_data_manuscript_title ; 'Coordination vs. Coupling of Dicyanamide in Molybdenum and Manganese Pyrazole Complexes' ; _audit_creation_method SHELXL _pub_requested_journal 'Inorg. Chem.' _publ_contact_author ; FERNANDO VILLAFAÑE IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_phone '+34-983-184620' _publ_contact_author_fax '+34-983-423013' _publ_contact_author_email 'fervilla@qi.uva.es' loop_ _publ_author_name _publ_author_address 'Marta Arroyo' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Patricia Gómez-Iglesias' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Jose Miguel Martín-Alvarez' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Celedonio M. Alvarez' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Daniel Miguel' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Fernando Villafañe' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; #---------data section of block ----------------------- data_Compound_1b_ma385am _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Mo2 N10 O6' _chemical_formula_weight 882.69 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' 'Mo' 'Mo' -1.6832 0.6857 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.897(4) _cell_length_b 14.105(5) _cell_length_c 14.454(5) _cell_angle_alpha 67.379(5) _cell_angle_beta 85.495(7) _cell_angle_gamma 69.564(7) _cell_volume 2093.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 650 _cell_measurement_theta_min 2.309 _cell_measurement_theta_max 23.268 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.363603 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 9429 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.38 _reflns_number_total 5968 _reflns_number_gt 1912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0827P)^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 5968 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2536 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 0.840 _refine_ls_restrained_S_all 0.840 _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 O90 O 0.5053(11) 0.6196(17) 0.2854(16) 0.147(7) Uani 1 1 d G . . C91 C 0.579(2) 0.5945(18) 0.3669(11) 0.193(15) Uani 1 1 d G . . H91A H 0.5320 0.6223 0.4149 0.231 Uiso 1 1 calc R . . H91B H 0.6165 0.5157 0.4000 0.231 Uiso 1 1 calc R . . C92 C 0.6652(19) 0.642(2) 0.333(2) 0.29(3) Uani 1 1 d G . . H92A H 0.6603 0.6930 0.3640 0.343 Uiso 1 1 calc R . . H92B H 0.7447 0.5864 0.3490 0.343 Uiso 1 1 calc R . . C93 C 0.645(2) 0.6967(19) 0.230(2) 0.224(19) Uani 1 1 d G . . H93A H 0.6305 0.7739 0.2116 0.269 Uiso 1 1 calc R . . H93B H 0.7149 0.6674 0.1967 0.269 Uiso 1 1 calc R . . C94 C 0.546(2) 0.6827(16) 0.2007(11) 0.167(13) Uani 1 1 d G . . H94A H 0.5683 0.6467 0.1534 0.200 Uiso 1 1 calc R . . H94B H 0.4839 0.7533 0.1683 0.200 Uiso 1 1 calc R . . Mo1 Mo 0.29662(13) 0.42092(11) 0.26541(10) 0.0546(6) Uani 1 1 d . . . Mo2 Mo 0.02075(13) 0.85594(11) -0.25481(10) 0.0500(5) Uani 1 1 d . . . N1 N 0.2014(15) 0.5569(10) 0.3216(9) 0.055(4) Uani 1 1 d . . . N2 N 0.2633(11) 0.6200(12) 0.3298(9) 0.058(4) Uani 1 1 d . . . H2 H 0.3346 0.6151 0.3104 0.070 Uiso 1 1 calc R . . N3 N 0.1267(12) 0.4950(11) 0.1711(10) 0.052(4) Uani 1 1 d . . . N4 N -0.0446(12) 0.6069(12) 0.0467(11) 0.069(4) Uani 1 1 d . . . N5 N -0.0315(12) 0.7393(10) -0.1207(10) 0.053(4) Uani 1 1 d . . . C1 C 0.428(2) 0.3762(15) 0.3568(13) 0.091(8) Uani 1 1 d . . . O1 O 0.5081(13) 0.3441(11) 0.4188(10) 0.110(5) Uani 1 1 d . . . C2 C 0.2520(17) 0.3246(16) 0.3824(12) 0.079(7) Uani 1 1 d . . . O2 O 0.2253(13) 0.2646(11) 0.4593(10) 0.109(5) Uani 1 1 d . . . C3 C 0.4719(18) 0.3207(15) 0.2180(14) 0.090(7) Uani 1 1 d . . . H3A H 0.5216 0.3610 0.1772 0.109 Uiso 1 1 calc R . . H3B H 0.5175 0.2504 0.2685 0.109 Uiso 1 1 calc R . . C4 C 0.3732(18) 0.3246(15) 0.1680(14) 0.066(5) Uani 1 1 d . . . C5 C 0.3030(16) 0.2674(14) 0.2378(15) 0.084(6) Uani 1 1 d . . . H5A H 0.3470 0.1967 0.2886 0.101 Uiso 1 1 calc R . . H5B H 0.2294 0.2703 0.2105 0.101 Uiso 1 1 calc R . . C6 C 0.3436(16) 0.3815(16) 0.0550(13) 0.100(7) Uani 1 1 d . . . H6A H 0.3820 0.3306 0.0235 0.150 Uiso 1 1 calc R . . H6B H 0.3719 0.4421 0.0288 0.150 Uiso 1 1 calc R . . H6C H 0.2581 0.4076 0.0414 0.150 Uiso 1 1 calc R . . C7 C 0.0492(17) 0.5469(14) 0.1113(13) 0.047(5) Uani 1 1 d . . . C8 C -0.0301(14) 0.6764(13) -0.0416(14) 0.051(5) Uani 1 1 d . . . C11 C 0.096(2) 0.5883(17) 0.3560(14) 0.076(6) Uani 1 1 d . . . C12 C 0.088(2) 0.6763(18) 0.3914(14) 0.091(7) Uani 1 1 d . . . H12 H 0.0238 0.7136 0.4200 0.110 Uiso 1 1 calc R . . C13 C 0.199(2) 0.6894(15) 0.3716(12) 0.071(6) Uani 1 1 d . . . C14 C 0.2505(18) 0.7677(14) 0.3899(14) 0.101(7) Uani 1 1 d . . . H14A H 0.3178 0.7257 0.4385 0.152 Uiso 1 1 calc R . . H14B H 0.1896 0.8163 0.4145 0.152 Uiso 1 1 calc R . . H14C H 0.2764 0.8096 0.3280 0.152 Uiso 1 1 calc R . . C15 C -0.0071(17) 0.5485(17) 0.3583(15) 0.118(8) Uani 1 1 d . . . H15A H -0.0516 0.5868 0.2943 0.177 Uiso 1 1 calc R . . H15B H -0.0590 0.5620 0.4096 0.177 Uiso 1 1 calc R . . H15C H 0.0238 0.4713 0.3725 0.177 Uiso 1 1 calc R . . N51 N -0.0578(14) 0.9716(11) -0.1749(9) 0.058(4) Uani 1 1 d . . . N52 N 0.0063(12) 1.0337(11) -0.1659(9) 0.061(4) Uani 1 1 d . . . H52 H 0.0782 1.0277 -0.1844 0.073 Uiso 1 1 calc R . . N53 N 0.1785(12) 0.8057(10) -0.1486(10) 0.054(4) Uani 1 1 d . . . N54 N 0.3324(12) 0.7172(12) -0.0118(11) 0.064(4) Uani 1 1 d . . . N55 N 0.3348(13) 0.5633(12) 0.1420(11) 0.071(5) Uani 1 1 d . . . C51 C -0.1263(18) 0.9165(12) -0.3354(12) 0.062(5) Uani 1 1 d . . . O51 O -0.2178(12) 0.9617(10) -0.3884(9) 0.086(4) Uani 1 1 d . . . C52 C 0.0439(16) 0.9792(14) -0.3615(13) 0.066(5) Uani 1 1 d . . . O52 O 0.0490(11) 1.0597(10) -0.4287(8) 0.080(4) Uani 1 1 d . . . C53 C 0.0095(16) 0.7371(12) -0.3281(12) 0.067(5) Uani 1 1 d . . . H53A H -0.0273 0.6833 -0.2903 0.080 Uiso 1 1 calc R . . H53B H -0.0102 0.7683 -0.4000 0.080 Uiso 1 1 calc R . . C54 C 0.1373(18) 0.7141(16) -0.2943(14) 0.066(5) Uani 1 1 d . . . C55 C 0.1726(16) 0.8021(14) -0.3510(13) 0.077(6) Uani 1 1 d . . . H55A H 0.1535 0.8324 -0.4228 0.092 Uiso 1 1 calc R . . H55B H 0.2517 0.7980 -0.3332 0.092 Uiso 1 1 calc R . . C56 C 0.2052(16) 0.6088(12) -0.2122(13) 0.084(6) Uani 1 1 d . . . H56A H 0.2401 0.6235 -0.1639 0.125 Uiso 1 1 calc R . . H56B H 0.2678 0.5648 -0.2399 0.125 Uiso 1 1 calc R . . H56C H 0.1515 0.5702 -0.1801 0.125 Uiso 1 1 calc R . . C57 C 0.2484(16) 0.7613(13) -0.0805(12) 0.042(4) Uani 1 1 d . . . C58 C 0.3291(14) 0.6344(15) 0.0690(14) 0.048(5) Uani 1 1 d . . . C61 C -0.1663(18) 1.0071(14) -0.1370(13) 0.063(5) Uani 1 1 d . . . C62 C -0.167(2) 1.0917(16) -0.1066(14) 0.086(7) Uani 1 1 d . . . H62 H -0.2301 1.1312 -0.0791 0.103 Uiso 1 1 calc R . . C63 C -0.060(2) 1.1046(15) -0.1244(12) 0.071(6) Uani 1 1 d . . . C64 C -0.2611(16) 0.9583(17) -0.1305(15) 0.108(8) Uani 1 1 d . . . H64A H -0.2650 0.9455 -0.1906 0.162 Uiso 1 1 calc R . . H64B H -0.3374 1.0078 -0.1233 0.162 Uiso 1 1 calc R . . H64C H -0.2417 0.8902 -0.0735 0.162 Uiso 1 1 calc R . . C65 C -0.0077(18) 1.1804(14) -0.1091(13) 0.101(7) Uani 1 1 d . . . H65A H 0.0303 1.1477 -0.0426 0.152 