data_Complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5 H3 N6)2 (H2 O)2 Zn' _chemical_formula_sum 'C10 H10 N12 O2 Zn' _chemical_formula_weight 395.67 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 6.0910(6) _cell_length_b 11.4576(12) _cell_length_c 10.6860(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.626(2) _cell_angle_gamma 90.00 _cell_volume 718.19(13) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6591 _exptl_absorpt_correction_T_max 0.6789 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4470 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.86 _reflns_number_total 1629 _reflns_number_gt 1443 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0458P)^2^+0.1979P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1629 _refine_ls_number_parameters 135 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.049 _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 Zn1 Zn 0.5000 0.5000 0.5000 0.02745(13) Uani 1 2 d S . . O1W O 0.4178(3) 0.53651(16) 0.67475(17) 0.0424(4) Uani 1 1 d D . . N1 N 0.3646(3) 0.32247(14) 0.50153(15) 0.0272(4) Uani 1 1 d . . . N2 N 0.2631(4) 0.08803(17) 0.5255(2) 0.0488(5) Uani 1 1 d . . . N3 N 0.7900(3) 0.40965(14) 0.61163(16) 0.0297(4) Uani 1 1 d . . . N4 N 1.0055(3) 0.42579(16) 0.68145(18) 0.0373(4) Uani 1 1 d . . . N5 N 1.0846(3) 0.32753(17) 0.73934(19) 0.0404(4) Uani 1 1 d . . . N6 N 0.9233(3) 0.24547(16) 0.70824(17) 0.0337(4) Uani 1 1 d . . . C1 C 0.1592(4) 0.27889(19) 0.4451(2) 0.0328(5) Uani 1 1 d D . . C2 C 0.1097(4) 0.1624(2) 0.4572(2) 0.0406(5) Uani 1 1 d D . . C3 C 0.4683(4) 0.13172(19) 0.5813(2) 0.0396(5) Uani 1 1 d D . . C4 C 0.5210(3) 0.24814(17) 0.57025(18) 0.0263(4) Uani 1 1 d . . . C5 C 0.7450(3) 0.29811(17) 0.63055(19) 0.0268(4) Uani 1 1 d . . . H1W1 H 0.290(3) 0.513(2) 0.680(3) 0.042(8) Uiso 1 1 d D . . H1W2 H 0.462(5) 0.6005(15) 0.713(3) 0.063(9) Uiso 1 1 d D . . H1 H 0.048(3) 0.3312(17) 0.3954(19) 0.038(6) Uiso 1 1 d D . . H2 H -0.040(2) 0.133(2) 0.420(2) 0.055(8) Uiso 1 1 d D . . H3 H 0.583(3) 0.0816(19) 0.631(2) 0.044(7) Uiso 1 1 d D . . 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 Zn1 0.0280(2) 0.01918(19) 0.0322(2) 0.00323(12) 0.00305(13) 0.00047(12) O1W 0.0471(11) 0.0402(9) 0.0443(9) -0.0134(8) 0.0201(8) -0.0167(8) N1 0.0275(9) 0.0259(8) 0.0268(8) 0.0004(6) 0.0050(7) 0.0006(7) N2 0.0436(12) 0.0311(10) 0.0649(14) 0.0001(9) 0.0026(10) -0.0095(9) N3 0.0261(9) 0.0248(9) 0.0350(9) 0.0015(7) 0.0026(7) -0.0021(7) N4 0.0302(10) 0.0342(10) 0.0432(11) -0.0001(8) 0.0023(8) -0.0050(8) N5 0.0302(10) 0.0427(11) 0.0428(10) 0.0047(8) 0.0005(8) -0.0018(8) N6 0.0271(9) 0.0325(9) 0.0375(9) 0.0077(7) 0.0019(7) 0.0018(7) C1 0.0276(10) 0.0350(11) 0.0320(11) -0.0005(8) 0.0014(8) 0.0011(9) C2 0.0325(12) 0.0379(12) 0.0468(13) -0.0066(10) 0.0030(10) -0.0090(10) C3 0.0379(13) 0.0242(11) 0.0515(14) 0.0057(9) 0.0032(10) 0.0013(9) C4 0.0266(10) 0.0239(9) 0.0275(10) 0.0011(7) 0.0058(8) 0.0008(8) C5 0.0270(10) 0.0245(9) 0.0276(9) 0.0027(7) 0.0052(8) 0.0032(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 Zn1 O1W 2.1016(17) 3_666 ? Zn1 O1W 2.1016(17) . ? Zn1 N3 2.1166(16) 3_666 ? Zn1 N3 2.1166(17) . ? Zn1 N1 2.1965(16) 3_666 ? Zn1 N1 2.1965(16) . ? N1 C1 1.331(3) . ? N1 C4 1.340(2) . ? N2 C2 1.328(3) . ? N2 C3 1.329(3) . ? N3 N4 1.337(2) . ? N3 C5 1.334(2) . ? N4 N5 1.312(3) . ? N5 N6 1.335(3) . ? N6 C5 1.322(2) . ? C1 C2 1.382(3) . ? C3 C4 1.385(3) . ? C4 C5 1.460(3) . ? 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 O1W Zn1 O1W 180.000(1) 3_666 . ? O1W Zn1 N3 87.65(7) 3_666 3_666 ? O1W Zn1 N3 92.35(7) . 3_666 ? O1W Zn1 N3 92.35(7) 3_666 . ? O1W Zn1 N3 87.65(7) . . ? N3 Zn1 N3 180.0 3_666 . ? O1W Zn1 N1 89.88(6) 3_666 3_666 ? O1W Zn1 N1 90.12(6) . 3_666 ? N3 Zn1 N1 78.52(6) 3_666 3_666 ? N3 Zn1 N1 101.48(6) . 3_666 ? O1W Zn1 N1 90.12(6) 3_666 . ? O1W Zn1 N1 89.88(6) . . ? N3 Zn1 N1 101.48(6) 3_666 . ? N3 Zn1 N1 78.52(6) . . ? N1 Zn1 N1 180.0 3_666 . ? C1 N1 C4 116.92(18) . . ? C1 N1 Zn1 130.76(14) . . ? C4 N1 Zn1 112.31(13) . . ? C2 N2 C3 116.2(2) . . ? N4 N3 C5 105.01(16) . . ? N4 N3 Zn1 142.38(13) . . ? C5 N3 Zn1 112.31(13) . . ? N5 N4 N3 108.97(17) . . ? N4 N5 N6 109.56(17) . . ? C5 N6 N5 105.07(17) . . ? N1 C1 C2 121.5(2) . . ? N2 C2 C1 122.1(2) . . ? N2 C3 C4 122.5(2) . . ? N1 C4 C3 120.79(19) . . ? N1 C4 C5 115.77(17) . . ? C3 C4 C5 123.44(18) . . ? N6 C5 N3 111.40(18) . . ? N6 C5 C4 127.62(18) . . ? N3 C5 C4 120.98(17) . . ? 