data_Compound 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H40 N12 Ni5 O28 S2, 2(C6 H16 N), 2(H2 O)' _chemical_formula_sum 'C50 H76 N14 Ni5 O30 S2' _chemical_formula_weight 1710.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.578(4) _cell_length_b 12.193(4) _cell_length_c 13.787(4) _cell_angle_alpha 66.907(4) _cell_angle_beta 86.720(5) _cell_angle_gamma 80.131(5) _cell_volume 1763.7(10) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1594 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.82 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 1.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7586 _exptl_absorpt_correction_T_max 0.8676 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9107 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6069 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6069 _refine_ls_number_parameters 563 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1739 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.5000 0.5000 0.0391(3) Uani 1 2 d S . . Ni2 Ni 0.63800(7) 0.53857(7) 0.26077(6) 0.0486(3) Uani 1 1 d . . . Ni3 Ni 0.43772(7) 0.81212(6) 0.42642(6) 0.0451(3) Uani 1 1 d . . . C1 C 0.6642(6) 0.2637(6) 0.3621(6) 0.0566(18) Uani 1 1 d D . . C2 C 0.6848(6) 0.1326(6) 0.4050(6) 0.0535(17) Uani 1 1 d . . . C3 C 0.7516(6) 0.0917(6) 0.3303(5) 0.0509(16) Uani 1 1 d . . . C4 C 0.7946(6) -0.0228(6) 0.3340(6) 0.0589(18) Uani 1 1 d . . . H4 H 0.7795 -0.0904 0.3919 0.071 Uiso 1 1 calc R . . C5 C 0.8588(7) -0.0361(7) 0.2528(6) 0.071(2) Uani 1 1 d . . . H5 H 0.8900 -0.1133 0.2567 0.085 Uiso 1 1 calc R . . C6 C 0.8790(7) 0.0657(8) 0.1620(7) 0.076(2) Uani 1 1 d . . . H6 H 0.9217 0.0549 0.1062 0.091 Uiso 1 1 calc R . . C7 C 0.8347(6) 0.1826(6) 0.1562(6) 0.067(2) Uani 1 1 d . . . H7 H 0.8474 0.2503 0.0972 0.080 Uiso 1 1 calc R . . C8 C 0.7715(6) 0.1946(6) 0.2408(5) 0.0524(17) Uani 1 1 d . . . C9 C 0.7189(6) 0.3036(5) 0.2581(5) 0.0538(17) Uani 1 1 d . . . N11 N 0.6105(9) 0.3049(7) 0.4326(8) 0.054(3) Uani 0.631(7) 1 d PD . 1 O11 O 0.5843(7) 0.4256(6) 0.3986(7) 0.058(2) Uani 0.631(7) 1 d PD . 1 N12 N 0.6169(14) 0.3664(12) 0.3724(11) 0.049(4) Uani 0.369(7) 1 d PD . 2 O12 O 0.5669(12) 0.3528(13) 0.4655(9) 0.051(4) Uani 0.369(7) 1 d PD . 2 N2 N 0.7171(5) 0.4174(5) 0.2026(5) 0.0618(15) Uani 1 1 d . . . O2 O 0.7698(5) 0.4516(4) 0.1081(4) 0.0750(14) Uani 1 1 d . . . H2 H 0.7610 0.5282 0.0875 0.113 Uiso 1 1 d R . . N3 N 0.6422(5) 0.0801(5) 0.5005(5) 0.0623(16) Uani 1 1 d . . . O3 O 0.6585(4) -0.0393(4) 0.5485(4) 0.0698(14) Uani 1 1 d . . . C10 C 0.5712(6) 0.7943(5) 0.2352(5) 0.0508(17) Uani 1 1 d D . . C11 C 0.6399(6) 0.7907(6) 0.1441(5) 0.0573(18) Uani 1 1 d . . . C12 C 0.6498(6) 0.9154(6) 0.0757(5) 0.0568(18) Uani 1 1 d . . . C13 C 0.7053(7) 0.9616(7) -0.0209(5) 0.073(2) Uani 1 1 d . . . H13 H 0.7454 0.9108 -0.0517 0.088 Uiso 1 1 calc R . . C14 C 0.6987(8) 1.0848(8) -0.0690(6) 0.087(3) Uani 1 1 d . . . H14 H 0.7359 1.1169 -0.1332 0.104 Uiso 1 1 calc R . . C15 C 0.6404(8) 1.1611(7) -0.0269(7) 0.084(3) Uani 1 1 d . . . H15 H 0.6375 1.2440 -0.0627 0.100 Uiso 1 1 calc R . . C16 C 0.5842(7) 1.1167(6) 0.0700(6) 0.066(2) Uani 1 1 d . . . H16 H 0.5443 1.1690 0.0993 0.079 Uiso 1 1 calc R . . C17 C 0.5894(6) 0.9930(5) 0.1211(5) 0.0504(17) Uani 1 1 d . . . C18 C 0.5405(6) 0.9202(6) 0.2218(5) 0.0526(17) Uani 1 1 d . . . N41 N 0.5612(8) 0.6822(8) 0.2998(6) 0.046(2) Uani 0.631(7) 1 d PD . 1 O41 O 0.4963(6) 0.6722(7) 0.3850(5) 0.046(2) Uani 0.631(7) 1 d PD . 1 N42 N 0.5223(13) 0.7332(10) 0.3265(9) 0.043(5) Uani 0.369(7) 1 d PD . 2 O42 O 0.5383(10) 0.6135(9) 0.3488(10) 0.036(3) Uani 0.369(7) 1 d PD . 2 N5 N 0.6774(6) 0.6862(5) 0.1386(4) 0.0646(16) Uani 1 1 d . . . O5 O 0.7403(5) 0.6799(5) 0.0553(4) 0.0822(16) Uani 1 1 d . . . N6 N 0.4802(5) 0.9447(5) 0.2942(4) 0.0576(15) Uani 1 1 d . . . O6 O 0.4542(5) 1.0659(4) 0.2788(4) 0.0783(15) Uani 1 1 d . . . H6A H 0.3993 1.0764 0.3197 0.117 Uiso 1 1 d R . . O7 O 0.4800(4) 0.5491(4) 0.1852(3) 0.0659(13) Uani 1 1 d . . . H71 H 0.4270 0.5251 0.2300 0.099 Uiso 1 1 d R . . H72 H 0.4893 0.5121 0.1437 0.099 Uiso 1 1 d R . . O8 O 0.7909(4) 0.5187(4) 0.3479(3) 0.0581(12) Uani 1 1 d . . . H81 H 0.7756 0.4917 0.4134 0.087 Uiso 1 1 d R . . H82 H 0.8183 0.5840 0.3282 0.087 Uiso 1 1 d R . . O9 O 0.2769(4) 0.8199(4) 0.3567(4) 0.0635(13) Uani 1 1 d . . . H9 H 0.2964 0.7520 0.3521 0.095 Uiso 1 1 d R . . C19 C 0.1684(10) 0.8810(15) 0.3605(13) 0.206(8) Uani 1 1 d . . . H191 H 0.1752 0.9516 0.3734 0.309 Uiso 1 1 calc R . . H192 H 0.1249 0.8299 0.4164 0.309 Uiso 1 1 calc R . . H193 H 0.1283 0.9049 0.2946 0.309 Uiso 1 1 calc R . . O10 O 0.6034(4) 0.7925(4) 0.4871(3) 0.0599(12) Uani 1 1 d . . . H101 H 0.6288 0.7239 0.5331 0.090 Uiso 1 1 d R . . H102 H 0.6192 0.8507 0.4987 0.090 Uiso 1 1 d R . . S11 S 0.2535(6) 0.5216(6) 0.3763(5) 0.0367(16) Uani 0.631(7) 1 d P . 1 O111 O 0.3288(10) 0.4977(9) 0.4698(7) 0.046(2) Uani 0.631(7) 1 d P . 1 O121 O 0.2687(15) 0.6352(12) 0.2926(11) 0.084(5) Uani 0.631(7) 1 d P . 1 O131 O 0.1410(9) 0.5030(11) 0.3998(9) 0.082(3) Uani 0.631(7) 1 d P . 1 O141 O 0.3106(7) 0.4259(7) 0.3314(6) 0.073(3) Uani 0.631(7) 1 d P . 1 S12 S 0.2635(18) 0.5190(16) 0.3772(16) 0.101(6) Uani 0.369(7) 1 d P . 2 O112 O 0.3585(15) 0.4604(16) 0.4429(14) 0.050(4) Uani 0.369(7) 1 d P . 2 O122 O 0.278(2) 0.591(2) 0.2650(15) 0.073(6) Uani 0.369(7) 1 d P . 2 O132 O 0.1734(15) 0.4331(14) 0.3967(13) 0.055(4) Uani 0.369(7) 1 d P . 2 O142 O 0.1865(10) 0.6138(9) 0.4252(10) 0.056(4) Uani 0.369(7) 1 d P . 2 O15 O 0.0728(5) 0.3422(5) 0.6092(5) 0.0973(18) Uani 1 1 d . . . H151 H 0.0858 0.3363 0.5502 0.146 Uiso 1 1 d R . . H152 H 0.0085 0.3888 0.6066 0.146 Uiso 1 1 d R . . N7 N 0.1210(7) 0.3761(7) 0.2393(6) 0.094(2) Uani 1 1 d D . . H7A H 0.1502 0.3977 0.2863 0.141 Uiso 1 1 d RD A . C20 C 0.0136(11) 0.3288(14) 0.2891(11) 0.181(6) Uani 1 1 d D A . H20A H -0.0199 0.2980 0.2439 0.217 Uiso 1 1 calc R . . H20B H -0.0431 0.3951 0.2936 0.217 Uiso 1 1 calc R . . C21 C 0.0321(13) 0.2313(13) 0.3964(11) 0.172(6) Uani 1 1 d DU . . H21A H 0.0766 0.1597 0.3914 0.258 Uiso 1 1 calc R A . H21B H -0.0425 0.2142 0.4275 0.258 Uiso 1 1 calc R . . H21C H 0.0740 0.2571 0.4396 0.258 Uiso 1 1 calc R . . C22 C 0.0960(16) 0.4768(12) 0.1339(10) 0.213(7) Uani 1 1 d DU A . H22A H 0.1690 0.4885 0.0960 0.255 Uiso 1 1 calc R . . H22B H 0.0453 0.4538 0.0941 0.255 Uiso 1 1 calc R . . C23 C 0.0398(12) 0.5926(13) 0.1395(9) 0.171(6) Uani 1 1 d D . . H23A H -0.0396 0.5872 0.1626 0.256 Uiso 1 1 calc R A . H23B H 0.0402 0.6564 0.0710 0.256 Uiso 1 1 calc R . . H23C H 0.0824 0.6093 0.1886 0.256 Uiso 1 1 calc R . . C241 C 0.2112(13) 0.295(3) 0.206(3) 0.142(10) Uani 0.59(2) 1 d PD A 1 H24A H 0.2226 0.2164 0.2646 0.170 Uiso 0.59(2) 1 calc PR A 1 H24B H 0.1778 0.2839 0.1483 0.170 Uiso 0.59(2) 1 calc PR A 1 C251 C 0.329(2) 0.328(2) 0.173(3) 0.239(18) Uani 0.59(2) 1 d PD A 1 H25A H 0.3707 0.2750 0.1418 0.359 Uiso 0.59(2) 1 calc PR A 1 H25B H 0.3725 0.3198 0.2337 0.359 Uiso 0.59(2) 1 calc PR A 1 H25C H 0.3211 0.4098 0.1229 0.359 Uiso 0.59(2) 1 calc PR A 1 C242 C 0.186(4) 0.251(3) 0.262(4) 0.23(3) Uani 0.41(2) 1 d PDU A 2 H24C H 0.1713 0.2005 0.3344 0.276 Uiso 0.41(2) 1 calc PR A 2 H24D H 0.2691 0.2544 0.2557 0.276 Uiso 0.41(2) 1 calc PR A 2 C252 C 0.154(3) 0.193(3) 0.192(2) 0.153(15) Uani 0.41(2) 1 d PD A 2 H25D H 0.0889 0.1514 0.2213 0.230 Uiso 0.41(2) 1 calc PR A 2 H25E H 0.2197 0.1367 0.1856 0.230 Uiso 0.41(2) 1 calc PR A 2 H25F H 0.1320 0.2541 0.1231 0.230 Uiso 0.41(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0518(7) 0.0296(5) 0.0353(6) -0.0100(5) -0.0011(5) -0.0109(5) Ni2 0.0652(6) 0.0357(4) 0.0434(5) -0.0134(4) 0.0046(4) -0.0104(4) Ni3 0.0607(6) 0.0330(4) 0.0436(5) -0.0149(3) 0.0012(4) -0.0126(4) C1 0.048(4) 0.067(5) 0.075(5) -0.049(4) 0.003(4) -0.013(3) C2 0.056(4) 0.062(4) 0.056(4) -0.032(4) 0.010(4) -0.023(3) C3 0.055(4) 0.050(4) 0.057(4) -0.028(3) 0.002(3) -0.017(3) C4 0.066(5) 0.047(4) 0.072(5) -0.032(4) 0.003(4) -0.010(3) C5 0.082(6) 0.056(5) 0.086(6) -0.042(4) -0.004(5) -0.002(4) C6 0.075(6) 0.089(6) 0.083(6) -0.057(5) 0.010(4) -0.011(4) C7 0.077(5) 0.060(5) 0.074(5) -0.036(4) 0.003(4) -0.016(4) C8 0.064(4) 0.047(4) 0.055(4) -0.028(3) 0.002(3) -0.013(3) C9 0.061(4) 0.039(4) 0.066(5) -0.025(3) -0.004(4) -0.008(3) N11 0.062(7) 0.043(6) 0.054(7) -0.011(6) -0.001(6) -0.015(6) O11 0.074(6) 0.038(4) 0.055(6) -0.012(4) 0.008(4) -0.012(4) N12 0.052(10) 0.043(11) 0.052(12) -0.024(9) -0.007(9) 0.008(9) O12 0.071(10) 0.029(8) 0.043(8) -0.004(7) -0.002(7) -0.008(7) N2 0.075(4) 0.055(4) 0.058(4) -0.026(3) -0.002(3) -0.007(3) O2 0.101(4) 0.059(3) 0.072(4) -0.033(3) 0.010(3) -0.014(3) N3 0.063(4) 0.063(4) 0.077(4) -0.043(3) -0.002(3) -0.014(3) O3 0.087(4) 0.050(3) 0.083(4) -0.034(3) -0.007(3) -0.014(3) C10 0.056(4) 0.047(4) 0.039(4) 0.003(3) -0.013(3) -0.025(3) C11 0.079(5) 0.039(4) 0.051(4) -0.009(3) -0.013(4) -0.015(3) C12 0.070(5) 0.053(4) 0.038(4) -0.002(3) -0.007(3) -0.023(4) C13 0.099(6) 0.073(5) 0.048(4) -0.015(4) 0.008(4) -0.040(5) C14 0.112(8) 0.080(6) 0.055(5) -0.002(5) 0.008(5) -0.043(6) C15 0.116(7) 0.050(5) 0.063(5) 0.014(4) -0.014(5) -0.037(5) C16 0.079(5) 0.042(4) 0.068(5) -0.010(4) -0.012(4) -0.011(4) C17 0.057(4) 0.043(3) 0.044(4) -0.006(3) -0.013(3) -0.011(3) C18 0.055(4) 0.048(4) 0.047(4) -0.005(3) -0.005(3) -0.017(3) N41 0.067(7) 0.027(6) 0.037(6) -0.002(5) -0.001(5) -0.016(5) O41 0.056(5) 0.040(5) 0.044(5) -0.018(4) 0.003(4) -0.013(4) N42 0.057(11) 0.028(9) 0.043(12) -0.011(8) -0.007(9) -0.006(8) O42 0.053(7) 0.022(6) 0.029(7) -0.008(6) 0.004(5) -0.004(5) N5 0.091(5) 0.051(3) 0.050(4) -0.012(3) 0.007(3) -0.027(3) O5 0.106(4) 0.075(4) 0.055(3) -0.012(3) 0.017(3) -0.027(3) N6 0.070(4) 0.043(3) 0.052(4) -0.010(3) 0.001(3) -0.011(3) O6 0.092(4) 0.048(3) 0.083(4) -0.016(3) 0.006(3) -0.006(3) O7 0.075(3) 0.070(3) 0.056(3) -0.026(2) 0.000(2) -0.017(3) O8 0.071(3) 0.053(3) 0.050(3) -0.017(2) 0.006(2) -0.018(2) O9 0.064(3) 0.047(3) 0.083(3) -0.027(2) -0.012(3) -0.008(2) C19 0.076(8) 0.35(2) 0.316(19) -0.269(19) -0.017(10) 0.000(11) O10 0.072(3) 0.042(2) 0.071(3) -0.023(2) -0.011(2) -0.016(2) S11 0.040(3) 0.036(3) 0.031(3) -0.008(3) -0.018(2) -0.004(2) O111 0.060(6) 0.060(6) 0.027(5) -0.022(4) 0.000(4) -0.019(5) O121 0.131(11) 0.072(8) 0.046(8) -0.005(5) -0.029(7) -0.043(7) O131 0.052(7) 0.099(9) 0.081(7) -0.014(7) -0.012(5) -0.020(6) O141 0.095(7) 0.061(5) 0.077(6) -0.044(4) -0.020(5) -0.003(4) S12 0.123(15) 0.071(11) 0.119(14) -0.035(10) 0.021(10) -0.055(9) O112 0.048(10) 0.074(11) 0.036(9) -0.031(7) -0.021(8) 0.002(8) O122 0.064(10) 0.11(2) 0.022(9) -0.004(10) 0.001(7) -0.018(12) O132 0.050(10) 0.060(10) 0.062(9) -0.023(9) -0.002(7) -0.028(8) O142 0.050(8) 0.038(6) 0.089(10) -0.039(6) 0.004(6) 0.003(5) O15 0.094(4) 0.079(4) 0.111(5) -0.025(3) -0.002(4) -0.018(3) N7 0.091(6) 0.108(6) 0.103(6) -0.057(5) -0.024(5) -0.021(5) C20 0.141(13) 0.210(16) 0.235(18) -0.122(15) 0.006(12) -0.057(12) C21 0.175(9) 0.161(9) 0.165(9) -0.045(7) 0.005(7) -0.037(7) C22 0.230(11) 0.231(11) 0.190(10) -0.087(9) -0.048(8) -0.042(9) C23 0.179(13) 0.209(15) 0.090(8) -0.031(9) -0.066(8) 0.012(11) C241 0.094(15) 0.18(2) 0.23(3) -0.18(2) 0.008(17) -0.012(15) C251 0.15(3) 0.19(3) 0.33(4) -0.04(3) 0.04(3) -0.08(2) C242 0.23(3) 0.23(3) 0.23(3) -0.091(15) -0.002(10) -0.034(11) C252 0.16(3) 0.20(3) 0.18(3) -0.17(3) 0.02(2) -0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O12 2.049(15) . ? Ni1 O12 2.049(15) 2_666 ? Ni1 O111 2.056(11) . ? Ni1 O111 2.056(11) 2_666 ? Ni1 O112 2.062(18) . ? Ni1 O112 2.062(18) 2_666 ? Ni1 O11 2.064(9) . ? Ni1 O11 2.064(9) 2_666 ? Ni1 O41 2.071(8) . ? Ni1 O41 2.071(8) 2_666 ? Ni1 O42 2.074(13) . ? Ni1 O42 2.074(13) 2_666 ? Ni2 O42 1.997(12) . ? Ni2 O11 2.000(9) . ? Ni2 N2 2.012(6) . ? Ni2 N5 2.025(5) . ? Ni2 N41 2.073(10) . ? Ni2 N12 2.106(15) . ? Ni2 O7 2.117(4) . ? Ni2 O8 2.122(4) . ? Ni3 O12 1.986(13) 2_666 ? Ni3 O41 2.005(8) . ? Ni3 N6 2.009(5) . ? Ni3 N11 2.025(9) 2_666 ? Ni3 N3 2.029(6) 2_666 ? Ni3 O10 2.075(4) . ? Ni3 N42 2.084(13) . ? Ni3 O9 2.115(5) . ? C1 N12 1.335(9) . ? C1 N11 1.337(9) . ? C1 C2 1.451(9) . ? C1 C9 1.466(9) . ? C2 N3 1.326(8) . ? C2 C3 1.446(9) . ? C3 C4 1.381(9) . ? C3 C8 1.415(8) . ? C4 C5 1.356(9) . ? C4 H4 0.9300 . ? C5 C6 1.418(10) . ? C5 H5 0.9300 . ? C6 C7 1.403(10) . ? C6 H6 0.9300 . ? C7 C8 1.383(9) . ? C7 H7 0.9300 . ? C8 C9 1.466(9) . ? C9 N2 1.292(8) . ? N11 O11 1.343(8) . ? N11 Ni3 2.025(9) 2_666 ? N12 O12 1.338(10) . ? O12 Ni3 1.986(13) 2_666 ? N2 O2 1.347(7) . ? O2 H2 0.8521 . ? N3 O3 1.326(7) . ? N3 Ni3 2.029(6) 2_666 ? C10 N41 1.328(8) . ? C10 N42 1.336(10) . ? C10 C18 1.454(9) . ? C10 C11 1.459(10) . ? C11 N5 1.304(8) . ? C11 C12 1.462(8) . ? C12 C13 1.394(9) . ? C12 C17 1.401(9) . ? C13 C14 1.373(10) . ? C13 H13 0.9300 . ? C14 C15 1.349(12) . ? C14 H14 0.9300 . ? C15 C16 1.398(11) . ? C15 H15 0.9300 . ? C16 C17 1.384(8) . ? C16 H16 0.9300 . ? C17 C18 1.467(9) . ? C18 N6 1.287(8) . ? N41 O41 1.333(8) . ? N42 O42 1.350(9) . ? N5 O5 1.346(7) . ? N6 O6 1.389(7) . ? O6 H6A 0.8520 . ? O7 H71 0.8483 . ? O7 H72 0.8486 . ? O8 H81 0.8513 . ? O8 H82 0.8463 . ? O9 C19 1.356(11) . ? O9 H9 0.8461 . ? C19 H191 0.9600 . ? C19 H192 0.9600 . ? C19 H193 0.9600 . ? O10 H101 0.8427 . ? O10 H102 0.8379 . ? S11 O131 1.359(14) . ? S11 O121 1.445(16) . ? S11 O111 1.502(11) . ? S11 O141 1.561(11) . ? S12 O112 1.37(2) . ? S12 O122 1.47(3) . ? S12 O132 1.54(2) . ? S12 O142 1.66(2) . ? O15 H151 0.8480 . ? O15 H152 0.8495 . ? N7 C20 1.479(8) . ? N7 C241 1.492(9) . ? N7 C22 1.493(9) . ? N7 C242 1.496(10) . ? N7 H7A 0.8898 . ? C20 C21 1.49(2) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.48(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C241 C251 1.489(10) . ? C241 H24A 0.9700 . ? C241 H24B 0.9700 . ? C251 H25A 0.9600 . ? C251 H25B 0.9600 . ? C251 H25C 0.9600 . ? C242 C252 1.500(10) . ? C242 H24C 0.9700 . ? C242 H24D 0.9700 . ? C252 H25D 0.9600 . ? C252 H25E 0.9600 . ? C252 H25F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Ni1 O12 180.0(6) . 2_666 ? O12 Ni1 O111 94.7(5) . . ? O12 Ni1 O111 85.3(5) 2_666 . ? O12 Ni1 O111 85.3(5) . 2_666 ? O12 Ni1 O111 94.7(5) 2_666 2_666 ? O111 Ni1 O111 180.000(1) . 2_666 ? O12 Ni1 O112 75.4(6) . . ? O12 Ni1 O112 104.6(6) 2_666 . ? O111 Ni1 O112 20.3(4) . . ? O111 Ni1 O112 159.7(4) 2_666 . ? O12 Ni1 O112 104.6(6) . 2_666 ? O12 Ni1 O112 75.4(6) 2_666 2_666 ? O111 Ni1 O112 159.7(4) . 2_666 ? O111 Ni1 O112 20.3(4) 2_666 2_666 ? O112 Ni1 O112 180.0(9) . 2_666 ? O12 Ni1 O11 29.2(3) . . ? O12 Ni1 O11 150.8(4) 2_666 . ? O111 Ni1 O11 99.8(3) . . ? O111 Ni1 O11 80.2(3) 2_666 . ? O112 Ni1 O11 79.9(5) . . ? O112 Ni1 O11 100.1(5) 2_666 . ? O12 Ni1 O11 150.8(4) . 2_666 ? O12 Ni1 O11 29.2(4) 2_666 2_666 ? O111 Ni1 O11 80.2(3) . 2_666 ? O111 Ni1 O11 99.8(3) 2_666 2_666 ? O112 Ni1 O11 100.1(5) . 2_666 ? O112 Ni1 O11 79.9(5) 2_666 2_666 ? O11 Ni1 O11 180.000(1) . 2_666 ? O12 Ni1 O41 119.7(4) . . ? O12 Ni1 O41 60.3(4) 2_666 . ? O111 Ni1 O41 92.3(3) . . ? O111 Ni1 O41 87.7(3) 2_666 . ? O112 Ni1 O41 96.4(5) . . ? O112 Ni1 O41 83.6(5) 2_666 . ? O11 Ni1 O41 90.6(3) . . ? O11 Ni1 O41 89.4(3) 2_666 . ? O12 Ni1 O41 60.3(4) . 2_666 ? O12 Ni1 O41 119.7(4) 2_666 2_666 ? O111 Ni1 O41 87.7(3) . 2_666 ? O111 Ni1 O41 92.3(3) 2_666 2_666 ? O112 Ni1 O41 83.6(5) . 2_666 ? O112 Ni1 O41 96.4(5) 2_666 2_666 ? O11 Ni1 O41 89.4(3) . 2_666 ? O11 Ni1 O41 90.6(3) 2_666 2_666 ? O41 Ni1 O41 180.000(1) . 2_666 ? O12 Ni1 O42 89.9(4) . . ? O12 Ni1 O42 90.1(4) 2_666 . ? O111 Ni1 O42 96.7(4) . . ? O111 Ni1 O42 83.3(4) 2_666 . ? O112 Ni1 O42 90.5(6) . . ? O112 Ni1 O42 89.5(6) 2_666 . ? O11 Ni1 O42 60.8(4) . . ? O11 Ni1 O42 119.2(4) 2_666 . ? O41 Ni1 O42 29.7(3) . . ? O41 Ni1 O42 150.3(3) 2_666 . ? O12 Ni1 O42 90.1(4) . 2_666 ? O12 Ni1 O42 89.9(4) 2_666 2_666 ? O111 Ni1 O42 83.3(4) . 2_666 ? O111 Ni1 O42 96.7(4) 2_666 2_666 ? O112 Ni1 O42 89.5(6) . 2_666 ? O112 Ni1 O42 90.5(6) 2_666 2_666 ? O11 Ni1 O42 119.2(4) . 2_666 ? O11 Ni1 O42 60.8(4) 2_666 2_666 ? O41 Ni1 O42 150.3(3) . 2_666 ? O41 Ni1 O42 29.7(3) 2_666 2_666 ? O42 Ni1 O42 180.000(2) . 2_666 ? O42 Ni2 O11 63.2(4) . . ? O42 Ni2 N2 161.9(4) . . ? O11 Ni2 N2 99.4(3) . . ? O42 Ni2 N5 101.6(4) . . ? O11 Ni2 N5 164.4(3) . . ? N2 Ni2 N5 96.0(3) . . ? O42 Ni2 N41 25.9(3) . . ? O11 Ni2 N41 88.8(3) . . ? N2 Ni2 N41 171.8(3) . . ? N5 Ni2 N41 75.9(3) . . ? O42 Ni2 N12 89.4(4) . . ? O11 Ni2 N12 26.4(3) . . ? N2 Ni2 N12 73.0(3) . . ? N5 Ni2 N12 169.0(3) . . ? N41 Ni2 N12 115.1(4) . . ? O42 Ni2 O7 86.2(3) . . ? O11 Ni2 O7 91.4(3) . . ? N2 Ni2 O7 89.4(2) . . ? N5 Ni2 O7 91.0(2) . . ? N41 Ni2 O7 89.6(3) . . ? N12 Ni2 O7 89.8(5) . . ? O42 Ni2 O8 91.7(3) . . ? O11 Ni2 O8 84.0(3) . . ? N2 Ni2 O8 91.5(2) . . ? N5 Ni2 O8 93.4(2) . . ? N41 Ni2 O8 90.2(3) . . ? N12 Ni2 O8 86.1(5) . . ? O7 Ni2 O8 175.41(16) . . ? O12 Ni3 O41 62.5(4) 2_666 . ? O12 Ni3 N6 160.0(4) 2_666 . ? O41 Ni3 N6 98.1(3) . . ? O12 Ni3 N11 27.1(4) 2_666 2_666 ? O41 Ni3 N11 89.2(3) . 2_666 ? N6 Ni3 N11 172.6(3) . 2_666 ? O12 Ni3 N3 102.8(4) 2_666 2_666 ? O41 Ni3 N3 164.6(3) . 