Uiso 1 1 calc R . . H65B H -0.0707 1.2484 -0.1173 0.152 Uiso 1 1 calc R . . H65C H 0.0507 1.1936 -0.1576 0.152 Uiso 1 1 calc R . . O95 O 0.2429(14) 1.0463(13) -0.2284(17) 0.167(8) Uani 1 1 d G . . C96 C 0.278(2) 1.0582(15) -0.3277(14) 0.196(15) Uiso 1 1 d G . . H96A H 0.2469 1.0167 -0.3522 0.235 Uiso 1 1 calc R . . H96B H 0.2468 1.1346 -0.3726 0.235 Uiso 1 1 calc R . . C97 C 0.406(2) 1.0187(19) -0.3245(18) 0.220(16) Uiso 1 1 d G . . H97A H 0.4348 1.0766 -0.3679 0.264 Uiso 1 1 calc R . . H97B H 0.4349 0.9586 -0.3474 0.264 Uiso 1 1 calc R . . C98 C 0.4502(18) 0.9824(16) -0.223(2) 0.26(3) Uani 1 1 d G . . H98A H 0.4992 0.9053 -0.1988 0.318 Uiso 1 1 calc R . . H98B H 0.4991 1.0233 -0.2192 0.318 Uiso 1 1 calc R . . C99 C 0.349(2) 0.9994(15) -0.1638(13) 0.26(3) Uani 1 1 d G . . H99A H 0.3510 0.9304 -0.1117 0.316 Uiso 1 1 calc R . . H99B H 0.3509 1.0483 -0.1321 0.316 Uiso 1 1 calc 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 O90 0.108(13) 0.27(2) 0.129(14) -0.115(16) -0.007(11) -0.100(14) C91 0.13(3) 0.37(5) 0.12(2) -0.13(3) 0.02(2) -0.10(3) C92 0.18(4) 0.56(8) 0.31(6) -0.26(6) 0.03(4) -0.24(4) C93 0.26(5) 0.32(5) 0.22(4) -0.14(4) 0.03(3) -0.22(4) C94 0.18(3) 0.14(3) 0.14(3) 0.00(2) 0.01(2) -0.08(2) Mo1 0.0576(13) 0.0546(11) 0.0545(11) -0.0209(9) -0.0112(9) -0.0198(9) Mo2 0.0625(13) 0.0459(10) 0.0478(10) -0.0202(8) -0.0080(9) -0.0208(9) N1 0.068(12) 0.061(10) 0.038(8) -0.016(7) 0.008(8) -0.030(9) N2 0.040(10) 0.082(11) 0.071(10) -0.045(9) 0.011(7) -0.026(9) N3 0.042(10) 0.063(10) 0.068(10) -0.023(8) -0.008(8) -0.038(8) N4 0.053(11) 0.091(12) 0.062(10) -0.004(9) -0.017(9) -0.048(9) N5 0.072(11) 0.047(9) 0.050(9) -0.016(7) -0.008(8) -0.033(8) C1 0.111(19) 0.076(15) 0.053(13) -0.030(11) -0.041(12) 0.022(13) O1 0.119(13) 0.108(11) 0.097(11) -0.045(9) -0.059(9) -0.013(9) C2 0.098(17) 0.104(17) 0.021(10) -0.017(11) -0.012(11) -0.023(13) O2 0.154(14) 0.113(12) 0.058(9) -0.016(8) -0.007(9) -0.058(10) C3 0.091(17) 0.085(15) 0.095(16) -0.054(12) -0.022(13) -0.003(13) C4 0.065(15) 0.065(13) 0.064(14) -0.033(11) 0.000(12) -0.008(11) C5 0.071(15) 0.049(12) 0.129(18) -0.044(12) -0.013(13) -0.002(11) C6 0.106(17) 0.150(19) 0.079(15) -0.075(14) 0.018(12) -0.055(15) C7 0.046(13) 0.056(12) 0.051(12) -0.020(10) 0.002(10) -0.032(11) C8 0.065(13) 0.040(11) 0.056(12) -0.013(10) -0.023(11) -0.026(10) C11 0.055(16) 0.102(17) 0.073(14) -0.039(12) 0.022(11) -0.028(14) C12 0.086(19) 0.109(19) 0.068(14) -0.035(13) -0.015(12) -0.016(16) C13 0.098(19) 0.062(13) 0.054(12) -0.037(10) 0.001(12) -0.013(13) C14 0.15(2) 0.068(13) 0.105(16) -0.050(12) -0.028(13) -0.027(13) C15 0.062(16) 0.14(2) 0.15(2) -0.062(17) 0.023(13) -0.038(15) N51 0.061(12) 0.080(11) 0.053(9) -0.037(8) 0.006(8) -0.034(10) N52 0.061(11) 0.053(9) 0.073(10) -0.025(8) -0.013(8) -0.020(8) N53 0.066(11) 0.043(9) 0.052(10) -0.018(8) -0.007(8) -0.016(8) N54 0.057(11) 0.079(11) 0.053(10) -0.012(9) -0.015(8) -0.028(9) N55 0.078(12) 0.070(11) 0.066(11) -0.024(9) -0.015(10) -0.022(10) C51 0.102(17) 0.032(10) 0.038(11) -0.005(8) -0.009(10) -0.014(11) O51 0.099(11) 0.075(9) 0.087(10) -0.029(8) -0.027(8) -0.027(8) C52 0.086(15) 0.056(12) 0.052(12) -0.015(10) 0.007(11) -0.026(11) O52 0.112(11) 0.071(9) 0.053(8) -0.005(7) -0.003(7) -0.047(8) C53 0.092(16) 0.056(12) 0.074(13) -0.042(10) 0.032(11) -0.038(11) C54 0.057(14) 0.078(15) 0.069(13) -0.049(12) -0.001(11) -0.007(12) C55 0.093(16) 0.082(14) 0.090(14) -0.046(12) 0.019(12) -0.060(13) C56 0.104(16) 0.043(11) 0.114(16) -0.048(12) -0.016(13) -0.014(11) C57 0.046(13) 0.048(11) 0.031(10) -0.012(9) 0.001(9) -0.020(10) C58 0.040(12) 0.052(13) 0.055(13) -0.020(10) -0.016(11) -0.016(10) C61 0.067(16) 0.057(12) 0.071(13) -0.022(10) 0.009(11) -0.032(12) C62 0.070(17) 0.078(15) 0.115(18) -0.069(13) -0.028(14) 0.011(13) C63 0.11(2) 0.042(12) 0.051(12) -0.016(9) -0.022(12) -0.013(13) C64 0.059(15) 0.15(2) 0.16(2) -0.102(17) 0.047(14) -0.052(15) C65 0.16(2) 0.074(14) 0.099(15) -0.043(12) -0.009(14) -0.064(14) O95 0.109(15) 0.150(16) 0.23(2) -0.036(14) -0.029(14) -0.062(13) C98 0.17(4) 0.15(3) 0.47(7) -0.14(4) -0.19(4) 0.03(3) C99 0.11(3) 0.065(19) 0.57(7) -0.03(3) -0.08(4) -0.05(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 O90 C94 1.379(10) . ? O90 C91 1.379(10) . ? C91 C92 1.379(10) . ? C92 C93 1.379(10) . ? C93 C94 1.379(10) . ? Mo1 C1 1.89(2) . ? Mo1 C2 1.89(2) . ? Mo1 N3 2.213(14) . ? Mo1 C4 2.250(17) . ? Mo1 N1 2.272(14) . ? Mo1 N55 2.275(16) . ? Mo1 C3 2.298(18) . ? Mo1 C5 2.323(16) . ? Mo2 C51 1.91(2) . ? Mo2 C52 1.919(18) . ? Mo2 N5 2.219(13) . ? Mo2 N53 2.251(14) . ? Mo2 C54 2.251(17) . ? Mo2 N51 2.255(13) . ? Mo2 C55 2.287(17) . ? Mo2 C53 2.345(15) . ? N1 C11 1.301(19) . ? N1 N2 1.378(16) . ? N2 C13 1.330(19) . ? N3 C7 1.140(18) . ? N4 C7 1.32(2) . ? N4 C8 1.319(19) . ? N5 C8 1.143(17) . ? C1 O1 1.201(18) . ? C2 O2 1.209(18) . ? C3 C4 1.40(2) . ? C4 C5 1.44(2) . ? C4 C6 1.52(2) . ? C11 C12 1.49(2) . ? C11 C15 1.51(2) . ? C12 C13 1.39(2) . ? C13 C14 1.55(2) . ? N51 C61 1.366(19) . ? N51 N52 1.392(16) . ? N52 C63 1.35(2) . ? N53 C57 1.160(17) . ? N54 C57 1.272(19) . ? N54 C58 1.306(19) . ? N55 C58 1.129(18) . ? C51 O51 1.204(18) . ? C52 O52 1.194(16) . ? C53 C54 1.52(2) . ? C54 C55 1.38(2) . ? C54 C56 1.49(2) . ? C61 C62 1.42(2) . ? C61 C64 1.49(2) . ? C62 C63 1.34(2) . ? C63 C65 1.50(2) . ? O95 C99 1.426(11) . ? O95 C96 1.426(11) . ? C96 C97 1.426(11) . ? C97 C98 1.426(11) . ? C98 C99 1.426(11) . ? 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 C94 O90 C91 108.0 . . ? C92 C91 O90 108.0 . . ? C93 C92 C91 108.0 . . ? C94 C93 C92 108.0 . . ? C93 C94 O90 108.0 . . ? C1 Mo1 C2 78.8(9) . . ? C1 Mo1 N3 169.6(6) . . ? C2 Mo1 N3 99.7(7) . . ? C1 Mo1 C4 102.9(7) . . ? C2 Mo1 C4 105.9(8) . . ? N3 Mo1 C4 87.5(6) . . ? C1 Mo1 N1 88.0(6) . . ? C2 Mo1 N1 87.5(7) . . ? N3 Mo1 N1 81.6(5) . . ? C4 Mo1 N1 164.0(6) . . ? C1 Mo1 N55 98.5(8) . . ? C2 Mo1 N55 167.3(7) . . ? N3 Mo1 N55 80.6(5) . . ? C4 Mo1 N55 86.8(6) . . ? N1 Mo1 N55 80.0(5) . . ? C1 Mo1 C3 68.5(7) . . ? C2 Mo1 C3 107.8(8) . . ? N3 Mo1 C3 121.4(6) . . ? C4 Mo1 C3 35.9(6) . . ? N1 Mo1 C3 148.0(7) . . ? N55 Mo1 C3 82.4(6) . . ? C1 Mo1 C5 107.0(7) . . ? C2 Mo1 C5 71.2(7) . . ? N3 Mo1 C5 82.0(5) . . ? C4 Mo1 C5 36.7(6) . . ? N1 Mo1 C5 150.4(6) . . ? N55 Mo1 C5 121.2(6) . . ? C3 Mo1 C5 60.9(7) . . ? C51 Mo2 C52 78.7(7) . . ? C51 Mo2 N5 98.0(6) . . ? C52 Mo2 N5 168.2(6) . . ? C51 Mo2 N53 170.4(6) . . ? C52 Mo2 N53 100.1(6) . . ? N5 Mo2 N53 81.3(5) . . ? C51 Mo2 C54 105.8(7) . . ? C52 Mo2 C54 102.6(7) . . ? N5 Mo2 C54 89.2(6) . . ? N53 Mo2 C54 83.8(6) . . ? C51 Mo2 N51 90.2(6) . . ? C52 Mo2 N51 85.6(6) . . ? N5 Mo2 N51 83.0(5) . . ? N53 Mo2 N51 80.1(5) . . ? C54 Mo2 N51 163.0(6) . . ? C51 Mo2 C55 107.0(7) . . ? C52 Mo2 C55 68.4(7) . . ? N5 Mo2 C55 123.3(5) . . ? N53 Mo2 C55 81.1(6) . . ? C54 Mo2 C55 35.5(5) . . ? N51 Mo2 C55 144.5(6) . . ? C51 Mo2 C53 69.3(6) . . ? C52 Mo2 C53 106.5(6) . . ? N5 Mo2 C53 82.5(5) . . ? N53 Mo2 C53 119.9(5) . . ? C54 Mo2 C53 38.6(5) . . ? N51 Mo2 C53 152.9(6) . . ? C55 Mo2 C53 61.6(6) . . ? C11 N1 N2 107.4(15) . . ? C11 N1 Mo1 