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 O1W H1W1 N4 0.840(10) 2.003(11) 2.831(3) 168(2) 1_455 O1W H1W2 N6 0.847(10) 1.908(11) 2.753(2) 176(3) 2_656 _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.489 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.065 data_Complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5 H3 N6)2 (H2 O) Cu, H2 O' _chemical_formula_sum 'C10 H12 Cu N12 O3' _chemical_formula_weight 411.86 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' 'Cu' 'Cu' 0.3201 1.2651 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y, z-1/2' _cell_length_a 13.0083(10) _cell_length_b 7.3160(6) _cell_length_c 16.8582(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.922(1) _cell_angle_gamma 90.00 _cell_volume 1569.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2195 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.7 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.436 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6334 _exptl_absorpt_correction_T_max 0.7154 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4699 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.92 _reflns_number_total 1791 _reflns_number_gt 1629 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0574P)^2^+2.4865P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1791 _refine_ls_number_parameters 120 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean '<0.001' 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 Cu1 Cu 0.2500 0.2500 0.5000 0.03058(18) Uani 1 2 d S . . O1 O 0.35914(16) 0.1119(3) 0.41423(14) 0.0441(5) Uani 1 1 d . . . H11 H 0.4168 0.1716 0.4267 0.053 Uiso 1 1 d . . . H12 H 0.3727 -0.0002 0.4267 0.053 Uiso 1 1 d . . . O2 O 0.2500 0.0662(10) 0.2500 0.159(3) Uani 1 2 d SU . . H21 H 0.2766 0.1365 0.2901 0.190 Uiso 1 1 d . . . N1 N 0.15762(16) 0.0321(3) 0.48356(13) 0.0299(5) Uani 1 1 d . . . N2 N 0.07551(19) -0.0372(3) 0.43115(16) 0.0392(6) Uani 1 1 d . . . N3 N 0.0525(2) -0.1971(4) 0.45921(17) 0.0405(6) Uani 1 1 d . . . N4 N 0.1184(2) -0.2351(3) 0.52948(17) 0.0355(5) Uani 1 1 d . . . N5 N 0.3930(2) -0.1309(4) 0.72912(17) 0.0506(7) Uani 1 1 d . . . N6 N 0.32217(18) 0.1002(3) 0.59854(14) 0.0314(5) Uani 1 1 d . . . C1 C 0.1811(2) -0.0916(3) 0.54233(16) 0.0293(5) Uani 1 1 d . . . C2 C 0.2717(2) -0.0570(4) 0.60770(16) 0.0305(5) Uani 1 1 d . . . C3 C 0.3085(3) -0.1707(4) 0.67253(19) 0.0418(7) Uani 1 1 d . . . H3 H 0.2729 -0.2793 0.6769 0.050 Uiso 1 1 calc R . . C4 C 0.4428(3) 0.0221(5) 0.7185(2) 0.0519(9) Uani 1 1 d . . . H4 H 0.5034 0.0523 0.7561 0.062 Uiso 1 1 calc R . . C5 C 0.4086(3) 0.1390(4) 0.65392(19) 0.0430(7) Uani 1 1 d . . . H5 H 0.4460 0.2454 0.6491 0.052 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 Cu1 0.0328(3) 0.0217(3) 0.0328(3) 0.00511(16) -0.00344(19) -0.00739(17) O1 0.0399(11) 0.0346(11) 0.0559(13) -0.0004(9) 0.0055(10) -0.0054(9) O2 0.252(7) 0.106(5) 0.092(4) 0.000 -0.023(5) 0.000 N1 0.0287(11) 0.0252(11) 0.0337(11) -0.0004(9) 0.0019(9) -0.0050(9) N2 0.0379(13) 0.0317(13) 0.0450(14) -0.0024(10) 0.0019(11) -0.0069(10) N3 0.0381(13) 0.0314(12) 0.0504(15) -0.0040(11) 0.0056(11) -0.0082(11) N4 0.0372(13) 0.0234(11) 0.0467(14) 0.0007(9) 0.0103(11) -0.0038(9) N5 0.0594(18) 0.0429(16) 0.0441(15) 0.0133(12) -0.0019(13) 0.0012(13) N6 0.0342(12) 0.0246(11) 0.0332(11) 0.0025(9) 0.0020(9) -0.0015(9) C1 0.0305(13) 0.0214(12) 0.0377(14) 0.0007(10) 0.0112(11) -0.0015(9) C2 0.0340(13) 0.0242(12) 0.0344(13) 0.0014(10) 0.0095(11) 0.0008(10) C3 0.0511(17) 0.0299(15) 0.0443(16) 0.0092(12) 0.0102(14) -0.0016(13) C4 0.0524(19) 0.0459(19) 0.0476(19) 0.0073(15) -0.0127(15) -0.0031(15) C5 0.0439(16) 0.0348(15) 0.0441(17) 0.0039(13) -0.0054(13) -0.0064(13) 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 Cu1 N1 1.981(2) 7_556 ? Cu1 N1 1.981(2) . ? Cu1 N6 2.049(2) 7_556 ? Cu1 N6 2.049(2) . ? Cu1 O1 2.444(2) 7_556 ? Cu1 O1 2.444(2) . ? O1 H11 0.86 . ? O1 H12 0.86 . ? O2 H21 0.86 . ? N1 C1 1.330(3) . ? N1 N2 1.337(3) . ? N2 N3 1.319(4) . ? N3 N4 1.340(4) . ? N4 C1 1.319(3) . ? N5 C4 1.325(4) . ? N5 C3 1.330(4) . ? N6 C5 1.335(4) . ? N6 C2 1.348(3) . ? C1 C2 1.460(4) . ? C2 C3 1.378(4) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? 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 N1 Cu1 N1 180.0 7_556 . ? N1 Cu1 N6 81.14(9) 7_556 7_556 ? N1 Cu1 N6 98.86(9) . 