2_666 ? N6 Ni3 N3 96.9(3) . 2_666 ? N11 Ni3 N3 75.8(3) 2_666 2_666 ? O12 Ni3 O10 85.4(4) 2_666 . ? O41 Ni3 O10 88.5(2) . . ? N6 Ni3 O10 89.04(19) . . ? N11 Ni3 O10 90.2(3) 2_666 . ? N3 Ni3 O10 95.11(19) 2_666 . ? O12 Ni3 N42 88.5(5) 2_666 . ? O41 Ni3 N42 26.3(3) . . ? N6 Ni3 N42 71.9(3) . . ? N11 Ni3 N42 115.4(4) 2_666 . ? N3 Ni3 N42 168.7(3) 2_666 . ? O10 Ni3 N42 85.9(5) . . ? O12 Ni3 O9 93.1(4) 2_666 . ? O41 Ni3 O9 85.6(2) . . ? N6 Ni3 O9 90.4(2) . . ? N11 Ni3 O9 91.1(3) 2_666 . ? N3 Ni3 O9 90.9(2) 2_666 . ? O10 Ni3 O9 173.96(18) . . ? N42 Ni3 O9 88.2(5) . . ? N12 C1 C2 149.1(9) . . ? N11 C1 C2 110.7(7) . . ? N12 C1 C9 104.2(8) . . ? N11 C1 C9 142.3(7) . . ? C2 C1 C9 106.8(5) . . ? N3 C2 C3 135.7(6) . . ? N3 C2 C1 115.3(6) . . ? C3 C2 C1 109.0(6) . . ? C4 C3 C8 120.1(6) . . ? C4 C3 C2 131.7(6) . . ? C8 C3 C2 108.1(6) . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.1(7) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 120.0(7) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 118.1(7) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C7 C8 C3 120.9(6) . . ? C7 C8 C9 130.1(6) . . ? C3 C8 C9 109.0(6) . . ? N2 C9 C1 120.2(6) . . ? N2 C9 C8 132.6(7) . . ? C1 C9 C8 107.1(5) . . ? C1 N11 O11 115.0(9) . . ? C1 N11 Ni3 120.2(6) . 2_666 ? O11 N11 Ni3 124.5(8) . 2_666 ? N11 O11 Ni2 123.4(8) . . ? N11 O11 Ni1 118.6(7) . . ? Ni2 O11 Ni1 117.6(3) . . ? C1 N12 O12 115.1(14) . . ? C1 N12 Ni2 123.3(9) . . ? O12 N12 Ni2 121.1(10) . . ? N12 O12 Ni3 119.7(12) . 2_666 ? N12 O12 Ni1 120.8(11) . . ? Ni3 O12 Ni1 119.4(6) 2_666 . ? C9 N2 O2 119.1(6) . . ? C9 N2 Ni2 119.1(5) . . ? O2 N2 Ni2 121.7(4) . . ? N2 O2 H2 103.1 . . ? C2 N3 O3 120.5(6) . . ? C2 N3 Ni3 117.9(5) . 2_666 ? O3 N3 Ni3 121.5(5) . 2_666 ? N41 C10 C18 143.4(8) . . ? N42 C10 C18 104.5(8) . . ? N41 C10 C11 109.0(7) . . ? N42 C10 C11 147.9(7) . . ? C18 C10 C11 107.6(5) . . ? N5 C11 C10 118.7(6) . . ? N5 C11 C12 134.1(7) . . ? C10 C11 C12 107.2(6) . . ? C13 C12 C17 120.6(6) . . ? C13 C12 C11 130.3(7) . . ? C17 C12 C11 109.1(6) . . ? C14 C13 C12 117.6(8) . . ? C14 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? C15 C14 C13 122.7(8) . . ? C15 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C14 C15 C16 120.6(7) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.4(7) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C12 120.1(6) . . ? C16 C17 C18 131.2(7) . . ? C12 C17 C18 108.8(5) . . ? N6 C18 C10 118.3(6) . . ? N6 C18 C17 134.4(6) . . ? C10 C18 C17 107.3(6) . . ? C10 N41 O41 115.4(9) . . ? C10 N41 Ni2 119.7(6) . . ? O41 N41 Ni2 124.8(7) . . ? N41 O41 Ni3 123.0(7) . . ? N41 O41 Ni1 116.8(7) . . ? Ni3 O41 Ni1 117.5(3) . . ? C10 N42 O42 112.1(11) . . ? C10 N42 Ni3 124.1(7) . . ? O42 N42 Ni3 123.7(9) . . ? N42 O42 Ni2 122.5(11) . . ? N42 O42 Ni1 117.7(9) . . ? Ni2 O42 Ni1 117.3(5) . . ? C11 N5 O5 120.1(6) . . ? C11 N5 Ni2 116.8(5) . . ? O5 N5 Ni2 123.1(4) . . ? C18 N6 O6 116.4(5) . . ? C18 N6 Ni3 120.9(4) . . ? O6 N6 Ni3 122.6(5) . . ? N6 O6 H6A 110.1 . . ? Ni2 O7 H71 110.9 . . ? Ni2 O7 H72 112.7 . . ? H71 O7 H72 111.7 . . ? Ni2 O8 H81 109.3 . . ? Ni2 O8 H82 111.8 . . ? H81 O8 H82 111.9 . . ? C19 O9 Ni3 131.1(6) . . ? C19 O9 H9 129.3 . . ? Ni3 O9 H9 94.3 . . ? O9 C19 H191 109.5 . . ? O9 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? O9 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? Ni3 O10 H101 115.8 . . ? Ni3 O10 H102 116.9 . . ? H101 O10 H102 114.7 . . ? O131 S11 O121 116.2(9) . . ? O131 S11 O111 114.7(8) . . ? O121 S11 O111 110.3(8) . . ? O131 S11 O141 106.3(8) . . ? O121 S11 O141 103.4(7) . . ? O111 S11 O141 104.5(6) . . ? S11 O111 Ni1 138.1(7) . . ? O112 S12 O122 121(2) . . ? O112 S12 O132 109.6(16) . . ? O122 S12 O132 112.9(17) . . ? O112 S12 O142 106.9(15) . . ? O122 S12 O142 105.4(15) . . ? O132 S12 O142 98.0(15) . . ? S12 O112 Ni1 139.4(14) . . ? H151 O15 H152 109.8 . . ? C20 N7 C241 117.6(13) . . ? C20 N7 C22 112.0(11) . . ? C241 N7 C22 98.4(16) . . ? C20 N7 C242 92(3) . . ? C22 N7 C242 127(2) . . ? C20 N7 H7A 104.3 . . ? C241 N7 H7A 111.3 . . ? C22 N7 H7A 113.7 . . ? C242 N7 H7A 103.9 . . ? N7 C20 C21 114.6(11) . . ? N7 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? N7 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N7 113.7(12) . . ? C23 C22 H22A 108.8 . . ? N7 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? N7 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C251 C241 N7 120.2(19) . . ? C251 C241 H24A 107.3 . . ? N7 C241 H24A 107.3 . . ? C251 C241 H24B 107.3 . . ? N7 C241 H24B 107.3 . . ? H24A C241 H24B 106.9 . . ? N7 C242 C252 115.0(19) . . ? N7 C242 H24C 108.5 . . ? C252 C242 H24C 108.5 . . ? N7 C242 H24D 108.5 . . ? C252 C242 H24D 108.5 . . ? H24C C242 H24D 107.5 . . ? C242 C252 H25D 109.5 . . ? C242 C252 H25E 109.5 . . ? H25D C252 H25E 109.5 . . ? C242 C252 H25F 109.5 . . ? H25D C252 H25F 109.5 . . ? H25E C252 H25F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 C1 C2 N3 -2(2) . . . . ? N11 C1 C2 N3 3.5(9) . . . . ? C9 C1 C2 N3 179.2(5) . . . . ? N12 C1 C2 C3 179.1(16) . . . . ? N11 C1 C2 C3 -175.2(7) . . . . ? C9 C1 C2 C3 0.6(7) . . . . ? N3 C2 C3 C4 0.7(13) . . . . ? C1 C2 C3 C4 178.9(7) . . . . ? N3 C2 C3 C8 -179.2(7) . . . . ? C1 C2 C3 C8 -0.9(7) . . . . ? C8 C3 C4 C5 1.9(10) . . . . ? C2 C3 C4 C5 -178.0(7) . . . . ? C3 C4 C5 C6 -2.4(11) . . . . ? C4 C5 C6 C7 1.5(11) . . . . ? C5 C6 C7 C8 -0.1(11) . . . . ? C6 C7 C8 C3 -0.4(10) . . . . ? C6 C7 C8 C9 177.8(7) . . . . ? C4 C3 C8 C7 -0.5(10) . . . . ? C2 C3 C8 C7 179.4(6) . . . . ? C4 C3 C8 C9 -179.0(6) . . . . ? C2 C3 C8 C9 0.9(7) . . . . ? N12 C1 C9 N2 2.9(11) . . . . ? N11 C1 C9 N2 -4.4(15) . . . . ? C2 C1 C9 N2 -177.9(6) . . . . ? N12 C1 C9 C8 -179.2(9) . . . . ? N11 C1 C9 C8 173.4(11) . . . . ? C2 C1 C9 C8 0.0(7) . . . . ? C7 C8 C9 N2 -1.4(13) . . . . ? C3 C8 C9 N2 177.0(7) . . . . ? C7 C8 C9 C1 -178.9(7) . . . . ? C3 C8 C9 C1 -0.5(7) . . . . ? N12 C1 N11 O11 -2.7(13) . . . . ? C2 C1 N11 O11 -177.9(8) . . . . ? C9 C1 N11 O11 8.8(17) . . . . ? N12 C1 N11 Ni3 172.1(19) . . . 2_666 ? C2 C1 N11 Ni3 -3.1(10) . . . 2_666 ? C9 C1 N11 Ni3 -176.4(7) . . . 2_666 ? C1 N11 O11 Ni2 -7.5(13) . . . . ? Ni3 N11 O11 Ni2 177.9(5) 2_666 . . . ? C1 N11 O11 Ni1 179.5(6) . . . . ? Ni3 N11 O11 Ni1 4.9(12) 2_666 . . . ? O42 Ni2 O11 N11 179.0(9) . . . . ? N2 Ni2 O11 N11 4.4(8) . . . . ? N5 Ni2 O11 N11 -167.1(9) . . . . ? N41 Ni2 O11 N11 -176.4(8) . . . . ? N12 Ni2 O11 N11 7.4(13) . . . . ? O7 Ni2 O11 N11 94.0(8) . . . . ? O8 Ni2 O11 N11 -86.1(8) . . . . ? O42 Ni2 O11 Ni1 -7.9(4) . . . . ? N2 Ni2 O11 Ni1 177.5(4) . . . . ? N5 Ni2 O11 Ni1 6.0(13) . . . . ? N41 Ni2 O11 Ni1 -3.4(5) . . . . ? N12 Ni2 O11 Ni1 -179.6(14) . . . . ? O7 Ni2 O11 Ni1 -92.9(4) . . . . ? O8 Ni2 O11 Ni1 87.0(4) . . . . ? O12 Ni1 O11 N11 -4.5(11) . . . . ? O12 Ni1 O11 N11 175.5(11) 2_666 . . . ? O111 Ni1 O11 N11 -86.5(8) . . . . ? O111 Ni1 O11 N11 93.5(8) 2_666 . . . ? O112 Ni1 O11 N11 -82.6(9) . . . . ? O112 Ni1 O11 N11 97.4(9) 2_666 . . . ? O41 Ni1 O11 N11 -179.0(8) . . . . ? O41 Ni1 O11 N11 1.0(8) 2_666 . . . ? O42 Ni1 O11 N11 -178.8(9) . . . . ? O42 Ni1 O11 N11 1.2(9) 2_666 . . . ? O12 Ni1 O11 Ni2 -177.9(11) . . . . ? O12 Ni1 O11 Ni2 2.1(11) 2_666 . . . ? O111 Ni1 O11 Ni2 100.1(5) . . . . ? O111 Ni1 O11 Ni2 -79.9(5) 2_666 . . . ? O112 Ni1 O11 Ni2 104.1(6) . . . . ? O112 Ni1 O11 Ni2 -75.9(6) 2_666 . . . ? O41 Ni1 O11 Ni2 7.6(4) . . . . ? O41 Ni1 O11 Ni2 -172.4(4) 2_666 . . . ? O42 Ni1 O11 Ni2 7.8(4) . . . . ? O42 Ni1 O11 Ni2 -172.2(4) 2_666 . . . ? N11 C1 N12 O12 -3.5(11) . . . . ? C2 C1 N12 O12 5(3) . . . . ? C9 C1 N12 O12 -176.3(11) . . . . ? N11 C1 N12 Ni2 168(2) . . . . ? C2 C1 N12 Ni2 177.0(9) . . . . ? C9 C1 N12 Ni2 -4.5(13) . . . . ? O42 Ni2 N12 C1 179.3(12) . . . . ? O11 Ni2 N12 C1 -173(2) . . . . ? N2 Ni2 N12 C1 3.7(11) . . . . ? N5 Ni2 N12 C1 -1(4) . . . . ? N41 Ni2 N12 C1 -177.4(10) . . . . ? O7 Ni2 N12 C1 93.1(12) . . . . ? O8 Ni2 N12 C1 -89.0(12) . . . . ? O42 Ni2 N12 O12 -9.3(13) . . . . ? O11 Ni2 N12 O12 -1.9(9) . . . . ? N2 Ni2 N12 O12 175.1(14) . . . . ? N5 Ni2 N12 O12 170.3(17) . . . . ? N41 Ni2 N12 O12 -6.1(15) . . . . ? O7 Ni2 N12 O12 -95.5(12) . . . . ? O8 Ni2 N12 O12 82.4(12) . . . . ? C1 N12 O12 Ni3 -2.3(18) . . . 2_666 ? Ni2 N12 O12 Ni3 -174.3(7) . . . 2_666 ? C1 N12 O12 Ni1 175.6(10) . . . . ? Ni2 N12 O12 Ni1 3.6(17) . . . . ? O111 Ni1 O12 N12 100.8(12) . . . . ? O111 Ni1 O12 N12 -79.2(12) 2_666 . . . ? O112 Ni1 O12 N12 94.6(13) . . . . ? O112 Ni1 O12 N12 -85.4(13) 2_666 . . . ? O11 Ni1 O12 N12 -0.9(10) . . . . ? O11 Ni1 O12 N12 179.1(10) 2_666 . . . ? O41 Ni1 O12 N12 5.4(14) . . . . ? O41 Ni1 O12 N12 -174.6(14) 2_666 . . . ? O42 Ni1 O12 N12 4.0(12) . . . . ? O42 Ni1 O12 N12 -176.0(12) 2_666 . . . ? O111 Ni1 O12 Ni3 -81.3(7) . . . 2_666 ? O111 Ni1 O12 Ni3 98.7(7) 2_666 . . 2_666 ? O112 Ni1 O12 Ni3 -87.5(9) . . . 2_666 ? O112 Ni1 O12 Ni3 92.5(9) 2_666 . . 2_666 ? O11 Ni1 O12 Ni3 177.0(15) . . . 2_666 ? O11 Ni1 O12 Ni3 -3.0(15) 2_666 . . 2_666 ? O41 Ni1 O12 Ni3 -176.7(5) . . . 2_666 ? O41 Ni1 O12 Ni3 3.3(5) 2_666 . . 2_666 ? O42 Ni1 O12 Ni3 -178.1(7) . . . 2_666 ? O42 Ni1 O12 Ni3 1.9(7) 2_666 . . 2_666 ? C1 C9 N2 O2 178.8(5) . . . . ? C8 C9 N2 O2 1.6(11) . . . . ? C1 C9 N2 Ni2 -0.2(8) . . . . ? C8 C9 N2 Ni2 -177.5(6) . . . . ? O42 Ni2 N2 C9 -16.0(13) . . . . ? O11 Ni2 N2 C9 -0.3(6) . . . . ? N5 Ni2 N2 C9 177.5(5) . . . . ? N12 Ni2 N2 C9 -1.6(7) . . . . ? O7 Ni2 N2 C9 -91.6(5) . . . . ? O8 Ni2 N2 C9 83.9(5) . . . . ? O42 Ni2 N2 O2 165.0(10) . . . . ? O11 Ni2 N2 O2 -179.3(5) . . . . ? N5 Ni2 N2 O2 -1.6(5) . . . . ? N12 Ni2 N2 O2 179.4(7) . . . . ? O7 Ni2 N2 O2 89.4(5) . . . . ? O8 Ni2 N2 O2 -95.1(5) . . . . ? C3 C2 N3 O3 -0.1(11) . . . . ? C1 C2 N3 O3 -178.3(5) . . . . ? C3 C2 N3 Ni3 175.7(6) . . . 2_666 ? C1 C2 N3 Ni3 -2.5(8) . . . 2_666 ? N41 C10 C11 N5 0.9(9) . . . . ? N42 C10 C11 N5 -0.6(18) . . . . ? C18 C10 C11 N5 -179.9(6) . . . . ? N41 C10 C11 C12 -179.4(6) . . . . ? N42 C10 C11 C12 179.1(15) . . . . ? C18 C10 C11 C12 -0.2(7) . . . . ? N5 C11 C12 C13 0.1(13) . . . . ? C10 C11 C12 C13 -179.5(7) . . . . ? N5 C11 C12 C17 179.0(7) . . . . ? C10 C11 C12 C17 -0.6(7) . . . . ? C17 C12 C13 C14 0.1(10) . . . . ? C11 C12 C13 C14 178.9(7) . . . . ? C12 C13 C14 C15 -0.6(12) . . . . ? C13 C14 C15 C16 0.7(13) . . . . ? C14 C15 C16 C17 -0.3(11) . . . . ? C15 C16 C17 C12 -0.1(10) . . . . ? C15 C16 C17 C18 180.0(6) . . . . ? C13 C12 C17 C16 0.2(10) . . . . ? C11 C12 C17 C16 -178.8(6) . . . . ? C13 C12 C17 C18 -179.9(6) . . . . ? C11 C12 C17 C18 1.1(7) . . . . ? N41 C10 C18 N6 -0.5(14) . . . . ? N42 C10 C18 N6 1.1(10) . . . . ? C11 C10 C18 N6 -179.3(6) . . . . ? N41 C10 C18 C17 179.7(9) . . . . ? N42 C10 C18 C17 -178.7(8) . . . . ? C11 C10 C18 C17 0.9(7) . . . . ? C16 C17 C18 N6 -1.1(12) . . . . ? C12 C17 C18 N6 178.9(7) . . . . ? C16 C17 C18 C10 178.7(6) . . . . ? C12 C17 C18 C10 -1.2(7) . . . . ? N42 C10 N41 O41 1.2(12) . . . . ? C18 C10 N41 O41 3.7(15) . . . . ? C11 C10 N41 O41 -177.5(7) . . . . ? N42 C10 N41 Ni2 178.6(17) . . . . ? C18 C10 N41 Ni2 -179.0(7) . . . . ? C11 C10 N41 Ni2 -0.2(9) . . . . ? O42 Ni2 N41 C10 -173.5(14) . . . . ? O11 Ni2 N41 C10 177.1(7) . . . . ? N5 Ni2 N41 C10 -0.3(6) . . . . ? N12 Ni2 N41 C10 179.0(7) . . . . ? O7 Ni2 N41 C10 -91.5(7) . . . . ? O8 Ni2 N41 C10 93.1(7) . . . . ? O42 Ni2 N41 O41 3.6(8) . . . . ? O11 Ni2 N41 O41 -5.8(8) . . . . ? N5 Ni2 N41 O41 176.8(8) . . . . ? N12 Ni2 N41 O41 -3.9(10) . . . . ? O7 Ni2 N41 O41 85.7(8) . . . . ? O8 Ni2 N41 O41 -89.8(8) . . . . ? C10 N41 O41 Ni3 -9.1(11) . . . . ? Ni2 N41 O41 Ni3 173.6(4) . . . . ? C10 N41 O41 Ni1 -170.3(6) . . . . ? Ni2 N41 O41 Ni1 12.5(10) . . . . ? O12 Ni3 O41 N41 -164.3(9) 2_666 . . . ? N6 Ni3 O41 N41 10.2(7) . . . . ? N11 Ni3 O41 N41 -168.9(7) 2_666 . . . ? N3 Ni3 O41 N41 177.4(8) 2_666 . . . ? O10 Ni3 O41 N41 -78.6(7) . . . . ? N42 Ni3 O41 N41 5.1(12) . . . . ? O9 Ni3 O41 N41 99.9(7) . . . . ? O12 Ni3 O41 Ni1 -3.3(5) 2_666 . . . ? N6 Ni3 O41 Ni1 171.2(3) . . . . ? N11 Ni3 O41 Ni1 -7.8(4) 2_666 . . . ? N3 Ni3 O41 Ni1 -21.6(12) 2_666 . . . ? O10 Ni3 O41 Ni1 82.4(3) . . . . ? N42 Ni3 O41 Ni1 166.1(13) . . . . ? O9 Ni3 O41 Ni1 -99.0(3) . . . . ? O12 Ni1 O41 N41 -14.6(8) . . . . ? O12 Ni1 O41 N41 165.4(8) 2_666 . . . ? O111 Ni1 O41 N41 -111.4(7) . . . . ? O111 Ni1 O41 N41 68.6(7) 2_666 . . . ? O112 Ni1 O41 N41 -91.4(8) . . . . ? O112 Ni1 O41 N41 88.6(8) 2_666 . . . ? O11 Ni1 O41 N41 -11.5(6) . . . . ? O11 Ni1 O41 N41 168.5(6) 2_666 . . . ? O42 Ni1 O41 N41 -11.8(8) . . . . ? O42 Ni1 O41 N41 168.2(8) 2_666 . . . ? O12 Ni1 O41 Ni3 -176.8(5) . . . . ? O12 Ni1 O41 Ni3 3.2(5) 2_666 . . . ? O111 Ni1 O41 Ni3 86.5(4) . . . . ? O111 Ni1 O41 Ni3 -93.5(4) 2_666 . . . ? O112 Ni1 O41 Ni3 106.4(6) . . . . ? O112 Ni1 O41 Ni3 -73.6(6) 2_666 . . . ? O11 Ni1 O41 Ni3 -173.7(4) . . . . ? O11 Ni1 O41 Ni3 6.3(4) 2_666 . . . ? O42 Ni1 O41 Ni3 -174.0(9) . . . . ? O42 Ni1 O41 Ni3 6.0(9) 2_666 . . . ? N41 C10 N42 O42 -4.3(8) . . . . ? C18 C10 N42 O42 177.2(10) . . . . ? C11 C10 N42 O42 -2(2) . . . . ? N41 C10 N42 Ni3 173(2) . . . . ? C18 C10 N42 Ni3 -5.4(13) . . . . ? C11 C10 N42 Ni3 175.4(8) . . . . ? O12 Ni3 N42 C10 -170.1(12) 2_666 . . . ? O41 Ni3 N42 C10 -180(2) . . . . ? N6 Ni3 N42 C10 5.7(10) . . . . ? N11 Ni3 N42 C10 -172.8(10) 2_666 . . . ? N3 Ni3 N42 C10 11(3) 2_666 . . . ? O10 Ni3 N42 C10 -84.6(11) . . . . ? O9 Ni3 N42 C10 96.7(12) . . . . ? O12 Ni3 N42 O42 7.0(13) 2_666 . . . ? O41 Ni3 N42 O42 -2.5(7) . . . . ? N6 Ni3 N42 O42 -177.2(14) . . . . ? N11 Ni3 N42 O42 4.3(15) 2_666 . . . ? N3 Ni3 N42 O42 -172.0(15) 2_666 . . . ? O10 Ni3 N42 O42 92.5(12) . . . . ? O9 Ni3 N42 O42 -86.2(12) . . . . ? C10 N42 O42 Ni2 5.8(17) . . . . ? Ni3 N42 O42 Ni2 -171.6(6) . . . . ? C10 N42 O42 Ni1 167.5(8) . . . . ? Ni3 N42 O42 Ni1 -9.9(16) . . . . ? O11 Ni2 O42 N42 169.6(12) . . . . ? N2 Ni2 O42 N42 -173.0(10) . . . . ? N5 Ni2 O42 N42 -6.6(11) . . . . ? N41 Ni2 O42 N42 0.1(11) . . . . ? N12 Ni2 O42 N42 173.3(12) . . . . ? O7 Ni2 O42 N42 -96.8(11) . . . . ? O8 Ni2 O42 N42 87.2(11) . . . . ? O11 Ni2 O42 Ni1 7.9(4) . . . . ? N2 Ni2 O42 Ni1 25.3(15) . . . . ? N5 Ni2 O42 Ni1 -168.4(5) . . . . ? N41 Ni2 O42 Ni1 -161.6(13) . . . . ? N12 Ni2 O42 Ni1 11.6(7) . . . . ? O7 Ni2 O42 Ni1 101.4(5) . . . . ? O8 Ni2 O42 Ni1 -74.5(5) . . . . ? O12 Ni1 O42 N42 -173.3(11) . . . . ? O12 Ni1 O42 N42 6.7(11) 2_666 . . . ? O111 Ni1 O42 N42 92.0(11) . . . . ? O111 Ni1 O42 N42 -88.0(11) 2_666 . . . ? O112 Ni1 O42 N42 111.3(11) . . . . ? O112 Ni1 O42 N42 -68.7(11) 2_666 . . . ? O11 Ni1 O42 N42 -170.5(12) . . . . ? O11 Ni1 O42 N42 9.5(12) 2_666 . . . ? O41 Ni1 O42 N42 9.2(9) . . . . ? O41 Ni1 O42 N42 -170.8(9) 2_666 . . . ? O12 Ni1 O42 Ni2 -10.6(6) . . . . ? O12 Ni1 O42 Ni2 169.4(6) 2_666 . . . ? O111 Ni1 O42 Ni2 -105.3(6) . . . . ? O111 Ni1 O42 Ni2 74.7(6) 2_666 . . . ? O112 Ni1 O42 Ni2 -86.0(7) . . . . ? O112 Ni1 O42 Ni2 94.0(7) 2_666 . . . ? O11 Ni1 O42 Ni2 -7.8(4) . . . . ? O11 Ni1 O42 Ni2 172.2(4) 2_666 . . . ? O41 Ni1 O42 Ni2 171.8(11) . . . . ? O41 Ni1 O42 Ni2 -8.2(11) 2_666 . . . ? C10 C11 N5 O5 179.5(6) . . . . ? C12 C11 N5 O5 0.0(12) . . . . ? C10 C11 N5 Ni2 -1.2(8) . . . . ? C12 C11 N5 Ni2 179.2(6) . . . . ? O42 Ni2 N5 C11 3.8(6) . . . . ? O11 Ni2 N5 C11 -8.8(13) . . . . ? N2 Ni2 N5 C11 179.6(5) . . . . ? N41 Ni2 N5 C11 0.8(5) . . . . ? N12 Ni2 N5 C11 -176(2) . . . . ? O7 Ni2 N5 C11 90.2(5) . . . . ? O8 Ni2 N5 C11 -88.6(5) . . . . ? O42 Ni2 N5 O5 -176.9(6) . . . . ? O11 Ni2 N5 O5 170.4(9) . . . . ? N2 Ni2 N5 O5 -1.2(5) . . . . ? N41 Ni2 N5 O5 -180.0(6) . . . . ? N12 Ni2 N5 O5 3(3) . . . . ? O7 Ni2 N5 O5 -90.6(5) . . . . ? O8 Ni2 N5 O5 90.7(5) . . . . ? C10 C18 N6 O6 179.2(5) . . . . ? C17 C18 N6 O6 -1.0(11) . . . . ? C10 C18 N6 Ni3 3.5(8) . . . . ? C17 C18 N6 Ni3 -176.7(5) . . . . ? O12 Ni3 N6 C18 7.5(14) 2_666 . . . ? O41 Ni3 N6 C18 -7.0(6) . . . . ? N3 Ni3 N6 C18 176.4(5) 2_666 . . . ? O10 Ni3 N6 C18 81.4(5) . . . . ? N42 Ni3 N6 C18 -4.6(6) . . . . ? O9 Ni3 N6 C18 -92.6(5) . . . . ? O12 Ni3 N6 O6 -167.9(12) 2_666 . . . ? O41 Ni3 N6 O6 177.6(5) . . . . ? N3 Ni3 N6 O6 1.0(5) 2_666 . . . ? O10 Ni3 N6 O6 -94.1(5) . . . . ? N42 Ni3 N6 O6 180.0(7) . . . . ? O9 Ni3 N6 O6 91.9(5) . . . . ? O12 Ni3 O9 C19 105.6(12) 2_666 . . . ? O41 Ni3 O9 C19 167.7(11) . . . . ? N6 Ni3 O9 C19 -94.2(11) . . . . ? N11 Ni3 O9 C19 78.5(11) 2_666 . . . ? N3 Ni3 O9 C19 2.7(11) 2_666 . . . ? N42 Ni3 O9 C19 -166.1(11) . . . . ? O131 S11 O111 Ni1 178.0(8) . . . . ? O121 S11 O111 Ni1 -48.5(13) . . . . ? O141 S11 O111 Ni1 62.0(11) . . . . ? O12 Ni1 O111 S11 -69.2(10) . . . . ? O12 Ni1 O111 S11 110.8(10) 2_666 . . . ? O112 Ni1 O111 S11 -51.5(17) . . . . ? O112 Ni1 O111 S11 128.5(17) 2_666 . . . ? O11 Ni1 O111 S11 -40.2(10) . . . . ? O11 Ni1 O111 S11 139.8(10) 2_666 . . . ? O41 Ni1 O111 S11 50.9(9) . . . . ? O41 Ni1 O111 S11 -129.1(9) 2_666 . . . ? O42 Ni1 O111 S11 21.3(10) . . . . ? O42 Ni1 O111 S11 -158.7(10) 2_666 . . . ? O122 S12 O112 Ni1 63(3) . . . . ? O132 S12 O112 Ni1 -163.2(14) . . . . ? O142 S12 O112 Ni1 -58(3) . . . . ? O12 Ni1 O112 S12 -138(2) . . . . ? O12 Ni1 O112 S12 42(2) 2_666 . . . ? O111 Ni1 O112 S12 60(2) . . . . ? O111 Ni1 O112 S12 -120(2) 2_666 . . . ? O11 Ni1 O112 S12 -108(2) . . . . ? O11 Ni1 O112 S12 72(2) 2_666 . . . ? O41 Ni1 O112 S12 -19(2) . . . . ? O41 Ni1 O112 S12 161(2) 2_666 . . . ? O42 Ni1 O112 S12 -48(2) . . . . ? O42 Ni1 O112 S12 132(2) 2_666 . . . ? C241 N7 C20 C21 69.5(19) . . . . ? C22 N7 C20 C21 -177.7(12) . . . . ? C242 N7 C20 C21 50.5(17) . . . . ? C20 N7 C22 C23 75.2(16) . . . . ? C241 N7 C22 C23 -160.4(14) . . . . ? C242 N7 C22 C23 -174(3) . . . . ? C20 N7 C241 C251 -169(2) . . . . ? C22 N7 C241 C251 70(3) . . . . ? C242 N7 C241 C251 -131(5) . . . . ? C20 N7 C242 C252 76(4) . . . . ? C241 N7 C242 C252 -71(4) . . . . ? C22 N7 C242 C252 -44(6) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.995 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.089 #===END data_Compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H52 N12 Ni5 O26 S2, C H4 O, 0.5(H4 O2), 5(H2 O)' _chemical_formula_sum 'C50 H68 N12 Ni5 O33 S2' _chemical_formula_weight 1722.