133.6(15) . . ? N2 N1 Mo1 118.9(12) . . ? C13 N2 N1 111.4(15) . . ? C7 N3 Mo1 167.0(13) . . ? C7 N4 C8 118.6(14) . . ? C8 N5 Mo2 161.9(13) . . ? O1 C1 Mo1 176(2) . . ? O2 C2 Mo1 177.5(17) . . ? C4 C3 Mo1 70.2(11) . . ? C3 C4 C5 111.0(18) . . ? C3 C4 C6 124.7(19) . . ? C5 C4 C6 124.3(19) . . ? C3 C4 Mo1 73.9(11) . . ? C5 C4 Mo1 74.4(10) . . ? C6 C4 Mo1 118.8(11) . . ? C4 C5 Mo1 68.9(10) . . ? N3 C7 N4 176.6(19) . . ? N5 C8 N4 171.9(17) . . ? N1 C11 C12 109.4(19) . . ? N1 C11 C15 128(2) . . ? C12 C11 C15 123(2) . . ? C13 C12 C11 103.2(19) . . ? N2 C13 C12 108.6(19) . . ? N2 C13 C14 121(2) . . ? C12 C13 C14 131(2) . . ? C61 N51 N52 105.5(14) . . ? C61 N51 Mo2 134.7(12) . . ? N52 N51 Mo2 119.5(12) . . ? C63 N52 N51 110.6(16) . . ? C57 N53 Mo2 163.9(13) . . ? C57 N54 C58 119.2(15) . . ? C58 N55 Mo1 162.3(15) . . ? O51 C51 Mo2 175.4(15) . . ? O52 C52 Mo2 175.0(16) . . ? C54 C53 Mo2 67.4(9) . . ? C55 C54 C56 129.9(19) . . ? C55 C54 C53 109.5(16) . . ? C56 C54 C53 120.7(17) . . ? C55 C54 Mo2 73.7(11) . . ? C56 C54 Mo2 119.2(11) . . ? C53 C54 Mo2 74.1(9) . . ? C54 C55 Mo2 70.8(10) . . ? N53 C57 N54 174.0(18) . . ? N55 C58 N54 174.0(19) . . ? N51 C61 C62 108.0(17) . . ? N51 C61 C64 122.3(17) . . ? C62 C61 C64 130(2) . . ? C63 C62 C61 107.9(19) . . ? C62 C63 N52 108.1(18) . . ? C62 C63 C65 133(2) . . ? N52 C63 C65 119(2) . . ? C99 O95 C96 108.0 . . ? C97 C96 O95 108.0 . . ? C96 C97 C98 108.0 . . ? C99 C98 C97 108.0 . . ? O95 C99 C98 108.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.38 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.884 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.118 #===END data_Compound_2a_ma369am _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 Mn N7 O3' _chemical_formula_weight 341.18 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)/n 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 7.7764(18) _cell_length_b 13.535(3) _cell_length_c 13.609(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.601(5) _cell_angle_gamma 90.00 _cell_volume 1397.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 783 _cell_measurement_theta_min 3.665 _cell_measurement_theta_max 22.941 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787786 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 6114 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 23.29 _reflns_number_total 2016 _reflns_number_gt 1597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0558P)^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 2016 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.19012(5) 0.21779(3) 0.24478(3) 0.03995(19) Uani 1 1 d . . . N1 N -0.0372(3) 0.29383(18) 0.23615(17) 0.0403(6) Uani 1 1 d . . . N2 N -0.1765(3) 0.25478(18) 0.16838(17) 0.0406(6) Uani 1 1 d . . . N3 N 0.0090(3) 0.12900(18) 0.15507(17) 0.0432(6) Uani 1 1 d . . . H3 H 0.0368 0.0708 0.1385 0.052 Uiso 1 1 calc R . . N4 N 0.2052(3) 0.28824(17) 0.11195(16) 0.0390(6) Uani 1 1 d . . . N5 N 0.2374(3) 0.24010(19) 0.03147(16) 0.0436(6) Uani 1 1 d . . . H5 H 0.2514 0.1772 0.0288 0.052 Uiso 1 1 calc R . . N6 N -0.2907(3) 0.1307(2) 0.05935(19) 0.0512(7) Uani 1 1 d . . . N7 N -0.2734(3) -0.0315(2) -0.0203(2) 0.0579(7) Uani 1 1 d . . . C1 C 0.1719(5) 0.1569(3) 0.3593(3) 0.0583(9) Uani 1 1 d . . . O1 O 0.1661(5) 0.1185(2) 0.4321(2) 0.1009(11) Uani 1 1 d . . . C2 C 0.3295(4) 0.3107(3) 0.3167(2) 0.0468(8) Uani 1 1 d . . . O2 O 0.4191(3) 0.3696(2) 0.36117(18) 0.0719(7) Uani 1 1 d . . . C3 C 0.3814(5) 0.1436(2) 0.2438(2) 0.0476(8) Uani 1 1 d . . . O3 O 0.5065(3) 0.0976(2) 0.24743(17) 0.0712(7) Uani 1 1 d . . . C4 C -0.1479(4) 0.1630(2) 0.1242(2) 0.0410(7) Uani 1 1 d . . . C5 C -0.2759(4) 0.0430(3) 0.0185(2) 0.0450(8) Uani 1 1 d . . . C11 C -0.0972(4) 0.3755(2) 0.2689(2) 0.0464(8) Uani 1 1 d . . . H11 H -0.0306 0.4176 0.3164 0.056 Uiso 1 1 calc R . . C12 C -0.2732(4) 0.3905(2) 0.2234(2) 0.0524(8) Uani 1 1 d . . . H12 H -0.3447 0.4428 0.2338 0.063 Uiso 1 1 calc R . . C13 C -0.3185(4) 0.3124(3) 0.1603(2) 0.0512(8) Uani 1 1 d . . . H13 H -0.4287 0.3011 0.1189 0.061 Uiso 1 1 calc R . . C14 C 0.1946(4) 0.3823(2) 0.0856(2) 0.0534(8) Uani 1 1 d . . . H14 H 0.1738 0.4336 0.1269 0.064 Uiso 1 1 calc R . . C15 C 0.2184(5) 0.3946(3) -0.0113(2) 0.0641(10) Uani 1 1 d . . . H15 H 0.2169 0.4533 -0.0469 0.077 Uiso 1 1 calc R . . C16 C 0.2446(4) 0.3017(3) -0.0432(2) 0.0556(9) Uani 1 1 d . . . H16 H 0.2641 0.2845 -0.1060 0.067 Uiso 1 1 calc 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 0.0466(3) 0.0357(3) 0.0369(3) -0.00347(19) 0.0076(2) 0.0024(2) N1 0.0446(14) 0.0358(15) 0.0416(13) -0.0059(11) 0.0118(11) -0.0031(12) N2 0.0405(14) 0.0386(15) 0.0442(13) -0.0089(12) 0.0121(11) -0.0042(12) N3 0.0461(15) 0.0326(15) 0.0527(15) -0.0094(11) 0.0147(12) 0.0018(12) N4 0.0441(13) 0.0354(16) 0.0364(13) -0.0059(11) 0.0066(10) -0.0018(11) N5 0.0541(15) 0.0365(15) 0.0401(13) -0.0080(12) 0.0099(11) -0.0038(12) N6 0.0462(15) 0.0475(18) 0.0597(16) -0.0168(14) 0.0109(13) -0.0067(13) N7 0.0612(17) 0.0441(19) 0.0651(17) -0.0161(15) 0.0065(13) -0.0074(14) C1 0.078(2) 0.048(2) 0.053(2) 0.0015(18) 0.0231(17) 0.0143(19) O1 0.162(3) 0.083(2) 0.0723(18) 0.0314(17) 0.0569(19) 0.033(2) C2 0.0446(18) 0.053(2) 0.0431(18) -0.0077(16) 0.0101(15) 0.0106(16) O2 0.0624(15) 0.0775(19) 0.0727(16) -0.0355(15) 0.0078(12) -0.0130(14) C3 0.062(2) 0.044(2) 0.0351(16) -0.0058(14) 0.0049(14) 0.0052(17) O3 0.0730(16) 0.0722(18) 0.0626(15) -0.0113(13) 0.0022(12) 0.0328(14) C4 0.0466(18) 0.0366(19) 0.0428(16) -0.0061(14) 0.0165(14) -0.0092(15) C5 0.0398(17) 0.048(2) 0.0449(17) -0.0038(17) 0.0050(13) -0.0076(15) C11 0.0548(19) 0.0361(19) 0.0513(18) -0.0098(15) 0.0180(15) -0.0033(16) C12 0.054(2) 0.042(2) 0.065(2) -0.0091(17) 0.0212(17) 0.0097(16) C13 0.0379(17) 0.055(2) 0.0616(19) -0.0068(17) 0.0139(14) -0.0006(16) C14 0.076(2) 0.033(2) 0.0523(19) -0.0024(15) 0.0157(16) 0.0040(17) C15 0.094(3) 0.046(2) 0.052(2) 0.0107(18) 0.0155(18) -0.002(2) C16 0.069(2) 0.058(3) 0.0400(18) -0.0014(16) 0.0119(15) -0.0061(18) _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 C1 1.795(4) . ? Mn1 C3 1.798(4) . ? Mn1 C2 1.803(4) . ? Mn1 N1 2.026(2) . ? Mn1 N3 2.042(2) . ? Mn1 N4 2.070(2) . ? N1 C11 1.315(4) . ? N1 N2 1.367(3) . ? N2 C13 1.337(4) . ? N2 C4 1.419(4) . ? N3 C4 1.286(4) . ? N4 C14 1.320(4) . ? N4 N5 1.344(3) . ? N5 C16 1.325(4) . ? N6 C5 1.327(4) . ? N6 C4 1.332(4) . ? N7 C5 1.139(4) . ? C1 O1 1.129(4) . ? C2 O2 1.142(4) . ? C3 O3 1.147(4) . ? C11 C12 1.388(4) . ? C12 C13 1.359(4) . ? C14 C15 1.381(5) . ? C15 C16 1.359(5) . ? 