7_556 ? N1 Cu1 N6 98.86(9) 7_556 . ? N1 Cu1 N6 81.14(9) . . ? N6 Cu1 N6 180.00(9) 7_556 . ? N1 Cu1 O1 89.67(8) 7_556 7_556 ? N1 Cu1 O1 90.33(8) . 7_556 ? N6 Cu1 O1 91.93(8) 7_556 7_556 ? N6 Cu1 O1 88.07(8) . 7_556 ? N1 Cu1 O1 90.33(8) 7_556 . ? N1 Cu1 O1 89.67(8) . . ? N6 Cu1 O1 88.07(8) 7_556 . ? N6 Cu1 O1 91.93(8) . . ? O1 Cu1 O1 180.00(8) 7_556 . ? Cu1 O1 H11 103.4 . . ? Cu1 O1 H12 111.5 . . ? H11 O1 H12 107.6 . . ? C1 N1 N2 105.3(2) . . ? C1 N1 Cu1 113.83(17) . . ? N2 N1 Cu1 140.90(19) . . ? N3 N2 N1 108.0(2) . . ? N2 N3 N4 110.5(2) . . ? C1 N4 N3 103.9(2) . . ? C4 N5 C3 116.3(3) . . ? C5 N6 C2 117.4(2) . . ? C5 N6 Cu1 129.2(2) . . ? C2 N6 Cu1 113.37(18) . . ? N4 C1 N1 112.3(2) . . ? N4 C1 C2 129.6(2) . . ? N1 C1 C2 118.0(2) . . ? N6 C2 C3 120.5(3) . . ? N6 C2 C1 113.4(2) . . ? C3 C2 C1 126.0(3) . . ? N5 C3 C2 122.5(3) . . ? N5 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? N5 C4 C5 122.8(3) . . ? N5 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? N6 C5 C4 120.4(3) . . ? N6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? 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 Cu1 N1 C1 -97(100) 7_556 . . . ? N6 Cu1 N1 C1 -176.37(18) 7_556 . . . ? N6 Cu1 N1 C1 3.63(18) . . . . ? O1 Cu1 N1 C1 -84.37(19) 7_556 . . . ? O1 Cu1 N1 C1 95.63(19) . . . . ? N1 Cu1 N1 N2 83(100) 7_556 . . . ? N6 Cu1 N1 N2 3.5(3) 7_556 . . . ? N6 Cu1 N1 N2 -176.5(3) . . . . ? O1 Cu1 N1 N2 95.5(3) 7_556 . . . ? O1 Cu1 N1 N2 -84.5(3) . . . . ? C1 N1 N2 N3 -0.1(3) . . . . ? Cu1 N1 N2 N3 -180.0(2) . . . . ? N1 N2 N3 N4 -0.1(3) . . . . ? N2 N3 N4 C1 0.3(3) . . . . ? N1 Cu1 N6 C5 -2.7(3) 7_556 . . . ? N1 Cu1 N6 C5 177.3(3) . . . . ? N6 Cu1 N6 C5 145(100) 7_556 . . . ? O1 Cu1 N6 C5 -92.0(3) 7_556 . . . ? O1 Cu1 N6 C5 88.0(3) . . . . ? N1 Cu1 N6 C2 175.76(18) 7_556 . . . ? N1 Cu1 N6 C2 -4.24(18) . . . . ? N6 Cu1 N6 C2 -36(100) 7_556 . . . ? O1 Cu1 N6 C2 86.40(19) 7_556 . . . ? O1 Cu1 N6 C2 -93.60(19) . . . . ? N3 N4 C1 N1 -0.3(3) . . . . ? N3 N4 C1 C2 -177.1(3) . . . . ? N2 N1 C1 N4 0.3(3) . . . . ? Cu1 N1 C1 N4 -179.81(18) . . . . ? N2 N1 C1 C2 177.5(2) . . . . ? Cu1 N1 C1 C2 -2.6(3) . . . . ? C5 N6 C2 C3 0.6(4) . . . . ? Cu1 N6 C2 C3 -178.0(2) . . . . ? C5 N6 C2 C1 -177.4(3) . . . . ? Cu1 N6 C2 C1 4.0(3) . . . . ? N4 C1 C2 N6 175.6(3) . . . . ? N1 C1 C2 N6 -1.0(4) . . . . ? N4 C1 C2 C3 -2.2(5) . . . . ? N1 C1 C2 C3 -178.9(3) . . . . ? C4 N5 C3 C2 -2.3(5) . . . . ? N6 C2 C3 N5 1.1(5) . . . . ? C1 C2 C3 N5 178.8(3) . . . . ? C3 N5 C4 C5 1.9(6) . . . . ? C2 N6 C5 C4 -1.0(5) . . . . ? Cu1 N6 C5 C4 177.4(3) . . . . ? N5 C4 C5 N6 -0.3(6) . . . . ? 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 H11 N3 0.86 1.99 2.840(3) 178 3 O1 H12 N4 0.86 2.07 2.910(3) 168 7_546 O2 H21 O1 0.86 2.15 2.858(2) 139 . _diffrn_measured_fraction_theta_max 0.95 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.95 _refine_diff_density_max 0.54 _refine_diff_density_min -0.85 _refine_diff_density_rms 0.08 data_Complex_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5 H3 N6)2 Cd' _chemical_formula_sum 'C10 H6 Cd N12' _chemical_formula_weight 406.67 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' 'Cd' 'Cd' -0.8075 1.2024 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7615(6) _cell_length_b 18.5982(13) _cell_length_c 9.0395(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.5030(10) _cell_angle_gamma 90.00 _cell_volume 1419.38(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.560 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9576 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.04 _reflns_number_total 5516 _reflns_number_gt 5367 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0513P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 5516 _refine_ls_number_parameters 416 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Cd1 Cd 0.35949(3) 0.124301(14) 0.81957(3) 0.03077(9) Uani 1 1 d . . . Cd2 Cd -0.16036(3) 0.181865(16) 0.75305(3) 0.02971(8) Uani 1 1 d . . . N19 N 0.4304(4) 0.1756(3) 0.6174(4) 0.0338(8) Uani 1 1 d . . . N5 N 0.3687(4) 0.0862(2) 1.0732(4) 0.0331(8) Uani 1 1 d . . . N1 N 0.6248(4) 0.1170(2) 0.9673(4) 0.0301(7) Uani 1 1 d . . . C16 C 0.5575(5) 0.2083(2) 0.4587(5) 0.0290(8) Uani 1 1 d . . . N13 N 0.1174(4) 0.0688(2) 0.7102(4) 0.0298(7) Uani 1 1 d . . . N7 N 0.2386(5) 