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.2288(15) _cell_length_b 15.8791(12) _cell_length_c 22.8186(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.8130(10) _cell_angle_gamma 90.00 _cell_volume 7090.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7658 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.91 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5600 _exptl_absorpt_correction_T_max 0.7592 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34840 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12240 _reflns_number_gt 6794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+12.9773P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12240 _refine_ls_number_parameters 875 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2169 _refine_ls_wR_factor_gt 0.1768 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.501244(11) 0.541667(16) 0.254007(12) 0.02502(7) Uani 1 1 d . . . Ni2 Ni 0.607375(11) 0.611900(16) 0.200787(12) 0.02545(8) Uani 1 1 d . . . Ni3 Ni 0.458672(13) 0.768099(18) 0.287438(14) 0.04000(9) Uani 1 1 d . . . Ni4 Ni 0.392343(12) 0.470847(16) 0.304190(12) 0.02641(8) Uani 1 1 d . . . Ni5 Ni 0.545349(12) 0.315295(17) 0.222515(14) 0.03998(9) Uani 1 1 d . . . C1 C 0.61586(9) 0.79530(13) 0.21520(10) 0.0297(6) Uani 1 1 d . . . C2 C 0.56206(9) 0.78822(13) 0.24027(10) 0.0306(6) Uani 1 1 d . . . C3 C 0.54484(10) 0.87274(15) 0.25405(12) 0.0445(8) Uani 1 1 d . . . C4 C 0.58897(10) 0.93032(13) 0.23704(12) 0.0413(7) Uani 1 1 d . . . C5 C 0.59232(11) 1.01812(15) 0.24255(14) 0.0604(10) Uani 1 1 d . . . H5 H 0.5635 1.0477 0.2572 0.072 Uiso 1 1 calc R . . C6 C 0.63959(11) 1.05881(15) 0.22556(14) 0.0602(9) Uani 1 1 d . . . H6 H 0.6435 1.1171 0.2294 0.072 Uiso 1 1 calc R . . C7 C 0.68098(11) 1.01541(15) 0.20309(13) 0.0581(9) Uani 1 1 d . . . H7 H 0.7126 1.0450 0.1921 0.070 Uiso 1 1 calc R . . C8 C 0.67733(10) 0.92765(14) 0.19594(11) 0.0383(7) Uani 1 1 d . . . H8 H 0.7048 0.8986 0.1795 0.046 Uiso 1 1 calc R . . C9 C 0.63073(9) 0.88622(13) 0.21465(10) 0.0323(7) Uani 1 1 d . . . C10 C 0.32332(9) 0.61056(13) 0.33696(9) 0.0292(6) Uani 1 1 d . . . C11 C 0.36860(9) 0.66508(14) 0.32031(10) 0.0321(6) Uani 1 1 d . . . C12 C 0.34922(10) 0.75354(14) 0.32438(11) 0.0399(7) Uani 1 1 d . . . C13 C 0.29288(10) 0.75177(14) 0.34565(10) 0.0348(7) Uani 1 1 d . . . C14 C 0.25529(10) 0.81710(15) 0.35504(11) 0.0431(7) Uani 1 1 d . . . H14 H 0.2648 0.8726 0.3482 0.052 Uiso 1 1 calc R . . C15 C 0.20349(11) 0.79849(15) 0.37469(11) 0.0474(8) Uani 1 1 d . . . H15 H 0.1785 0.8419 0.3827 0.057 Uiso 1 1 calc R . . C16 C 0.18804(10) 0.71577(15) 0.38278(11) 0.0417(7) Uani 1 1 d . . . H16 H 0.1519 0.7048 0.3951 0.050 Uiso 1 1 calc R . . C17 C 0.22473(10) 0.64852(14) 0.37306(10) 0.0384(7) Uani 1 1 d . . . H17 H 0.2145 0.5934 0.3800 0.046 Uiso 1 1 calc R . . C18 C 0.27774(9) 0.66626(13) 0.35250(10) 0.0312(6) Uani 1 1 d . . . C19 C 0.38352(9) 0.28886(13) 0.28855(10) 0.0309(6) Uani 1 1 d . . . C20 C 0.43955(9) 0.29619(13) 0.26747(10) 0.0340(7) Uani 1 1 d . . . C21 C 0.45794(10) 0.21117(14) 0.25398(12) 0.0448(7) Uani 1 1 d . . . C22 C 0.41322(10) 0.15351(14) 0.26821(12) 0.0447(8) Uani 1 1 d . . . C23 C 0.40948(11) 0.06547(15) 0.26131(13) 0.0538(9) Uani 1 1 d . . . H23 H 0.4384 0.0363 0.2465 0.065 Uiso 1 1 calc R . . C24 C 0.36087(11) 0.02364(15) 0.27749(14) 0.0598(10) Uani 1 1 d . . . H24 H 0.3578 -0.0348 0.2747 0.072 Uiso 1 1 calc R . . C25 C 0.31762(10) 0.06796(15) 0.29751(12) 0.0471(8) Uani 1 1 d . . . H25 H 0.2853 0.0386 0.3076 0.057 Uiso 1 1 calc R . . C26 C 0.32018(10) 0.15630(14) 0.30336(11) 0.0394(7) Uani 1 1 d . . . H26 H 0.2904 0.1853 0.3172 0.047 Uiso 1 1 calc R . . C27 C 0.36811(9) 0.19794(13) 0.28794(10) 0.0304(6) Uani 1 1 d . . . C28 C 0.67604(9) 0.47288(13) 0.16723(9) 0.0279(6) Uani 1 1 d . . . C29 C 0.63193(9) 0.41762(13) 0.18525(10) 0.0288(6) Uani 1 1 d . . . C30 C 0.65190(9) 0.33021(14) 0.18177(10) 0.0343(7) Uani 1 1 d . . . C31 C 0.70805(9) 0.33278(14) 0.15943(10) 0.0319(7) Uani 1 1 d . . . C32 C 0.74361(10) 0.26817(14) 0.14764(10) 0.0345(7) Uani 1 1 d . . . H32 H 0.7349 0.2128 0.1555 0.041 Uiso 1 1 calc R . . C33 C 0.79277(10) 0.28621(15) 0.12391(10) 0.0387(7) Uani 1 1 d . . . H33 H 0.8169 0.2428 0.1148 0.046 Uiso 1 1 calc R . . C34 C 0.80620(10) 0.36961(15) 0.11363(10) 0.0416(7) Uani 1 1 d . . . H34 H 0.8400 0.3809 0.0983 0.050 Uiso 1 1 calc R . . C35 C 0.77101(10) 0.43550(15) 0.12553(10) 0.0360(7) Uani 1 1 d . . . H35 H 0.7801 0.4908 0.1178 0.043 Uiso 1 1 calc R . . C36 C 0.72139(9) 0.41741(13) 0.14948(9) 0.0283(6) Uani 1 1 d . . . N1 N 0.64207(7) 0.72942(11) 0.19957(8) 0.0288(5) Uani 1 1 d . . . N2 N 0.52801(8) 0.72729(10) 0.25156(8) 0.0299(5) Uani 1 1 d . . . N3 N 0.32569(8) 0.52827(10) 0.33360(8) 0.0286(5) Uani 1 1 d . . . N4 N 0.42179(8) 0.65615(11) 0.30548(8) 0.0306(5) Uani 1 1 d . . . N5 N 0.35493(8) 0.35399(11) 0.30227(8) 0.0302(5) Uani 1 1 d . . . N6 N 0.47598(8) 0.35677(11) 0.25866(8) 0.0320(6) Uani 1 1 d . . . N7 N 0.67324(7) 0.55462(11) 0.16981(8) 0.0297(5) Uani 1 1 d . . . N8 N 0.58132(8) 0.42748(11) 0.20349(8) 0.0307(5) Uani 1 1 d . . . O1 O 0.69227(6) 0.74480(9) 0.17889(7) 0.0393(5) Uani 1 1 d . . . H1 H 0.7062 0.6984 0.1695 0.059 Uiso 1 1 d R . . O2 O 0.53638(6) 0.65073(8) 0.23354(6) 0.0268(4) Uani 1 1 d . . . O3 O 0.49857(7) 0.88635(9) 0.27348(8) 0.0553(5) Uani 1 1 d . . . O4 O 0.28164(6) 0.48357(9) 0.34871(7) 0.0369(4) Uani 1 1 d . . . O5 O 0.44499(6) 0.57881(8) 0.30485(6) 0.0294(4) Uani 1 1 d . . . O6 O 0.38118(7) 0.81331(10) 0.31546(8) 0.0571(6) Uani 1 1 d . . . O7 O 0.30249(6) 0.33863(9) 0.31928(7) 0.0360(4) Uani 1 1 d . . . H7A H 0.2876 0.3852 0.3275 0.054 Uiso 1 1 d R . . O8 O 0.46668(6) 0.43278(8) 0.27535(7) 0.0305(4) Uani 1 1 d . . . O9 O 0.50669(8) 0.19724(11) 0.23719(9) 0.0650(6) Uani 1 1 d . . . O10 O 0.71620(6) 0.60007(9) 0.15288(7) 0.0368(5) Uani 1 1 d . . . O11 O 0.55652(6) 0.50398(8) 0.20329(7) 0.0313(4) Uani 1 1 d . . . O12 O 0.62270(7) 0.26923(10) 0.19342(8) 0.0504(6) Uani 1 1 d . . . S1 S 0.34237(2) 0.54426(3) 0.16117(2) 0.03015(16) Uani 1 1 d . . . O13 O 0.41633(6) 0.54598(9) 0.17248(6) 0.0320(4) Uani 1 1 d . . . O14 O 0.33207(6) 0.49191(9) 0.21017(6) 0.0332(5) Uani 1 1 d . . . O15 O 0.31868(7) 0.62862(9) 0.16481(8) 0.0429(5) Uani 1 1 d . . . O16 O 0.30478(7) 0.50674(11) 0.09871(7) 0.0449(5) Uani 1 1 d . . . S2 S 0.66179(2) 0.54188(3) 0.34498(2) 0.03003(16) Uani 1 1 d . . . O17 O 0.67110(6) 0.59266(9) 0.29496(6) 0.0323(4) Uani 1 1 d . . . O18 O 0.58801(6) 0.53750(9) 0.33450(7) 0.0355(5) Uani 1 1 d . . . O19 O 0.69857(7) 0.58202(11) 0.40660(7) 0.0453(5) Uani 1 1 d . . . O20 O 0.68693(7) 0.45587(9) 0.34359(7) 0.0403(5) Uani 1 1 d . . . O21 O 0.54055(6) 0.62846(10) 0.10707(6) 0.0355(5) Uani 1 1 d . . . C37 C 0.48052(10) 0.64848(15) 0.09207(10) 0.0394(7) Uani 1 1 d . . . H37 H 0.4672 0.6625 0.1252 0.047 Uiso 1 1 calc R . . N9 N 0.43339(10) 0.65220(18) 0.03488(10) 0.0690(9) Uani 1 1 d . . . C38 C 0.45182(17) 0.6300(4) -0.01907(16) 0.202(3) Uani 1 1 d . . . H38A H 0.4992 0.6144 -0.0035 0.303 Uiso 1 1 calc R . . H38B H 0.4441 0.6776 -0.0470 0.303 Uiso 1 1 calc R . . H38C H 0.4242 0.5836 -0.0419 0.303 Uiso 1 1 calc R . . C39 C 0.36344(13) 0.6777(2) 0.02201(14) 0.0787(13) Uani 1 1 d . . . H39A H 0.3347 0.6288 0.0134 0.118 Uiso 1 1 calc R . . H39B H 0.3476 0.7145 -0.0142 0.118 Uiso 1 1 calc R . . H39C H 0.3619 0.7068 0.0583 0.118 Uiso 1 1 calc R . . O22 O 0.45426(7) 0.44281(10) 0.39732(7) 0.0388(5) Uani 1 1 d . . . C40 C 0.51739(11) 0.44520(18) 0.41607(11) 0.0535(9) Uani 1 1 d . . . H40 H 0.5362 0.4711 0.3901 0.064 Uiso 1 1 calc R . . N10 N 0.55939(9) 0.41340(14) 0.47039(9) 0.0531(7) Uani 1 1 d . . . C41 C 0.63210(13) 0.4221(3) 0.49166(15) 0.1220(17) Uani 1 1 d . . . H41A H 0.6429 0.4537 0.4609 0.183 Uiso 1 1 calc R . . H41B H 0.6527 0.3674 0.4967 0.183 Uiso 1 1 calc R . . H41C H 0.6494 0.4512 0.5317 0.183 Uiso 1 1 calc R . . C42 C 0.53416(13) 0.3708(2) 0.51357(12) 0.0645(10) Uani 1 1 d . . . H42A H 0.4854 0.3769 0.4982 0.097 Uiso 1 1 calc R . . H42B H 0.5547 0.3955 0.5551 0.097 Uiso 1 1 calc R . . H42C H 0.5457 0.3122 0.5158 0.097 Uiso 1 1 calc R . . O23 O 0.47616(8) 0.30566(12) 0.13169(9) 0.0713(6) Uani 1 1 d D . . C43 C 0.44189(13) 0.37090(19) 0.09668(13) 0.0713(6) Uani 1 1 d D . . H43 H 0.4474 0.4219 0.1182 0.086 Uiso 1 1 calc R . . N11 N 0.40111(14) 0.3729(2) 0.03552(14) 0.3085(17) Uani 1 1 d D . . C44 C 0.3787(5) 0.2934(4) -0.0057(3) 0.444(6) Uani 1 1 d D . . H44A H 0.4018 0.2453 0.0185 0.666 Uiso 1 1 calc R . . H44B H 0.3900 0.2992 -0.0424 0.666 Uiso 1 1 calc R . . H44C H 0.3302 0.2862 -0.0191 0.666 Uiso 1 1 calc R . . C45 C 0.3576(2) 0.4407(3) -0.00187(18) 0.196(2) Uani 1 1 d D . . H45A H 0.3614 0.4886 0.0250 0.295 Uiso 1 1 calc R . . H45B H 0.3110 0.4220 -0.0196 0.295 Uiso 1 1 calc R . . H45C H 0.3717 0.4562 -0.0356 0.295 Uiso 1 1 calc R . . O24 O 0.52669(8) 0.77725(11) 0.37940(8) 0.0618(7) Uani 1 1 d D . . C46 C 0.5623(2) 0.7098(3) 0.40825(17) 0.243(2) Uani 1 1 d D . . H46 H 0.5537 0.6609 0.3840 0.291 Uiso 1 1 calc R . . N12 N 0.60682(18) 0.7037(3) 0.46499(16) 0.243(2) Uani 1 1 d D . . C47 C 0.6463(2) 0.6379(3) 0.5052(2) 0.243(2) Uani 1 1 d D . . H47A H 0.6776 0.6616 0.5444 0.364 Uiso 1 1 calc R . . H47B H 0.6716 0.6089 0.4844 0.364 Uiso 1 1 calc R . . H47C H 0.6165 0.5989 0.5139 0.364 Uiso 1 1 calc R . . C48 C 0.6100(2) 0.7819(3) 0.50560(19) 0.243(2) Uani 1 1 d D . . H48A H 0.6562 0.8020 0.5241 0.364 Uiso 1 1 calc R . . H48B H 0.5947 0.7675 0.5388 0.364 Uiso 1 1 calc R . . H48C H 0.5811 0.8251 0.4793 0.364 Uiso 1 1 calc R . . O25 O 0.38980(7) 0.76988(10) 0.19692(9) 0.0571(6) Uani 1 1 d . . . H251 H 0.3767 0.7196 0.1855 0.086 Uiso 1 1 d R . . H252 H 0.3712 0.8134 0.1756 0.086 Uiso 1 1 d R . . O26 O 0.61697(7) 0.31552(10) 0.31323(8) 0.0539(6) Uani 1 1 d . . . H261 H 0.6273 0.3612 0.3347 0.081 Uiso 1 1 d R . . C49 C 0.6652(2) 0.2495(3) 0.3515(2) 0.165(2) Uani 1 1 d . . . H49A H 0.6870 0.2682 0.3947 0.248 Uiso 1 1 calc R . . H49B H 0.6992 0.2394 0.3343 0.248 Uiso 1 1 calc R . . H49C H 0.6405 0.1984 0.3501 0.248 Uiso 1 1 calc R . . O27 O 0.33264(18) 0.9047(3) 0.13068(18) 0.1979(17) Uiso 1 1 d . . . H271 H 0.3280 0.9182 0.0932 0.297 Uiso 1 1 d R . . H272 H 0.2995 0.9280 0.1365 0.297 Uiso 1 1 d R . . O28 O 0.4802(3) 0.1454(4) 0.0763(3) 0.334(3) Uiso 1 1 d . . . H281 H 0.5038 0.1361 0.0543 0.500 Uiso 1 1 d R . . H282 H 0.4774 0.1922 0.0932 0.500 Uiso 1 1 d R . . O29 O 0.8158(3) 0.5507(5) 0.5117(3) 0.353(4) Uiso 1 1 d . . . H291 H 0.7882 0.5566 0.5307 0.530 Uiso 1 1 d R . . H292 H 0.8504 0.5678 0.5051 0.530 Uiso 1 1 d R . . O30 O 0.7854(3) 0.3871(4) 0.4636(3) 0.354(4) Uiso 1 1 d . . . H301 H 0.7555 0.4046 0.4287 0.532 Uiso 1 1 d R . . H302 H 0.7948 0.4373 0.4771 0.532 Uiso 1 1 d R . . C50 C 0.5012(4) 0.1237(6) -0.0549(3) 0.307(5) Uiso 1 1 d D . . H50A H 0.4558 0.1255 -0.0557 0.460 Uiso 1 1 calc R . . H50B H 0.5057 0.0758 -0.0786 0.460 Uiso 1 1 calc R . . H50C H 0.5099 0.1742 -0.0737 0.460 Uiso 1 1 calc R . . O31 O 0.5533(3) 0.1167(4) 0.0146(2) 0.332(3) Uiso 1 1 d D . . H31 H 0.5878 0.0995 0.0078 0.498 Uiso 1 1 d R . . O321 O 0.1807(4) 0.4845(6) 0.0176(4) 0.222(4) Uiso 0.50 1 d P A 1 H321 H 0.2206 0.4998 0.0427 0.333 Uiso 0.50 1 d PR A 1 H322 H 0.1447 0.5123 -0.0033 0.333 Uiso 0.50 1 d PR A 1 O322 O 0.1680(6) 0.3902(9) -0.0325(6) 0.360(7) Uiso 0.50 1 d P B 2 H323 H 0.1738 0.4429 -0.0256 0.540 Uiso 0.50 1 d PR B 2 H324 H 0.1263 0.3803 -0.0395 0.540 Uiso 0.50 1 d PR B 2 O331 O 0.5711(5) 0.9239(7) 0.4539(5) 0.276(5) Uiso 0.50 1 d P C 1 H331 H 0.5787 0.9745 0.4671 0.414 Uiso 0.50 1 d PR C 1 H332 H 0.5415 0.8914 0.4281 0.414 Uiso 0.50 1 d PR C 1 O332 O 0.5267(7) 1.1401(9) 0.4435(6) 0.352(7) Uiso 0.50 1 d P D 2 H333 H 0.5458 1.1189 0.4203 0.528 Uiso 0.50 1 d PR D 2 H334 H 0.5034 1.1027 0.4523 0.528 Uiso 0.50 1 d PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02061(9) 0.01867(12) 0.04277(12) 0.00449(11) 0.01995(8) 0.00120(9) Ni2 0.02216(10) 0.02264(13) 0.03681(12) 0.00286(12) 0.01721(8) 0.00061(10) Ni3 0.03566(11) 0.02437(14) 0.07633(16) -0.00073(14) 0.03965(10) -0.00257(11) Ni4 0.02358(10) 0.02097(13) 0.04129(12) 0.00424(12) 0.01984(8) 0.00224(10) Ni5 0.03530(11) 0.02314(14) 0.07959(16) 0.00039(14) 0.04211(9) -0.00115(11) C1 0.0276(9) 0.0254(11) 0.0374(10) 0.0089(9) 0.0140(7) 0.0020(9) C2 0.0226(8) 0.0262(11) 0.0489(11) 0.0103(10) 0.0205(7) 0.0008(8) C3 0.0360(10) 0.0315(12) 0.0781(14) -0.0044(12) 0.0353(8) -0.0091(9) C4 0.0397(10) 0.0177(10) 0.0754(14) 0.0111(11) 0.0320(9) -0.0024(9) C5 0.0396(11) 0.0323(13) 0.1224(19) 0.0051(14) 0.0459(10) 0.0040(10) C6 0.0436(10) 0.0160(11) 0.1391(19) 0.0080(13) 0.0551(10) -0.0013(9) C7 0.0342(10) 0.0348(13) 0.1104(18) 0.0267(13) 0.0336(10) -0.0042(10) C8 0.0285(9) 0.0314(12) 0.0588(12) 0.0115(11) 0.0212(8) 0.0027(9) C9 0.0186(8) 0.0264(11) 0.0505(12) 0.0111(10) 0.0120(8) -0.0002(8) C10 0.0312(9) 0.0256(11) 0.0381(10) 0.0016(9) 0.0215(7) -0.0021(8) C11 0.0227(8) 0.0304(11) 0.0529(11) 0.0062(10) 0.0254(7) 0.0047(8) C12 0.0387(10) 0.0218(11) 0.0694(13) 0.0006(11) 0.0321(8) 0.0006(9) C13 0.0354(9) 0.0319(12) 0.0435(11) 0.0026(10) 0.0225(8) 0.0061(9) C14 0.0433(10) 0.0339(13) 0.0640(12) -0.0078(11) 0.0339(8) 0.0008(10) C15 0.0460(10) 0.0362(13) 0.0735(13) -0.0011(12) 0.0379(8) 0.0118(10) C16 0.0349(9) 0.0449(14) 0.0595(11) -0.0096(11) 0.0339(7) 0.0015(10) C17 0.0373(9) 0.0276(12) 0.0627(12) 0.0018(11) 0.0330(8) 0.0016(9) C18 0.0249(8) 0.0291(11) 0.0442(10) -0.0050(10) 0.0184(7) 0.0016(8) C19 0.0248(9) 0.0296(11) 0.0412(10) 0.0166(10) 0.0159(7) 0.0010(8) C20 0.0246(8) 0.0281(11) 0.0580(11) 0.0027(10) 0.0256(7) 0.0028(8) C21 0.0393(9) 0.0226(11) 0.0915(14) 0.0049(11) 0.0462(8) 0.0029(9) C22 0.0301(9) 0.0300(12) 0.0861(14) 0.0117(12) 0.0359(8) -0.0011(9) C23 0.0466(11) 0.0244(12) 0.1028(17) -0.0012(13) 0.0427(10) -0.0054(10) C24 0.0509(12) 0.0230(12) 0.1203(19) 0.0034(14) 0.0493(11) -0.0007(10) C25 0.0302(9) 0.0352(13) 0.0877(14) 0.0123(12) 0.0357(8) -0.0085(9) C26 0.0227(9) 0.0300(12) 0.0697(13) 0.0083(11) 0.0225(8) 0.0010(9) C27 0.0273(9) 0.0173(10) 0.0502(11) 0.0050(10) 0.0189(7) 0.0023(8) C28 0.0270(8) 0.0288(11) 0.0329(9) 0.0035(9) 0.0172(7) 0.0023(8) C29 0.0266(9) 0.0232(11) 0.0417(10) 0.0054(9) 0.0188(7) 0.0054(8) C30 0.0285(9) 0.0320(12) 0.0507(11) -0.0054(10) 0.0245(7) -0.0044(9) C31 0.0209(8) 0.0346(12) 0.0432(11) -0.0052(10) 0.0155(7) 0.0059(9) C32 0.0287(9) 0.0318(12) 0.0458(11) 0.0039(10) 0.0173(8) 0.0044(9) C33 0.0346(10) 0.0378(13) 0.0461(12) -0.0013(11) 0.0185(8) 0.0087(10) C34 0.0374(9) 0.0494(14) 0.0529(11) 0.0066(11) 0.0336(7) 0.0061(10) C35 0.0380(10) 0.0347(12) 0.0440(11) -0.0016(10) 0.0255(7) -0.0009(9) C36 0.0242(8) 0.0293(11) 0.0371(10) -0.0017(9) 0.0181(7) 0.0040(8) N1 0.0208(7) 0.0297(9) 0.0379(8) 0.0071(8) 0.0136(6) 0.0017(7) N2 0.0226(7) 0.0207(9) 0.0519(9) 0.0033(8) 0.0206(6) 0.0034(7) N3 0.0309(7) 0.0201(9) 0.0416(8) 0.0049(8) 0.0216(6) 0.0060(7) N4 0.0300(7) 0.0235(9) 0.0457(9) 0.0018(8) 0.0228(6) 0.0057(7) N5 0.0278(7) 0.0278(9) 0.0423(8) 0.0068(8) 0.0218(6) 0.0017(7) N6 0.0250(7) 0.0212(9) 0.0551(10) -0.0038(8) 0.0214(6) -0.0023(7) N7 0.0229(7) 0.0316(9) 0.0398(8) 0.0028(8) 0.0179(6) 0.0010(7) N8 0.0272(7) 0.0244(9) 0.0440(9) -0.0002(8) 0.0177(6) 0.0030(7) O1 0.0356(6) 0.0313(8) 0.0652(8) 0.0053(7) 0.0350(5) -0.0025(6) O2 0.0253(6) 0.0179(7) 0.0436(7) -0.0005(6) 0.0204(5) -0.0020(5) O3 0.0536(7) 0.0207(8) 0.1199(10) -0.0042(8) 0.0646(6) -0.0051(6) O4 0.0357(6) 0.0289(8) 0.0624(7) 0.0076(7) 0.0370(5) 0.0030(6) O5 0.0297(6) 0.0203(7) 0.0473(7) 0.0029(6) 0.0250(5) 0.0028(5) O6 0.0643(7) 0.0206(8) 0.1157(10) 0.0079(8) 0.0671(6) 0.0050(7) O7 0.0331(6) 0.0249(7) 0.0678(7) 0.0056(7) 0.0391(5) -0.0020(6) O8 0.0294(6) 0.0211(7) 0.0472(7) 0.0001(7) 0.0215(5) -0.0013(6) O9 0.0630(8) 0.0347(9) 0.1283(11) -0.0130(9) 0.0710(6) -0.0062(7) O10 0.0360(6) 0.0349(8) 0.0508(7) 0.0070(7) 0.0292(5) -0.0036(6) O11 0.0290(6) 0.0208(7) 0.0530(7) -0.0004(7) 