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 C1 Mn1 C3 88.41(14) . . ? C1 Mn1 C2 90.06(15) . . ? C3 Mn1 C2 89.61(13) . . ? C1 Mn1 N1 92.89(13) . . ? C3 Mn1 N1 175.01(11) . . ? C2 Mn1 N1 95.21(11) . . ? C1 Mn1 N3 94.24(13) . . ? C3 Mn1 N3 97.51(12) . . ? C2 Mn1 N3 171.78(12) . . ? N1 Mn1 N3 77.59(9) . . ? C1 Mn1 N4 178.76(13) . . ? C3 Mn1 N4 92.63(12) . . ? C2 Mn1 N4 90.62(11) . . ? N1 Mn1 N4 86.01(9) . . ? N3 Mn1 N4 84.96(9) . . ? C11 N1 N2 105.4(2) . . ? C11 N1 Mn1 141.0(2) . . ? N2 N1 Mn1 113.32(17) . . ? C13 N2 N1 110.4(2) . . ? C13 N2 C4 132.8(3) . . ? N1 N2 C4 116.7(2) . . ? C4 N3 Mn1 117.8(2) . . ? C14 N4 N5 104.9(2) . . ? C14 N4 Mn1 132.0(2) . . ? N5 N4 Mn1 123.00(18) . . ? C16 N5 N4 111.5(3) . . ? C5 N6 C4 115.8(3) . . ? O1 C1 Mn1 177.8(3) . . ? O2 C2 Mn1 179.0(3) . . ? O3 C3 Mn1 177.0(3) . . ? N3 C4 N6 133.9(3) . . ? N3 C4 N2 113.6(2) . . ? N6 C4 N2 112.5(3) . . ? N7 C5 N6 175.7(3) . . ? N1 C11 C12 111.1(3) . . ? C13 C12 C11 105.2(3) . . ? N2 C13 C12 107.8(3) . . ? N4 C14 C15 111.2(3) . . ? C16 C15 C14 104.7(3) . . ? N5 C16 C15 107.6(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.399 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.056 #===END data_Compound_2b_ma409am _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H24 Mn N7 O4' _chemical_formula_weight 469.39 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.733(7) _cell_length_b 10.655(8) _cell_length_c 13.642(11) _cell_angle_alpha 98.909(13) _cell_angle_beta 96.890(13) _cell_angle_gamma 107.068(13) _cell_volume 1180.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1009 _cell_measurement_theta_min 2.676 _cell_measurement_theta_max 22.817 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.368812 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 11278 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.59 _reflns_number_total 5682 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0389P)^2^+1.3085P] 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 5682 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _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 0.62589(7) 0.89335(5) 0.68426(4) 0.04459(17) Uani 1 1 d . . . N1 N 0.6406(4) 0.7061(3) 0.6952(2) 0.0455(7) Uani 1 1 d . . . N2 N 0.5931(4) 0.6640(3) 0.7812(2) 0.0445(7) Uani 1 1 d . . . N3 N 0.5339(3) 0.8591(3) 0.8110(2) 0.0431(6) Uani 1 1 d . . . H3 H 0.4914 0.9141 0.8411 0.052 Uiso 1 1 calc R . . N4 N 0.8524(4) 0.9811(3) 0.7826(2) 0.0485(7) Uani 1 1 d . . . N5 N 0.8587(4) 1.0673(3) 0.8699(2) 0.0520(7) Uani 1 1 d . . . H5 H 0.7746 1.0832 0.8889 0.062 Uiso 1 1 calc R . . N6 N 0.5050(4) 0.7147(3) 0.9322(2) 0.0520(7) Uani 1 1 d . . . N7 N 0.4103(5) 0.8572(3) 1.0558(3) 0.0658(9) Uani 1 1 d . . . C1 C 0.4306(6) 0.8159(4) 0.6011(3) 0.0578(10) Uani 1 1 d . . . O1 O 0.3102(5) 0.7678(4) 0.5458(3) 0.0947(11) Uani 1 1 d . . . C2 C 0.7201(6) 0.9208(4) 0.5745(3) 0.0628(10) Uani 1 1 d . . . O2 O 0.7726(5) 0.9424(4) 0.5032(3) 0.1045(13) Uani 1 1 d . . . C3 C 0.5924(5) 1.0549(4) 0.6883(3) 0.0542(9) Uani 1 1 d . . . O3 O 0.5632(5) 1.1521(3) 0.6867(3) 0.0871(10) Uani 1 1 d . . . C5 C 0.4537(5) 0.7941(3) 0.9953(3) 0.0480(8) Uani 1 1 d . . . C4 C 0.5395(4) 0.7542(3) 0.8464(2) 0.0415(7) Uani 1 1 d . . . C11 C 0.6678(5) 0.6012(4) 0.6412(3) 0.0554(9) Uani 1 1 d . . . C12 C 0.6379(6) 0.4941(4) 0.6918(3) 0.0632(11) Uani 1 1 d . . . H12 H 0.6484 0.4106 0.6692 0.076 Uiso 1 1 calc R . . C13 C 0.5907(5) 0.5336(3) 0.7799(3) 0.0553(9) Uani 1 1 d . . . C14 C 0.7197(7) 0.6046(5) 0.5403(3) 0.0801(14) Uani 1 1 d . . . H14A H 0.6449 0.6312 0.4971 0.120 Uiso 1 1 calc R . . H14B H 0.7206 0.5172 0.5104 0.120 Uiso 1 1 calc R . . H14C H 0.8269 0.6677 0.5487 0.120 Uiso 1 1 calc R . . C15 C 0.5457(7) 0.4557(4) 0.8608(3) 0.0800(15) Uani 1 1 d . . . H15A H 0.5482 0.3660 0.8403 0.120 Uiso 1 1 calc R . . H15B H 0.4382 0.4528 0.8717 0.120 Uiso 1 1 calc R . . H15C H 0.6219 0.4984 0.9222 0.120 Uiso 1 1 calc R . . C16 C 1.0083(5) 0.9852(4) 0.7821(3) 0.0616(10) Uani 1 1 d . . . C17 C 1.1085(6) 1.0719(5) 0.8678(4) 0.0783(13) Uani 1 1 d . . . H17 H 1.2203 1.0910 0.8850 0.094 Uiso 1 1 calc R . . C18 C 1.0108(6) 1.1243(4) 0.9224(3) 0.0665(11) Uani 1 1 d . . . C19 C 1.0578(6) 0.9030(5) 0.6990(4) 0.0902(16) Uani 1 1 d . . . H19A H 0.9875 0.8118 0.6861 0.135 Uiso 1 1 calc R . . H19B H 1.1682 0.9059 0.7191 0.135 Uiso 1 1 calc R . . H19C H 1.0491 0.9388 0.6390 0.135 Uiso 1 1 calc R . . C20 C 1.0444(7) 1.2227(5) 1.0203(4) 0.0917(16) Uani 1 1 d . . . H20A H 0.9452 1.2381 1.0336 0.137 Uiso 1 1 calc R . . H20B H 1.1222 1.3057 1.0158 0.137 Uiso 1 1 calc R . . H20C H 1.0872 1.1871 1.0739 0.137 Uiso 1 1 calc R . . O90 O 0.070(2) 0.385(2) 0.6587(11) 0.408(11) Uani 1 1 d . . . C91 C 0.1270(18) 0.5189(16) 0.6872(12) 0.217(6) Uani 1 1 d . . . H91A H 0.0802 0.5600 0.6379 0.261 Uiso 1 1 calc R . . H91B H 0.2444 0.5504 0.6928 0.261 Uiso 1 1 calc R . . C92 C 0.0841(13) 0.5518(13) 0.7789(13) 0.187(5) Uani 1 1 d . . . H92A H -0.0039 0.5898 0.7715 0.224 Uiso 1 1 calc R . . H92B H 0.1761 0.6167 0.8253 0.224 Uiso 1 1 calc R . . C93 C 0.035(3) 0.434(3) 0.8136(14) 0.280(12) Uani 1 1 d . . . H93A H 0.1164 0.4332 0.8683 0.336 Uiso 1 1 calc R . . H93B H -0.0669 0.4244 0.8379 0.336 Uiso 1 1 calc R . . C94 C 0.017(3) 0.3355(14) 0.735(2) 0.304(14) Uani 1 1 d . . . H94A H 0.0773 0.2772 0.7544 0.365 Uiso 1 1 calc R . . H94B H -0.0969 0.2825 0.7154 0.365 Uiso 1 1 calc 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 0.0616(4) 0.0335(3) 0.0419(3) 0.0071(2) 0.0127(2) 0.0186(2) N1 0.0626(19) 0.0371(15) 0.0411(14) 0.0054(12) 0.0161(13) 0.0208(14) N2 0.0620(18) 0.0349(14) 0.0416(14) 0.0075(11) 0.0164(13) 0.0202(13) N3 0.0550(17) 0.0308(14) 0.0476(15) 0.0047(11) 0.0159(13) 0.0187(13) N4 0.0577(19) 0.0422(16) 0.0497(16) 0.0078(13) 0.0163(14) 0.0200(14) N5 0.0547(19) 0.0488(17) 0.0504(17) 0.0034(14) 0.0085(14) 0.0171(15) N6 0.075(2) 0.0428(16) 0.0482(16) 0.0126(13) 0.0242(15) 0.0266(15) N7 0.094(3) 0.0526(19) 0.063(2) 0.0112(16) 0.0369(19) 0.0326(19) C1 0.082(3) 0.0391(19) 0.052(2) 0.0023(16) 0.010(2) 0.023(2) O1 0.091(3) 0.084(2) 0.088(2) -0.0036(19) -0.020(2) 0.021(2) C2 0.085(3) 0.056(2) 0.055(2) 0.0173(19) 0.018(2) 0.028(2) O2 0.147(3) 0.119(3) 0.075(2) 0.046(2) 0.059(2) 0.053(3) C3 0.073(3) 0.0387(19) 0.051(2) 0.0084(16) 0.0063(18) 0.0195(18) O3 0.128(3) 0.0500(17) 0.096(2) 0.0213(16) 0.014(2) 0.0463(19) C5 0.062(2) 0.0374(18) 0.0486(19) 0.0137(15) 0.0187(17) 0.0163(17) C4 0.0490(19) 0.0323(16) 0.0431(17) 0.0024(13) 0.0111(15) 0.0143(14) C11 0.078(3) 0.0426(19) 0.052(2) 0.0035(16) 0.0227(19) 0.0271(19) C12 0.098(3) 0.0374(19) 0.065(2) 0.0042(17) 0.025(2) 0.036(2) C13 0.081(3) 0.0368(18) 0.055(2) 0.0093(16) 0.0178(19) 0.0257(19) C14 0.126(4) 0.064(3) 0.061(3) 0.005(2) 0.042(3) 0.041(3) C15 0.140(5) 0.041(2) 0.078(3) 0.023(2) 0.041(3) 0.042(3) C16 0.056(2) 0.058(2) 0.075(3) 0.013(2) 0.016(2) 0.021(2) C17 0.055(3) 0.081(3) 0.096(4) 0.014(3) 0.005(2) 0.023(2) C18 0.068(3) 0.058(2) 0.065(2) 0.006(2) -0.002(2) 0.015(2) C19 0.079(3) 0.096(4) 0.109(4) 0.011(3) 0.040(3) 0.044(3) C20 0.096(4) 0.082(3) 0.072(3) -0.010(3) -0.014(3) 0.016(3) O90 0.50(2) 0.34(2) 0.303(15) -0.043(15) 0.245(16) -0.004(18) C91 0.283(16) 0.154(10) 0.194(12) 0.071(10) 0.094(12) -0.001(11) C92 0.149(9) 0.174(11) 0.190(11) -0.056(9) -0.020(8) 0.046(8) C93 0.31(2) 0.40(3) 0.27(2) 0.25(2) 0.149(18) 0.20(2) C94 0.32(2) 0.113(9) 0.52(4) 0.135(17) 0.16(3) 0.058(12) _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 C1 1.815(5) . ? Mn1 C2 1.816(4) . ? Mn1 C3 1.822(4) . ? Mn1 N3 2.031(3) . ? Mn1 N1 2.063(3) . ? Mn1 N4 2.116(3) . ? N1 C11 1.338(4) . ? N1 N2 1.386(4) . ? N2 C13 1.380(4) . ? N2 C4 1.426(4) . ? N3 C4 1.296(4) . ? N4 C16 1.350(5) . ? N4 N5 1.372(4) . ? N5 C18 1.345(5) . ? N6 C5 1.322(4) . ? N6 C4 1.342(4) . ? N7 C5 1.153(4) . ? C1 O1 1.145(5) . ? C2 O2 1.150(5) . ? C3 O3 1.140(4) . ? C11 C12 1.400(5) . ? C11 C14 1.503(5) . ? C12 C13 1.362(5) . ? C13 C15 1.504(5) . ? C16 C17 1.390(6) . ? C16 C19 1.507(6) . ? C17 C18 1.378(6) . ? C18 C20 1.503(6) . ? O90 C94 1.32(2) . ? O90 C91 1.337(17) . ? C91 C92 1.372(14) . ? C92 C93 1.376(17) . ? C93 C94 1.34(2) . ? 