0.2272(2) 0.8814(5) 0.0369(8) Uani 1 1 d . . . N11 N -0.2064(5) 0.2990(2) 0.8488(4) 0.0358(8) Uani 1 1 d . . . C13 C 0.2796(7) -0.0918(3) 0.5596(6) 0.0448(11) Uani 1 1 d . . . H13 H 0.1858 -0.1139 0.5062 0.054 Uiso 1 1 calc R . . C12 C 0.2722(5) -0.0290(2) 0.6432(5) 0.0341(9) Uani 1 1 d . . . N24 N 0.8041(6) 0.2601(3) 0.1973(5) 0.0517(12) Uani 1 1 d . . . N17 N 0.4053(5) 0.0032(2) 0.7234(4) 0.0371(8) Uani 1 1 d . . . C7 C -0.0771(5) 0.3347(2) 0.9271(5) 0.0347(9) Uani 1 1 d . . . N15 N -0.1183(5) 0.0237(3) 0.6344(6) 0.0500(11) Uani 1 1 d . . . N10 N 0.0823(4) 0.2387(2) 0.8611(4) 0.0327(7) Uani 1 1 d . . . N9 N 0.2179(6) 0.3306(3) 0.9846(6) 0.0539(12) Uani 1 1 d . . . N6 N 0.4004(6) 0.0321(3) 1.3656(5) 0.0484(11) Uani 1 1 d . . . C14 C 0.5458(7) -0.0888(3) 0.6347(8) 0.0563(14) Uani 1 1 d . . . H14 H 0.6435 -0.1086 0.6357 0.068 Uiso 1 1 calc R . . N16 N -0.0201(5) -0.0250(3) 0.6021(6) 0.0487(11) Uani 1 1 d . . . C11 C 0.1246(5) 0.0042(2) 0.6501(5) 0.0318(9) Uani 1 1 d . . . N14 N -0.0361(4) 0.0798(2) 0.6990(4) 0.0366(8) Uani 1 1 d . . . N18 N 0.4166(7) -0.1205(3) 0.5545(7) 0.0574(13) Uani 1 1 d . . . N12 N -0.2279(7) 0.4222(3) 1.0156(6) 0.0555(12) Uani 1 1 d . . . N3 N 0.8728(5) 0.0943(3) 1.0665(6) 0.0640(16) Uani 1 1 d . . . C15 C 0.5414(6) -0.0264(3) 0.7183(7) 0.0462(11) Uani 1 1 d . . . H15 H 0.6360 -0.0050 0.7718 0.055 Uiso 1 1 calc R . . C10 C -0.3466(6) 0.3256(3) 0.8540(6) 0.0411(10) Uani 1 1 d . . . H10 H -0.4394 0.3028 0.8006 0.049 Uiso 1 1 calc R . . C18 C 0.6767(6) 0.2454(3) 0.2486(5) 0.0401(10) Uani 1 1 d . . . H18 H 0.5763 0.2492 0.1810 0.048 Uiso 1 1 calc R . . C6 C 0.0756(5) 0.3018(3) 0.9249(5) 0.0354(9) Uani 1 1 d . . . C4 C 0.2609(6) 0.0501(3) 1.2739(6) 0.0451(12) Uani 1 1 d . . . H4 H 0.1713 0.0449 1.3095 0.054 Uiso 1 1 calc R . . N2 N 0.7701(4) 0.1221(3) 0.9494(4) 0.0378(8) Uani 1 1 d . . . C17 C 0.6904(5) 0.2249(2) 0.3987(5) 0.0304(8) Uani 1 1 d . . . C9 C -0.3544(7) 0.3871(3) 0.9385(7) 0.0501(13) Uani 1 1 d . . . H9 H -0.4535 0.4043 0.9407 0.060 Uiso 1 1 calc R . . C19 C 0.9423(7) 0.2531(4) 0.2982(6) 0.0557(15) Uani 1 1 d . . . H19 H 1.0333 0.2612 0.2663 0.067 Uiso 1 1 calc R . . N4 N 0.7973(5) 0.0694(3) 1.1666(6) 0.0596(14) Uani 1 1 d . . . C2 C 0.5111(5) 0.0687(2) 1.1648(4) 0.0315(8) Uani 1 1 d . . . C3 C 0.5261(6) 0.0417(3) 1.3118(5) 0.0408(10) Uani 1 1 d . . . H3 H 0.6262 0.0302 1.3736 0.049 Uiso 1 1 calc R . . C5 C 0.2433(5) 0.0764(3) 1.1273(5) 0.0415(11) Uani 1 1 d . . . H5 H 0.1427 0.0873 1.0659 0.050 Uiso 1 1 calc R . . C1 C 0.6457(5) 0.0837(3) 1.1009(5) 0.0334(9) Uani 1 1 d . . . N22 N 0.5774(4) 0.1830(2) 0.6021(3) 0.0293(6) Uani 1 1 d . . . N20 N 0.3269(4) 0.1948(3) 0.4882(4) 0.0441(10) Uani 1 1 d . . . N21 N 0.4039(5) 0.2155(3) 0.3867(4) 0.0396(9) Uani 1 1 d . . . N23 N 0.8328(4) 0.2198(2) 0.4994(4) 0.0353(8) Uani 1 1 d . . . N8 N 0.3186(5) 0.2818(3) 0.9548(6) 0.0522(11) Uani 1 1 d . . . C8 C -0.0884(7) 0.3967(3) 1.0096(7) 0.0498(12) Uani 1 1 d . . . H8 H 0.0035 0.4206 1.0614 0.060 Uiso 1 1 calc R . . C20 C 0.9589(6) 0.2343(3) 0.4476(6) 0.0495(13) Uani 1 1 d . . . H20 H 1.0597 0.2316 0.5147 0.059 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 Cd1 0.02166(14) 0.04222(18) 0.02895(14) 0.00161(13) 0.00766(10) -0.00033(13) Cd2 0.02192(14) 0.03981(16) 0.02801(14) 0.00098(12) 0.00774(10) 0.00063(12) N19 0.0203(16) 0.047(2) 0.0353(16) 0.005(2) 0.0088(13) 0.0005(18) N5 0.0241(18) 0.048(2) 0.0285(16) 0.0021(15) 0.0096(14) 0.0003(16) N1 0.0190(15) 0.043(2) 0.0299(14) 0.0036(16) 0.0089(12) -0.0003(16) C16 0.0267(19) 0.0315(19) 0.0286(17) 0.0018(15) 0.0066(15) 0.0018(15) N13 0.0256(16) 0.0345(18) 0.0303(15) 0.0027(15) 0.0093(13) 0.0020(15) N7 0.0261(19) 0.044(2) 0.0432(19) -0.0007(17) 0.0131(16) 0.0002(16) N11 0.031(2) 0.045(2) 0.0341(17) 0.0012(17) 0.0145(15) 0.0033(17) C13 0.042(3) 0.032(2) 0.064(3) -0.002(2) 0.020(2) -0.001(2) C12 0.035(2) 0.035(2) 0.035(2) 0.0071(18) 0.0143(18) -0.0005(18) N24 0.043(3) 0.079(4) 0.038(2) 0.012(2) 0.0192(19) 0.000(2) N17 0.033(2) 0.044(2) 0.0372(18) 0.0038(17) 0.0147(16) 0.0022(17) C7 0.033(2) 0.038(2) 0.036(2) 0.0016(19) 0.0148(18) 0.0021(18) N15 0.033(2) 0.053(3) 0.065(3) -0.011(2) 0.014(2) -0.0046(19) N10 0.0262(17) 0.0397(19) 0.0340(16) 0.0008(16) 0.0112(14) 0.0012(16) N9 0.035(2) 0.052(3) 0.073(3) -0.017(2) 0.012(2) -0.005(2) N6 0.050(3) 0.062(3) 0.039(2) 0.010(2) 0.022(2) -0.001(2) C14 