0.0255(5) 0.0002(6) O12 0.0441(7) 0.0296(9) 0.0935(10) 0.0024(8) 0.0442(6) 0.0022(7) S1 0.0239(2) 0.0305(3) 0.0406(3) 0.0036(2) 0.01754(17) 0.0017(2) O13 0.0253(6) 0.0373(8) 0.0425(7) 0.0069(7) 0.0229(5) 0.0005(6) O14 0.0216(6) 0.0386(8) 0.0433(7) 0.0045(7) 0.0169(5) -0.0047(6) O15 0.0328(6) 0.0331(8) 0.0724(9) 0.0063(8) 0.0308(6) 0.0016(6) O16 0.0415(8) 0.0564(10) 0.0356(8) -0.0021(8) 0.0135(6) -0.0096(8) S2 0.0225(2) 0.0309(3) 0.0406(3) 0.0081(2) 0.01635(17) 0.0029(2) O17 0.0207(6) 0.0425(9) 0.0385(7) 0.0054(7) 0.0166(5) -0.0008(6) O18 0.0218(6) 0.0424(9) 0.0480(7) 0.0160(7) 0.0198(5) 0.0036(6) O19 0.0382(7) 0.0588(10) 0.0389(8) -0.0018(8) 0.0151(6) -0.0078(8) O20 0.0313(7) 0.0349(8) 0.0571(8) 0.0065(8) 0.0198(6) 0.0025(6) O21 0.0282(6) 0.0464(9) 0.0357(7) 0.0024(7) 0.0166(5) 0.0028(7) C37 0.0393(10) 0.0492(14) 0.0345(10) 0.0154(11) 0.0196(8) -0.0028(10) N9 0.0375(10) 0.128(2) 0.0442(11) 0.0066(14) 0.0187(8) 0.0154(13) C38 0.061(2) 0.487(9) 0.0417(19) -0.027(4) 0.0036(15) 0.067(4) C39 0.0391(14) 0.132(3) 0.0553(16) 0.0222(19) 0.0074(12) 0.0120(17) O22 0.0334(7) 0.0403(9) 0.0430(8) 0.0109(7) 0.0151(6) 0.0011(7) C40 0.0352(11) 0.0844(19) 0.0416(12) 0.0221(13) 0.0156(9) -0.0077(12) N10 0.0372(9) 0.0731(14) 0.0483(10) 0.0287(11) 0.0159(8) 0.0088(10) C41 0.0286(14) 0.252(4) 0.0761(18) 0.081(2) 0.0101(12) 0.008(2) C42 0.0591(14) 0.091(2) 0.0479(13) 0.0232(15) 0.0260(10) -0.0014(15) O23 0.0567(7) 0.0713(11) 0.0958(10) -0.0240(10) 0.0405(6) -0.0088(8) C43 0.0567(7) 0.0713(11) 0.0958(10) -0.0240(10) 0.0405(6) -0.0088(8) N11 0.0933(15) 0.575(4) 0.311(2) 0.383(2) 0.1372(13) 0.165(2) C44 0.654(10) 0.539(11) 0.168(5) -0.144(7) 0.190(6) -0.419(8) C45 0.231(3) 0.293(6) 0.093(2) 0.045(3) 0.092(2) 0.149(4) O24 0.0574(9) 0.0564(11) 0.0765(11) -0.0261(10) 0.0313(7) -0.0166(9) C46 0.1397(15) 0.423(5) 0.203(2) 0.115(3) 0.1075(12) 0.064(2) N12 0.1397(15) 0.423(5) 0.203(2) 0.115(3) 0.1075(12) 0.064(2) C47 0.1397(15) 0.423(5) 0.203(2) 0.115(3) 0.1075(12) 0.064(2) C48 0.1397(15) 0.423(5) 0.203(2) 0.115(3) 0.1075(12) 0.064(2) O25 0.0325(7) 0.0355(9) 0.0988(12) 0.0260(9) 0.0205(7) 0.0029(7) O26 0.0385(7) 0.0369(9) 0.0935(11) 0.0272(9) 0.0337(7) 0.0151(7) C49 0.173(3) 0.165(5) 0.208(4) -0.055(4) 0.129(2) -0.045(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O8 2.0105(14) . ? Ni1 O2 2.0110(14) . ? Ni1 O13 2.0285(11) . ? Ni1 O11 2.0316(16) . ? Ni1 O18 2.0365(11) . ? Ni1 O5 2.0479(16) . ? Ni2 N1 2.0103(17) . ? Ni2 N7 2.0121(19) . ? Ni2 O2 2.0208(15) . ? Ni2 O11 2.0380(14) . ? Ni2 O17 2.0704(12) . ? Ni2 O21 2.0742(12) . ? Ni3 O25 2.0157(16) . ? Ni3 O24 2.0396(16) . ? Ni3 N2 2.047(2) . ? Ni3 N4 2.0476(18) . ? Ni3 O6 2.1087(19) . ? Ni3 O3 2.1339(16) . ? Ni4 N3 2.0049(19) . ? Ni4 N5 2.0123(17) . ? Ni4 O8 2.0234(16) . ? Ni4 O5 2.0434(14) . ? Ni4 O14 2.0550(13) . ? Ni4 O22 2.0679(13) . ? Ni5 O23 2.0287(17) . ? Ni5 O26 2.0387(15) . ? Ni5 N8 2.0499(18) . ? Ni5 N6 2.055(2) . ? Ni5 O9 2.1244(18) . ? Ni5 O12 2.1255(18) . ? C1 N1 1.298(3) . ? C1 C2 1.466(3) . ? C1 C9 1.479(3) . ? C2 N2 1.292(3) . ? C2 C3 1.457(3) . ? C3 O3 1.243(3) . ? C3 C4 1.465(4) . ? C4 C9 1.374(3) . ? C4 C5 1.399(3) . ? C5 C6 1.370(4) . ? C5 H5 0.9300 . ? C6 C7 1.363(4) . ? C6 H6 0.9300 . ? C7 C8 1.402(3) . ? C7 H7 0.9300 . ? C8 C9 1.386(3) . ? C8 H8 0.9300 . ? C10 N3 1.311(3) . ? C10 C11 1.449(3) . ? C10 C18 1.453(3) . ? C11 N4 1.306(3) . ? C11 C12 1.477(3) . ? C12 O6 1.229(3) . ? C12 C13 1.455(4) . ? C13 C14 1.375(3) . ? C13 C18 1.418(3) . ? C14 C15 1.371(4) . ? C14 H14 0.9300 . ? C15 C16 1.383(3) . ? C15 H15 0.9300 . ? C16 C17 1.389(3) . ? C16 H16 0.9300 . ? C17 C18 1.406(3) . ? C17 H17 0.9300 . ? C19 N5 1.297(3) . ? C19 C20 1.450(3) . ? C19 C27 1.479(3) . ? C20 N6 1.298(3) . ? C20 C21 1.471(3) . ? C21 O9 1.255(3) . ? C21 C22 1.444(3) . ? C22 C27 1.397(3) . ? C22 C23 1.406(3) . ? C23 C24 1.392(4) . ? C23 H23 0.9300 . ? C24 C25 1.368(4) . ? C24 H24 0.9300 . ? C25 C26 1.408(3) . ? C25 H25 0.9300 . ? C26 C27 1.369(3) . ? C26 H26 0.9300 . ? C28 N7 1.302(3) . ? C28 C29 1.454(3) . ? C28 C36 1.473(3) . ? C29 N8 1.303(3) . ? C29 C30 1.463(3) . ? C30 O12 1.233(3) . ? C30 C31 1.468(3) . ? C31 C32 1.361(3) . ? C31 C36 1.410(3) . ? C32 C33 1.379(4) . ? C32 H32 0.9300 . ? C33 C34 1.393(3) . ? C33 H33 0.9300 . ? C34 C35 1.373(3) . ? C34 H34 0.9300 . ? C35 C36 1.392(3) . ? C35 H35 0.9300 . ? N1 O1 1.345(2) . ? N2 O2 1.317(2) . ? N3 O4 1.322(2) . ? N4 O5 1.325(2) . ? N5 O7 1.336(2) . ? N6 O8 1.304(2) . ? N7 O10 1.332(2) . ? N8 O11 1.323(2) . ? O1 H1 0.8508 . ? O7 H7A 0.8530 . ? S1 O15 1.4445(16) . ? S1 O16 1.4633(15) . ? S1 O14 1.4761(16) . ? S1 O13 1.4894(14) . ? S2 O19 1.4634(15) . ? S2 O20 1.4712(16) . ? S2 O17 1.4723(16) . ? S2 O18 1.4914(14) . ? O21 C37 1.226(3) . ? C37 N9 1.302(3) . ? C37 H37 0.9300 . ? N9 C39 1.455(3) . ? N9 C38 1.472(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? O22 C40 1.239(3) . ? C40 N10 1.315(3) . ? C40 H40 0.9300 . ? N10 C41 1.434(3) . ? N10 C42 1.457(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? O23 C43 1.338(3) . ? C43 N11 1.327(4) . ? C43 H43 0.9300 . ? N11 C45 1.460(5) . ? N11 C44 1.535(7) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? O24 C46 1.328(5) . ? C46 N12 1.277(4) . ? C46 H46 0.9300 . ? N12 C47 1.428(5) . ? N12 C48 1.536(6) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? O25 H251 0.8523 . ? O25 H252 0.8499 . ? O26 C49 1.489(5) . ? O26 H261 0.8549 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? O27 H271 0.8505 . ? O27 H272 0.8498 . ? O28 H281 0.8494 . ? O28 H282 0.8503 . ? O29 H291 0.8583 . ? O29 H292 0.8501 . ? O30 H301 0.8490 . ? O30 H302 0.8501 . ? C50 O31 1.546(7) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? O31 H31 0.8497 . ? O321 H321 0.8534 . ? O321 H322 0.8498 . ? O321 H323 1.1493 . ? O322 H323 0.8521 . ? O322 H324 0.8501 . ? O331 H331 0.8512 . ? O331 H332 0.8491 . ? O332 H333 0.8530 . ? O332 H334 0.8454 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Ni1 O2 179.45(5) . . ? O8 Ni1 O13 88.46(5) . . ? O2 Ni1 O13 92.05(5) . . ? O8 Ni1 O11 103.31(6) . . ? O2 Ni1 O11 76.89(6) . . ? O13 Ni1 O11 89.52(6) . . ? O8 Ni1 O18 92.35(5) . . ? O2 Ni1 O18 87.14(5) . . ? O13 Ni1 O18 178.52(7) . . ? O11 Ni1 O18 89.09(6) . . ? O8 Ni1 O5 76.27(6) . . ? O2 Ni1 O5 103.52(6) . . ? O13 Ni1 O5 90.22(5) . . ? O11 Ni1 O5 179.52(5) . . ? O18 Ni1 O5 91.18(6) . . ? N1 Ni2 N7 96.12(7) . . ? N1 Ni2 O2 92.96(7) . . ? N7 Ni2 O2 170.89(6) . . ? N1 Ni2 O11 169.06(7) . . ? N7 Ni2 O11 94.45(7) . . ? O2 Ni2 O11 76.53(6) . . ? N1 Ni2 O17 93.20(6) . . ? N7 Ni2 O17 91.97(6) . . ? O2 Ni2 O17 86.68(5) . . ? O11 Ni2 O17 89.25(5) . . ? N1 Ni2 O21 88.62(6) . . ? N7 Ni2 O21 89.19(6) . . ? O2 Ni2 O21 91.87(6) . . ? O11 Ni2 O21 88.71(6) . . ? O17 Ni2 O21 177.73(6) . . ? O25 Ni3 O24 174.99(7) . . ? O25 Ni3 N2 86.73(7) . . ? O24 Ni3 N2 95.86(7) . . ? O25 Ni3 N4 92.08(6) . . ? O24 Ni3 N4 91.62(7) . . ? N2 Ni3 N4 101.30(7) . . ? O25 Ni3 O6 87.98(7) . . ? O24 Ni3 O6 89.32(7) . . ? N2 Ni3 O6 174.54(6) . . ? N4 Ni3 O6 80.24(7) . . ? O25 Ni3 O3 90.39(6) . . ? O24 Ni3 O3 85.83(7) . . ? N2 Ni3 O3 80.23(7) . . ? N4 Ni3 O3 177.16(7) . . ? O6 Ni3 O3 98.46(6) . . ? N3 Ni4 N5 95.90(7) . . ? N3 Ni4 O8 170.16(6) . . ? N5 Ni4 O8 93.93(7) . . ? N3 Ni4 O5 94.07(6) . . ? N5 Ni4 O5 169.73(7) . . ? O8 Ni4 O5 76.09(6) . . ? N3 Ni4 O14 92.34(6) . . ? N5 Ni4 O14 92.67(6) . . ? O8 Ni4 O14 87.56(6) . . ? O5 Ni4 O14 89.34(5) . . ? N3 Ni4 O22 90.22(6) . . ? N5 Ni4 O22 84.95(6) . . ? O8 Ni4 O22 90.28(6) . . ? O5 Ni4 O22 92.59(5) . . ? O14 Ni4 O22 176.68(6) . . ? O23 Ni5 O26 175.55(7) . . ? O23 Ni5 N8 91.77(7) . . ? O26 Ni5 N8 91.21(6) . . ? O23 Ni5 N6 94.96(7) . . ? O26 Ni5 N6 87.72(7) . . ? N8 Ni5 N6 100.96(7) . . ? O23 Ni5 O9 85.61(7) . . ? O26 Ni5 O9 91.32(6) . . ? N8 Ni5 O9 177.01(7) . . ? N6 Ni5 O9 80.72(7) . . ? O23 Ni5 O12 89.77(7) . . ? O26 Ni5 O12 87.45(7) . . ? N8 Ni5 O12 80.59(7) . . ? N6 Ni5 O12 174.95(6) . . ? O9 Ni5 O12 97.93(7) . . ? N1 C1 C2 121.80(19) . . ? N1 C1 C9 132.0(2) . . ? C2 C1 C9 106.21(19) . . ? N2 C2 C3 116.1(2) . . ? N2 C2 C1 135.7(2) . . ? C3 C2 C1 108.19(19) . . ? O3 C3 C2 122.4(2) . . ? O3 C3 C4 131.4(2) . . ? C2 C3 C4 106.1(2) . . ? C9 C4 C5 121.6(2) . . ? C9 C4 C3 110.58(19) . . ? C5 C4 C3 127.8(2) . . ? C6 C5 C4 117.5(3) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C7 C6 C5 121.2(2) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 122.1(3) . . ? C6 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C9 C8 C7 116.7(2) . . ? C9 C8 H8 121.6 . . ? C7 C8 H8 121.6 . . ? C4 C9 C8 120.9(2) . . ? C4 C9 C1 108.9(2) . . ? C8 C9 C1 130.3(2) . . ? N3 C10 C11 122.4(2) . . ? N3 C10 C18 131.7(2) . . ? C11 C10 C18 105.81(18) . . ? N4 C11 C10 137.0(2) . . ? N4 C11 C12 114.2(2) . . ? C10 C11 C12 108.81(19) . . ? O6 C12 C13 130.4(2) . . ? O6 C12 C11 122.6(2) . . ? C13 C12 C11 106.72(19) . . ? C14 C13 C18 122.4(2) . . ? C14 C13 C12 129.7(2) . . ? C18 C13 C12 107.8(2) . . ? C15 C14 C13 118.4(2) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 120.7(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 122.1(2) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C16 C17 C18 118.1(2) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C17 C18 C13 118.3(2) . . ? C17 C18 C10 130.9(2) . . ? C13 C18 C10 110.8(2) . . ? N5 C19 C20 122.5(2) . . ? N5 C19 C27 131.1(2) . . ? C20 C19 C27 106.38(19) . . ? N6 C20 C19 136.5(2) . . ? N6 C20 C21 115.2(2) . . ? C19 C20 C21 108.31(19) . . ? O9 C21 C22 130.5(2) . . ? O9 C21 C20 122.9(2) . . ? C22 C21 C20 106.5(2) . . ? C27 C22 C23 121.5(2) . . ? C27 C22 C21 110.2(2) . . ? C23 C22 C21 128.3(2) . . ? C24 C23 C22 117.4(3) . . ? C24 C23 H23 121.3 . . ? C22 C23 H23 121.3 . . ? C25 C24 C23 120.4(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 122.5(2) . . ? C24 C25 H25 118.7 . . ? C26 C25 H25 118.7 . . ? C27 C26 C25 117.5(2) . . ? C27 C26 H26 121.2 . . ? C25 C26 H26 121.2 . . ? C26 C27 C22 120.6(2) . . ? C26 C27 C19 130.7(2) . . ? C22 C27 C19 108.6(2) . . ? N7 C28 C29 122.9(2) . . ? N7 C28 C36 130.9(2) . . ? C29 C28 C36 106.15(18) . . ? N8 C29 C28 135.95(19) . . ? N8 C29 C30 115.07(19) . . ? C28 C29 C30 108.98(19) . . ? O12 C30 C29 123.6(2) . . ? O12 C30 C31 129.8(2) . . ? C29 C30 C31 106.51(19) . . ? C32 C31 C36 121.7(2) . . ? C32 C31 C30 129.4(2) . . ? C36 C31 C30 108.87(19) . . ? C31 C32 C33 118.9(2) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C32 C33 C34 119.9(2) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 121.9(2) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 C36 118.2(2) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C35 C36 C31 119.3(2) . . ? C35 C36 C28 131.3(2) . . ? C31 C36 C28 109.4(2) . . ? C1 N1 O1 115.63(17) . . ? C1 N1 Ni2 123.09(15) . . ? O1 N1 Ni2 121.18(13) . . ? C2 N2 O2 118.37(19) . . ? C2 N2 Ni3 112.79(14) . . ? O2 N2 Ni3 128.46(13) . . ? C10 N3 O4 118.21(18) . . ? C10 N3 Ni4 121.40(16) . . ? O4 N3 Ni4 120.37(12) . . ? C11 N4 O5 117.76(18) . . ? C11 N4 Ni3 113.22(14) . . ? O5 N4 Ni3 129.02(14) . . ? C19 N5 O7 116.44(17) . . ? C19 N5 Ni4 121.51(15) . . ? O7 N5 Ni4 121.90(13) . . ? C20 N6 O8 118.31(19) . . ? C20 N6 Ni5 112.79(15) . . ? O8 N6 Ni5 128.84(14) . . ? C28 N7 O10 118.60(18) . . ? C28 N7 Ni2 121.12(16) . . ? O10 N7 Ni2 120.27(13) . . ? C29 N8 O11 119.04(18) . . ? C29 N8 Ni5 112.59(14) . . ? O11 N8 Ni5 128.18(14) . . ? N1 O1 H1 109.3 . . ? N2 O2 Ni1 127.97(13) . . ? N2 O2 Ni2 127.39(12) . . ? Ni1 O2 Ni2 102.71(6) . . ? C3 O3 Ni3 108.33(14) . . ? N4 O5 Ni4 124.96(12) . . ? N4 O5 Ni1 125.02(13) . . ? Ni4 O5 Ni1 101.05(6) . . ? C12 O6 Ni3 109.45(15) . . ? N5 O7 H7A 109.1 . . ? N6 O8 Ni1 127.93(14) . . ? N6 O8 Ni4 126.67(12) . . ? Ni1 O8 Ni4 103.05(6) . . ? C21 O9 Ni5 107.90(15) . . ? N8 O11 Ni1 125.83(13) . . ? N8 O11 Ni2 123.89(12) . . ? Ni1 O11 Ni2 101.39(6) . . ? C30 O12 Ni5 108.12(15) . . ? O15 S1 O16 111.29(9) . . ? O15 S1 O14 108.75(10) . . ? O16 S1 O14 108.88(9) . . ? O15 S1 O13 109.88(9) . . ? O16 S1 O13 108.44(9) . . ? O14 S1 O13 109.57(8) . . ? S1 O13 Ni1 131.34(10) . . ? S1 O14 Ni4 131.86(8) . . ? O19 S2 O20 111.23(9) . . ? O19 S2 O17 108.93(9) . . ? O20 S2 O17 109.43(10) . . ? O19 S2 O18 108.08(10) . . ? O20 S2 O18 108.69(9) . . ? O17 S2 O18 110.46(8) . . ? S2 O17 Ni2 130.95(8) . . ? S2 O18 Ni1 132.02(10) . . ? C37 O21 Ni2 122.82(15) . . ? O21 C37 N9 127.1(2) . . ? O21 C37 H37 116.5 . . ? N9 C37 H37 116.5 . . ? C37 N9 C39 122.8(2) . . ? C37 N9 C38 118.5(2) . . ? C39 N9 C38 118.6(2) . . ? N9 C38 H38A 109.5 . . ? N9 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N9 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N9 C39 H39A 109.5 . . ? N9 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N9 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 O22 Ni4 121.31(17) . . ? O22 C40 N10 124.1(3) . . ? O22 C40 H40 117.9 . . ? N10 C40 H40 117.9 . . ? C40 N10 C41 122.0(3) . . ? C40 N10 C42 121.5(2) . . ? C41 N10 C42 116.5(2) . . ? N10 C41 H41A 109.5 . . ? N10 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N10 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N10 C42 H42A 109.5 . . ? N10 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N10 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C43 O23 Ni5 124.22(17) . . ? N11 C43 O23 128.9(3) . . ? N11 C43 H43 115.5 . . ? O23 C43 H43 115.5 . . ? C43 N11 C45 129.7(3) . . ? C43 N11 C44 123.1(4) . . ? C45 N11 C44 105.8(3) . . ? N11 C44 H44A 109.5 . . ? N11 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N11 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N11 C45 H45A 109.5 . . ? N11 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N11 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 O24 Ni3 119.5(2) . . ? N12 C46 O24 128.3(4) . . ? N12 C46 H46 115.9 . . ? O24 C46 H46 115.9 . . ? C46 N12 C47 136.7(4) . . ? C46 N12 C48 113.1(4) . . ? C47 N12 C48 109.1(3) . . ? N12 C47 H47A 109.5 . . ? N12 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N12 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N12 C48 H48A 109.5 . . ? N12 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N12 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Ni3 O25 H251 108.7 . . ? Ni3 O25 H252 126.1 . . ? H251 O25 H252 124.4 . . ? C49 O26 Ni5 131.8(2) . . ? C49 O26 H261 107.2 . . ? Ni5 O26 H261 120.5 . . ? O26 C49 H49A 109.5 . . ? O26 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O26 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? H271 O27 H272 105.6 . . ? H281 O28 H282 125.5 . . ? H291 O29 H292 149.3 . . ? H301 O30 H302 91.1 . . ? O31 C50 H50A 109.5 . . ? O31 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O31 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C50 O31 H31 99.2 . . ? H321 O321 H322 132.2 . . ? H321 O321 H323 120.1 . . ? H322 O321 H323 91.6 . . ? H323 O322 H324 106.4 . . ? H331 O331 H332 143.8 . . ? H333 O332 H334 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -1.9(3) . . . . ? C9 C1 C2 N2 179.4(2) . . . . ? N1 C1 C2 C3 179.00(17) . . . . ? C9 C1 C2 C3 0.3(2) . . . . ? N2 C2 C3 O3 -2.4(3) . . . . ? C1 C2 C3 O3 176.93(19) . . . . ? N2 C2 C3 C4 -179.41(17) . . . . ? C1 C2 C3 C4 -0.1(2) . . . . ? O3 C3 C4 C9 -176.8(2) . . . . ? C2 C3 C4 C9 -0.2(2) . . . . ? O3 C3 C4 C5 4.4(4) . . . . ? C2 C3 C4 C5 -179.0(2) . . . . ? C9 C4 C5 C6 -0.9(3) . . . . ? C3 C4 C5 C6 177.8(2) . . . . ? C4 C5 C6 C7 1.1(4) . . . . ? C5 C6 C7 C8 0.3(4) . . . . ? C6 C7 C8 C9 -1.8(3) . . . . ? C5 C4 C9 C8 -0.8(3) . . . . ? C3 C4 C9 C8 -179.61(18) . . . . ? C5 C4 C9 C1 179.3(2) . . . . ? C3 C4 C9 C1 0.4(2) . . . . ? C7 C8 C9 C4 2.1(3) . . . . ? C7 C8 C9 C1 -178.0(2) . . . . ? N1 C1 C9 C4 -178.9(2) . . . . ? C2 C1 C9 C4 -0.4(2) . . . . ? N1 C1 C9 C8 1.1(3) . . . . ? C2 C1 C9 C8 179.57(19) . . . . ? N3 C10 C11 N4 -7.6(3) . . . . ? C18 C10 C11 N4 175.6(2) . . . . ? N3 C10 C11 C12 175.58(17) . . . . ? C18 C10 C11 C12 -1.3(2) . . . . ? N4 C11 C12 O6 -1.0(3) . . . . ? C10 C11 C12 O6 176.64(19) . . . . ? N4 C11 C12 C13 -175.95(17) . . . . ? C10 C11 C12 C13 1.7(2) . . . . ? O6 C12 C13 C14 7.8(4) . . . . ? C11 C12 C13 C14 -177.8(2) . . . . ? O6 C12 C13 C18 -175.8(2) . . . . ? C11 C12 C13 C18 -1.4(2) . . . . ? C18 C13 C14 C15 3.2(3) . . . . ? C12 C13 C14 C15 179.1(2) . . . . ? C13 C14 C15 C16 -2.1(3) . . . . ? C14 C15 C16 C17 1.6(3) . . . . ? C15 C16 C17 C18 -1.9(3) . . . . ? C16 C17 C18 C13 2.9(3) . . . . ? C16 C17 C18 C10 -178.30(19) . . . . ? C14 C13 C18 C17 -3.6(3) . . . . ? C12 C13 C18 C17 179.73(17) . . . . ? C14 C13 C18 C10 177.32(18) . . . . ? C12 C13 C18 C10 0.7(2) . . . . ? N3 C10 C18 C17 5.0(4) . . . . ? C11 C10 C18 C17 -178.5(2) . . . . ? N3 C10 C18 C13 -176.07(19) . . . . ? C11 C10 C18 C13 0.4(2) . . . . ? N5 C19 C20 N6 2.8(4) . . . . ? C27 C19 C20 N6 -179.0(2) . . . . ? N5 C19 C20 C21 -178.02(17) . . . . ? C27 C19 C20 C21 0.2(2) . . . . ? N6 C20 C21 O9 2.3(3) . . . . ? C19 C20 C21 O9 -177.1(2) . . . . ? N6 C20 C21 C22 178.49(17) . . . . ? C19 C20 C21 C22 -0.9(2) . . . . ? O9 C21 C22 C27 177.2(2) . . . . ? C20 C21 C22 C27 1.4(2) . . . . ? O9 C21 