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 C1 Mn1 C2 88.9(2) . . ? C1 Mn1 C3 88.49(17) . . ? C2 Mn1 C3 87.77(17) . . ? C1 Mn1 N3 94.15(16) . . ? C2 Mn1 N3 176.05(16) . . ? C3 Mn1 N3 94.86(14) . . ? C1 Mn1 N1 89.88(15) . . ? C2 Mn1 N1 100.65(15) . . ? C3 Mn1 N1 171.38(14) . . ? N3 Mn1 N1 76.82(10) . . ? C1 Mn1 N4 179.05(15) . . ? C2 Mn1 N4 91.84(17) . . ? C3 Mn1 N4 92.18(15) . . ? N3 Mn1 N4 85.13(12) . . ? N1 Mn1 N4 89.36(12) . . ? C11 N1 N2 105.1(3) . . ? C11 N1 Mn1 140.7(2) . . ? N2 N1 Mn1 113.80(18) . . ? C13 N2 N1 111.2(3) . . ? C13 N2 C4 132.6(3) . . ? N1 N2 C4 115.8(2) . . ? C4 N3 Mn1 119.8(2) . . ? C16 N4 N5 104.5(3) . . ? C16 N4 Mn1 137.4(3) . . ? N5 N4 Mn1 118.0(2) . . ? C18 N5 N4 112.5(3) . . ? C5 N6 C4 116.9(3) . . ? O1 C1 Mn1 177.6(4) . . ? O2 C2 Mn1 175.5(4) . . ? O3 C3 Mn1 175.9(4) . . ? N7 C5 N6 174.7(4) . . ? N3 C4 N6 132.4(3) . . ? N3 C4 N2 113.3(3) . . ? N6 C4 N2 114.3(3) . . ? N1 C11 C12 110.1(3) . . ? N1 C11 C14 122.3(3) . . ? C12 C11 C14 127.6(3) . . ? C13 C12 C11 108.0(3) . . ? C12 C13 N2 105.5(3) . . ? C12 C13 C15 128.7(3) . . ? N2 C13 C15 125.8(3) . . ? N4 C16 C17 110.1(4) . . ? N4 C16 C19 122.5(4) . . ? C17 C16 C19 127.3(4) . . ? C18 C17 C16 107.1(4) . . ? N5 C18 C17 105.8(4) . . ? N5 C18 C20 121.0(4) . . ? C17 C18 C20 133.2(5) . . ? C94 O90 C91 108.1(14) . . ? O90 C91 C92 107.5(11) . . ? C91 C92 C93 106.1(12) . . ? C94 C93 C92 106.1(14) . . ? O90 C94 C93 110.3(14) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.59 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.609 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.059 #===END data_Compound_3_ma369bm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Br Mn2 N11 O6' _chemical_formula_weight 696.23 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' 'Br' 'Br' -0.2901 2.4595 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 16.232(7) _cell_length_b 9.622(4) _cell_length_c 27.200(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.354(7) _cell_angle_gamma 90.00 _cell_volume 4213(3) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 959 _cell_measurement_theta_min 2.765 _cell_measurement_theta_max 22.475 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 2.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.748043 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26351 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 23.29 _reflns_number_total 6052 _reflns_number_gt 4546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0607P)^2^+23.1651P] 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 6052 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.1763 _refine_ls_wR_factor_gt 0.1656 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 0.15846(8) 0.08129(18) 0.69101(5) 0.0574(4) Uani 1 1 d . . . Mn2 Mn -0.22531(8) 0.34801(15) 0.57036(5) 0.0475(4) Uani 1 1 d . . . Mn3 Mn 0.55126(8) 0.90153(13) 0.62827(4) 0.0357(3) Uani 1 1 d . . . Br1 Br -0.04473(6) 0.00827(10) 0.56905(4) 0.0513(3) Uani 1 1 d . . . Br2 Br 0.5000 0.61941(14) 0.7500 0.0647(5) Uani 1 2 d S . . N1 N 0.1903(5) 0.2779(10) 0.7117(3) 0.065(2) Uani 1 1 d . . . N2 N 0.1292(5) 0.3714(10) 0.7008(3) 0.064(2) Uani 1 1 d . . . N3 N 0.0545(4) 0.1901(9) 0.6672(3) 0.050(2) Uani 1 1 d . . . H3 H 0.0116 0.1480 0.6523 0.060 Uiso 1 1 calc R . . N4 N -0.0017(5) 0.4259(8) 0.6626(3) 0.060(2) Uani 1 1 d . . . N5 N -0.1153(5) 0.5376(8) 0.6263(3) 0.055(2) Uani 1 1 d . . . N6 N -0.1882(5) 0.5379(8) 0.5954(3) 0.056(2) Uani 1 1 d . . . N7 N -0.1155(4) 0.3068(8) 0.6134(3) 0.0448(18) Uani 1 1 d . . . H7 H -0.0973 0.2231 0.6173 0.054 Uiso 1 1 calc R . . N8 N 0.1963(4) 0.1320(9) 0.6232(3) 0.054(2) Uani 1 1 d . . . N9 N 0.1505(5) 0.1073(9) 0.5792(3) 0.058(2) Uani 1 1 d . . . H9 H 0.1012 0.0726 0.5759 0.070 Uiso 1 1 calc R . . N10 N -0.1522(5) 0.3805(8) 0.5134(3) 0.054(2) Uani 1 1 d . . . N11 N -0.0969(5) 0.2896(9) 0.5006(3) 0.055(2) Uani 1 1 d . . . H11 H -0.0852 0.2123 0.5157 0.066 Uiso 1 1 calc R . . N21 N 0.5094(4) 1.1024(7) 0.6223(2) 0.0365(16) Uani 1 1 d . . . N22 N 0.4985(4) 1.1592(7) 0.6666(2) 0.0331(16) Uani 1 1 d . . . N23 N 0.5300(4) 0.9474(7) 0.6984(2) 0.0325(15) Uani 1 1 d . . . H23 H 0.5351 0.8843 0.7210 0.039 Uiso 1 1 calc R . . N24 N 0.5000 1.1399(9) 0.7500 0.036(2) Uani 1 2 d S . . N25 N 0.4303(4) 0.8390(7) 0.6155(2) 0.0406(17) Uani 1 1 d . . . N26 N 0.3974(5) 0.7454(8) 0.6446(3) 0.054(2) Uani 1 1 d . . . H26 H 0.4247 0.7071 0.6702 0.065 Uiso 1 1 calc R . . C1 C 0.1226(7) 0.0438(14) 0.7492(5) 0.078(4) Uani 1 1 d . . . O1 O 0.0982(5) 0.0197(13) 0.7861(3) 0.116(4) Uani 1 1 d . . . C2 C 0.1214(6) -0.0856(14) 0.6706(4) 0.063(3) Uani 1 1 d . . . O2 O 0.1011(6) -0.1978(10) 0.6596(4) 0.100(3) Uani 1 1 d . . . C3 C 0.2582(7) 0.0025(14) 0.7122(4) 0.075(3) Uani 1 1 d . . . O3 O 0.3195(5) -0.0511(12) 0.7251(3) 0.116(4) Uani 1 1 d . . . C4 C -0.2818(6) 0.3213(9) 0.6215(4) 0.050(2) Uani 1 1 d . . . O4 O -0.3201(5) 0.3014(8) 0.6537(3) 0.072(2) Uani 1 1 d . . . C5 C -0.2506(6) 0.1712(13) 0.5512(3) 0.052(3) Uani 1 1 d . . . O5 O -0.2713(5) 0.0631(9) 0.5389(3) 0.073(2) Uani 1 1 d . . . C6 C -0.3188(7) 0.4099(13) 0.5329(4) 0.074(3) Uani 1 1 d . . . O6 O -0.3780(5) 0.4453(12) 0.5098(4) 0.121(4) Uani 1 1 d . . . C7 C 0.6561(6) 0.9589(9) 0.6432(3) 0.045(2) Uani 1 1 d . . . O7 O 0.7236(4) 0.9918(8) 0.6538(3) 0.072(2) Uani 1 1 d . . . C8 C 0.5870(6) 0.7237(12) 0.6393(4) 0.056(3) Uani 1 1 d . . . O8 O 0.6138(5) 0.6140(8) 0.6432(3) 0.089(3) Uani 1 1 d . . . C9 C 0.5649(6) 0.8812(11) 0.5640(4) 0.057(3) Uani 1 1 d . . . O9 O 0.5756(5) 0.8633(11) 0.5245(3) 0.097(3) Uani 1 1 d . . . C11 C 0.2542(8) 0.3518(16) 0.7347(4) 0.086(4) Uani 1 1 d . . . H11A H 0.3058 0.3151 0.7469 0.103 Uiso 1 1 calc R . . C12 C 0.2325(9) 0.4889(18) 0.7378(5) 0.109(5) Uani 1 1 d . . . H12 H 0.2658 0.5612 0.7516 0.131 Uiso 1 1 calc R . . C13 C 0.1534(9) 0.4971(15) 0.7166(5) 0.102(5) Uani 1 1 d . . . H13A H 0.1210 0.5772 0.7135 0.123 Uiso 1 1 calc R . . C14 C 0.0523(6) 0.3227(11) 0.6742(3) 0.051(2) Uani 1 1 d . . . C15 C -0.0742(5) 0.4095(10) 0.6345(3) 0.045(2) Uani 1 1 d . . . C16 C -0.0939(7) 0.6667(12) 0.6423(6) 0.087(4) Uani 1 1 d . . . H16 H -0.0462 0.6926 0.6629 0.105 Uiso 1 1 calc R . . C17 C -0.1565(8) 0.7519(12) 0.6220(6) 0.097(5) Uani 1 1 d . . . H17 H -0.1607 0.8472 0.6270 0.116 Uiso 1 1 calc R . . C18 C -0.2118(8) 0.6703(12) 0.5930(5) 0.074(3) Uani 1 1 d . . . H18 H -0.2596 0.7030 0.5741 0.089 Uiso 1 1 calc R . . C21 C 0.2667(6) 0.1828(12) 0.6112(4) 0.061(3) Uani 1 1 d . . . H21 H 0.3115 0.2088 0.6342 0.074 Uiso 1 1 calc R . . C22 C 0.2658(6) 0.1926(12) 0.5603(4) 0.063(3) Uani 