0.042(3) 0.047(3) 0.086(4) 0.004(3) 0.027(3) 0.015(2) N16 0.032(2) 0.047(2) 0.065(3) -0.010(2) 0.010(2) -0.0055(19) C11 0.032(2) 0.035(2) 0.0305(18) 0.0059(17) 0.0105(16) -0.0021(17) N14 0.0234(17) 0.047(2) 0.0389(18) 0.0001(17) 0.0077(15) 0.0001(17) N18 0.061(3) 0.037(2) 0.082(3) -0.004(2) 0.033(3) 0.007(2) N12 0.054(3) 0.047(3) 0.068(3) -0.007(2) 0.021(3) 0.013(2) N3 0.026(2) 0.111(4) 0.058(3) 0.038(3) 0.0163(19) 0.011(2) C15 0.031(2) 0.047(3) 0.060(3) 0.004(2) 0.013(2) 0.003(2) C10 0.032(2) 0.047(3) 0.047(2) -0.004(2) 0.015(2) 0.005(2) C18 0.038(2) 0.049(3) 0.032(2) 0.0037(19) 0.0082(18) -0.001(2) C6 0.030(2) 0.040(2) 0.038(2) -0.0029(19) 0.0100(18) -0.0011(18) C4 0.038(3) 0.062(3) 0.043(2) 0.007(2) 0.024(2) -0.005(2) N2 0.0249(17) 0.055(2) 0.0356(16) 0.011(2) 0.0116(14) 0.003(2) C17 0.030(2) 0.033(2) 0.0282(17) -0.0014(15) 0.0075(15) 0.0003(16) C9 0.049(3) 0.049(3) 0.059(3) -0.001(2) 0.024(3) 0.007(2) C19 0.036(3) 0.092(5) 0.042(2) 0.007(3) 0.016(2) -0.002(3) N4 0.029(2) 0.096(4) 0.055(3) 0.036(3) 0.0138(19) 0.011(2) C2 0.028(2) 0.037(2) 0.0308(18) 0.0042(17) 0.0115(15) 0.0000(18) C3 0.034(2) 0.050(3) 0.040(2) 0.010(2) 0.0126(19) 0.003(2) C5 0.025(2) 0.057(3) 0.044(2) -0.002(2) 0.0117(18) -0.001(2) C1 0.0222(19) 0.046(2) 0.0329(19) 0.0054(17) 0.0086(15) 0.0023(17) N22 0.0227(15) 0.0377(17) 0.0284(14) -0.0007(16) 0.0082(12) -0.0014(16) N20 0.0231(17) 0.064(3) 0.0432(19) 0.0084(19) 0.0057(15) 0.0006(18) N21 0.0258(19) 0.054(2) 0.0376(19) 0.0093(18) 0.0065(16) -0.0034(17) N23 0.0261(18) 0.048(2) 0.0331(17) 0.0080(16) 0.0097(14) 0.0063(16) N8 0.031(2) 0.058(3) 0.066(3) -0.009(2) 0.011(2) -0.004(2) C8 0.051(3) 0.044(3) 0.057(3) -0.009(2) 0.020(3) 0.000(2) C20 0.028(2) 0.083(4) 0.042(2) 0.013(3) 0.0163(19) 0.003(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 Cd1 N19 2.290(4) . ? Cd1 N7 2.326(4) . ? Cd1 N13 2.328(4) . ? Cd1 N1 2.355(3) . ? Cd1 N5 2.380(3) . ? Cd1 N17 2.484(4) . ? Cd2 N14 2.305(4) . ? Cd2 N2 2.310(4) 1_455 ? Cd2 N22 2.338(3) 1_455 ? Cd2 N10 2.341(4) . ? Cd2 N23 2.385(3) 1_455 ? Cd2 N11 2.418(4) . ? N19 N20 1.322(5) . ? N19 N22 1.339(5) . ? N5 C5 1.330(6) . ? N5 C2 1.340(5) . ? N1 C1 1.325(5) . ? N1 N2 1.329(5) . ? C16 N21 1.336(6) . ? C16 N22 1.346(5) . ? C16 C17 1.443(6) . ? N13 C11 1.327(6) . ? N13 N14 1.338(5) . ? N7 N8 1.309(6) . ? N7 N10 1.349(5) . ? N11 C10 1.336(6) . ? N11 C7 1.341(6) . ? C13 N18 1.326(7) . ? C13 C12 1.402(7) . ? C12 N17 1.339(6) . ? C12 C11 1.450(6) . ? N24 C19 1.313(7) . ? N24 C18 1.346(6) . ? N17 C15 1.325(6) . ? C7 C8 1.390(7) . ? C7 C6 1.476(6) . ? N15 N14 1.312(6) . ? N15 N16 1.334(6) . ? N10 C6 1.316(6) . ? N9 C6 1.331(7) . ? N9 N8 1.342(7) . ? N6 C4 1.323(7) . ? N6 C3 1.329(7) . ? C14 N18 1.310(9) . ? C14 C15 1.391(8) . ? N16 C11 1.340(6) . ? N12 C9 1.315(8) . ? N12 C8 1.326(8) . ? N3 N2 1.299(6) . ? N3 N4 1.339(6) . ? C10 C9 1.387(7) . ? C18 C17 1.383(6) . ? C4 C5 1.381(7) . ? N2 Cd2 2.310(4) 1_655 ? C17 N23 1.337(6) . ? C19 C20 1.364(7) . ? N4 C1 1.329(6) . ? C2 C3 1.393(6) . ? C2 C1 1.472(6) . ? N22 Cd2 2.338(3) 1_655 ? N20 N21 1.333(5) . ? N23 C20 1.337(6) . ? N23 Cd2 2.385(3) 1_655 ? 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 N19 Cd1 N7 95.00(14) . . ? N19 Cd1 N13 104.86(12) . . ? N7 Cd1 N13 92.58(13) . . ? N19 Cd1 N1 92.26(12) . . ? N7 Cd1 N1 110.81(14) . . ? N13 Cd1 N1 149.80(13) . . ? N19 Cd1 N5 161.11(13) . . ? N7 Cd1 N5 85.06(14) . . ? N13 Cd1 N5 94.00(12) . . ? N1 Cd1 N5 70.26(12) . . ? N19 Cd1 N17 89.71(14) . . ? N7 Cd1 N17 162.93(13) . . ? N13 Cd1 N17 70.35(13) . . ? N1 Cd1 N17 85.33(14) . . ? N5 Cd1 N17 95.74(13) . . ? N14 Cd2 N2 90.15(15) . 1_455 ? N14 Cd2 N22 109.27(13) . 1_455 ? N2 Cd2 N22 91.89(12) 1_455 1_455 ? N14 Cd2 N10 91.88(13) . . ? N2 Cd2 N10 107.07(13) 1_455 . ? N22 Cd2 N10 151.70(14) 1_455 . ? N14 Cd2 N23 86.12(13) . 1_455 ? N2 Cd2 N23 159.62(14) 1_455 1_455 ? N22 Cd2 N23 70.61(12) 1_455 1_455 ? N10 Cd2 N23 93.09(13) . 