C22 C23 -6.2(4) . . . . ? C20 C21 C22 C23 178.0(2) . . . . ? C27 C22 C23 C24 -2.7(3) . . . . ? C21 C22 C23 C24 -179.0(2) . . . . ? C22 C23 C24 C25 1.8(4) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C25 C26 C27 C22 -1.0(3) . . . . ? C25 C26 C27 C19 179.61(19) . . . . ? C23 C22 C27 C26 2.3(3) . . . . ? C21 C22 C27 C26 179.25(19) . . . . ? C23 C22 C27 C19 -178.2(2) . . . . ? C21 C22 C27 C19 -1.3(2) . . . . ? N5 C19 C27 C26 -1.9(4) . . . . ? C20 C19 C27 C26 -179.9(2) . . . . ? N5 C19 C27 C22 178.6(2) . . . . ? C20 C19 C27 C22 0.7(2) . . . . ? N7 C28 C29 N8 3.9(3) . . . . ? C36 C28 C29 N8 -177.9(2) . . . . ? N7 C28 C29 C30 -175.43(16) . . . . ? C36 C28 C29 C30 2.8(2) . . . . ? N8 C29 C30 O12 1.8(3) . . . . ? C28 C29 C30 O12 -178.74(18) . . . . ? N8 C29 C30 C31 178.93(16) . . . . ? C28 C29 C30 C31 -1.6(2) . . . . ? O12 C30 C31 C32 -2.2(3) . . . . ? C29 C30 C31 C32 -179.08(19) . . . . ? O12 C30 C31 C36 176.63(19) . . . . ? C29 C30 C31 C36 -0.3(2) . . . . ? C36 C31 C32 C33 -1.6(3) . . . . ? C30 C31 C32 C33 177.08(19) . . . . ? C31 C32 C33 C34 1.3(3) . . . . ? C32 C33 C34 C35 -1.0(3) . . . . ? C33 C34 C35 C36 1.0(3) . . . . ? C34 C35 C36 C31 -1.3(3) . . . . ? C34 C35 C36 C28 179.56(18) . . . . ? C32 C31 C36 C35 1.6(3) . . . . ? C30 C31 C36 C35 -177.31(16) . . . . ? C32 C31 C36 C28 -179.06(17) . . . . ? C30 C31 C36 C28 2.0(2) . . . . ? N7 C28 C36 C35 -5.7(3) . . . . ? C29 C28 C36 C35 176.27(19) . . . . ? N7 C28 C36 C31 175.03(18) . . . . ? C29 C28 C36 C31 -3.0(2) . . . . ? C2 C1 N1 O1 -178.24(15) . . . . ? C9 C1 N1 O1 0.1(3) . . . . ? C2 C1 N1 Ni2 5.2(2) . . . . ? C9 C1 N1 Ni2 -176.47(15) . . . . ? N7 Ni2 N1 C1 179.00(14) . . . . ? O2 Ni2 N1 C1 -1.83(15) . . . . ? O11 Ni2 N1 C1 14.1(4) . . . . ? O17 Ni2 N1 C1 -88.66(15) . . . . ? O21 Ni2 N1 C1 89.97(15) . . . . ? N7 Ni2 N1 O1 2.66(13) . . . . ? O2 Ni2 N1 O1 -178.17(12) . . . . ? O11 Ni2 N1 O1 -162.3(3) . . . . ? O17 Ni2 N1 O1 94.99(12) . . . . ? O21 Ni2 N1 O1 -86.38(12) . . . . ? C3 C2 N2 O2 172.79(15) . . . . ? C1 C2 N2 O2 -6.3(3) . . . . ? C3 C2 N2 Ni3 -0.7(2) . . . . ? C1 C2 N2 Ni3 -179.76(18) . . . . ? O25 Ni3 N2 C2 92.92(13) . . . . ? O24 Ni3 N2 C2 -82.77(13) . . . . ? N4 Ni3 N2 C2 -175.61(12) . . . . ? O3 Ni3 N2 C2 1.96(13) . . . . ? O25 Ni3 N2 O2 -79.73(14) . . . . ? O24 Ni3 N2 O2 104.57(14) . . . . ? N4 Ni3 N2 O2 11.73(15) . . . . ? O3 Ni3 N2 O2 -170.70(15) . . . . ? C11 C10 N3 O4 -178.88(15) . . . . ? C18 C10 N3 O4 -2.9(3) . . . . ? C11 C10 N3 Ni4 -0.5(2) . . . . ? C18 C10 N3 Ni4 175.49(16) . . . . ? N5 Ni4 N3 C10 -173.16(14) . . . . ? O5 Ni4 N3 C10 9.28(14) . . . . ? O14 Ni4 N3 C10 -80.22(14) . . . . ? O22 Ni4 N3 C10 101.89(14) . . . . ? N5 Ni4 N3 O4 5.20(13) . . . . ? O5 Ni4 N3 O4 -172.36(12) . . . . ? O14 Ni4 N3 O4 98.13(12) . . . . ? O22 Ni4 N3 O4 -79.75(12) . . . . ? C10 C11 N4 O5 -0.9(3) . . . . ? C12 C11 N4 O5 175.82(15) . . . . ? C10 C11 N4 Ni3 179.95(19) . . . . ? C12 C11 N4 Ni3 -3.3(2) . . . . ? O25 Ni3 N4 C11 -83.32(14) . . . . ? O24 Ni3 N4 C11 93.30(14) . . . . ? N2 Ni3 N4 C11 -170.40(13) . . . . ? O6 Ni3 N4 C11 4.28(13) . . . . ? O25 Ni3 N4 O5 97.69(15) . . . . ? O24 Ni3 N4 O5 -85.69(15) . . . . ? N2 Ni3 N4 O5 10.61(15) . . . . ? O6 Ni3 N4 O5 -174.72(15) . . . . ? C20 C19 N5 O7 178.05(16) . . . . ? C27 C19 N5 O7 0.3(3) . . . . ? C20 C19 N5 Ni4 -6.4(2) . . . . ? C27 C19 N5 Ni4 175.84(15) . . . . ? N3 Ni4 N5 C19 -176.46(14) . . . . ? O8 Ni4 N5 C19 3.17(15) . . . . ? O5 Ni4 N5 C19 -10.2(4) . . . . ? O14 Ni4 N5 C19 90.91(15) . . . . ? O22 Ni4 N5 C19 -86.76(15) . . . . ? N3 Ni4 N5 O7 -1.20(13) . . . . ? O8 Ni4 N5 O7 178.43(12) . . . . ? O5 Ni4 N5 O7 165.0(3) . . . . ? O14 Ni4 N5 O7 -93.83(13) . . . . ? O22 Ni4 N5 O7 88.50(13) . . . . ? C19 C20 N6 O8 5.5(3) . . . . ? C21 C20 N6 O8 -173.70(16) . . . . ? C19 C20 N6 Ni5 -177.10(19) . . . . ? C21 C20 N6 Ni5 3.7(2) . . . . ? O23 Ni5 N6 C20 79.33(14) . . . . ? O26 Ni5 N6 C20 -97.11(14) . . . . ? N8 Ni5 N6 C20 172.10(13) . . . . ? O9 Ni5 N6 C20 -5.39(13) . . . . ? O23 Ni5 N6 O8 -103.59(15) . . . . ? O26 Ni5 N6 O8 79.97(15) . . . . ? N8 Ni5 N6 O8 -10.82(15) . . . . ? O9 Ni5 N6 O8 171.69(15) . . . . ? C29 C28 N7 O10 179.37(15) . . . . ? C36 C28 N7 O10 1.7(3) . . . . ? C29 C28 N7 Ni2 1.0(2) . . . . ? C36 C28 N7 Ni2 -176.74(15) . . . . ? N1 Ni2 N7 C28 173.95(13) . . . . ? O11 Ni2 N7 C28 -8.89(14) . . . . ? O17 Ni2 N7 C28 80.52(14) . . . . ? O21 Ni2 N7 C28 -97.53(14) . . . . ? N1 Ni2 N7 O10 -4.44(12) . . . . ? O11 Ni2 N7 O10 172.73(12) . . . . ? O17 Ni2 N7 O10 -97.87(12) . . . . ? O21 Ni2 N7 O10 84.08(12) . . . . ? C28 C29 N8 O11 5.8(3) . . . . ? C30 C29 N8 O11 -174.87(15) . . . . ? C28 C29 N8 Ni5 -178.90(18) . . . . ? C30 C29 N8 Ni5 0.4(2) . . . . ? O23 Ni5 N8 C29 -90.80(14) . . . . ? O26 Ni5 N8 C29 85.89(14) . . . . ? N6 Ni5 N8 C29 173.80(13) . . . . ? O12 Ni5 N8 C29 -1.32(13) . . . . ? O23 Ni5 N8 O11 83.94(15) . . . . ? O26 Ni5 N8 O11 -99.37(15) . . . . ? N6 Ni5 N8 O11 -11.46(15) . . . . ? O12 Ni5 N8 O11 173.42(15) . . . . ? C2 N2 O2 Ni1 171.16(12) . . . . ? Ni3 N2 O2 Ni1 -16.54(19) . . . . ? C2 N2 O2 Ni2 9.7(2) . . . . ? Ni3 N2 O2 Ni2 -177.97(7) . . . . ? O13 Ni1 O2 N2 93.90(12) . . . . ? O11 Ni1 O2 N2 -177.07(12) . . . . ? O18 Ni1 O2 N2 -87.34(12) . . . . ? O5 Ni1 O2 N2 3.19(12) . . . . ? O13 Ni1 O2 Ni2 -101.13(6) . . . . ? O11 Ni1 O2 Ni2 -12.10(5) . . . . ? O18 Ni1 O2 Ni2 77.63(6) . . . . ? O5 Ni1 O2 Ni2 168.15(5) . . . . ? N1 Ni2 O2 N2 -5.90(13) . . . . ? O11 Ni2 O2 N2 177.16(13) . . . . ? O17 Ni2 O2 N2 87.14(13) . . . . ? O21 Ni2 O2 N2 -94.61(13) . . . . ? N1 Ni2 O2 Ni1 -170.98(6) . . . . ? O11 Ni2 O2 Ni1 12.08(5) . . . . ? O17 Ni2 O2 Ni1 -77.95(6) . . . . ? O21 Ni2 O2 Ni1 100.31(6) . . . . ? C2 C3 O3 Ni3 3.8(2) . . . . ? C4 C3 O3 Ni3 180.0(2) . . . . ? O25 Ni3 O3 C3 -89.66(15) . . . . ? O24 Ni3 O3 C3 93.64(15) . . . . ? N2 Ni3 O3 C3 -3.05(14) . . . . ? O6 Ni3 O3 C3 -177.68(14) . . . . ? C11 N4 O5 Ni4 15.4(2) . . . . ? Ni3 N4 O5 Ni4 -165.65(8) . . . . ? C11 N4 O5 Ni1 156.24(13) . . . . ? Ni3 N4 O5 Ni1 -24.80(18) . . . . ? N3 Ni4 O5 N4 -17.61(14) . . . . ? N5 Ni4 O5 N4 176.1(3) . . . . ? O8 Ni4 O5 N4 162.34(14) . . . . ? O14 Ni4 O5 N4 74.69(14) . . . . ? O22 Ni4 O5 N4 -108.01(14) . . . . ? N3 Ni4 O5 Ni1 -165.81(6) . . . . ? N5 Ni4 O5 Ni1 27.9(4) . . . . ? O8 Ni4 O5 Ni1 14.14(5) . . . . ? O14 Ni4 O5 Ni1 -73.52(6) . . . . ? O22 Ni4 O5 Ni1 103.78(6) . . . . ? O8 Ni1 O5 N4 -162.40(12) . . . . ? O2 Ni1 O5 N4 18.12(12) . . . . ? O13 Ni1 O5 N4 -74.03(12) . . . . ? O18 Ni1 O5 N4 105.47(12) . . . . ? O8 Ni1 O5 Ni4 -14.22(5) . . . . ? O2 Ni1 O5 Ni4 166.30(5) . . . . ? O13 Ni1 O5 Ni4 74.14(6) . . . . ? O18 Ni1 O5 Ni4 -106.35(6) . . . . ? C13 C12 O6 Ni3 178.12(19) . . . . ? C11 C12 O6 Ni3 4.5(2) . . . . ? O25 Ni3 O6 C12 87.85(15) . . . . ? O24 Ni3 O6 C12 -96.38(15) . . . . ? N4 Ni3 O6 C12 -4.61(14) . . . . ? O3 Ni3 O6 C12 177.94(14) . . . . ? C20 N6 O8 Ni1 -167.82(13) . . . . ? Ni5 N6 O8 Ni1 15.2(2) . . . . ? C20 N6 O8 Ni4 -8.2(2) . . . . ? Ni5 N6 O8 Ni4 174.82(7) . . . . ? O13 Ni1 O8 N6 87.18(13) . . . . ? O11 Ni1 O8 N6 -1.96(13) . . . . ? O18 Ni1 O8 N6 -91.58(13) . . . . ? O5 Ni1 O8 N6 177.78(13) . . . . ? O13 Ni1 O8 Ni4 -76.12(6) . . . . ? O11 Ni1 O8 Ni4 -165.27(5) . . . . ? O18 Ni1 O8 Ni4 105.11(6) . . . . ? O5 Ni1 O8 Ni4 14.47(5) . . . . ? N5 Ni4 O8 N6 4.33(14) . . . . ? O5 Ni4 O8 N6 -178.11(14) . . . . ? O14 Ni4 O8 N6 -88.19(14) . . . . ? O22 Ni4 O8 N6 89.29(14) . . . . ? N5 Ni4 O8 Ni1 167.92(6) . . . . ? O5 Ni4 O8 Ni1 -14.52(5) . . . . ? O14 Ni4 O8 Ni1 75.41(6) . . . . ? O22 Ni4 O8 Ni1 -107.12(6) . . . . ? C22 C21 O9 Ni5 178.2(2) . . . . ? C20 C21 O9 Ni5 -6.5(2) . . . . ? O23 Ni5 O9 C21 -89.55(15) . . . . ? O26 Ni5 O9 C21 93.69(15) . . . . ? N6 Ni5 O9 C21 6.21(14) . . . . ? O12 Ni5 O9 C21 -178.71(14) . . . . ? C29 N8 O11 Ni1 -159.24(13) . . . . ? Ni5 N8 O11 Ni1 26.31(19) . . . . ? C29 N8 O11 Ni2 -18.1(2) . . . . ? Ni5 N8 O11 Ni2 167.43(8) . . . . ? O8 Ni1 O11 N8 -19.66(12) . . . . ? O2 Ni1 O11 N8 159.83(12) . . . . ? O13 Ni1 O11 N8 -107.96(12) . . . . ? O18 Ni1 O11 N8 72.54(12) . . . . ? O8 Ni1 O11 Ni2 -167.54(5) . . . . ? O2 Ni1 O11 Ni2 11.94(5) . . . . ? O13 Ni1 O11 Ni2 104.15(6) . . . . ? O18 Ni1 O11 Ni2 -75.34(6) . . . . ? N1 Ni2 O11 N8 -176.9(3) . . . . ? N7 Ni2 O11 N8 18.07(14) . . . . ? O2 Ni2 O11 N8 -160.62(14) . . . . ? O17 Ni2 O11 N8 -73.86(14) . . . . ? O21 Ni2 O11 N8 107.15(14) . . . . ? N1 Ni2 O11 Ni1 -28.2(3) . . . . ? N7 Ni2 O11 Ni1 166.79(6) . . . . ? O2 Ni2 O11 Ni1 -11.90(5) . . . . ? O17 Ni2 O11 Ni1 74.87(6) . . . . ? O21 Ni2 O11 Ni1 -104.13(6) . . . . ? C29 C30 O12 Ni5 -2.7(2) . . . . ? C31 C30 O12 Ni5 -179.19(17) . . . . ? O23 Ni5 O12 C30 93.95(14) . . . . ? O26 Ni5 O12 C30 -89.52(13) . . . . ? N8 Ni5 O12 C30 2.13(13) . . . . ? O9 Ni5 O12 C30 179.49(13) . . . . ? O15 S1 O13 Ni1 86.69(13) . . . . ? O16 S1 O13 Ni1 -151.46(11) . . . . ? O14 S1 O13 Ni1 -32.74(14) . . . . ? O8 Ni1 O13 S1 56.40(12) . . . . ? O2 Ni1 O13 S1 -123.40(12) . . . . ? O11 Ni1 O13 S1 159.73(12) . . . . ? O5 Ni1 O13 S1 -19.86(12) . . . . ? O15 S1 O14 Ni4 -87.24(13) . . . . ? O16 S1 O14 Ni4 151.33(12) . . . . ? O13 S1 O14 Ni4 32.88(15) . . . . ? N3 Ni4 O14 S1 113.88(13) . . . . ? N5 Ni4 O14 S1 -150.09(13) . . . . ? O8 Ni4 O14 S1 -56.27(13) . . . . ? O5 Ni4 O14 S1 19.84(13) . . . . ? O19 S2 O17 Ni2 -148.76(11) . . . . ? O20 S2 O17 Ni2 89.44(12) . . . . ? O18 S2 O17 Ni2 -30.19(15) . . . . ? N1 Ni2 O17 S2 148.44(13) . . . . ? N7 Ni2 O17 S2 -115.32(13) . . . . ? O2 Ni2 O17 S2 55.66(12) . . . . ? O11 Ni2 O17 S2 -20.89(13) . . . . ? O19 S2 O18 Ni1 148.76(12) . . . . ? O20 S2 O18 Ni1 -90.41(13) . . . . ? O17 S2 O18 Ni1 29.67(15) . . . . ? O8 Ni1 O18 S2 125.69(13) . . . . ? O2 Ni1 O18 S2 -54.52(13) . . . . ? O11 Ni1 O18 S2 22.40(13) . . . . ? O5 Ni1 O18 S2 -158.00(12) . . . . ? N1 Ni2 O21 C37 -97.88(18) . . . . ? N7 Ni2 O21 C37 165.98(18) . . . . ? O2 Ni2 O21 C37 -4.97(18) . . . . ? O11 Ni2 O21 C37 71.51(18) . . . . ? Ni2 O21 C37 N9 -172.7(2) . . . . ? O21 C37 N9 C39 -179.3(3) . . . . ? O21 C37 N9 C38 0.4(5) . . . . ? N3 Ni4 O22 C40 -142.5(2) . . . . ? N5 Ni4 O22 C40 121.6(2) . . . . ? O8 Ni4 O22 C40 27.7(2) . . . . ? O5 Ni4 O22 C40 -48.4(2) . . . . ? Ni4 O22 C40 N10 -166.7(2) . . . . ? O22 C40 N10 C41 -176.2(3) . . . . ? O22 C40 N10 C42 0.8(4) . . . . ? N8 Ni5 O23 C43 -37.5(2) . . . . ? N6 Ni5 O23 C43 63.7(2) . . . . ? O9 Ni5 O23 C43 143.9(2) . . . . ? O12 Ni5 O23 C43 -118.1(2) . . . . ? Ni5 O23 C43 N11 172.6(3) . . . . ? O23 C43 N11 C45 172.6(4) . . . . ? O23 C43 N11 C44 7.8(7) . . . . ? N2 Ni3 O24 C46 -57.4(3) . . . . ? N4 Ni3 O24 C46 44.1(3) . . . . ? O6 Ni3 O24 C46 124.3(3) . . . . ? O3 Ni3 O24 C46 -137.1(3) . . . . ? Ni3 O24 C46 N12 179.8(4) . . . . ? O24 C46 N12 C47 175.0(5) . . . . ? O24 C46 N12 C48 9.5(7) . . . . ? N8 Ni5 O26 C49 -131.5(3) . . . . ? N6 Ni5 O26 C49 127.6(3) . . . . ? O9 Ni5 O26 C49 46.9(3) . . . . ? O12 Ni5 O26 C49 -51.0(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O10 0.85 1.64 2.475(2) 166.1 . O1 H1 N7 0.85 2.39 3.043(2) 134.1 . O7 H7A O4 0.85 1.65 2.485(2) 163.6 . O7 H7A N3 0.85 2.40 3.048(2) 133.5 . O25 H251 O15 0.85 1.84 2.644(2) 157.2 . O25 H251 S1 0.85 2.88 3.7254(17) 173.7 . O26 H261 O20 0.85 1.92 2.618(2) 137.4 . O26 H261 S2 0.85 2.95 3.7170(17) 150.8 . O27 H271 O29 0.85 1.84 2.693(8) 178.3 4_575 O27 H272 O4 0.85 2.08 2.925(5) 179.3 2 O28 H281 O31 0.85 1.66 2.509(10) 177.1 . O28 H282 O23 0.85 2.01 2.857(7) 176.1 . O29 H291 O27 0.86 2.19 2.693(8) 117.0 4_676 O29 H292 O31 0.85 2.39 3.237(10) 179.2 2_655 O30 H301 O20 0.85 2.09 2.936(6) 175.5 . O30 H302 O29 0.85 1.95 2.796(10) 177.4 . O31 H31 O29 0.85 2.39 3.237(10) 179.7 2_645 O321 H321 O16 0.85 1.75 2.590(7) 166.9 . O321 H322 O331 0.85 1.80 2.649(12) 177.0 4_575 O322 H324 O332 0.85 2.02 2.874(19) 178.6 4_575 O331 H331 O321 0.85 2.12 2.649(12) 119.7 4_676 O331 H332 O24 0.85 2.09 2.821(11) 144.7 . O332 H333 O322 0.85 2.40 2.87(2) 116.0 4_676 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.590 _refine_diff_density_min -1.135 _refine_diff_density_rms 0.124 #===END data_Compound 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H33 Mn3 N8 O16, H2 O' _chemical_formula_sum 'C35 H35 Mn3 N8 O17' _chemical_formula_weight 1004.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.293(7) _cell_length_b 17.769(4) _cell_length_c 13.601(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.72(3) _cell_angle_gamma 90.00 _cell_volume 8520(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 16692 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.70 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6726 _exptl_absorpt_correction_T_max 0.8697 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18191 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7111 _reflns_number_gt 4710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1784P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7111 _refine_ls_number_parameters 559 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2857 _refine_ls_wR_factor_gt 0.2511 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.20586(3) 0.32547(6) 0.36952(8) 0.0385(3) Uani 1 1 d . . . Mn2 Mn 0.11699(3) 0.27621(6) 0.38651(9) 0.0424(4) Uani 1 1 d . . . Mn3 Mn 0.14267(3) 0.45166(6) 0.35036(10) 0.0469(4) Uani 1 1 d . . . C1 C 0.2561(2) 0.4573(4) 0.3701(5) 0.0344(15) Uani 1 1 d . . . C2 C 0.2883(2) 0.4058(4) 0.3682(5) 0.0398(16) Uani 1 1 d . . . C3 C 0.3238(2) 0.4526(5) 0.3674(6) 0.0469(19) Uani 1 1 d . . . C4 C 0.3106(2) 0.5317(4) 0.3640(5) 0.0441(18) Uani 1 1 d . . . C5 C 0.3327(2) 0.5978(4) 0.3564(6) 0.0472(18) Uani 1 1 d . . . H5 H 0.3593 0.5953 0.3564 0.057 Uiso 1 1 calc R . . C6 C 0.3145(3) 0.6649(4) 0.3492(6) 0.053(2) Uani 1 1 d . . . H6 H 0.3287 0.7093 0.3442 0.064 Uiso 1 1 calc R . . C7 C 0.2739(3) 0.6695(4) 0.3491(7) 0.053(2) Uani 1 1 d . . . H7 H 0.2618 0.7163 0.3409 0.064 Uiso 1 1 calc R . . C8 C 0.2527(2) 0.6051(4) 0.3612(6) 0.0451(18) Uani 1 1 d . . . H8 H 0.2263 0.6078 0.3662 0.054 Uiso 1 1 calc R . . C9 C 0.2716(2) 0.5351(4) 0.3658(5) 0.0405(17) Uani 1 1 d . . . C10 C 0.1521(2) 0.1247(4) 0.3948(5) 0.0459(18) Uani 1 1 d . . . C11 C 0.1143(2) 0.0962(4) 0.4063(6) 0.050(2) Uani 1 1 d . . . C12 C 0.1190(4) 0.0101(5) 0.4063(7) 0.068(3) Uani 1 1 d . . . C13 C 0.1579(3) -0.0040(5) 0.3958(6) 0.052(2) Uani 1 1 d . . . C14 C 0.1772(3) -0.0741(4) 0.3907(6) 0.059(2) Uani 1 1 d . . . H14 H 0.1638 -0.1197 0.3942 0.070 Uiso 1 1 calc R . . C15 C 0.2155(3) -0.0738(4) 0.3809(6) 0.057(2) Uani 1 1 d . . . H15 H 0.2284 -0.1199 0.3773 0.069 Uiso 1 1 calc R . . C16 C 0.2360(3) -0.0074(5) 0.3759(7) 0.060(2) Uani 1 1 d . . . H16 H 0.2623 -0.0097 0.3681 0.072 Uiso 1 1 calc R . . C17 C 0.2188(3) 0.0621(4) 0.3821(6) 0.0480(19) Uani 1 1 d . . . H17 H 0.2330 0.1069 0.3830 0.058 Uiso 1 1 calc R . . C18 C 0.1794(3) 0.0631(4) 0.3870(5) 0.0463(19) Uani 1 1 d . . . C19 C 0.0606(2) 0.4727(5) 0.3630(6) 0.0462(18) Uani 1 1 d . . . C20 C 0.0678(2) 0.5544(5) 0.3588(6) 0.0461(18) Uani 1 1 d . . . C21 C 0.0307(2) 0.5942(5) 0.3688(6) 0.0482(18) Uani 1 1 d . . . C22 C 0.0016(2) 0.5356(5) 0.3743(6) 0.0485(19) Uani 1 1 d . . . C23 C -0.0368(2) 0.5422(5) 0.3805(6) 0.055(2) Uani 1 1 d . . . H23 H -0.0482 0.5899 0.3818 0.066 Uiso 1 1 calc R . . C24 C -0.0592(2) 0.4757(7) 0.3852(7) 0.069(3) Uani 1 1 d . . . H24 H -0.0856 0.4789 0.3903 0.082 Uiso 1 1 calc R . . C25 C -0.0414(3) 0.4059(6) 0.3821(7) 0.066(3) Uani 1 1 d . . . H25 H -0.0564 0.3622 0.3836 0.079 Uiso 1 1 calc R . . C26 C -0.0027(2) 0.3984(5) 0.3770(7) 0.056(2) Uani 1 1 d . . . H26 H 0.0087 0.3506 0.3749 0.068 Uiso 1 1 calc R . . C27 C 0.0188(2) 0.4629(4) 0.3751(6) 0.0441(17) Uani 1 1 d . . . C28 C 0.1745(2) 0.3822(4) 0.1605(6) 0.0477(19) Uani 1 1 d . . . C29 C 0.1723(4) 0.3713(6) 0.0504(8) 0.081(3) Uani 1 1 d . . . H29A H 0.1935 0.3405 0.0314 0.122 Uiso 1 1 calc R . . H29B H 0.1735 0.4199 0.0181 0.122 Uiso 1 1 calc R . . H29C H 0.1487 0.3465 0.0308 0.122 Uiso 1 1 calc R . . C30 C 0.0749(3) 0.2270(5) 0.1920(7) 0.067(3) Uani 1 1 d . . . H30 H 0.0570 0.2172 0.2393 0.081 Uiso 1 1 calc R . . C31 C 0.0907(4) 0.2231(7) 0.0243(8) 0.089(4) Uani 1 1 d D . . H31A H 0.1163 0.2247 0.0534 0.133 Uiso 1 1 calc R . . H31B H 0.0854 0.2694 -0.0116 0.133 Uiso 1 1 calc R . . H31C H 0.0882 0.1807 -0.0205 0.133 Uiso 1 1 calc R . . C32 C 0.0237(5) 0.1871(11) 0.0786(15) 0.162(9) Uani 1 1 d D . . H32A H 0.0115 0.2193 0.0291 0.243 Uiso 1 1 calc R . . H32B H 0.0094 0.1881 0.1378 0.243 Uiso 1 1 calc R . . H32C H 0.0246 0.1359 0.0538 0.243 Uiso 1 1 calc R . . O14 O 0.1259(3) 0.2911(5) 0.5532(6) 0.1052(17) Uani 1 1 d . . . C33 C 0.1085(5) 0.2527(8) 0.6115(10) 0.1052(17) Uani 1 1 d . . . H33 H 0.0902 0.2211 0.5807 0.126 Uiso 1 1 calc R . . N8 N 0.1101(4) 0.2472(6) 0.7027(8) 0.1052(17) Uani 1 1 d D . . C34 C 0.0848(4) 0.1989(7) 0.7551(10) 0.1052(17) Uani 1 1 d D . . H34A H 0.0741 0.1611 0.7104 0.158 Uiso 1 1 calc R . . H34B H 0.0645 0.2289 0.7806 0.158 Uiso 1 1 calc R . . H34C H 0.0988 0.1744 0.8092 0.158 Uiso 1 1 calc R . . C35 C 0.1475(5) 0.2733(7) 0.7495(10) 0.1052(17) Uani 1 1 d . . . H35A H 0.1681 0.2464 0.7203 0.158 Uiso 1 1 calc R . . H35B H 0.1480 0.2633 0.8197 0.158 Uiso 1 1 calc R . . H35C H 0.1504 0.3268 0.7385 0.158 Uiso 1 1 calc R . . N1 N 0.22186(17) 0.4355(3) 0.3745(5) 0.0399(14) Uani 1 1 d . . . N2 N 0.29037(17) 0.3343(3) 0.3682(5) 0.0420(14) Uani 1 1 d . . . N3 N 0.15864(18) 0.1983(3) 0.3876(4) 0.0392(14) Uani 1 1 d . . . N4 N 0.0814(2) 0.1272(4) 0.4146(6) 0.0553(18) Uani 1 1 d . . . N5 N 0.08729(18) 0.4246(3) 0.3624(5) 0.0419(14) Uani 1 1 d . . . N6 N 0.09782(19) 0.5927(4) 0.3440(6) 0.0556(18) Uani 1 1 d . . . N7 N 0.0636(3) 0.2148(5) 0.1024(7) 0.090(3) Uani 1 1 d D . . O1 O 0.15456(14) 0.3507(3) 0.3787(4) 0.0407(11) Uani 1 1 d . . . O2 O 0.19367(15) 0.4877(3) 0.3757(4) 0.0478(13) Uani 1 1 d . . . O3 O 0.25717(15) 0.2943(3) 0.3677(4) 0.0488(13) Uani 1 1 d . . . O4 O 0.35634(15) 0.4286(3) 0.3690(5) 0.0565(14) Uani 1 1 d . . . O5 O 0.19473(14) 0.2190(3) 0.3758(4) 0.0428(12) Uani 1 1 d . . . O6 O 0.07935(16) 0.2024(3) 0.4117(5) 0.0563(15) Uani 1 1 d . . . O7 O 0.0927(2) -0.0348(4) 0.4188(7) 0.084(2) Uani 1 1 d . . . O8 O 0.07662(14) 0.3505(3) 0.3740(4) 0.0514(13) Uani 1 1 d . . . O9 O 0.13015(16) 0.5550(3) 0.3328(5) 0.0599(16) Uani 1 1 d . . . O10 O 0.02568(19) 0.6632(4) 0.3717(6) 0.0754(19) Uani 1 1 d . . . O11 O 0.15219(17) 0.4325(3) 0.1952(4) 0.0560(14) Uani 1 1 d . . . O12 O 0.19834(15) 0.3432(3) 0.2111(4) 0.0487(13) Uani 1 1 d . . . O13 O 0.10616(17) 0.2497(4) 0.2251(4) 0.0591(15) Uani 1 1 d . . . O15 O 0.1389(2) 0.4554(4) 0.5357(6) 0.083(2) Uani 1 1 d . . . H151 H 0.1427 0.4875 0.5815 0.125 Uiso 1 1 d R . . H152 H 0.1279 0.4159 0.5552 0.125 Uiso 1 1 d R . . O16 O 0.20818(17) 0.3291(3) 0.5372(4) 0.0557(15) Uani 1 1 d . . . H161 H 0.2195 0.2919 0.5644 0.084 Uiso 1 1 d R . . H162 H 0.1866 0.3356 0.5610 0.084 Uiso 1 1 d R . . O171 O 0.0214(8) -0.012(2) 0.170(2) 0.089(14) Uani 0.25(2) 1 d PD A 1 H171 H 0.0101 -0.0495 0.1434 0.134 Uiso 0.25(2) 1 d PRD A 1 H172 H 0.0072 0.0104 0.2095 0.134 Uiso 0.25(2) 1 d PRD A 1 O172 O 0.0686(11) 0.015(2) 0.161(3) 0.46(5) Uani 0.75(2) 1 d PD A 2 H173 H 0.0667 0.0342 0.2160 0.695 Uiso 0.75(2) 1 d PRD A 2 H174 H 0.0893 -0.0082 0.1527 0.695 Uiso 0.75(2) 1 d PRD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0469(7) 0.0260(5) 0.0426(7) 0.0012(4) 0.0000(5) -0.0019(5) Mn2 0.0486(7) 0.0306(6) 0.0480(7) 0.0010(4) 0.0013(5) -0.0051(5) Mn3 0.0447(7) 0.0299(6) 0.0663(9) 0.0017(5) 0.0055(5) 0.0012(5) C1 0.052(4) 0.025(3) 0.026(4) 0.002(2) 0.001(3) -0.004(3) C2 0.048(4) 0.031(4) 0.041(4) 0.004(3) 0.005(3) -0.003(3) C3 0.046(4) 0.060(5) 0.034(4) -0.002(3) 0.003(3) -0.019(4) C4 0.061(5) 0.042(4) 0.030(4) 0.001(3) 0.005(3) -0.014(4) C5 0.052(4) 0.044(4) 0.046(5) 0.001(3) 0.009(3) -0.012(4) C6 0.071(5) 0.039(4) 0.051(5) -0.008(3) 0.009(4) -0.018(4) C7 0.073(6) 0.027(4) 0.059(6) 0.004(3) 0.010(4) 0.001(4) C8 0.063(5) 0.025(3) 0.049(5) 0.003(3) 0.015(4) -0.002(3) C9 0.059(5) 0.027(3) 0.035(4) 0.004(3) -0.001(3) -0.003(3) C10 0.067(5) 0.042(4) 0.028(4) 0.002(3) 0.001(3) -0.010(4) C11 0.065(5) 0.037(4) 0.049(5) 0.014(3) 0.000(4) -0.010(4) C12 0.125(9) 0.029(4) 0.050(6) 0.001(3) -0.003(5) -0.027(5) C13 0.071(6) 0.032(4) 0.054(5) 0.001(3) 0.000(4) -0.010(4) C14 0.098(7) 0.027(4) 0.049(5) 0.001(3) -0.009(4) 0.000(4) C15 0.103(8) 0.031(4) 0.038(5) -0.003(3) -0.006(4) 0.006(4) C16 0.079(6) 0.049(5) 0.051(5) -0.001(4) 0.001(4) 0.011(5) C17 0.078(6) 0.030(4) 0.037(4) 0.001(3) 0.005(4) 0.000(4) C18 0.084(6) 0.028(4) 0.027(4) -0.002(3) 0.002(3) -0.008(4) C19 0.050(4) 0.046(4) 0.042(5) 0.000(3) -0.005(3) -0.003(4) C20 0.049(4) 0.041(4) 0.047(5) -0.005(3) -0.009(3) 0.003(4) C21 0.053(4) 0.047(5) 0.044(5) -0.002(3) -0.007(3) 0.006(4) C22 0.048(4) 0.057(5) 0.040(5) -0.011(3) 0.006(3) 0.007(4) C23 0.058(5) 0.065(6) 0.041(5) -0.012(4) -0.010(4) 0.012(4) C24 0.042(4) 0.105(9) 0.059(6) 0.007(5) 0.001(4) -0.012(5) C25 0.056(5) 0.078(7) 0.062(6) -0.007(5) -0.001(4) -0.017(5) C26 0.047(4) 0.061(5) 0.062(6) -0.003(4) 0.003(4) -0.015(4) C27 0.048(4) 0.049(4) 0.035(4) -0.001(3) -0.007(3) -0.009(4) C28 0.050(4) 0.038(4) 0.055(5) 0.005(4) -0.002(4) -0.004(4) C29 0.119(9) 0.074(7) 0.050(6) 0.012(5) -0.003(5) -0.004(6) C30 0.080(6) 0.065(6) 0.055(6) -0.001(4) -0.023(5) -0.024(5) C31 0.119(9) 0.101(9) 0.046(6) -0.015(5) -0.008(6) 0.037(7) C32 0.167(16) 0.155(17) 0.153(18) 0.012(13) -0.094(14) -0.055(13) O14 0.165(5) 0.085(3) 0.069(3) 0.009(2) 0.038(3) 0.006(3) C33 0.165(5) 0.085(3) 0.069(3) 0.009(2) 0.038(3) 0.006(3) N8 0.165(5) 0.085(3) 0.069(3) 0.009(2) 0.038(3) 0.006(3) C34 0.165(5) 0.085(3) 0.069(3) 0.009(2) 0.038(3) 0.006(3) C35 0.165(5) 0.085(3) 0.069(3) 0.009(2) 0.038(3) 0.006(3) N1 0.044(3) 0.035(3) 0.041(4) 0.000(3) 0.000(2) -0.005(3) N2 0.042(3) 0.039(3) 0.046(4) 0.003(3) 0.002(3) 0.000(3) N3 0.060(4) 0.023(3) 0.035(3) -0.007(2) 0.006(3) -0.004(3) N4 0.062(4) 0.040(4) 0.064(5) 0.004(3) 0.002(3) -0.018(3) N5 0.053(4) 0.023(3) 0.049(4) -0.002(2) -0.001(3) 0.000(3) N6 0.044(4) 0.041(4) 0.082(5) -0.002(3) 0.001(3) 0.007(3) N7 0.116(8) 0.062(5) 0.089(8) -0.007(5) -0.049(6) -0.009(5) O1 0.053(3) 0.025(2) 0.044(3) 0.006(2) -0.004(2) -0.006(2) O2 0.052(3) 0.030(3) 0.062(4) -0.001(2) 0.007(2) 0.001(2) O3 0.051(3) 0.031(3) 0.064(4) 0.003(2) -0.001(2) -0.005(2) O4 0.046(3) 0.049(3) 0.075(4) 0.005(3) 0.008(3) -0.004(3) O5 0.046(3) 0.030(3) 0.051(3) -0.004(2) -0.001(2) 0.000(2) O6 0.064(3) 0.038(3) 0.068(4) 0.002(3) 0.013(3) -0.012(3) O7 0.088(5) 0.053(4) 0.111(7) 0.009(4) -0.003(4) -0.017(4) O8 0.047(3) 0.038(3) 0.069(4) 0.001(3) -0.002(2) -0.008(2) O9 0.050(3) 0.035(3) 0.095(5) 0.003(3) 0.010(3) 0.003(3) O10 0.073(4) 0.068(4) 0.084(5) -0.008(4) -0.003(3) 0.013(4) O11 0.070(4) 0.040(3) 0.058(4) 0.011(3) -0.001(3) -0.001(3) O12 0.062(3) 0.040(3) 0.044(3) -0.004(2) 0.012(2) -0.003(3) O13 0.070(4) 0.058(4) 0.048(4) -0.003(3) 0.000(3) 0.000(3) O15 0.097(5) 0.057(4) 0.095(6) -0.014(4) 0.001(4) -0.006(4) O16 0.074(4) 0.045(3) 0.047(4) 0.000(2) -0.005(3) 0.020(3) O171 0.070(19) 0.13(3) 0.07(2) -0.064(19) 0.001(13) 0.000(17) O172 0.43(5) 0.53(6) 0.47(6) 0.35(5) 0.35(5) 0.36(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.875(5) . ? Mn1 O3 1.895(5) . ? Mn1 O5 1.934(5) . ? Mn1 N1 2.035(6) . ? Mn1 O12 2.181(6) . ? Mn1 O16 2.279(6) . ? Mn1 Mn3 3.1646(16) . ? Mn2 O1 1.880(5) . ? Mn2 O6 1.909(5) . ? Mn2 O8 1.943(6) . ? Mn2 N3 2.018(6) . ? Mn2 O13 2.260(6) . ? Mn2 O14 2.289(9) . ? Mn3 O1 1.878(5) . ? Mn3 O9 1.901(6) . ? Mn3 O2 1.926(5) . ? Mn3 N5 2.027(6) . ? Mn3 O11 2.179(6) . ? Mn3 O15 2.531(8) . ? C1 N1 1.273(9) . ? C1 C2 1.462(10) . ? C1 C9 1.488(9) . ? C2 N2 1.272(10) . ? C2 C3 1.502(11) . ? C3 O4 1.226(10) . ? C3 C4 1.479(12) . ? C4 C9 1.381(11) . ? C4 C5 1.416(11) . ? C5 C6 1.355(12) . ? C5 H5 0.9400 . ? C6 C7 1.433(12) . ? C6 H6 0.9400 . ? C7 C8 1.382(11) . ? C7 H7 0.9400 . ? C8 C9 1.410(11) . ? C8 H8 0.9400 . ? C10 N3 1.333(10) . ? C10 C11 1.442(11) . ? C10 C18 1.465(12) . ? C11 N4 1.298(11) . ? C11 C12 1.538(12) . ? C12 O7 1.242(12) . ? C12 C13 1.411(14) . ? C13 C18 1.420(11) . ? C13 C14 1.422(12) . ? C14 C15 1.367(13) . ? C14 H14 0.9400 . ? C15 C16 1.387(13) . ? C15 H15 0.9400 . ? C16 C17 1.381(12) . ? C16 H16 0.9400 . ? C17 C18 1.395(12) . ? C17 H17 0.9400 . ? C19 N5 1.272(10) . ? C19 C20 1.474(11) . ? C19 C27 1.503(11) . ? C20 N6 1.283(11) . ? C20 C21 1.501(11) . ? C21 O10 1.240(11) . ? C21 C22 1.467(12) . ? C22 C23 1.366(11) . ? C22 C27 1.427(11) . ? C23 C24 1.425(14) . ? C23 H23 0.9400 . ? C24 C25 1.391(15) . ? C24 H24 0.9400 . ? C25 C26 1.379(12) . ? C25 H25 0.9400 . ? C26 C27 1.376(12) . ? C26 H26 0.9400 . ? C28 O12 1.268(9) . ? C28 O11 1.296(10) . ? C28 C29 1.508(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 O13 1.238(10) . ? C30 N7 1.284(13) . ? C30 H30 0.9400 . ? C31 N7 1.469(13) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 N7 1.513(13) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? O14 C33 1.232(15) . ? C33 N8 1.243(16) . ? C33 H33 0.9400 . ? N8 C34 1.451(13) . ? N8 C35 1.510(19) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? N1 O2 1.362(8) . ? N2 O3 1.370(8) . ? N3 O5 1.343(8) . ? N4 O6 1.338(9) . ? N5 O8 1.380(8) . ? N6 O9 1.338(9) . ? O15 H151 0.8500 . ? O15 H152 0.8514 . ? O16 H161 0.8491 . ? O16 H162 0.8513 . ? O171 H171 0.8524 . ? O171 H172 0.8527 . ? O172 H173 0.8300 . ? O172 H174 0.8490 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O3 175.6(2) . . ? O1 Mn1 O5 91.8(2) . . ? O3 Mn1 O5 84.9(2) . . ? O1 Mn1 N1 92.0(2) . . ? O3 Mn1 N1 91.0(2) . . ? O5 Mn1 N1 173.9(2) . . ? O1 Mn1 O12 87.6(2) . . ? O3 Mn1 O12 95.8(2) . . ? O5 Mn1 O12 99.8(2) . . ? N1 Mn1 O12 85.1(2) . . ? O1 Mn1 O16 85.2(2) . . ? O3 Mn1 O16 91.9(2) . . ? O5 Mn1 O16 88.9(2) . . ? N1 Mn1 O16 86.7(2) . . ? O12 Mn1 O16 168.9(2) . . ? O1 Mn1 Mn3 32.55(14) . . ? O3 Mn1 Mn3 151.19(16) . . ? O5 Mn1 Mn3 123.54(16) . . ? N1 Mn1 Mn3 61.02(17) . . ? O12 Mn1 Mn3 76.36(15) . . ? O16 Mn1 Mn3 93.10(14) . . ? O1 Mn2 O6 172.9(3) . . ? O1 Mn2 O8 91.9(2) . . ? O6 Mn2 O8 88.2(2) . . ? O1 Mn2 N3 88.2(2) . . ? O6 Mn2 N3 92.3(2) . . ? O8 Mn2 N3 175.4(2) . . ? O1 Mn2 O13 100.3(2) . . ? O6 Mn2 O13 86.8(3) . . ? O8 Mn2 O13 88.1(2) . . ? N3 Mn2 O13 87.4(2) . . ? O1 Mn2 O14 84.9(3) . . ? O6 Mn2 O14 88.0(3) . . ? O8 Mn2 O14 94.3(3) . . ? N3 Mn2 O14 90.3(3) . . ? O13 Mn2 O14 174.3(3) . . ? O1 Mn3 O9 175.4(3) . . ? O1 Mn3 O2 94.8(2) . . ? O9 Mn3 O2 84.9(2) . . ? O1 Mn3 N5 87.9(2) . . ? O9 Mn3 N5 91.2(2) . . ? O2 Mn3 N5 163.9(2) . . ? O1 Mn3 O11 90.4(2) . . ? O9 Mn3 O11 94.3(3) . . ? O2 Mn3 O11 92.3(2) . . ? N5 Mn3 O11 103.6(2) . . ? O1 Mn3 O15 81.0(2) . . ? O9 Mn3 O15 94.4(3) . . ? O2 Mn3 O15 84.6(2) . . ? N5 Mn3 O15 80.2(3) . . ? O11 Mn3 O15 170.5(2) . . ? O1 Mn3 Mn1 32.50(15) . . ? O9 Mn3 Mn1 148.59(18) . . ? O2 Mn3 Mn1 64.67(15) . . ? N5 Mn3 Mn1 120.23(17) . . ? O11 Mn3 Mn1 80.14(16) . . ? O15 Mn3 Mn1 90.38(17) . . ? N1 C1 C2 123.5(6) . . ? N1 C1 C9 129.4(7) . . ? C2 C1 C9 107.1(6) . . ? N2 C2 C1 132.0(7) . . ? N2 C2 C3 120.5(7) . . ? C1 C2 C3 107.5(6) . . ? O4 C3 C4 128.6(7) . . ? O4 C3 C2 125.9(8) . . ? C4 C3 C2 105.5(7) . . ? C9 C4 C5 121.2(7) . . ? C9 C4 C3 110.6(6) . . ? C5 C4 C3 128.1(7) . . ? C6 C5 C4 118.3(8) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 121.4(7) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 119.9(7) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 118.6(7) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C4 C9 C8 120.5(7) . . ? C4 C9 C1 109.2(6) . . ? C8 C9 C1 130.4(7) . . ? N3 C10 C11 121.1(7) . . ? N3 C10 C18 127.8(7) . . ? C11 C10 C18 111.0(7) . . ? N4 C11 C10 134.2(7) . . ? N4 C11 C12 121.3(8) . . ? C10 C11 C12 104.5(8) . . ? O7 C12 C13 129.7(9) . . ? O7 C12 C11 123.9(10) . . ? C13 C12 C11 106.3(7) . . ? C12 C13 C18 112.6(8) . . ? C12 C13 C14 129.1(8) . . ? C18 C13 C14 118.3(8) . . ? C15 C14 C13 118.6(8) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 122.0(8) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C17 C16 C15 121.7(9) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 117.2(8) . . ? C16 C17 H17 121.4 . . ? C18 C17 H17 121.4 . . ? C17 C18 C13 122.0(8) . . ? C17 C18 C10 132.2(7) . . ? C13 C18 C10 105.5(7) . . ? N5 C19 C20 122.2(7) . . ? N5 C19 C27 130.7(7) . . ? C20 C19 C27 106.9(7) . . ? N6 C20 C19 132.3(7) . . ? N6 C20 C21 119.6(7) . . ? C19 C20 C21 107.9(7) . . ? O10 C21 C22 126.8(8) . . ? O10 C21 C20 126.5(8) . . ? C22 C21 C20 106.6(7) . . ? C23 C22 C27 120.0(8) . . ? C23 C22 C21 129.9(8) . . ? C27 C22 C21 110.1(7) . . ? C22 C23 C24 119.1(9) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 119.0(8) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C24 122.5(9) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C27 C26 C25 118.0(9) . . ? C27 C26 H26 121.0 . . ? C25 C26 H26 121.0 . . ? C26 C27 C22 121.2(7) . . ? C26 C27 C19 130.2(8) . . ? C22 C27 C19 108.3(6) . . ? O12 C28 O11 125.3(8) . . ? O12 C28 C29 118.0(8) . . ? O11 C28 C29 116.6(8) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O13 C30 N7 129.2(11) . . ? O13 C30 H30 115.4 . . ? N7 C30 H30 115.4 . . ? N7 C31 H31A 109.5 . . ? N7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N7 C32 H32A 109.5 . . ? N7 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N7 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O14 Mn2 121.6(11) . . ? O14 C33 N8 133.2(17) . . ? O14 C33 H33 113.4 . . ? N8 C33 H33 113.4 . . ? C33 N8 C34 122.4(14) . . ? C33 N8 C35 113.2(12) . . ? C34 N8 C35 121.5(12) . . ? N8 C34 H34A 109.5 . . ? N8 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N8 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N8 C35 H35A 109.5 . . ? N8 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N8 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C1 N1 O2 119.2(6) . . ? C1 N1 Mn1 123.6(5) . . ? O2 N1 Mn1 117.0(4) . . ? C2 N2 O3 118.0(6) . . ? C10 N3 O5 116.5(6) . . ? C10 N3 Mn2 123.0(5) . . ? O5 N3 Mn2 120.4(4) . . ? C11 N4 O6 117.9(6) . . ? C19 N5 O8 115.8(6) . . ? C19 N5 Mn3 123.8(5) . . ? O8 N5 Mn3 120.3(4) . . ? C20 N6 O9 117.8(7) . . ? C30 N7 C31 119.0(9) . . ? C30 N7 C32 120.2(12) . . ? C31 N7 C32 120.6(12) . . ? Mn1 O1 Mn3 114.9(2) . . ? Mn1 O1 Mn2 121.4(3) . . ? Mn3 O1 Mn2 122.2(3) . . ? N1 O2 Mn3 116.6(4) . . ? N2 O3 Mn1 131.8(4) . . ? N3 O5 Mn1 118.0(4) . . ? N4 O6 Mn2 130.9(5) . . ? N5 O8 Mn2 117.0(4) . . ? N6 O9 Mn3 131.6(5) . . ? C28 O11 Mn3 125.8(5) . . ? C28 O12 Mn1 131.5(5) . . ? C30 O13 Mn2 121.8(6) . . ? Mn3 O15 H151 137.2 . . ? Mn3 O15 H152 109.6 . . ? H151 O15 H152 112.5 . . ? Mn1 O16 H161 114.1 . . ? Mn1 O16 H162 113.2 . . ? H161 O16 H162 110.6 . . ? H171 O171 H172 110.6 . . ? H173 O172 H174 115.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn1 Mn3 O1 -175.6(5) . . . . ? O5 Mn1 Mn3 O1 14.7(3) . . . . ? N1 Mn1 Mn3 O1 -160.5(4) . . . . ? O12 Mn1 Mn3 O1 107.5(3) . . . . ? O16 Mn1 Mn3 O1 -76.0(3) . . . . ? O1 Mn1 Mn3 O9 171.5(5) . . . . ? O3 Mn1 Mn3 O9 -4.1(6) . . . . ? O5 Mn1 Mn3 O9 -173.8(5) . . . . ? N1 Mn1 Mn3 O9 10.9(5) . . . . ? O12 Mn1 Mn3 O9 -81.0(4) . . . . ? O16 Mn1 Mn3 O9 95.5(4) . . . . ? O1 Mn1 Mn3 O2 156.2(4) . . . . ? O3 Mn1 Mn3 O2 -19.4(4) . . . . ? O5 Mn1 Mn3 O2 170.9(3) . . . . ? N1 Mn1 Mn3 O2 -4.4(3) . . . . ? O12 Mn1 Mn3 O2 -96.3(2) . . . . ? O16 Mn1 Mn3 O2 80.1(2) . . . . ? O1 Mn1 Mn3 N5 -6.5(3) . . . . ? O3 Mn1 Mn3 N5 177.9(4) . . . . ? O5 Mn1 Mn3 N5 8.2(3) . . . . ? N1 Mn1 Mn3 N5 -167.0(3) . . . . ? O12 Mn1 Mn3 N5 101.0(3) . . . . ? O16 Mn1 Mn3 N5 -82.5(3) . . . . ? O1 Mn1 Mn3 O11 -106.6(3) . . . . ? O3 Mn1 Mn3 O11 77.9(4) . . . . ? O5 Mn1 Mn3 O11 -91.8(2) . . . . ? N1 Mn1 Mn3 O11 92.9(3) . . . . ? O12 Mn1 Mn3 O11 0.9(2) . . . . ? O16 Mn1 Mn3 O11 177.4(2) . . . . ? O1 Mn1 Mn3 O15 72.4(3) . . . . ? O3 Mn1 Mn3 O15 -103.2(4) . . . . ? O5 Mn1 Mn3 O15 87.1(3) . . . . ? N1 Mn1 Mn3 O15 -88.2(3) . . . . ? O12 Mn1 Mn3 O15 179.9(2) . . . . ? O16 Mn1 Mn3 O15 -3.7(2) . . . . ? N1 C1 C2 N2 1.6(13) . . . . ? C9 C1 C2 N2 -178.3(8) . . . . ? N1 C1 C2 C3 -177.5(6) . . . . ? C9 C1 C2 C3 2.6(8) . . . . ? N2 C2 C3 O4 -1.7(12) . . . . ? C1 C2 C3 O4 177.5(7) . . . . ? N2 C2 C3 C4 178.1(7) . . . . ? C1 C2 C3 C4 -2.7(8) . . . . ? O4 C3 C4 C9 -178.4(8) . . . . ? C2 C3 C4 C9 1.8(8) . . . . ? O4 C3 C4 C5 3.8(14) . . . . ? C2 C3 C4 C5 -176.0(7) . . . . ? C9 C4 C5 C6 -1.1(12) . . . . ? C3 C4 C5 C6 176.5(8) . . . . ? C4 C5 C6 C7 0.0(12) . . . . ? C5 C6 C7 C8 3.0(13) . . . . ? C6 C7 C8 C9 -4.8(12) . . . . ? C5 C4 C9 C8 -0.7(11) . . . . ? C3 C4 C9 C8 -178.8(7) . . . . ? C5 C4 C9 C1 177.7(7) . . . . ? C3 C4 C9 C1 -0.3(8) . . . . ? C7 C8 C9 C4 3.7(12) . . . . ? C7 C8 C9 C1 -174.4(7) . . . . ? N1 C1 C9 C4 178.6(7) . . . . ? C2 C1 C9 C4 -1.5(8) . . . . ? N1 C1 C9 C8 -3.1(13) . . . . ? C2 C1 C9 C8 176.8(8) . . . . ? N3 C10 C11 N4 -2.1(14) . . . . ? C18 C10 C11 N4 -178.9(9) . . . . ? N3 C10 C11 C12 177.2(7) . . . . ? C18 C10 C11 C12 0.5(8) . . . . ? N4 C11 C12 O7 -3.7(14) . . . . ? C10 C11 C12 O7 176.9(9) . . . . ? N4 C11 C12 C13 179.8(8) . . . . ? C10 C11 C12 C13 0.4(9) . . . . ? O7 C12 C13 C18 -177.4(10) . . . . ? C11 C12 C13 C18 -1.1(10) . . . . ? O7 C12 C13 C14 4.3(17) . . . . ? C11 C12 C13 C14 -179.5(8) . . . . ? C12 C13 C14 C15 -179.7(9) . . . . ? C18 C13 C14 C15 2.0(12) . . . . ? C13 C14 C15 C16 0.2(13) . . . . ? C14 C15 C16 C17 0.9(13) . . . . ? C15 C16 C17 C18 -4.2(12) . . . . ? C16 C17 C18 C13 6.5(11) . . . . ? C16 C17 C18 C10 179.4(8) . . . . ? C12 C13 C18 C17 175.9(7) . . . . ? C14 C13 C18 C17 -5.5(12) . . . . ? C12 C13 C18 C10 1.4(9) . . . . ? C14 C13 C18 C10 179.9(7) . . . . ? N3 C10 C18 C17 8.7(13) . . . . ? C11 C10 C18 C17 -174.8(8) . . . . ? N3 C10 C18 C13 -177.6(7) . . . . ? C11 C10 C18 C13 -1.1(8) . . . . ? N5 C19 C20 N6 8.4(14) . . . . ? C27 C19 C20 N6 -175.7(9) . . . . ? N5 C19 C20 C21 -175.6(7) . . . . ? C27 C19 C20 C21 0.3(8) . . . . ? N6 C20 C21 O10 -5.8(13) . . . . ? C19 C20 C21 O10 177.6(8) . . . . ? N6 C20 C21 C22 174.0(8) . . . . ? C19 C20 C21 C22 -2.5(9) . . . . ? O10 C21 C22 C23 2.2(15) . . . . ? C20 C21 C22 C23 -177.7(8) . . . . ? O10 C21 C22 C27 -176.2(8) . . . . ? C20 C21 C22 C27 