1 1 d . . . H22 H 0.3074 0.2256 0.5429 0.076 Uiso 1 1 calc R . . C23 C 0.1899(6) 0.1425(10) 0.5421(4) 0.053(2) Uani 1 1 d . . . H23A H 0.1694 0.1346 0.5087 0.064 Uiso 1 1 calc R . . C24 C -0.1539(7) 0.4796(12) 0.4802(4) 0.073(3) Uani 1 1 d . . . H24 H -0.1885 0.5570 0.4790 0.088 Uiso 1 1 calc R . . C25 C -0.0980(8) 0.4542(13) 0.4472(4) 0.079(4) Uani 1 1 d . . . H25 H -0.0876 0.5095 0.4207 0.095 Uiso 1 1 calc R . . C26 C -0.0617(7) 0.3322(13) 0.4615(4) 0.071(3) Uani 1 1 d . . . H26A H -0.0203 0.2868 0.4469 0.085 Uiso 1 1 calc R . . C31 C 0.4980(6) 1.2056(10) 0.5899(3) 0.049(2) Uani 1 1 d . . . H31 H 0.5028 1.1974 0.5563 0.058 Uiso 1 1 calc R . . C32 C 0.4777(6) 1.3276(10) 0.6127(3) 0.049(2) Uani 1 1 d . . . H32 H 0.4650 1.4131 0.5977 0.059 Uiso 1 1 calc R . . C33 C 0.4804(5) 1.2965(9) 0.6613(3) 0.041(2) Uani 1 1 d . . . H33 H 0.4714 1.3579 0.6865 0.049 Uiso 1 1 calc R . . C34 C 0.5090(4) 1.0716(8) 0.7086(3) 0.0274(18) Uani 1 1 d . . . C35 C 0.3667(6) 0.8641(11) 0.5803(3) 0.060(3) Uani 1 1 d . . . H35 H 0.3697 0.9254 0.5542 0.072 Uiso 1 1 calc R . . C36 C 0.2964(7) 0.7905(14) 0.5867(4) 0.078(4) Uani 1 1 d . . . H36 H 0.2457 0.7898 0.5664 0.094 Uiso 1 1 calc R . . C37 C 0.3180(6) 0.7195(13) 0.6290(4) 0.071(3) Uani 1 1 d . . . H37 H 0.2833 0.6621 0.6446 0.086 Uiso 1 1 calc 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 0.0372(8) 0.0835(12) 0.0489(9) 0.0048(8) -0.0046(6) 0.0058(8) Mn2 0.0406(8) 0.0474(9) 0.0537(9) 0.0067(7) 0.0034(6) 0.0085(7) Mn3 0.0393(7) 0.0412(8) 0.0272(7) -0.0059(6) 0.0066(5) -0.0019(6) Br1 0.0450(5) 0.0482(6) 0.0584(6) -0.0019(5) -0.0019(4) 0.0016(5) Br2 0.1147(13) 0.0325(8) 0.0446(8) 0.000 0.0008(8) 0.000 N1 0.036(5) 0.107(7) 0.046(5) -0.002(5) -0.011(4) -0.018(5) N2 0.046(5) 0.084(7) 0.055(5) -0.001(5) -0.017(4) -0.017(5) N3 0.033(4) 0.058(6) 0.056(5) -0.005(4) -0.006(3) 0.002(4) N4 0.057(5) 0.044(5) 0.074(6) -0.010(4) -0.005(4) -0.009(4) N5 0.043(5) 0.039(5) 0.086(6) -0.005(4) 0.016(4) -0.008(4) N6 0.048(5) 0.045(5) 0.079(6) 0.002(4) 0.023(4) 0.003(4) N7 0.043(4) 0.035(4) 0.054(5) 0.002(4) -0.003(4) 0.001(4) N8 0.026(4) 0.081(6) 0.050(5) -0.004(4) -0.008(3) 0.002(4) N9 0.045(5) 0.071(6) 0.055(5) 0.004(4) -0.003(4) -0.009(4) N10 0.057(5) 0.054(5) 0.051(5) 0.011(4) 0.011(4) 0.009(4) N11 0.049(5) 0.053(5) 0.064(5) 0.006(4) 0.006(4) 0.014(4) N21 0.030(4) 0.049(4) 0.028(4) 0.007(3) -0.003(3) -0.009(3) N22 0.037(4) 0.037(4) 0.025(4) 0.001(3) 0.003(3) -0.002(3) N23 0.046(4) 0.027(4) 0.025(3) 0.004(3) 0.008(3) 0.007(3) N24 0.059(6) 0.019(5) 0.034(6) 0.000 0.017(5) 0.000 N25 0.045(4) 0.048(5) 0.028(4) 0.002(3) 0.001(3) 0.000(4) N26 0.044(5) 0.068(6) 0.047(5) -0.001(4) -0.006(4) -0.019(4) C1 0.055(7) 0.116(11) 0.061(8) 0.018(7) -0.007(6) 0.018(7) O1 0.084(6) 0.198(11) 0.070(6) 0.047(7) 0.021(5) 0.053(7) C2 0.042(6) 0.074(8) 0.067(7) 0.019(6) -0.008(5) 0.012(6) O2 0.095(7) 0.068(6) 0.131(8) 0.022(6) -0.009(6) 0.008(5) C3 0.054(7) 0.119(10) 0.052(6) -0.011(7) 0.002(5) 0.011(7) O3 0.059(5) 0.186(11) 0.094(7) -0.021(6) -0.023(5) 0.047(6) C4 0.044(6) 0.038(5) 0.065(7) 0.000(5) -0.002(5) 0.011(4) O4 0.066(5) 0.083(6) 0.071(5) -0.011(4) 0.024(4) -0.008(4) C5 0.043(5) 0.076(8) 0.039(5) 0.003(5) 0.007(4) -0.002(5) O5 0.074(5) 0.070(5) 0.073(5) -0.019(4) 0.006(4) -0.022(4) C6 0.055(7) 0.089(9) 0.078(8) 0.011(7) 0.005(6) 0.018(7) O6 0.062(5) 0.161(10) 0.132(8) 0.035(7) -0.024(5) 0.041(6) C7 0.054(6) 0.045(6) 0.039(5) -0.001(4) 0.017(4) 0.008(5) O7 0.042(4) 0.082(5) 0.091(6) -0.006(4) 0.005(4) -0.004(4) C8 0.056(6) 0.058(7) 0.058(6) -0.009(5) 0.025(5) -0.001(6) O8 0.087(6) 0.044(5) 0.145(8) -0.001(5) 0.047(5) 0.018(4) C9 0.048(6) 0.066(7) 0.055(7) -0.018(5) 0.004(5) -0.017(5) O9 0.103(6) 0.166(9) 0.026(4) -0.035(5) 0.023(4) -0.031(6) C11 0.061(8) 0.112(12) 0.077(8) -0.004(8) -0.016(6) -0.027(8) C12 0.097(11) 0.113(13) 0.102(11) -0.008(9) -0.049(8) -0.039(10) C13 0.098(10) 0.085(10) 0.111(11) -0.015(8) -0.038(8) -0.017(8) C14 0.051(6) 0.059(7) 0.043(6) -0.003(5) 0.004(4) -0.011(5) C15 0.038(5) 0.040(6) 0.057(6) 0.002(5) 0.009(4) 0.005(5) C16 0.059(7) 0.050(7) 0.159(13) -0.018(8) 0.039(8) -0.004(6) C17 0.073(8) 0.034(7) 0.196(15) -0.014(8) 0.066(10) -0.004(7) C18 0.075(8) 0.045(7) 0.108(10) 0.001(6) 0.036(7) 0.020(7) C21 0.039(6) 0.092(8) 0.052(6) -0.007(6) 0.005(5) -0.008(5) C22 0.049(6) 0.080(8) 0.062(7) 0.009(6) 0.017(5) 0.010(6) C23 0.049(6) 0.061(7) 0.046(6) 0.003(5) -0.004(5) 0.009(5) C24 0.081(8) 0.065(8) 0.077(8) 0.027(6) 0.025(7) 0.013(6) C25 0.104(10) 0.069(8) 0.069(8) 0.032(6) 0.023(7) -0.004(7) C26 0.068(7) 0.077(9) 0.071(8) 0.000(6) 0.027(6) -0.009(6) C31 0.061(6) 0.057(6) 0.026(5) 0.012(5) -0.003(4) -0.008(5) C32 0.052(6) 0.044(6) 0.049(6) 0.021(5) -0.002(4) 0.001(5) C33 0.044(5) 0.028(5) 0.051(6) 0.003(4) 0.003(4) 0.000(4) C34 0.026(4) 0.034(5) 0.022(4) 0.002(4) 0.001(3) -0.004(4) C35 0.065(7) 0.065(7) 0.044(6) 0.005(5) -0.013(5) -0.013(6) C36 0.047(6) 0.112(10) 0.070(8) -0.007(7) -0.018(6) -0.031(7) C37 0.053(7) 0.088(9) 0.070(8) 0.004(7) -0.001(6) -0.032(6) _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 C2 1.779(14) . ? Mn1 C1 1.791(13) . ? Mn1 C3 1.814(12) . ? Mn1 N3 2.021(7) . ? Mn1 N1 2.022(10) . ? Mn1 N8 2.077(8) . ? Mn2 C4 1.780(12) . ? Mn2 C5 1.811(12) . ? Mn2 C6 1.817(12) . ? Mn2 N6 2.015(8) . ? Mn2 N7 2.042(7) . ? Mn2 N10 2.091(8) . ? Mn3 C7 1.786(11) . ? Mn3 C9 1.800(11) . ? Mn3 C8 1.820(12) . ? Mn3 N23 2.029(6) . ? Mn3 N25 2.041(7) . ? Mn3 N21 2.048(7) . ? N1 N2 1.344(12) . ? N1 C11 1.345(13) . ? N2 C13 1.327(15) . ? N2 C14 1.438(12) . ? N3 C14 1.291(12) . ? N4 C15 1.327(11) . ? N4 C14 1.336(13) . ? N5 C16 1.347(13) . ? N5 N6 1.360(11) . ? N5 C15 1.406(11) . ? N6 C18 1.330(12) . ? N7 C15 1.288(11) . ? N8 C21 1.321(12) . ? N8 N9 1.347(10) . ? N9 C23 1.308(12) . ? N10 C24 1.312(12) . ? N10 N11 1.332(10) . ? N11 C26 1.335(12) . ? N21 C31 1.325(10) . ? N21 N22 1.357(9) . ? N22 C33 1.358(10) . ? N22 C34 1.412(10) . ? N23 C34 1.283(10) . ? N24 C34 1.328(9) . ? N24 C34 1.328(9) 2_656 ? N25 C35 1.336(11) . ? N25 N26 1.353(10) . ? N26 C37 1.327(12) . ? C1 O1 1.151(13) . ? C2 O2 1.157(13) . ? C3 O3 1.136(13) . ? C4 O4 1.153(11) . ? C5 O5 1.132(12) . ? C6 O6 1.131(12) . ? C7 O7 1.141(11) . ? C8 O8 1.141(12) . ? C9 O9 1.124(11) . ? C11 C12 1.371(19) . ? C12 C13 1.342(18) . ? C16 C17 1.366(17) . ? C17 C18 1.365(17) . ? C21 C22 1.386(13) . ? C22 C23 1.356(13) . ? C24 C25 1.377(16) . ? C25 C26 1.348(15) . ? C31 C32 1.387(13) . ? C32 C33 1.349(12) . ? C35 C36 1.372(14) . ? C36 C37 1.346(15) . ? 