1_455 ? N14 Cd2 N11 162.12(13) . . ? N2 Cd2 N11 93.15(16) 1_455 . ? N22 Cd2 N11 88.20(14) 1_455 . ? N10 Cd2 N11 70.34(13) . . ? N23 Cd2 N11 96.53(13) 1_455 . ? N20 N19 N22 109.4(3) . . ? N20 N19 Cd1 123.3(3) . . ? N22 N19 Cd1 126.8(3) . . ? C5 N5 C2 117.6(4) . . ? C5 N5 Cd1 125.2(3) . . ? C2 N5 Cd1 117.0(3) . . ? C1 N1 N2 104.0(3) . . ? C1 N1 Cd1 114.8(3) . . ? N2 N1 Cd1 139.4(3) . . ? N21 C16 N22 111.0(4) . . ? N21 C16 C17 127.2(4) . . ? N22 C16 C17 121.8(4) . . ? C11 N13 N14 105.3(4) . . ? C11 N13 Cd1 116.0(3) . . ? N14 N13 Cd1 138.4(3) . . ? N8 N7 N10 109.4(4) . . ? N8 N7 Cd1 122.9(3) . . ? N10 N7 Cd1 127.5(3) . . ? C10 N11 C7 117.0(4) . . ? C10 N11 Cd2 126.1(3) . . ? C7 N11 Cd2 115.9(3) . . ? N18 C13 C12 121.8(5) . . ? N17 C12 C13 120.4(4) . . ? N17 C12 C11 116.3(4) . . ? C13 C12 C11 123.3(4) . . ? C19 N24 C18 115.8(4) . . ? C15 N17 C12 117.1(4) . . ? C15 N17 Cd1 128.3(4) . . ? C12 N17 Cd1 113.4(3) . . ? N11 C7 C8 121.5(5) . . ? N11 C7 C6 115.4(4) . . ? C8 C7 C6 123.1(5) . . ? N14 N15 N16 109.1(4) . . ? C6 N10 N7 104.1(4) . . ? C6 N10 Cd2 116.4(3) . . ? N7 N10 Cd2 139.5(3) . . ? C6 N9 N8 104.0(4) . . ? C4 N6 C3 117.0(4) . . ? N18 C14 C15 122.1(5) . . ? N15 N16 C11 105.3(4) . . ? N13 C11 N16 110.8(4) . . ? N13 C11 C12 123.0(4) . . ? N16 C11 C12 126.2(5) . . ? N15 N14 N13 109.5(4) . . ? N15 N14 Cd2 121.0(3) . . ? N13 N14 Cd2 129.2(3) . . ? C14 N18 C13 117.1(5) . . ? C9 N12 C8 117.2(5) . . ? N2 N3 N4 109.2(4) . . ? N17 C15 C14 121.4(5) . . ? N11 C10 C9 120.4(5) . . ? N24 C18 C17 122.1(4) . . ? N10 C6 N9 112.9(4) . . ? N10 C6 C7 121.5(4) . . ? N9 C6 C7 125.6(5) . . ? N6 C4 C5 122.5(4) . . ? N3 N2 N1 110.5(3) . . ? N3 N2 Cd2 123.4(3) . 1_655 ? N1 N2 Cd2 125.9(3) . 1_655 ? N23 C17 C18 120.5(4) . . ? N23 C17 C16 115.4(4) . . ? C18 C17 C16 124.1(4) . . ? N12 C9 C10 122.8(5) . . ? N24 C19 C20 123.2(5) . . ? C1 N4 N3 104.1(4) . . ? N5 C2 C3 120.8(4) . . ? N5 C2 C1 115.0(3) . . ? C3 C2 C1 124.1(4) . . ? N6 C3 C2 121.4(5) . . ? N5 C5 C4 120.6(5) . . ? N1 C1 N4 112.3(4) . . ? N1 C1 C2 121.1(4) . . ? N4 C1 C2 126.6(4) . . ? N19 N22 C16 104.8(3) . . ? N19 N22 Cd2 139.6(2) . 1_655 ? C16 N22 Cd2 114.8(3) . 1_655 ? N19 N20 N21 109.4(3) . . ? N20 N21 C16 105.4(4) . . ? C17 N23 C20 117.1(4) . . ? C17 N23 Cd2 117.0(3) . 1_655 ? C20 N23 Cd2 125.8(3) . 1_655 ? N7 N8 N9 109.6(4) . . ? N12 C8 C7 121.1(6) . . ? N23 C20 C19 121.2(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.953 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.096 data_Complex_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C5 H3 N6) Ag' _chemical_formula_sum 'C5 H3 Ag N6' _chemical_formula_weight 255.00 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' 'Ag' 'Ag' -0.8971 1.1015 '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 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 3.5465(6) _cell_length_b 12.373(2) _cell_length_c 14.679(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.638(3) _cell_angle_gamma 90.00 _cell_volume 643.45(19) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description club _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 3.069 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4156 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.25 _reflns_number_total 1559 _reflns_number_gt 1391 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0262P)^2^+0.8442P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1559 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 N3 N 0.9933(7) 0.54039(19) 0.21410(17) 0.0293(5) Uani 1 1 d . . . Ag1 Ag 1.29350(10) 0.70011(2) 0.215984(16) 0.04781(12) Uani 1 1 d . . . N5 N 0.5180(7) 0.22161(18) 0.12069(16) 0.0269(5) Uani 1 1 d . . . N2 N 0.9690(8) 0.4691(2) 0.28063(17) 0.0322(6) Uani 1 1 d . . . C1 C 0.7790(8) 0.3970(2) 0.15534(18) 0.0230(5) Uani 1 1 d . . . N6 N 0.5185(7) 0.2646(2) -0.06598(17) 0.0305(5) Uani 1 1 d . . . C2 C 0.6360(7) 0.3164(2) 0.08916(18) 0.0224(5) Uani 1 1 d . . . N4 N 0.8763(7) 0.49680(19) 0.13391(16) 0.0289(5) Uani 1 1 d . . . N1 N 0.8331(7) 0.37744(19) 0.24470(16) 0.0296(5) Uani 1 1 d . . . C3 C 0.6317(8) 0.3381(2) -0.00425(19) 0.0265(6) Uani 1 1 d . . . H10 H 0.7099 0.4056 -0.0239 0.032 Uiso 1 1 calc R . . C5 C 0.4017(8) 0.1486(2) 0.0582(2) 0.0303(6) Uani 1 1 d . . . H12 H 0.3163 0.0818 0.0777 0.036 Uiso 1 1 calc R . . C4 C 0.4042(9) 0.1690(2) -0.0339(2) 0.0303(6) Uani 1 1 d . . . H13 H 0.3249 0.1154 -0.0748 0.036 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 N3 0.0382(14) 0.0225(11) 0.0269(12) -0.0027(9) -0.0019(10) -0.0016(10) Ag1 0.0918(3) 0.02611(15) 0.02554(14) -0.00707(9) 0.00246(13) -0.01088(12) N5 0.0328(13) 0.0218(11) 0.0260(12) 0.0024(9) 0.0005(10) 0.0015(9) N2 0.0446(16) 0.0274(12) 0.0241(12) -0.0016(10) -0.0028(10) 0.0007(11) C1 0.0273(13) 0.0216(12) 0.0202(12) 