4.0(9) . . . . ? C27 C22 C23 C24 -1.7(12) . . . . ? C21 C22 C23 C24 -179.9(8) . . . . ? C22 C23 C24 C25 -0.7(13) . . . . ? C23 C24 C25 C26 1.6(15) . . . . ? C24 C25 C26 C27 0.1(14) . . . . ? C25 C26 C27 C22 -2.6(13) . . . . ? C25 C26 C27 C19 -175.4(8) . . . . ? C23 C22 C27 C26 3.4(12) . . . . ? C21 C22 C27 C26 -178.1(7) . . . . ? C23 C22 C27 C19 177.6(7) . . . . ? C21 C22 C27 C19 -3.9(9) . . . . ? N5 C19 C27 C26 -8.9(15) . . . . ? C20 C19 C27 C26 175.7(8) . . . . ? N5 C19 C27 C22 177.6(8) . . . . ? C20 C19 C27 C22 2.2(8) . . . . ? O1 Mn2 O14 C33 -178.0(11) . . . . ? O6 Mn2 O14 C33 2.4(11) . . . . ? O8 Mn2 O14 C33 90.5(11) . . . . ? N3 Mn2 O14 C33 -89.9(11) . . . . ? Mn2 O14 C33 N8 174.8(13) . . . . ? O14 C33 N8 C34 177.3(15) . . . . ? O14 C33 N8 C35 -22(2) . . . . ? C2 C1 N1 O2 -179.9(6) . . . . ? C9 C1 N1 O2 0.0(11) . . . . ? C2 C1 N1 Mn1 -4.7(9) . . . . ? C9 C1 N1 Mn1 175.3(6) . . . . ? O1 Mn1 N1 C1 -179.4(6) . . . . ? O3 Mn1 N1 C1 3.8(6) . . . . ? O12 Mn1 N1 C1 -91.9(6) . . . . ? O16 Mn1 N1 C1 95.6(6) . . . . ? Mn3 Mn1 N1 C1 -169.0(6) . . . . ? O1 Mn1 N1 O2 -4.0(5) . . . . ? O3 Mn1 N1 O2 179.1(5) . . . . ? O12 Mn1 N1 O2 83.4(5) . . . . ? O16 Mn1 N1 O2 -89.1(5) . . . . ? Mn3 Mn1 N1 O2 6.3(4) . . . . ? C1 C2 N2 O3 1.8(12) . . . . ? C3 C2 N2 O3 -179.2(6) . . . . ? C11 C10 N3 O5 -179.1(6) . . . . ? C18 C10 N3 O5 -2.9(11) . . . . ? C11 C10 N3 Mn2 -2.5(10) . . . . ? C18 C10 N3 Mn2 173.7(6) . . . . ? O1 Mn2 N3 C10 178.6(6) . . . . ? O6 Mn2 N3 C10 5.6(6) . . . . ? O13 Mn2 N3 C10 -81.1(6) . . . . ? O14 Mn2 N3 C10 93.7(6) . . . . ? O1 Mn2 N3 O5 -5.0(5) . . . . ? O6 Mn2 N3 O5 -177.9(5) . . . . ? O13 Mn2 N3 O5 95.4(5) . . . . ? O14 Mn2 N3 O5 -89.8(5) . . . . ? C10 C11 N4 O6 0.8(14) . . . . ? C12 C11 N4 O6 -178.4(7) . . . . ? C20 C19 N5 O8 175.4(7) . . . . ? C27 C19 N5 O8 0.6(12) . . . . ? C20 C19 N5 Mn3 -2.5(11) . . . . ? C27 C19 N5 Mn3 -177.3(6) . . . . ? O1 Mn3 N5 C19 171.0(7) . . . . ? O9 Mn3 N5 C19 -4.4(7) . . . . ? O2 Mn3 N5 C19 71.0(11) . . . . ? O11 Mn3 N5 C19 -99.1(6) . . . . ? O15 Mn3 N5 C19 89.8(7) . . . . ? Mn1 Mn3 N5 C19 174.5(6) . . . . ? O1 Mn3 N5 O8 -6.8(5) . . . . ? O9 Mn3 N5 O8 177.7(5) . . . . ? O2 Mn3 N5 O8 -106.8(9) . . . . ? O11 Mn3 N5 O8 83.1(5) . . . . ? O15 Mn3 N5 O8 -88.0(5) . . . . ? Mn1 Mn3 N5 O8 -3.3(6) . . . . ? C19 C20 N6 O9 -2.6(14) . . . . ? C21 C20 N6 O9 -178.2(7) . . . . ? O13 C30 N7 C31 4.6(17) . . . . ? O13 C30 N7 C32 -179.7(13) . . . . ? O5 Mn1 O1 Mn3 -167.8(3) . . . . ? N1 Mn1 O1 Mn3 16.9(3) . . . . ? O12 Mn1 O1 Mn3 -68.1(3) . . . . ? O16 Mn1 O1 Mn3 103.5(3) . . . . ? O5 Mn1 O1 Mn2 -1.2(3) . . . . ? N1 Mn1 O1 Mn2 -176.5(3) . . . . ? O12 Mn1 O1 Mn2 98.5(3) . . . . ? O16 Mn1 O1 Mn2 -89.9(3) . . . . ? Mn3 Mn1 O1 Mn2 166.6(5) . . . . ? O2 Mn3 O1 Mn1 -21.5(3) . . . . ? N5 Mn3 O1 Mn1 174.4(3) . . . . ? O11 Mn3 O1 Mn1 70.8(3) . . . . ? O15 Mn3 O1 Mn1 -105.2(3) . . . . ? O2 Mn3 O1 Mn2 172.0(3) . . . . ? N5 Mn3 O1 Mn2 7.9(3) . . . . ? O11 Mn3 O1 Mn2 -95.7(3) . . . . ? O15 Mn3 O1 Mn2 88.3(3) . . . . ? Mn1 Mn3 O1 Mn2 -166.5(5) . . . . ? O8 Mn2 O1 Mn1 -172.4(3) . . . . ? N3 Mn2 O1 Mn1 3.0(3) . . . . ? O13 Mn2 O1 Mn1 -84.0(3) . . . . ? O14 Mn2 O1 Mn1 93.5(4) . . . . ? O8 Mn2 O1 Mn3 -6.8(3) . . . . ? N3 Mn2 O1 Mn3 168.6(3) . . . . ? O13 Mn2 O1 Mn3 81.6(3) . . . . ? O14 Mn2 O1 Mn3 -100.9(4) . . . . ? C1 N1 O2 Mn3 165.4(5) . . . . ? Mn1 N1 O2 Mn3 -10.2(6) . . . . ? O1 Mn3 O2 N1 19.0(5) . . . . ? O9 Mn3 O2 N1 -165.6(5) . . . . ? N5 Mn3 O2 N1 118.1(8) . . . . ? O11 Mn3 O2 N1 -71.6(5) . . . . ? O15 Mn3 O2 N1 99.4(5) . . . . ? Mn1 Mn3 O2 N1 6.4(4) . . . . ? C2 N2 O3 Mn1 -1.5(10) . . . . ? O5 Mn1 O3 N2 -176.3(6) . . . . ? N1 Mn1 O3 N2 -0.8(6) . . . . ? O12 Mn1 O3 N2 84.4(6) . . . . ? O16 Mn1 O3 N2 -87.5(6) . . . . ? Mn3 Mn1 O3 N2 12.3(9) . . . . ? C10 N3 O5 Mn1 -178.0(5) . . . . ? Mn2 N3 O5 Mn1 5.3(6) . . . . ? O1 Mn1 O5 N3 -2.6(5) . . . . ? O3 Mn1 O5 N3 174.5(5) . . . . ? O12 Mn1 O5 N3 -90.5(5) . . . . ? O16 Mn1 O5 N3 82.6(5) . . . . ? Mn3 Mn1 O5 N3 -10.4(5) . . . . ? C11 N4 O6 Mn2 5.6(11) . . . . ? O8 Mn2 O6 N4 167.8(7) . . . . ? N3 Mn2 O6 N4 -7.6(7) . . . . ? O13 Mn2 O6 N4 79.7(7) . . . . ? O14 Mn2 O6 N4 -97.8(7) . . . . ? C19 N5 O8 Mn2 -174.1(5) . . . . ? Mn3 N5 O8 Mn2 3.9(7) . . . . ? O1 Mn2 O8 N5 1.4(5) . . . . ? O6 Mn2 O8 N5 174.3(5) . . . . ? O13 Mn2 O8 N5 -98.9(5) . . . . ? O14 Mn2 O8 N5 86.4(5) . . . . ? C20 N6 O9 Mn3 -8.9(12) . . . . ? O2 Mn3 O9 N6 -153.5(8) . . . . ? N5 Mn3 O9 N6 10.9(8) . . . . ? O11 Mn3 O9 N6 114.6(8) . . . . ? O15 Mn3 O9 N6 -69.4(8) . . . . ? Mn1 Mn3 O9 N6 -167.4(5) . . . . ? O12 C28 O11 Mn3 -10.6(11) . . . . ? C29 C28 O11 Mn3 171.2(6) . . . . ? O1 Mn3 O11 C28 -27.1(6) . . . . ? O9 Mn3 O11 C28 152.8(6) . . . . ? O2 Mn3 O11 C28 67.7(6) . . . . ? N5 Mn3 O11 C28 -115.0(6) . . . . ? Mn1 Mn3 O11 C28 3.9(6) . . . . ? O11 C28 O12 Mn1 12.9(11) . . . . ? C29 C28 O12 Mn1 -168.8(6) . . . . ? O1 Mn1 O12 C28 23.8(6) . . . . ? O3 Mn1 O12 C28 -158.9(6) . . . . ? O5 Mn1 O12 C28 115.3(6) . . . . ? N1 Mn1 O12 C28 -68.4(7) . . . . ? O16 Mn1 O12 C28 -25.6(15) . . . . ? Mn3 Mn1 O12 C28 -7.1(6) . . . . ? N7 C30 O13 Mn2 174.4(9) . . . . ? O1 Mn2 O13 C30 -151.3(7) . . . . ? O6 Mn2 O13 C30 28.6(7) . . . . ? O8 Mn2 O13 C30 -59.7(7) . . . . ? N3 Mn2 O13 C30 121.1(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15 H151 O11 0.85 2.12 2.966(9) 179.9 6_566 O15 H152 O14 0.85 2.22 2.968(12) 146.5 . O16 H161 O3 0.85 1.95 2.797(7) 176.4 7_556 O16 H161 N2 0.85 2.45 3.174(8) 143.4 7_556 O16 H162 O14 0.85 2.28 2.999(12) 142.4 . O171 H172 O171 0.85 2.01 2.72(6) 139.9 2 O172 H174 O4 0.85 2.26 3.10(2) 179.2 4_545 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.243 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.132 #===END data_Compound 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H35 Mn3 N8 O16, H2 O' _chemical_formula_sum 'C36 H37 Mn3 N8 O17' _chemical_formula_weight 1018.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3831(10) _cell_length_b 17.8693(11) _cell_length_c 13.7435(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.6490(10) _cell_angle_gamma 90.00 _cell_volume 4003.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9189 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6296 _exptl_absorpt_correction_T_max 0.8221 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22036 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 26.06 _reflns_number_total 7909 _reflns_number_gt 6000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+2.1268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7909 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.25447(3) 0.88494(3) 0.14683(4) 0.02287(14) Uani 1 1 d . . . Mn2 Mn 0.30088(3) 1.05510(3) 0.21793(4) 0.02450(14) Uani 1 1 d . . . Mn3 Mn 0.11592(3) 1.01481(3) 0.14439(4) 0.01932(13) Uani 1 1 d . . . C1 C 0.1080(2) 0.79167(17) 0.1134(2) 0.0214(7) Uani 1 1 d . . . C2 C 0.1626(2) 0.72672(18) 0.1287(2) 0.0244(7) Uani 1 1 d . . . C3 C 0.1093(2) 0.65894(18) 0.1339(3) 0.0276(8) Uani 1 1 d . . . C4 C 0.0243(2) 0.68641(19) 0.1099(2) 0.0259(7) Uani 1 1 d . . . C5 C -0.0478(2) 0.6445(2) 0.1012(3) 0.0327(9) Uani 1 1 d . . . H5 H -0.0469 0.5928 0.1095 0.039 Uiso 1 1 calc R . . C6 C -0.1204(2) 0.6825(2) 0.0797(3) 0.0343(9) Uani 1 1 d . . . H6 H -0.1695 0.6560 0.0735 0.041 Uiso 1 1 calc R . . C7 C -0.1218(2) 0.7594(2) 0.0673(3) 0.0316(8) Uani 1 1 d . . . H7 H -0.1718 0.7834 0.0521 0.038 Uiso 1 1 calc R . . C8 C -0.0505(2) 0.80166(19) 0.0768(2) 0.0245(7) Uani 1 1 d . . . H8 H -0.0521 0.8534 0.0690 0.029 Uiso 1 1 calc R . . C9 C 0.0237(2) 0.76408(18) 0.0985(2) 0.0229(7) Uani 1 1 d . . . C10 C 0.4481(2) 0.9736(2) 0.3006(3) 0.0271(8) Uani 1 1 d . . . C11 C 0.4739(2) 1.0441(2) 0.3497(3) 0.0283(8) Uani 1 1 d . . . C12 C 0.5514(2) 1.0291(2) 0.4122(3) 0.0342(9) Uani 1 1 d . . . C13 C 0.5693(2) 0.9493(2) 0.3997(3) 0.0321(8) Uani 1 1 d . . . C14 C 0.6326(2) 0.9064(3) 0.4459(3) 0.0404(10) Uani 1 1 d . . . H14 H 0.6718 0.9278 0.4909 0.048 Uiso 1 1 calc R . . C15 C 0.6356(2) 0.8315(3) 0.4232(3) 0.0434(10) Uani 1 1 d . . . H15 H 0.6775 0.8020 0.4535 0.052 Uiso 1 1 calc R . . C16 C 0.5776(3) 0.7990(2) 0.3561(3) 0.0465(11) Uani 1 1 d . . . H16 H 0.5817 0.7484 0.3414 0.056 Uiso 1 1 calc R . . C17 C 0.5133(2) 0.8407(2) 0.3103(3) 0.0374(9) Uani 1 1 d . . . H17 H 0.4740 0.8186 0.2660 0.045 Uiso 1 1 calc R . . C18 C 0.5093(2) 0.9161(2) 0.3325(3) 0.0291(8) Uani 1 1 d . . . C19 C 0.0961(2) 1.17774(17) 0.1635(2) 0.0206(7) Uani 1 1 d . . . C20 C 0.0067(2) 1.16541(17) 0.1478(2) 0.0219(7) Uani 1 1 d . . . C21 C -0.0335(2) 1.24051(18) 0.1542(2) 0.0249(7) Uani 1 1 d . . . C22 C 0.0338(2) 1.29524(18) 0.1709(2) 0.0262(8) Uani 1 1 d . . . C23 C 0.0283(3) 1.37226(19) 0.1821(3) 0.0333(9) Uani 1 1 d . . . H23 H -0.0224 1.3960 0.1794 0.040 Uiso 1 1 calc R . . C24 C 0.1005(3) 1.4126(2) 0.1973(3) 0.0398(10) Uani 1 1 d . . . H24 H 0.0986 1.4642 0.2047 0.048 Uiso 1 1 calc R . . C25 C 0.1756(3) 1.3764(2) 0.2017(3) 0.0412(10) Uani 1 1 d . . . H25 H 0.2234 1.4048 0.2110 0.049 Uiso 1 1 calc R . . C26 C 0.1821(2) 1.29901(18) 0.1925(3) 0.0298(8) Uani 1 1 d . . . H26 H 0.2329 1.2754 0.1964 0.036 Uiso 1 1 calc R . . C27 C 0.1100(2) 1.25875(17) 0.1774(2) 0.0227(7) Uani 1 1 d . . . C28 C 0.1797(2) 1.00333(18) 0.3630(3) 0.0264(8) Uani 1 1 d . . . C29 C 0.1689(3) 0.9731(2) 0.4632(3) 0.0403(10) Uani 1 1 d . . . H29A H 0.2202 0.9532 0.4920 0.060 Uiso 1 1 calc R . . H29B H 0.1283 0.9342 0.4579 0.060 Uiso 1 1 calc R . . H29C H 0.1515 1.0127 0.5036 0.060 Uiso 1 1 calc R . . C30 C 0.3470(3) 1.1149(3) 0.0231(4) 0.0655(15) Uani 1 1 d . . . H30 H 0.2958 1.1370 0.0249 0.079 Uiso 1 1 calc R . . C31 C 0.3586(4) 1.1830(5) -0.1257(6) 0.116(3) Uani 1 1 d . . . H31A H 0.3056 1.2006 -0.1116 0.174 Uiso 1 1 calc R . . H31B H 0.3536 1.1578 -0.1877 0.174 Uiso 1 1 calc R . . H31C H 0.3953 1.2247 -0.1281 0.174 Uiso 1 1 calc R . . C32 C 0.4630(4) 1.0922(4) -0.0631(5) 0.097(2) Uani 1 1 d . . . H32A H 0.4742 1.0593 -0.0082 0.146 Uiso 1 1 calc R . . H32B H 0.5079 1.1264 -0.0659 0.146 Uiso 1 1 calc R . . H32C H 0.4562 1.0634 -0.1223 0.146 Uiso 1 1 calc R . . C33 C 0.3201(3) 0.8783(2) -0.0515(3) 0.0438(10) Uani 1 1 d . . . H33 H 0.3515 0.8416 -0.0176 0.053 Uiso 1 1 calc R . . C34 C 0.2919(4) 0.9483(4) -0.1980(4) 0.088(2) Uani 1 1 d . . . H34A H 0.2678 0.9256 -0.2573 0.133 Uiso 1 1 calc R . . H34B H 0.3274 0.9884 -0.2136 0.133 Uiso 1 1 calc R . . H34C H 0.2493 0.9678 -0.1619 0.133 Uiso 1 1 calc R . . C35 C 0.4053(4) 0.8569(4) -0.1827(5) 0.087(2) Uani 1 1 d . . . H35A H 0.4301 0.8214 -0.1365 0.131 Uiso 1 1 calc R . . H35B H 0.4454 0.8933 -0.1974 0.131 Uiso 1 1 calc R . . H35C H 0.3848 0.8314 -0.2416 0.131 Uiso 1 1 calc R . . C36 C 0.2915(3) 0.8236(3) 0.3753(3) 0.0482(11) Uani 1 1 d . . . H36A H 0.3221 0.7850 0.3464 0.072 Uiso 1 1 calc R . . H36B H 0.2659 0.8032 0.4293 0.072 Uiso 1 1 calc R . . H36C H 0.3278 0.8634 0.3980 0.072 Uiso 1 1 calc R . . N1 N 0.13473(17) 0.86003(14) 0.1187(2) 0.0216(6) Uani 1 1 d . . . N2 N 0.24138(18) 0.72059(15) 0.1361(2) 0.0286(7) Uani 1 1 d . . . N3 N 0.38159(17) 0.96927(15) 0.2422(2) 0.0258(6) Uani 1 1 d . . . N4 N 0.44416(18) 1.11103(17) 0.3428(2) 0.0306(7) Uani 1 1 d . . . N5 N 0.14813(16) 1.12321(14) 0.1649(2) 0.0212(6) Uani 1 1 d . . . N6 N -0.03674(17) 1.10649(15) 0.1305(2) 0.0246(6) Uani 1 1 d . . . N7 N 0.3895(4) 1.1334(3) -0.0526(3) 0.0854(17) Uani 1 1 d . . . N8 N 0.3375(2) 0.8945(2) -0.1410(3) 0.0501(10) Uani 1 1 d . . . O1 O 0.22740(13) 0.98657(12) 0.15260(16) 0.0224(5) Uani 1 1 d . . . O2 O 0.07814(14) 0.91505(12) 0.10853(17) 0.0241(5) Uani 1 1 d . . . O3 O 0.28606(14) 0.78331(12) 0.13040(19) 0.0291(6) Uani 1 1 d . . . O4 O 0.13122(17) 0.59567(13) 0.1542(2) 0.0368(6) Uani 1 1 d . . . O5 O 0.36665(14) 0.90287(12) 0.19593(19) 0.0288(6) Uani 1 1 d . . . O6 O 0.37560(15) 1.12407(13) 0.28481(19) 0.0330(6) Uani 1 1 d . . . O7 O 0.59133(18) 1.07416(17) 0.4631(2) 0.0504(8) Uani 1 1 d . . . O8 O 0.22868(14) 1.14047(12) 0.18055(18) 0.0268(5) Uani 1 1 d . . . O9 O 0.00273(14) 1.04034(12) 0.12496(17) 0.0251(5) Uani 1 1 d . . . O10 O -0.10708(16) 1.25254(14) 0.1480(2) 0.0367(6) Uani 1 1 d . . . O11 O 0.11918(14) 0.99775(12) 0.29869(17) 0.0256(5) Uani 1 1 d . . . O12 O 0.24724(15) 1.03365(13) 0.35097(17) 0.0287(6) Uani 1 1 d . . . O13 O 0.36814(19) 1.07402(18) 0.0862(2) 0.0518(8) Uani 1 1 d . . . O14 O 0.26681(17) 0.90733(15) -0.0105(2) 0.0371(6) Uani 1 1 d . . . O15 O 0.13404(16) 1.02936(13) -0.02260(18) 0.0319(6) Uani 1 1 d . . . H152 H 0.1754 1.0040 -0.0364 0.048 Uiso 1 1 d R . . H151 H 0.0904 1.0144 -0.0549 0.048 Uiso 1 1 d R . . O16 O 0.22973(15) 0.85204(13) 0.30372(18) 0.0289(5) Uani 1 1 d . . . H161 H 0.1855 0.8311 0.3157 0.043 Uiso 1 1 d R . . O17 O 0.4434(2) 0.74513(18) 0.0703(3) 0.0717(11) Uani 1 1 d . . . H172 H 0.4570 0.6991 0.0742 0.108 Uiso 1 1 d R . . H171 H 0.3943 0.7523 0.0824 0.108 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0204(3) 0.0172(3) 0.0302(3) -0.0035(2) -0.0014(2) 0.0002(2) Mn2 0.0199(3) 0.0187(3) 0.0340(3) -0.0040(2) -0.0013(2) -0.0024(2) Mn3 0.0187(3) 0.0146(2) 0.0242(3) -0.00112(19) -0.00042(19) -0.00130(19) C1 0.0289(18) 0.0178(16) 0.0171(16) -0.0012(12) 0.0007(13) -0.0020(13) C2 0.030(2) 0.0187(16) 0.0239(18) -0.0029(13) 0.0006(14) -0.0005(14) C3 0.043(2) 0.0162(16) 0.0237(18) -0.0030(13) 0.0052(15) -0.0034(15) C4 0.037(2) 0.0229(17) 0.0179(17) -0.0032(14) 0.0012(14) -0.0052(15) C5 0.045(2) 0.0267(18) 0.0260(19) 0.0012(15) 0.0031(16) -0.0118(17) C6 0.033(2) 0.037(2) 0.031(2) 0.0038(17) 0.0011(16) -0.0152(17) C7 0.0256(19) 0.042(2) 0.0265(19) 0.0022(16) -0.0017(14) -0.0058(16) C8 0.0279(19) 0.0256(17) 0.0194(17) 0.0002(13) -0.0009(14) -0.0018(14) C9 0.0297(19) 0.0242(17) 0.0147(16) -0.0022(13) 0.0019(13) -0.0062(14) C10 0.0223(18) 0.0299(18) 0.0291(19) -0.0022(15) 0.0026(14) -0.0013(15) C11 0.0245(18) 0.0296(18) 0.0306(19) -0.0039(15) 0.0019(14) -0.0063(15) C12 0.027(2) 0.045(2) 0.030(2) -0.0066(17) -0.0003(15) -0.0056(17) C13 0.0211(18) 0.047(2) 0.028(2) -0.0022(17) 0.0018(14) -0.0014(16) C14 0.022(2) 0.062(3) 0.036(2) -0.003(2) -0.0027(16) -0.0009(19) C15 0.028(2) 0.057(3) 0.044(3) 0.004(2) -0.0013(18) 0.013(2) C16 0.036(2) 0.047(3) 0.054(3) -0.002(2) -0.004(2) 0.014(2) C17 0.030(2) 0.040(2) 0.040(2) -0.0053(18) -0.0072(17) 0.0028(17) C18 0.0240(19) 0.0355(19) 0.0278(19) -0.0020(16) 0.0019(14) -0.0005(15) C19 0.0275(18) 0.0180(15) 0.0166(16) 0.0022(12) 0.0036(13) -0.0018(13) C20 0.0279(18) 0.0197(16) 0.0183(16) 0.0002(13) 0.0034(13) 0.0025(14) C21 0.031(2) 0.0247(17) 0.0191(17) -0.0022(13) 0.0035(14) 0.0070(15) C22 0.036(2) 0.0219(17) 0.0209(17) -0.0001(13) 0.0027(14) 0.0036(15) C23 0.048(2) 0.0214(17) 0.031(2) 0.0036(15) 0.0054(17) 0.0102(16) C24 0.060(3) 0.0146(17) 0.045(2) 0.0000(16) 0.007(2) -0.0002(17) C25 0.048(3) 0.0238(19) 0.053(3) -0.0026(18) 0.009(2) -0.0081(18) C26 0.032(2) 0.0207(17) 0.037(2) -0.0014(15) 0.0055(16) -0.0020(15) C27 0.0325(19) 0.0171(15) 0.0191(17) 0.0008(13) 0.0050(13) -0.0008(14) C28 0.035(2) 0.0203(16) 0.0243(18) -0.0022(14) 0.0025(15) 0.0050(15) C29 0.046(3) 0.045(2) 0.028(2) 0.0034(18) -0.0020(17) -0.005(2) C30 0.062(3) 0.067(3) 0.073(4) -0.001(3) 0.032(3) 0.013(3) C31 0.088(5) 0.164(8) 0.100(6) 0.040(5) 0.029(4) 0.055(5) C32 0.069(4) 0.136(6) 0.089(5) 0.027(4) 0.024(4) -0.005(4) C33 0.055(3) 0.036(2) 0.042(2) 0.0057(19) 0.013(2) 0.003(2) C34 0.109(5) 0.117(5) 0.039(3) 0.012(3) 0.005(3) 0.032(4) C35 0.107(5) 0.084(4) 0.080(4) 0.002(3) 0.057(4) 0.010(4) C36 0.038(2) 0.062(3) 0.043(3) 0.013(2) -0.0060(19) 0.004(2) N1 0.0256(15) 0.0152(13) 0.0238(15) 0.0007(11) 0.0014(11) 0.0011(11) N2 0.0335(18) 0.0184(14) 0.0340(17) -0.0024(12) 0.0041(13) 0.0013(12) N3 0.0209(15) 0.0238(14) 0.0319(17) -0.0041(12) -0.0015(12) -0.0044(12) N4 0.0240(16) 0.0320(17) 0.0358(18) -0.0050(13) 0.0023(13) -0.0070(13) N5 0.0204(14) 0.0192(13) 0.0240(15) 0.0004(11) 0.0024(11) -0.0025(11) N6 0.0245(15) 0.0245(15) 0.0245(15) -0.0022(12) 0.0012(12) 0.0046(12) N7 0.124(5) 0.089(4) 0.051(3) 0.023(3) 0.052(3) 0.042(3) N8 0.065(3) 0.053(2) 0.035(2) 0.0001(17) 0.0182(18) 0.0052(19) O1 0.0200(12) 0.0171(11) 0.0292(13) -0.0020(9) -0.0015(9) 0.0006(9) O2 0.0207(12) 0.0166(11) 0.0337(14) -0.0028(10) -0.0034(10) 0.0017(9) O3 0.0248(13) 0.0202(12) 0.0426(15) -0.0034(11) 0.0042(11) -0.0007(10) O4 0.0474(17) 0.0184(13) 0.0450(17) -0.0001(11) 0.0070(13) -0.0005(11) O5 0.0232(13) 0.0216(12) 0.0400(15) -0.0069(10) -0.0041(11) 0.0010(10) O6 0.0270(14) 0.0241(12) 0.0462(16) -0.0058(11) -0.0049(11) -0.0038(10) O7 0.0414(17) 0.0529(18) 0.0532(19) -0.0172(15) -0.0144(14) -0.0066(15) O8 0.0214(12) 0.0184(11) 0.0403(15) -0.0015(10) 0.0010(10) -0.0030(10) O9 0.0221(12) 0.0175(11) 0.0350(14) -0.0046(10) -0.0008(10) 0.0015(9) O10 0.0286(15) 0.0339(14) 0.0472(17) -0.0070(12) 0.0018(12) 0.0097(11) O11 0.0263(13) 0.0254(12) 0.0249(13) 0.0015(10) 0.0011(10) -0.0013(10) O12 0.0289(14) 0.0283(13) 0.0278(13) -0.0040(10) -0.0019(10) -0.0058(11) O13 0.0495(19) 0.057(2) 0.050(2) 0.0058(16) 0.0127(15) -0.0036(16) O14 0.0422(16) 0.0353(14) 0.0337(15) -0.0029(12) 0.0035(12) 