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 C2 Mn1 C1 87.6(6) . . ? C2 Mn1 C3 88.5(5) . . ? C1 Mn1 C3 90.7(5) . . ? C2 Mn1 N3 97.6(4) . . ? C1 Mn1 N3 92.0(4) . . ? C3 Mn1 N3 173.4(5) . . ? C2 Mn1 N1 174.8(4) . . ? C1 Mn1 N1 92.5(5) . . ? C3 Mn1 N1 96.7(5) . . ? N3 Mn1 N1 77.2(3) . . ? C2 Mn1 N8 93.5(4) . . ? C1 Mn1 N8 177.5(4) . . ? C3 Mn1 N8 91.5(4) . . ? N3 Mn1 N8 85.6(3) . . ? N1 Mn1 N8 86.2(3) . . ? C4 Mn2 C5 88.2(4) . . ? C4 Mn2 C6 90.5(5) . . ? C5 Mn2 C6 90.3(5) . . ? C4 Mn2 N6 91.6(4) . . ? C5 Mn2 N6 174.9(4) . . ? C6 Mn2 N6 94.9(5) . . ? C4 Mn2 N7 91.4(3) . . ? C5 Mn2 N7 97.5(4) . . ? C6 Mn2 N7 172.0(5) . . ? N6 Mn2 N7 77.3(3) . . ? C4 Mn2 N10 176.4(4) . . ? C5 Mn2 N10 93.3(4) . . ? C6 Mn2 N10 92.7(4) . . ? N6 Mn2 N10 86.6(3) . . ? N7 Mn2 N10 85.2(3) . . ? C7 Mn3 C9 91.2(4) . . ? C7 Mn3 C8 88.8(4) . . ? C9 Mn3 C8 89.0(5) . . ? C7 Mn3 N23 89.5(3) . . ? C9 Mn3 N23 173.1(4) . . ? C8 Mn3 N23 97.9(4) . . ? C7 Mn3 N25 176.6(3) . . ? C9 Mn3 N25 92.2(3) . . ? C8 Mn3 N25 91.7(4) . . ? N23 Mn3 N25 87.1(3) . . ? C7 Mn3 N21 91.3(3) . . ? C9 Mn3 N21 96.1(4) . . ? C8 Mn3 N21 175.0(3) . . ? N23 Mn3 N21 77.0(3) . . ? N25 Mn3 N21 87.9(3) . . ? N2 N1 C11 104.6(10) . . ? N2 N1 Mn1 114.2(6) . . ? C11 N1 Mn1 141.2(9) . . ? C13 N2 N1 111.1(9) . . ? C13 N2 C14 131.4(11) . . ? N1 N2 C14 117.5(9) . . ? C14 N3 Mn1 120.1(7) . . ? C15 N4 C14 123.7(8) . . ? C16 N5 N6 111.4(9) . . ? C16 N5 C15 131.3(9) . . ? N6 N5 C15 117.3(8) . . ? C18 N6 N5 104.8(9) . . ? C18 N6 Mn2 141.3(9) . . ? N5 N6 Mn2 113.9(6) . . ? C15 N7 Mn2 118.3(6) . . ? C21 N8 N9 104.2(8) . . ? C21 N8 Mn1 132.0(6) . . ? N9 N8 Mn1 123.7(6) . . ? C23 N9 N8 111.7(8) . . ? C24 N10 N11 104.6(8) . . ? C24 N10 Mn2 130.9(7) . . ? N11 N10 Mn2 124.2(6) . . ? N10 N11 C26 112.3(8) . . ? C31 N21 N22 105.4(7) . . ? C31 N21 Mn3 141.1(6) . . ? N22 N21 Mn3 112.9(5) . . ? N21 N22 C33 110.4(6) . . ? N21 N22 C34 117.6(6) . . ? C33 N22 C34 132.1(7) . . ? C34 N23 Mn3 119.2(5) . . ? C34 N24 C34 120.6(9) . 2_656 ? C35 N25 N26 102.2(7) . . ? C35 N25 Mn3 135.0(6) . . ? N26 N25 Mn3 122.7(5) . . ? C37 N26 N25 112.2(8) . . ? O1 C1 Mn1 178.9(10) . . ? O2 C2 Mn1 175.5(9) . . ? O3 C3 Mn1 177.7(13) . . ? O4 C4 Mn2 177.9(9) . . ? O5 C5 Mn2 175.8(9) . . ? O6 C6 Mn2 178.2(12) . . ? O7 C7 Mn3 177.6(9) . . ? O8 C8 Mn3 174.2(9) . . ? O9 C9 Mn3 176.9(11) . . ? N1 C11 C12 110.4(12) . . ? C13 C12 C11 105.7(12) . . ? N2 C13 C12 108.2(14) . . ? N3 C14 N4 136.8(9) . . ? N3 C14 N2 111.0(9) . . ? N4 C14 N2 112.2(9) . . ? N7 C15 N4 136.1(9) . . ? N7 C15 N5 113.1(8) . . ? N4 C15 N5 110.8(8) . . ? N5 C16 C17 106.0(11) . . ? C18 C17 C16 106.7(10) . . ? N6 C18 C17 111.0(11) . . ? N8 C21 C22 111.8(9) . . ? C23 C22 C21 103.5(9) . . ? N9 C23 C22 108.8(9) . . ? N10 C24 C25 111.3(10) . . ? C26 C25 C24 105.5(10) . . ? N11 C26 C25 106.3(10) . . ? N21 C31 C32 111.0(8) . . ? C33 C32 C31 105.7(8) . . ? C32 C33 N22 107.4(8) . . ? N23 C34 N24 134.9(7) . . ? N23 C34 N22 112.9(6) . . ? N24 C34 N22 112.0(7) . . ? N25 C35 C36 113.3(9) . . ? C37 C36 C35 103.8(9) . . ? N26 C37 C36 108.3(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.696 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.104 #===END data_Compound_4_ma383v _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cl Mn2 N11 O11' _chemical_formula_weight 787.87 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 16.046(11) _cell_length_b 8.880(6) _cell_length_c 23.199(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3306(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 958 _cell_measurement_theta_min 2.621 _cell_measurement_theta_max 26.363 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.714322 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20702 _diffrn_reflns_av_R_equivalents 0.1021 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5354 _reflns_number_gt 3066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+22.5638P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(10) _refine_ls_number_reflns 5354 _refine_ls_number_parameters 384 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1830 _refine_ls_R_factor_gt 0.1054 _refine_ls_wR_factor_ref 0.2060 _refine_ls_wR_factor_gt 0.1751 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.002 _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 Cl1 Cl 0.2206(2) 0.0849(4) 0.0669(4) 0.0816(12) Uani 1 1 d G . . O11 O 0.2462(6) -0.0609(5) 0.0548(7) 0.169(8) Uani 1 1 d G . . O12 O 0.2152(8) 0.0940(17) 0.1269(4) 0.277(17) Uani 1 1 d G . . O13 O 0.2799(5) 0.1875(9) 0.0471(8) 0.189(12) Uani 1 1 d G . . O14 O 0.1432(4) 0.1182(11) 0.0429(5) 0.139(8) Uani 1 1 d G . . Mn1 Mn 0.27294(19) 0.6204(4) 0.22145(9) 0.0521(10) Uani 1 1 d . . . Mn2 Mn 0.26872(18) 0.6192(4) -0.09083(10) 0.0517(10) Uani 1 1 d . . . C1 C 0.2029(15) 0.466(3) 0.2190(11) 0.059(6) Uiso 1 1 d . . . O1 O 0.1588(11) 0.361(2) 0.2174(11) 0.110(7) Uani 1 1 d . . . C2 C 0.1842(14) 0.731(3) 0.2225(13) 0.070(7) Uiso 1 1 d . . . O2 O 0.1211(10) 0.8037(19) 0.2239(11) 0.111(7) Uani 1 1 d . . . C3 C 0.2729(12) 0.609(3) 0.2948(9) 0.063(7) Uani 1 1 d . . . O3 O 0.2707(14) 0.608(3) 0.3462(12) 0.132(9) Uani 1 1 d . . . C4 C 0.2027(15) 0.448(3) -0.0889(10) 0.064(6) Uani 1 1 d . . . O4 O 0.1534(12) 0.359(2) -0.0897(12) 0.115(8) Uani 1 1 d . . . C5 C 0.1733(11) 0.738(2) -0.0879(11) 0.058(6) Uani 1 1 d . . . O5 O 0.1139(9) 0.797(3) -0.0912(11) 0.134(9) Uani 1 1 d . . . C6 C 0.2596(14) 0.618(2) -0.1714(12) 0.071(8) Uani 1 1 d . . . O6 O 0.2599(15) 0.608(3) -0.2190(10) 0.136(10) Uani 1 1 d . . . N1 N 0.3795(10) 0.5027(18) 0.2185(7) 0.048(4) Uani 1 1 d . . . N2 N 0.4069(10) 0.4911(19) 0.1603(7) 0.045(4) Uiso 1 1 d . . . N3 N 0.2911(9) 0.6113(16) 0.1355(8) 0.040(4) Uani 1 1 d . . . H3 H 0.2556 0.6500 0.1120 0.048 Uiso 1 1 calc R . . N4 N 0.3922(5) 0.5103(9) 0.0683(9) 0.044(2) Uiso 1 1 d . . . N5 N 0.4090(9) 0.4897(16) -0.0333(8) 0.039(4) Uani 1 1 d . . . N6 N 0.3744(9) 0.4966(17) -0.0842(8) 0.049(5) Uani 1 1 d . . . N7 N 0.2910(10) 0.6094(17) -0.0037(7) 0.038(4) Uiso 1 1 d . . . H7 H 0.2561 0.6502 0.0198 0.046 Uiso 1 1 calc R . . N8 N 0.3489(11) 0.808(2) 0.2233(9) 0.061(5) Uani 1 1 d . . . N9 N 0.3376(10) 0.924(2) 0.1897(8) 0.056(5) Uani 1 1 d . . . H9 H 0.2972 0.9271 0.1654 0.067 Uiso 1 1 calc R . . N10 N 0.3460(10) 0.8047(17) -0.0905(7) 0.044(4) Uani 1 1 d . . . N11 N 0.3359(12) 0.9285(18) -0.0559(8) 0.064(6) Uani 1 1 d . . . H11 H 0.2994 0.9374 -0.0289 0.077 Uiso 1 1 calc R . . C11 C 0.4382(14) 0.441(2) 0.2472(11) 0.057(6) Uiso 1 1 d . . . H11A H 0.4357 0.4293 0.2869 0.068 Uiso 1 1 calc R . . C12 C 0.5058(14) 0.393(3) 0.2149(10) 0.063(6) Uiso 1 1 d . . . H12 H 0.5543 0.3470 0.2281 0.076 Uiso 1 1 calc R . . C13 C 0.4862(14) 0.426(3) 0.1616(10) 0.057(6) Uiso 1 1 d . . . H13 H 0.5198 0.4092 0.1296 0.068 Uiso 1 1 calc R . . C14 C 0.3572(10) 0.5462(19) 0.1170(8) 0.029(4) Uiso 1 1 d . . . C15 C 0.3585(13) 0.541(2) 0.0171(9) 0.048(5) Uiso 1 1 d . . . C16 C 0.4820(12) 0.422(2) -0.0318(10) 0.050(6) Uani 1 1 d . . . H16 H 0.5147 0.4002 0.0003 0.061 Uiso 1 1 calc R . . C17 C 0.4993(12) 0.389(2) -0.0906(11) 0.061(7) Uani 1 1 d . . . H17 H 0.5470 0.3426 -0.1050 0.073 Uiso 1 1 calc R . . C18 C 0.4328(15) 0.438(2) -0.1221(11) 0.062(7) Uani 1 1 d . . . H18 H 0.4275 0.4332 -0.1620 0.074 Uiso 1 1 calc R . . C21 C 0.4130(15) 0.866(2) 0.2562(10) 0.062(6) Uani 1 1 d . . . H21 H 0.4342 0.8133 0.2875 0.075 Uiso 1 1 calc R . . C22 C 0.4436(19) 1.002(3) 0.2415(14) 0.106(11) Uani 1 1 d . . . H22 H 0.4871 1.0562 0.2578 0.128 Uiso 1 1 calc R . . C23 C 0.3923(18) 1.038(2) 0.1950(12) 0.088(9) Uani 1 1 d . . . H23 H 0.3954 1.1235 0.1721 0.106 Uiso 1 1 calc R . . C24 C 0.4128(17) 0.824(2) -0.1222(12) 