0.0005(10) 0.0012(10) 0.0036(10) N6 0.0379(14) 0.0277(12) 0.0255(12) -0.0027(10) -0.0021(10) 0.0013(10) C2 0.0228(13) 0.0205(12) 0.0240(13) 0.0012(10) 0.0012(10) 0.0028(10) N4 0.0404(14) 0.0220(11) 0.0240(11) 0.0003(9) -0.0015(10) -0.0029(10) N1 0.0432(15) 0.0233(12) 0.0220(11) 0.0011(9) -0.0022(10) -0.0009(10) C3 0.0327(15) 0.0218(12) 0.0250(13) 0.0017(11) -0.0002(11) -0.0019(11) C5 0.0326(15) 0.0218(13) 0.0362(16) 0.0008(11) -0.0001(12) -0.0032(11) C4 0.0350(16) 0.0226(13) 0.0329(15) -0.0056(11) -0.0034(12) 0.0003(11) _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 N3 N2 1.322(3) . ? N3 N4 1.343(3) . ? N3 Ag1 2.244(2) . ? Ag1 N1 2.318(2) 2_755 ? Ag1 N6 2.370(3) 3_765 ? Ag1 N5 2.473(2) 2_755 ? N5 C2 1.336(3) . ? N5 C5 1.339(4) . ? N5 Ag1 2.473(2) 2_745 ? N2 N1 1.332(3) . ? C1 N4 1.324(4) . ? C1 N1 1.339(4) . ? C1 C2 1.466(4) . ? N6 C3 1.333(4) . ? N6 C4 1.343(4) . ? N6 Ag1 2.370(3) 3_765 ? C2 C3 1.397(4) . ? N1 Ag1 2.318(2) 2_745 ? C5 C4 1.375(4) . ? 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 N2 N3 N4 110.6(2) . . ? N2 N3 Ag1 128.73(19) . . ? N4 N3 Ag1 119.45(18) . . ? N3 Ag1 N1 137.68(9) . 2_755 ? N3 Ag1 N6 107.72(9) . 3_765 ? N1 Ag1 N6 97.05(9) 2_755 3_765 ? N3 Ag1 N5 102.33(8) . 2_755 ? N1 Ag1 N5 72.76(8) 2_755 2_755 ? N6 Ag1 N5 143.66(9) 3_765 2_755 ? C2 N5 C5 116.5(2) . . ? C2 N5 Ag1 110.82(18) . 2_745 ? C5 N5 Ag1 130.76(19) . 2_745 ? N3 N2 N1 108.1(2) . . ? N4 C1 N1 112.0(2) . . ? N4 C1 C2 124.2(2) . . ? N1 C1 C2 123.8(2) . . ? C3 N6 C4 116.7(3) . . ? C3 N6 Ag1 114.62(19) . 3_765 ? C4 N6 Ag1 126.21(19) . 3_765 ? N5 C2 C3 121.3(3) . . ? N5 C2 C1 118.2(2) . . ? C3 C2 C1 120.5(2) . . ? C1 N4 N3 103.9(2) . . ? N2 N1 C1 105.5(2) . . ? N2 N1 Ag1 141.10(19) . 2_745 ? C1 N1 Ag1 113.22(18) . 2_745 ? N6 C3 C2 121.7(3) . . ? N5 C5 C4 122.3(3) . . ? N6 C4 C5 121.5(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.504 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.090 data_Complex_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cd2(C5 H3 N6)(OH)(SO4)' _chemical_formula_sum 'C5 H4 Cd2 N6 O5 S' _chemical_formula_weight 485.00 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y, z-1/2' _cell_length_a 20.1345(5) _cell_length_b 10.5451(3) _cell_length_c 13.3534(3) _cell_angle_alpha 90.00 _cell_angle_beta 131.39 _cell_angle_gamma 90.00 _cell_volume 2127.07(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.49 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 4.224 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3195 _exptl_absorpt_correction_T_max 0.4181 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8513 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2399 _reflns_number_gt 2316 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0385P)^2^+1.2639P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00227(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2399 _refine_ls_number_parameters 179 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Cd1 Cd 0.2500 0.52722(3) 0.2500 0.02004(9) Uani 1 2 d S . . Cd2 Cd 0.0000 0.5000 0.0000 0.01864(10) Uani 1 2 d S . . Cd3 Cd 0.135753(12) 0.260221(16) 0.007201(18) 0.01723(9) Uani 1 1 d . . . S1 S 0.13191(4) 0.28178(6) 0.25274(6) 0.01549(14) Uani 1 1 d . . . O1 O 0.21870(11) 0.34820(19) 0.33384(19) 0.0279(4) Uani 1 1 d . . . O2 O 0.06107(12) 0.37603(19) 0.18838(19) 0.0266(4) Uani 1 1 d . . . O3 O 0.12114(14) 0.2003(2) 0.1538(2) 0.0292(4) Uani 1 1 d . . . O4 O 0.13024(13) 0.19841(18) 0.33957(18) 0.0235(4) Uani 1 1 d . . . O5 O 0.12565(12) 0.46971(17) 0.04020(17) 0.0190(4) Uani 1 1 d D . . H5O H 0.124(3) 0.514(3) -0.015(3) 0.042(11) Uiso 1 1 d D . . N1 N 0.34227(13) 0.6765(2) 0.2588(2) 0.0197(4) Uani 1 1 d . . . N2 N 0.43028(14) 0.6602(2) 0.3474(2) 0.0211(4) Uani 1 1 d . . . N3 N 0.46964(15) 0.7603(2) 0.3482(2) 0.0219(5) Uani 1 1 d . . . N4 N 0.40877(14) 0.8466(2) 0.2613(2) 0.0239(5) Uani 1 1 d . . . N5 N 0.15813(15) 1.0407(2) 0.0098(2) 0.0224(4) Uani 1 1 d . . . N6 N 0.17441(16) 0.7760(2) 0.0334(3) 0.0255(5) Uani 1 1 d . . . C1 C 0.33112(16) 0.7922(2) 0.2080(3) 0.0191(5) Uani 1 1 d . . . C2 C 0.24451(15) 0.8529(2) 0.1085(2) 0.0187(5) Uani 1 1 d . . . C3 C 0.23721(18) 0.9842(3) 0.0981(3) 0.0233(5) Uani 1 1 d . . . H3 H 0.2880 1.0337 0.1533 0.028 Uiso 1 1 calc R . . C4 C 0.08771(18) 0.9648(3) -0.0672(3) 0.0288(6) Uani 1 1 d . . . H4 H 0.0318 1.0006 -0.1302 