0.0016(13) O15 0.0340(14) 0.0302(13) 0.0305(14) -0.0013(11) -0.0011(11) -0.0036(11) O16 0.0261(13) 0.0281(13) 0.0315(14) 0.0030(11) -0.0020(10) -0.0011(11) O17 0.058(2) 0.0445(19) 0.117(3) 0.0151(19) 0.033(2) 0.0097(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.873(2) . ? Mn1 O3 1.908(2) . ? Mn1 O5 1.921(2) . ? Mn1 N1 2.012(3) . ? Mn1 O14 2.228(3) . ? Mn1 O16 2.309(2) . ? Mn2 O1 1.882(2) . ? Mn2 O6 1.908(2) . ? Mn2 O8 1.967(2) . ? Mn2 N3 2.031(3) . ? Mn2 O12 2.140(3) . ? Mn2 O13 2.236(3) . ? Mn2 Mn3 3.1809(7) . ? Mn3 O1 1.887(2) . ? Mn3 O9 1.903(2) . ? Mn3 O2 1.935(2) . ? Mn3 N5 2.020(3) . ? Mn3 O11 2.138(2) . ? Mn3 O15 2.357(2) . ? C1 N1 1.297(4) . ? C1 C9 1.461(5) . ? C1 C2 1.468(5) . ? C2 N2 1.289(4) . ? C2 C3 1.499(5) . ? C3 O4 1.211(4) . ? C3 C4 1.482(5) . ? C4 C5 1.395(5) . ? C4 C9 1.397(5) . ? C5 C6 1.376(5) . ? C5 H5 0.9300 . ? C6 C7 1.386(5) . ? C6 H6 0.9300 . ? C7 C8 1.386(5) . ? C7 H7 0.9300 . ? C8 C9 1.395(5) . ? C8 H8 0.9300 . ? C10 N3 1.291(4) . ? C10 C18 1.471(5) . ? C10 C11 1.471(5) . ? C11 N4 1.291(5) . ? C11 C12 1.485(5) . ? C12 O7 1.216(4) . ? C12 C13 1.468(6) . ? C13 C14 1.391(5) . ? C13 C18 1.412(5) . ? C14 C15 1.377(6) . ? C14 H14 0.9300 . ? C15 C16 1.385(6) . ? C15 H15 0.9300 . ? C16 C17 1.388(5) . ? C16 H16 0.9300 . ? C17 C18 1.385(5) . ? C17 H17 0.9300 . ? C19 N5 1.293(4) . ? C19 C27 1.475(4) . ? C19 C20 1.476(5) . ? C20 N6 1.279(4) . ? C20 C21 1.501(4) . ? C21 O10 1.219(4) . ? C21 C22 1.474(5) . ? C22 C23 1.389(5) . ? C22 C27 1.403(5) . ? C23 C24 1.383(6) . ? C23 H23 0.9300 . ? C24 C25 1.386(6) . ? C24 H24 0.9300 . ? C25 C26 1.394(5) . ? C25 H25 0.9300 . ? C26 C27 1.382(5) . ? C26 H26 0.9300 . ? C28 O12 1.257(4) . ? C28 O11 1.266(4) . ? C28 C29 1.506(5) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O13 1.159(6) . ? C30 N7 1.349(7) . ? C30 H30 0.9300 . ? C31 N7 1.397(8) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N7 1.430(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O14 1.202(5) . ? C33 N8 1.322(5) . ? C33 H33 0.9300 . ? C34 N8 1.408(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N8 1.461(6) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O16 1.433(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? N1 O2 1.349(3) . ? N2 O3 1.345(4) . ? N3 O5 1.357(3) . ? N4 O6 1.332(4) . ? N5 O8 1.352(3) . ? N6 O9 1.353(3) . ? O15 H152 0.8525 . ? O15 H151 0.8469 . ? O16 H161 0.8459 . ? O17 H172 0.8518 . ? O17 H171 0.8481 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O3 174.93(11) . . ? O1 Mn1 O5 92.62(10) . . ? O3 Mn1 O5 86.51(10) . . ? O1 Mn1 N1 89.56(10) . . ? O3 Mn1 N1 92.14(10) . . ? O5 Mn1 N1 170.21(11) . . ? O1 Mn1 O14 84.92(10) . . ? O3 Mn1 O14 90.25(10) . . ? O5 Mn1 O14 97.81(11) . . ? N1 Mn1 O14 91.89(11) . . ? O1 Mn1 O16 98.24(9) . . ? O3 Mn1 O16 86.72(10) . . ? O5 Mn1 O16 87.95(10) . . ? N1 Mn1 O16 82.29(10) . . ? O14 Mn1 O16 173.33(9) . . ? O1 Mn2 O6 179.61(11) . . ? O1 Mn2 O8 92.30(9) . . ? O6 Mn2 O8 88.03(10) . . ? O1 Mn2 N3 87.85(10) . . ? O6 Mn2 N3 91.84(11) . . ? O8 Mn2 N3 173.40(11) . . ? O1 Mn2 O12 89.65(10) . . ? O6 Mn2 O12 90.11(10) . . ? O8 Mn2 O12 94.31(10) . . ? N3 Mn2 O12 92.29(11) . . ? O1 Mn2 O13 93.16(11) . . ? O6 Mn2 O13 87.05(12) . . ? O8 Mn2 O13 90.16(11) . . ? N3 Mn2 O13 83.24(12) . . ? O12 Mn2 O13 174.63(11) . . ? O1 Mn2 Mn3 32.50(7) . . ? O6 Mn2 Mn3 147.69(8) . . ? O8 Mn2 Mn3 64.10(7) . . ? N3 Mn2 Mn3 117.75(8) . . ? O12 Mn2 Mn3 76.85(6) . . ? O13 Mn2 Mn3 107.87(9) . . ? O1 Mn3 O9 175.14(10) . . ? O1 Mn3 O2 93.00(9) . . ? O9 Mn3 O2 84.39(9) . . ? O1 Mn3 N5 90.58(10) . . ? O9 Mn3 N5 91.56(10) . . ? O2 Mn3 N5 172.57(10) . . ? O1 Mn3 O11 88.45(10) . . ? O9 Mn3 O11 95.87(10) . . ? O2 Mn3 O11 95.59(9) . . ? N5 Mn3 O11 91.02(10) . . ? O1 Mn3 O15 82.76(9) . . ? O9 Mn3 O15 92.94(10) . . ? O2 Mn3 O15 85.50(9) . . ? N5 Mn3 O15 88.50(10) . . ? O11 Mn3 O15 171.19(9) . . ? O1 Mn3 Mn2 32.39(6) . . ? O9 Mn3 Mn2 151.05(7) . . ? O2 Mn3 Mn2 124.08(7) . . ? N5 Mn3 Mn2 60.73(8) . . ? O11 Mn3 Mn2 77.71(6) . . ? O15 Mn3 Mn2 94.42(6) . . ? N1 C1 C9 129.4(3) . . ? N1 C1 C2 122.6(3) . . ? C9 C1 C2 107.9(3) . . ? N2 C2 C1 132.0(3) . . ? N2 C2 C3 120.7(3) . . ? C1 C2 C3 107.2(3) . . ? O4 C3 C4 127.7(3) . . ? O4 C3 C2 127.2(3) . . ? C4 C3 C2 105.1(3) . . ? C5 C4 C9 121.8(3) . . ? C5 C4 C3 127.7(3) . . ? C9 C4 C3 110.5(3) . . ? C6 C5 C4 117.5(3) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? C5 C6 C7 121.2(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 121.7(4) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 117.8(3) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? C8 C9 C4 119.9(3) . . ? C8 C9 C1 131.2(3) . . ? C4 C9 C1 108.9(3) . . ? N3 C10 C18 130.7(3) . . ? N3 C10 C11 121.5(3) . . ? C18 C10 C11 107.7(3) . . ? N4 C11 C10 132.1(3) . . ? N4 C11 C12 120.3(3) . . ? C10 C11 C12 107.5(3) . . ? O7 C12 C13 127.5(4) . . ? O7 C12 C11 126.4(4) . . ? C13 C12 C11 106.1(3) . . ? C14 C13 C18 120.5(4) . . ? C14 C13 C12 129.0(4) . . ? C18 C13 C12 110.5(3) . . ? C15 C14 C13 118.3(4) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 121.3(4) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C17 121.1(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 118.2(4) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 C10 131.3(3) . . ? C13 C18 C10 108.2(3) . . ? N5 C19 C27 130.1(3) . . ? N5 C19 C20 122.2(3) . . ? C27 C19 C20 107.7(3) . . ? N6 C20 C19 132.5(3) . . ? N6 C20 C21 120.5(3) . . ? C19 C20 C21 107.0(3) . . ? O10 C21 C22 127.8(3) . . ? O10 C21 C20 126.1(3) . . ? C22 C21 C20 106.1(3) . . ? C23 C22 C27 121.3(3) . . ? C23 C22 C21 128.3(3) . . ? C27 C22 C21 110.4(3) . . ? C24 C23 C22 118.0(4) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 122.2(4) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C27 C26 C25 117.3(4) . . ? C27 C26 H26 121.4 . . ? C25 C26 H26 121.4 . . ? C26 C27 C22 120.7(3) . . ? C26 C27 C19 130.5(3) . . ? C22 C27 C19 108.9(3) . . ? O12 C28 O11 125.5(3) . . ? O12 C28 C29 117.3(3) . . ? O11 C28 C29 117.2(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O13 C30 N7 126.3(5) . . ? O13 C30 H30 116.8 . . ? N7 C30 H30 116.8 . . ? N7 C31 H31A 109.5 . . ? N7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N7 C32 H32A 109.5 . . ? N7 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N7 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O14 C33 N8 125.1(4) . . ? O14 C33 H33 117.4 . . ? N8 C33 H33 117.4 . . ? N8 C34 H34A 109.5 . . ? N8 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N8 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N8 C35 H35A 109.5 . . ? N8 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N8 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O16 C36 H36A 109.5 . . ? O16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 O2 117.1(3) . . ? C1 N1 Mn1 122.5(2) . . ? O2 N1 Mn1 120.39(19) . . ? C2 N2 O3 118.1(3) . . ? C10 N3 O5 116.5(3) . . ? C10 N3 Mn2 123.6(2) . . ? O5 N3 Mn2 119.93(19) . . ? C11 N4 O6 119.7(3) . . ? C19 N5 O8 117.5(3) . . ? C19 N5 Mn3 123.9(2) . . ? O8 N5 Mn3 118.58(19) . . ? C20 N6 O9 118.0(3) . . ? C30 N7 C31 122.2(6) . . ? C30 N7 C32 117.1(5) . . ? C31 N7 C32 120.2(5) . . ? C33 N8 C34 121.0(4) . . ? C33 N8 C35 120.4(4) . . ? C34 N8 C35 118.6(5) . . ? Mn1 O1 Mn2 120.54(12) . . ? Mn1 O1 Mn3 119.24(11) . . ? Mn2 O1 Mn3 115.11(11) . . ? N1 O2 Mn3 116.47(18) . . ? N2 O3 Mn1 129.1(2) . . ? N3 O5 Mn1 115.63(19) . . ? N4 O6 Mn2 129.7(2) . . ? N5 O8 Mn2 114.65(17) . . ? N6 O9 Mn3 131.76(19) . . ? C28 O11 Mn3 128.5(2) . . ? C28 O12 Mn2 129.1(2) . . ? C30 O13 Mn2 124.4(3) . . ? C33 O14 Mn1 121.1(3) . . ? Mn3 O15 H152 109.7 . . ? Mn3 O15 H151 107.1 . . ? H152 O15 H151 111.4 . . ? C36 O16 Mn1 123.7(2) . . ? C36 O16 H161 105.6 . . ? Mn1 O16 H161 121.8 . . ? H172 O17 H171 112.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Mn2 Mn3 O1 -179.4(2) . . . . ? O8 Mn2 Mn3 O1 147.71(16) . . . . ? N3 Mn2 Mn3 O1 -25.19(16) . . . . ? O12 Mn2 Mn3 O1 -110.80(15) . . . . ? O13 Mn2 Mn3 O1 66.53(16) . . . . ? O1 Mn2 Mn3 O9 -173.3(2) . . . . ? O6 Mn2 Mn3 O9 7.4(2) . . . . ? O8 Mn2 Mn3 O9 -25.56(18) . . . . ? N3 Mn2 Mn3 O9 161.54(18) . . . . ? O12 Mn2 Mn3 O9 75.93(17) . . . . ? O13 Mn2 Mn3 O9 -106.74(18) . . . . ? O1 Mn2 Mn3 O2 18.52(16) . . . . ? O6 Mn2 Mn3 O2 -160.83(18) . . . . ? O8 Mn2 Mn3 O2 166.23(12) . . . . ? N3 Mn2 Mn3 O2 -6.67(13) . . . . ? O12 Mn2 Mn3 O2 -92.28(11) . . . . ? O13 Mn2 Mn3 O2 85.05(13) . . . . ? O1 Mn2 Mn3 N5 -154.81(16) . . . . ? O6 Mn2 Mn3 N5 25.83(18) . . . . ? O8 Mn2 Mn3 N5 -7.11(12) . . . . ? N3 Mn2 Mn3 N5 179.99(14) . . . . ? O12 Mn2 Mn3 N5 94.38(11) . . . . ? O13 Mn2 Mn3 N5 -88.29(13) . . . . ? O1 Mn2 Mn3 O11 106.97(14) . . . . ? O6 Mn2 Mn3 O11 -72.39(17) . . . . ? O8 Mn2 Mn3 O11 -105.32(10) . . . . ? N3 Mn2 Mn3 O11 81.78(12) . . . . ? O12 Mn2 Mn3 O11 -3.83(9) . . . . ? O13 Mn2 Mn3 O11 173.50(11) . . . . ? O1 Mn2 Mn3 O15 -69.02(14) . . . . ? O6 Mn2 Mn3 O15 111.62(17) . . . . ? O8 Mn2 Mn3 O15 78.68(10) . . . . ? N3 Mn2 Mn3 O15 -94.21(12) . . . . ? O12 Mn2 Mn3 O15 -179.83(9) . . . . ? O13 Mn2 Mn3 O15 -2.50(11) . . . . ? N1 C1 C2 N2 -10.5(6) . . . . ? C9 C1 C2 N2 172.8(4) . . . . ? N1 C1 C2 C3 170.6(3) . . . . ? C9 C1 C2 C3 -6.1(3) . . . . ? N2 C2 C3 O4 7.9(6) . . . . ? C1 C2 C3 O4 -173.1(3) . . . . ? N2 C2 C3 C4 -172.9(3) . . . . ? C1 C2 C3 C4 6.2(3) . . . . ? O4 C3 C4 C5 -3.5(6) . . . . ? C2 C3 C4 C5 177.3(3) . . . . ? O4 C3 C4 C9 175.1(4) . . . . ? C2 C3 C4 C9 -4.2(4) . . . . ? C9 C4 C5 C6 0.6(5) . . . . ? C3 C4 C5 C6 179.0(3) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C8 -0.7(6) . . . . ? C6 C7 C8 C9 0.7(5) . . . . ? C7 C8 C9 C4 -0.1(5) . . . . ? C7 C8 C9 C1 -179.7(3) . . . . ? C5 C4 C9 C8 -0.6(5) . . . . ? C3 C4 C9 C8 -179.2(3) . . . . ? C5 C4 C9 C1 179.1(3) . . . . ? C3 C4 C9 C1 0.5(4) . . . . ? N1 C1 C9 C8 6.8(6) . . . . ? C2 C1 C9 C8 -176.8(3) . . . . ? N1 C1 C9 C4 -172.8(3) . . . . ? C2 C1 C9 C4 3.6(4) . . . . ? N3 C10 C11 N4 -4.8(6) . . . . ? C18 C10 C11 N4 175.9(4) . . . . ? N3 C10 C11 C12 179.1(3) . . . . ? C18 C10 C11 C12 -0.2(4) . . . . ? N4 C11 C12 O7 2.7(6) . . . . ? C10 C11 C12 O7 179.3(4) . . . . ? N4 C11 C12 C13 -177.4(3) . . . . ? C10 C11 C12 C13 -0.7(4) . . . . ? O7 C12 C13 C14 3.6(7) . . . . ? C11 C12 C13 C14 -176.4(4) . . . . ? O7 C12 C13 C18 -178.6(4) . . . . ? C11 C12 C13 C18 1.4(4) . . . . ? C18 C13 C14 C15 1.0(6) . . . . ? C12 C13 C14 C15 178.6(4) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C14 C15 C16 C17 -1.1(7) . . . . ? C15 C16 C17 C18 0.9(7) . . . . ? C16 C17 C18 C13 0.2(6) . . . . ? C16 C17 C18 C10 -176.8(4) . . . . ? C14 C13 C18 C17 -1.1(6) . . . . ? C12 C13 C18 C17 -179.2(4) . . . . ? C14 C13 C18 C10 176.4(3) . . . . ? C12 C13 C18 C10 -1.6(4) . . . . ? N3 C10 C18 C17 -0.9(7) . . . . ? C11 C10 C18 C17 178.3(4) . . . . ? N3 C10 C18 C13 -178.1(4) . . . . ? C11 C10 C18 C13 1.1(4) . . . . ? N5 C19 C20 N6 -2.4(6) . . . . ? C27 C19 C20 N6 178.4(3) . . . . ? N5 C19 C20 C21 178.2(3) . . . . ? C27 C19 C20 C21 -1.0(3) . . . . ? N6 C20 C21 O10 3.0(5) . . . . ? C19 C20 C21 O10 -177.5(3) . . . . ? N6 C20 C21 C22 -178.0(3) . . . . ? C19 C20 C21 C22 1.5(3) . . . . ? O10 C21 C22 C23 -0.9(6) . . . . ? C20 C21 C22 C23 -179.9(3) . . . . ? O10 C21 C22 C27 177.5(3) . . . . ? C20 C21 C22 C27 -1.5(4) . . . . ? C27 C22 C23 C24 1.7(5) . . . . ? C21 C22 C23 C24 179.9(3) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C23 C24 C25 C26 -0.9(6) . . . . ? C24 C25 C26 C27 0.8(6) . . . . ? C25 C26 C27 C22 0.5(5) . . . . ? C25 C26 C27 C19 179.0(4) . . . . ? C23 C22 C27 C26 -1.8(5) . . . . ? C21 C22 C27 C26 179.7(3) . . . . ? C23 C22 C27 C19 179.4(3) . . . . ? C21 C22 C27 C19 0.9(4) . . . . ? N5 C19 C27 C26 2.4(6) . . . . ? C20 C19 C27 C26 -178.5(3) . . . . ? N5 C19 C27 C22 -179.0(3) . . . . ? C20 C19 C27 C22 0.1(4) . . . . ? C9 C1 N1 O2 -0.5(5) . . . . ? C2 C1 N1 O2 -176.4(3) . . . . ? C9 C1 N1 Mn1 176.7(3) . . . . ? C2 C1 N1 Mn1 0.8(4) . . . . ? O1 Mn1 N1 C1 -174.2(3) . . . . ? O3 Mn1 N1 C1 10.6(3) . . . . ? O14 Mn1 N1 C1 100.9(3) . . . . ? O16 Mn1 N1 C1 -75.8(3) . . . . ? O1 Mn1 N1 O2 3.0(2) . . . . ? O3 Mn1 N1 O2 -172.3(2) . . . . ? O14 Mn1 N1 O2 -81.9(2) . . . . ? O16 Mn1 N1 O2 101.3(2) . . . . ? C1 C2 N2 O3 0.8(5) . . . . ? C3 C2 N2 O3 179.6(3) . . . . ? C18 C10 N3 O5 -5.2(6) . . . . ? C11 C10 N3 O5 175.7(3) . . . . ? C18 C10 N3 Mn2 174.6(3) . . . . ? C11 C10 N3 Mn2 -4.6(5) . . . . ? O1 Mn2 N3 C10 -169.1(3) . . . . ? O6 Mn2 N3 C10 10.6(3) . . . . ? O12 Mn2 N3 C10 -79.5(3) . . . . ? O13 Mn2 N3 C10 97.5(3) . . . . ? Mn3 Mn2 N3 C10 -155.9(3) . . . . ? O1 Mn2 N3 O5 10.6(2) . . . . ? O6 Mn2 N3 O5 -169.6(2) . . . . ? O12 Mn2 N3 O5 100.2(2) . . . . ? O13 Mn2 N3 O5 -82.8(2) . . . . ? Mn3 Mn2 N3 O5 23.9(3) . . . . ? C10 C11 N4 O6 2.8(6) . . . . ? C12 C11 N4 O6 178.5(3) . . . . ? C27 C19 N5 O8 -0.5(5) . . . . ? C20 C19 N5 O8 -179.6(3) . . . . ? C27 C19 N5 Mn3 179.8(3) . . . . ? C20 C19 N5 Mn3 0.8(4) . . . . ? O1 Mn3 N5 C19 177.1(3) . . . . ? O9 Mn3 N5 C19 1.5(3) . . . . ? O11 Mn3 N5 C19 -94.4(3) . . . . ? O15 Mn3 N5 C19 94.4(3) . . . . ? Mn2 Mn3 N5 C19 -169.7(3) . . . . ? O1 Mn3 N5 O8 -2.5(2) . . . . ? O9 Mn3 N5 O8 -178.2(2) . . . . ? O11 Mn3 N5 O8 85.9(2) . . . . ? O15 Mn3 N5 O8 -85.3(2) . . . . ? Mn2 Mn3 N5 O8 10.63(17) . . . . ? C19 C20 N6 O9 0.3(5) . . . . ? C21 C20 N6 O9 179.6(3) . . . . ? O13 C30 N7 C31 179.6(7) . . . . ? O13 C30 N7 C32 8.2(10) . . . . ? O14 C33 N8 C34 -1.2(8) . . . . ? O14 C33 N8 C35 178.3(5) . . . . ? O5 Mn1 O1 Mn2 -11.18(15) . . . . ? N1 Mn1 O1 Mn2 159.27(15) . . . . ? O14 Mn1 O1 Mn2 -108.79(15) . . . . ? O16 Mn1 O1 Mn2 77.13(14) . . . . ? O5 Mn1 O1 Mn3 -164.66(14) . . . . ? N1 Mn1 O1 Mn3 5.79(14) . . . . ? O14 Mn1 O1 Mn3 97.73(14) . . . . ? O16 Mn1 O1 Mn3 -76.35(14) . . . . ? O8 Mn2 O1 Mn1 176.74(14) . . . . ? N3 Mn2 O1 Mn1 3.34(15) . . . . ? O12 Mn2 O1 Mn1 -88.97(14) . . . . ? O13 Mn2 O1 Mn1 86.45(15) . . . . ? Mn3 Mn2 O1 Mn1 -154.5(2) . . . . ? O8 Mn2 O1 Mn3 -28.75(14) . . . . ? N3 Mn2 O1 Mn3 157.86(14) . . . . ? O12 Mn2 O1 Mn3 65.55(13) . . . . ? O13 Mn2 O1 Mn3 -119.04(14) . . . . ? O2 Mn3 O1 Mn1 -9.85(14) . . . . ? N5 Mn3 O1 Mn1 176.66(14) . . . . ? O11 Mn3 O1 Mn1 85.66(13) . . . . ? O15 Mn3 O1 Mn1 -94.92(13) . . . . ? Mn2 Mn3 O1 Mn1 154.9(2) . . . . ? O2 Mn3 O1 Mn2 -164.72(13) . . . . ? N5 Mn3 O1 Mn2 21.79(13) . . . . ? O11 Mn3 O1 Mn2 -69.21(13) . . . . ? O15 Mn3 O1 Mn2 110.21(13) . . . . ? C1 N1 O2 Mn3 167.0(2) . . . . ? Mn1 N1 O2 Mn3 -10.3(3) . . . . ? O1 Mn3 O2 N1 11.7(2) . . . . ? O9 Mn3 O2 N1 -172.4(2) . . . . ? O11 Mn3 O2 N1 -77.1(2) . . . . ? O15 Mn3 O2 N1 94.2(2) . . . . ? Mn2 Mn3 O2 N1 1.9(2) . . . . ? C2 N2 O3 Mn1 18.4(4) . . . . ? O5 Mn1 O3 N2 149.0(3) . . . . ? N1 Mn1 O3 N2 -21.3(3) . . . . ? O14 Mn1 O3 N2 -113.2(3) . . . . ? O16 Mn1 O3 N2 60.9(3) . . . . ? C10 N3 O5 Mn1 159.4(3) . . . . ? Mn2 N3 O5 Mn1 -20.4(3) . . . . ? O1 Mn1 O5 N3 18.3(2) . . . . ? O3 Mn1 O5 N3 -166.7(2) . . . . ? O14 Mn1 O5 N3 103.6(2) . . . . ? O16 Mn1 O5 N3 -79.8(2) . . . . ? C11 N4 O6 Mn2 9.3(5) . . . . ? O8 Mn2 O6 N4 173.0(3) . . . . ? N3 Mn2 O6 N4 -13.6(3) . . . . ? O12 Mn2 O6 N4 78.7(3) . . . . ? O13 Mn2 O6 N4 -96.7(3) . . . . ? Mn3 Mn2 O6 N4 143.7(2) . . . . ? C19 N5 O8 Mn2 163.7(2) . . . . ? Mn3 N5 O8 Mn2 -16.6(3) . . . . ? O1 Mn2 O8 N5 26.9(2) . . . . ? O6 Mn2 O8 N5 -152.9(2) . . . . ? O12 Mn2 O8 N5 -62.9(2) . . . . ? O13 Mn2 O8 N5 120.1(2) . . . . ? Mn3 Mn2 O8 N5 10.22(17) . . . . ? C20 N6 O9 Mn3 3.5(4) . . . . ? O2 Mn3 O9 N6 -177.6(3) . . . . ? N5 Mn3 O9 N6 -3.8(3) . . . . ? O11 Mn3 O9 N6 87.3(3) . . . . ? O15 Mn3 O9 N6 -92.4(3) . . . . ? Mn2 Mn3 O9 N6 12.2(4) . . . . ? O12 C28 O11 Mn3 14.1(5) . . . . ? C29 C28 O11 Mn3 -167.8(2) . . . . ? O1 Mn3 O11 C28 28.0(3) . . . . ? O9 Mn3 O11 C28 -154.3(3) . . . . ? O2 Mn3 O11 C28 120.8(3) . . . . ? N5 Mn3 O11 C28 -62.6(3) . . . . ? Mn2 Mn3 O11 C28 -2.9(2) . . . . ? O11 C28 O12 Mn2 -21.1(5) . . . . ? C29 C28 O12 Mn2 160.8(2) . . . . ? O1 Mn2 O12 C28 -16.7(3) . . . . ? O6 Mn2 O12 C28 163.6(3) . . . . ? O8 Mn2 O12 C28 75.6(3) . . . . ? N3 Mn2 O12 C28 -104.6(3) . . . . ? Mn3 Mn2 O12 C28 13.4(3) . . . . ? N7 C30 O13 Mn2 173.1(5) . . . . ? O1 Mn2 O13 C30 82.5(5) . . . . ? O6 Mn2 O13 C30 -97.9(5) . . . . ? O8 Mn2 O13 C30 -9.9(5) . . . . ? N3 Mn2 O13 C30 169.9(5) . . . . ? Mn3 Mn2 O13 C30 52.9(5) . . . . ? N8 C33 O14 Mn1 -172.2(3) . . . . ? O1 Mn1 O14 C33 141.8(3) . . . . ? O3 Mn1 O14 C33 -36.7(3) . . . . ? O5 Mn1 O14 C33 49.8(3) . . . . ? N1 Mn1 O14 C33 -128.8(3) . . . . ? O1 Mn1 O16 C36 -118.3(3) . . . . ? O3 Mn1 O16 C36 60.7(3) . . . . ? O5 Mn1 O16 C36 -25.9(3) . . . . ? N1 Mn1 O16 C36 153.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15 H152 O14 0.85 2.29 3.073(4) 152.7 . O15 H151 O9 0.85 1.98 2.816(3) 168.8 3_575 O15 H151 N6 0.85 2.52 3.189(4) 136.8 3_575 O16 H161 O10 0.85 2.00 2.811(3) 160.6 2_545 O17 H172 O7 0.85 2.41 3.133(4) 143.5 2_645 O17 H172 N4 0.85 2.46 3.182(4) 143.4 2_645 O17 H171 O3 0.85 2.03 2.866(4) 169.2 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.249 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.091 #===END