0.079(8) Uani 1 1 d . . . H24 H 0.4381 0.7559 -0.1469 0.095 Uiso 1 1 calc R . . C25 C 0.4375(13) 0.975(2) -0.1100(12) 0.076(8) Uani 1 1 d . . . H25 H 0.4811 1.0253 -0.1282 0.091 Uiso 1 1 calc R . . C26 C 0.3917(11) 1.033(3) -0.0707(11) 0.071(8) Uani 1 1 d . . . H26 H 0.3963 1.1292 -0.0554 0.086 Uiso 1 1 calc R . . O90 O 0.1339(4) 0.6316(9) 0.0616(13) 0.081(3) Uani 1 1 d . . . C91 C 0.1018(11) 0.4822(16) 0.0733(19) 0.127(12) Uani 1 1 d . . . H91A H 0.1338 0.4080 0.0521 0.153 Uiso 1 1 calc R . . H91B H 0.1069 0.4602 0.1141 0.153 Uiso 1 1 calc R . . C92 C 0.0218(11) 0.4753(18) 0.058(3) 0.138(11) Uani 1 1 d . . . H92A H -0.0083 0.3996 0.0794 0.166 Uiso 1 1 calc R . . H92B H 0.0160 0.4550 0.0167 0.166 Uiso 1 1 calc R . . C93 C -0.0075(9) 0.6369(17) 0.073(3) 0.149(13) Uani 1 1 d . . . H93A H -0.0548 0.6663 0.0496 0.178 Uiso 1 1 calc R . . H93B H -0.0232 0.6432 0.1134 0.178 Uiso 1 1 calc R . . C94 C 0.0626(9) 0.7301(16) 0.0614(18) 0.099(6) Uani 1 1 d . . . H94A H 0.0684 0.8071 0.0908 0.119 Uiso 1 1 calc R . . H94B H 0.0567 0.7789 0.0242 0.119 Uiso 1 1 calc 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 Cl1 0.067(2) 0.071(2) 0.107(3) 0.009(6) 0.032(5) 0.0194(19) O11 0.204(15) 0.069(7) 0.24(2) -0.007(12) 0.164(18) 0.017(9) O12 0.31(3) 0.42(4) 0.094(15) -0.060(18) -0.024(16) 0.24(3) O13 0.094(10) 0.151(13) 0.32(4) -0.044(18) 0.060(17) -0.042(9) O14 0.086(9) 0.120(10) 0.21(2) 0.032(11) -0.080(11) -0.022(8) Mn1 0.0417(19) 0.059(2) 0.056(3) 0.000(2) 0.0145(16) -0.0055(16) Mn2 0.0422(18) 0.0446(18) 0.068(3) -0.0011(19) -0.0002(16) -0.0030(15) O1 0.077(11) 0.096(14) 0.156(19) -0.005(12) 0.028(13) -0.061(11) O2 0.065(10) 0.076(11) 0.19(2) -0.011(13) -0.015(12) 0.032(9) C3 0.052(11) 0.105(16) 0.031(11) 0.036(11) 0.028(8) 0.001(10) O3 0.129(18) 0.18(2) 0.082(17) -0.031(16) 0.049(12) -0.058(16) C4 0.066(11) 0.061(11) 0.064(13) -0.015(9) -0.021(9) 0.002(8) O4 0.104(13) 0.071(12) 0.17(2) -0.046(13) 0.029(15) -0.045(10) C5 0.026(8) 0.072(11) 0.076(14) 0.011(10) -0.025(9) -0.003(7) O5 0.034(8) 0.174(19) 0.19(2) 0.034(17) -0.063(12) 0.013(10) C6 0.074(15) 0.051(11) 0.09(2) 0.054(12) -0.038(12) -0.030(10) O6 0.18(2) 0.19(2) 0.038(12) -0.022(14) -0.015(11) -0.046(18) N1 0.054(10) 0.057(10) 0.033(10) -0.008(9) -0.012(8) -0.008(8) N3 0.009(5) 0.029(6) 0.082(10) 0.011(5) 0.002(5) 0.002(4) N5 0.011(5) 0.034(6) 0.073(10) -0.005(6) 0.009(5) -0.004(4) N6 0.032(8) 0.038(8) 0.076(14) -0.007(10) -0.007(9) 0.003(7) N8 0.062(12) 0.070(12) 0.050(13) 0.007(11) 0.023(11) -0.006(10) N9 0.034(9) 0.076(13) 0.058(13) -0.014(10) 0.010(8) -0.012(9) N10 0.047(9) 0.038(8) 0.046(12) 0.002(9) 0.017(9) 0.001(7) N11 0.083(13) 0.035(9) 0.075(14) -0.026(9) 0.023(10) 0.006(9) C16 0.024(8) 0.053(10) 0.075(12) -0.005(7) 0.017(7) -0.004(6) C17 0.035(8) 0.041(8) 0.108(17) -0.020(9) 0.039(10) 0.003(7) C18 0.064(12) 0.042(9) 0.080(14) -0.037(8) 0.040(10) -0.009(8) C21 0.090(14) 0.032(10) 0.064(12) 0.005(9) -0.041(11) -0.012(10) C22 0.15(3) 0.055(13) 0.11(2) 0.003(14) -0.002(19) -0.072(15) C23 0.16(3) 0.032(10) 0.077(17) 0.028(11) 0.019(16) -0.024(14) C24 0.088(16) 0.027(9) 0.122(19) 0.011(10) 0.010(13) -0.024(9) C25 0.051(12) 0.058(13) 0.12(2) 0.005(13) 0.057(14) -0.022(10) C26 0.026(10) 0.091(16) 0.096(18) 0.049(13) 0.012(11) -0.022(11) O90 0.029(4) 0.052(5) 0.163(9) 0.013(13) 0.018(12) 0.012(4) C91 0.107(14) 0.050(9) 0.22(3) -0.001(19) -0.09(3) 0.013(9) C92 0.093(14) 0.071(11) 0.25(3) 0.00(3) -0.03(3) 0.001(10) C93 0.055(10) 0.066(10) 0.33(4) 0.01(3) 0.06(3) 0.016(8) C94 0.073(10) 0.075(9) 0.150(16) 0.02(2) 0.051(18) 0.015(8) _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 Cl1 O11 1.3871 . ? Cl1 O14 1.3934 . ? Cl1 O13 1.3948 . ? Cl1 O12 1.3976 . ? Mn1 C3 1.70(2) . ? Mn1 C2 1.73(2) . ? Mn1 C1 1.77(2) . ? Mn1 N1 2.005(18) . ? Mn1 N3 2.017(18) . ? Mn1 N8 2.068(19) . ? Mn2 C4 1.85(2) . ? Mn2 C5 1.86(2) . ? Mn2 C6 1.88(3) . ? Mn2 N6 2.022(16) . ? Mn2 N7 2.054(17) . ? Mn2 N10 2.062(16) . ? C1 O1 1.17(3) . ? C2 O2 1.20(3) . ? C3 O3 1.19(3) . ? C4 O4 1.12(3) . ? C5 O5 1.09(2) . ? C6 O6 1.11(3) . ? N1 C11 1.28(3) . ? N1 N2 1.42(2) . ? N2 C14 1.37(2) . ? N2 C13 1.40(3) . ? N3 C14 1.28(2) . ? N4 C14 1.30(2) . ? N4 C15 1.33(2) . ? N5 N6 1.31(2) . ? N5 C16 1.32(2) . ? N5 C15 1.49(3) . ? N6 C18 1.39(2) . ? N7 C15 1.33(2) . ? N8 N9 1.30(3) . ? N8 C21 1.38(3) . ? N9 C23 1.35(3) . ? N10 C24 1.31(3) . ? N10 N11 1.37(2) . ? N11 C26 1.33(2) . ? C11 C12 1.39(3) . ? C12 C13 1.31(3) . ? C16 C17 1.42(3) . ? C17 C18 1.36(3) . ? C21 C22 1.34(3) . ? C22 C23 1.39(4) . ? C24 C25 1.43(3) . ? C25 C26 1.28(3) . ? O90 C94 1.440(14) . ? O90 C91 1.449(18) . ? C91 C92 1.34(2) . ? C92 C93 1.55(3) . ? C93 C94 1.42(2) . ? 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 O11 Cl1 O14 112.4 . . ? O11 Cl1 O13 109.9 . . ? O14 Cl1 O13 109.7 . . ? O11 Cl1 O12 106.0 . . ? O14 Cl1 O12 109.4 . . ? O13 Cl1 O12 109.4 . . ? C3 Mn1 C2 91.1(12) . . ? C3 Mn1 C1 89.3(11) . . ? C2 Mn1 C1 85.3(11) . . ? C3 Mn1 N1 90.2(9) . . ? C2 Mn1 N1 176.6(9) . . ? C1 Mn1 N1 97.9(9) . . ? C3 Mn1 N3 169.9(8) . . ? C2 Mn1 N3 99.0(11) . . ? C1 Mn1 N3 91.6(9) . . ? N1 Mn1 N3 79.8(7) . . ? C3 Mn1 N8 91.5(10) . . ? C2 Mn1 N8 91.5(10) . . ? C1 Mn1 N8 176.7(9) . . ? N1 Mn1 N8 85.3(7) . . ? N3 Mn1 N8 88.2(7) . . ? C4 Mn2 C5 89.5(10) . . ? C4 Mn2 C6 88.6(9) . . ? C5 Mn2 C6 88.5(11) . . ? C4 Mn2 N6 92.1(8) . . ? C5 Mn2 N6 173.3(9) . . ? C6 Mn2 N6 98.0(9) . . ? C4 Mn2 N7 92.4(9) . . ? C5 Mn2 N7 97.6(9) . . ? C6 Mn2 N7 173.9(9) . . ? N6 Mn2 N7 75.9(7) . . ? C4 Mn2 N10 177.4(9) . . ? C5 Mn2 N10 92.5(7) . . ? C6 Mn2 N10 93.1(7) . . ? N6 Mn2 N10 85.7(6) . . ? N7 Mn2 N10 85.8(6) . . ? O1 C1 Mn1 178(2) . . ? O2 C2 Mn1 178(2) . . ? O3 C3 Mn1 177(2) . . ? O4 C4 Mn2 170(2) . . ? O5 C5 Mn2 172(2) . . ? O6 C6 Mn2 173(2) . . ? C11 N1 N2 103.7(18) . . ? C11 N1 Mn1 146.6(16) . . ? N2 N1 Mn1 109.5(12) . . ? C14 N2 C13 133.8(17) . . ? C14 N2 N1 119.2(16) . . ? C13 N2 N1 106.9(16) . . ? C14 N3 Mn1 117.9(13) . . ? C14 N4 C15 123.3(9) . . ? N6 N5 C16 115.0(17) . . ? N6 N5 C15 117.6(15) . . ? C16 N5 C15 127.0(18) . . ? N5 N6 C18 105.7(18) . . ? N5 N6 Mn2 116.8(12) . . ? C18 N6 Mn2 136.1(17) . . ? C15 N7 Mn2 121.1(14) . . ? N9 N8 C21 98.2(17) . . ? N9 N8 Mn1 122.7(16) . . ? C21 N8 Mn1 138.8(16) . . ? N8 N9 C23 117(2) . . ? C24 N10 N11 108.6(17) . . ? C24 N10 Mn2 126.6(14) . . ? N11 N10 Mn2 124.8(13) . . ? C26 N11 N10 109.0(18) . . ? N1 C11 C12 115(2) . . ? C13 C12 C11 105(2) . . ? C12 C13 N2 109(2) . . ? N3 C14 N4 139.3(17) . . ? N3 C14 N2 113.4(17) . . ? N4 C14 N2 107.2(15) . . ? N7 C15 N4 138.2(19) . . ? N7 C15 N5 107.3(17) . . ? N4 C15 N5 114.5(16) . . ? N5 C16 C17 104(2) . . ? C18 C17 C16 107.2(17) . . ? C17 C18 N6 108(2) . . ? C22 C21 N8 118(2) . . ? C21 C22 C23 101(2) . . ? N9 C23 C22 106.4(18) . . ? N10 C24 C25 104(2) . . ? C26 C25 C24 111(2) . . ? C25 C26 N11 107(2) . . ? C94 O90 C91 105.9(10) . . ? C92 C91 O90 109.4(18) . . ? C91 C92 C93 101(2) . . ? C94 C93 C92 104.7(18) . . ? C93 C94 O90 105.9(12) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.557 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.092 #===END