0.035 Uiso 1 1 calc R . . C5 C 0.09588(18) 0.8341(3) -0.0557(3) 0.0318(6) Uani 1 1 d . . . H5 H 0.0451 0.7847 -0.1116 0.038 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 Cd1 0.01180(14) 0.01774(15) 0.02348(16) 0.000 0.00864(12) 0.000 Cd2 0.01103(14) 0.01748(15) 0.02025(15) -0.00386(9) 0.00729(12) 0.00068(9) Cd3 0.01928(13) 0.01657(12) 0.01803(13) 0.00074(6) 0.01326(11) 0.00236(6) S1 0.0142(3) 0.0178(3) 0.0144(3) 0.0014(2) 0.0094(3) -0.0002(2) O1 0.0145(8) 0.0330(11) 0.0269(10) 0.0019(8) 0.0097(8) -0.0046(8) O2 0.0203(9) 0.0253(10) 0.0306(10) 0.0084(8) 0.0153(8) 0.0055(8) O3 0.0450(12) 0.0255(10) 0.0282(10) -0.0044(8) 0.0290(10) -0.0047(9) O4 0.0335(10) 0.0212(9) 0.0250(9) 0.0038(7) 0.0233(9) 0.0025(8) O5 0.0160(8) 0.0182(9) 0.0218(9) 0.0018(7) 0.0121(8) 0.0022(7) N1 0.0147(9) 0.0164(10) 0.0218(10) 0.0028(8) 0.0095(9) 0.0007(8) N2 0.0150(9) 0.0197(10) 0.0222(10) 0.0033(8) 0.0097(9) 0.0008(8) N3 0.0166(10) 0.0194(11) 0.0248(12) 0.0030(8) 0.0116(10) 0.0004(8) N4 0.0153(10) 0.0188(11) 0.0275(11) 0.0034(9) 0.0098(9) -0.0010(8) N5 0.0224(11) 0.0201(11) 0.0234(11) 0.0037(8) 0.0146(10) 0.0053(9) N6 0.0182(11) 0.0201(11) 0.0299(13) 0.0002(9) 0.0123(10) -0.0010(9) C1 0.0158(12) 0.0148(11) 0.0213(12) 0.0016(9) 0.0100(11) 0.0008(9) C2 0.0159(11) 0.0176(12) 0.0196(11) 0.0008(9) 0.0105(10) 0.0002(9) C3 0.0183(12) 0.0188(13) 0.0249(13) 0.0008(10) 0.0109(11) 0.0003(10) C4 0.0182(13) 0.0297(15) 0.0279(14) 0.0025(11) 0.0108(12) 0.0047(11) C5 0.0161(12) 0.0259(14) 0.0356(15) -0.0030(12) 0.0095(12) -0.0019(11) _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 Cd1 O5 2.2825(18) . ? Cd1 O5 2.2825(18) 4_545 ? Cd1 N1 2.377(2) . ? Cd1 N1 2.377(2) 4_545 ? Cd1 O1 2.4794(19) 4_545 ? Cd1 O1 2.4794(19) . ? Cd2 O5 2.2348(18) 5_565 ? Cd2 O5 2.2348(18) . ? Cd2 N2 2.279(2) 8_465 ? Cd2 N2 2.279(2) 4_545 ? Cd2 O2 2.3364(18) 5_565 ? Cd2 O2 2.3364(18) . ? Cd3 O4 2.2102(17) 6_565 ? Cd3 O3 2.2535(19) . ? Cd3 O5 2.2879(18) . ? Cd3 N5 2.355(2) 1_545 ? Cd3 O1 2.3935(18) 4_545 ? Cd3 N3 2.520(2) 8_465 ? S1 O2 1.4629(19) . ? S1 O3 1.467(2) . ? S1 O4 1.4730(18) . ? S1 O1 1.4881(18) . ? O1 Cd3 2.3935(18) 4_545 ? O4 Cd3 2.2102(17) 6_566 ? O5 H5O 0.850(10) . ? N1 N2 1.341(3) . ? N1 C1 1.341(3) . ? N2 N3 1.316(3) . ? N2 Cd2 2.279(2) 4_545 ? N3 N4 1.340(3) . ? N3 Cd3 2.520(2) 8_566 ? N4 C1 1.345(3) . ? N5 C4 1.334(4) . ? N5 C3 1.341(3) . ? N5 Cd3 2.355(2) 1_565 ? N6 C2 1.336(3) . ? N6 C5 1.343(4) . ? C1 C2 1.467(3) . ? C2 C3 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? 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 O5 Cd1 O5 149.19(9) . 4_545 ? O5 Cd1 N1 115.08(7) . . ? O5 Cd1 N1 85.86(7) 4_545 . ? O5 Cd1 N1 85.86(7) . 4_545 ? O5 Cd1 N1 115.08(7) 4_545 4_545 ? N1 Cd1 N1 97.10(10) . 4_545 ? O5 Cd1 O1 69.12(6) . 4_545 ? O5 Cd1 O1 87.24(6) 4_545 4_545 ? N1 Cd1 O1 95.91(7) . 4_545 ? N1 Cd1 O1 154.85(6) 4_545 4_545 ? O5 Cd1 O1 87.24(6) . . ? O5 Cd1 O1 69.12(6) 4_545 . ? N1 Cd1 O1 154.85(6) . . ? N1 Cd1 O1 95.91(7) 4_545 . ? O1 Cd1 O1 80.83(10) 4_545 . ? O5 Cd2 O5 180.00(13) 5_565 . ? O5 Cd2 N2 87.76(7) 5_565 8_465 ? O5 Cd2 N2 92.24(7) . 8_465 ? O5 Cd2 N2 92.24(7) 5_565 4_545 ? O5 Cd2 N2 87.76(7) . 4_545 ? N2 Cd2 N2 180.00(12) 8_465 4_545 ? O5 Cd2 O2 87.43(6) 5_565 5_565 ? O5 Cd2 O2 92.57(6) . 5_565 ? N2 Cd2 O2 82.96(7) 8_465 5_565 ? N2 Cd2 O2 97.04(7) 4_545 5_565 ? O5 Cd2 O2 92.57(6) 5_565 . ? O5 Cd2 O2 87.43(6) . . ? N2 Cd2 O2 97.04(7) 8_465 . ? N2 Cd2 O2 82.96(7) 4_545 . ? O2 Cd2 O2 180.00(12) 5_565 . ? O4 Cd3 O3 170.77(7) 6_565 . ? O4 Cd3 O5 93.05(7) 6_565 . ? O3 Cd3 O5 91.39(7) . . ? O4 Cd3 N5 95.17(7) 6_565 1_545 ? O3 Cd3 N5 81.08(8) . 1_545 ? O5 Cd3 N5 170.80(7) . 1_545 ? O4 Cd3 O1 91.94(7) 6_565 4_545 ? O3 Cd3 O1 97.17(7) . 4_545 ? O5 Cd3 O1 70.59(6) . 4_545 ? N5 Cd3 O1 104.94(7) 1_545 4_545 ? O4 Cd3 N3 90.80(8) 6_565 8_465 ? O3 Cd3 N3 81.07(8) . 8_465 ? O5 Cd3 N3 90.45(7) . 8_465 ? N5 Cd3 N3 93.57(7) 1_545 8_465 ? O1 Cd3 N3 160.95(7) 4_545 8_465 ? O2 S1 O3 111.27(12) . . ? O2 S1 O4 110.31(11) . . ? O3 S1 O4 107.02(12) . . ? O2 S1 O1 109.11(12) . . ? O3 S1 O1 109.52(12) . . ? O4 S1 O1 109.57(11) . . ? S1 O1 Cd3 128.54(12) . 4_545 ? S1 O1 Cd1 123.82(11) . . ? Cd3 O1 Cd1 99.66(6) 4_545 . ? S1 O2 Cd2 128.85(11) . . ? S1 O3 Cd3 126.27(12) . . ? S1 O4 Cd3 131.87(12) . 6_566 ? Cd2 O5 Cd1 113.94(8) . . ? Cd2 O5 Cd3 108.81(7) . . ? Cd1 O5 Cd3 109.14(7) . . ? Cd2 O5 H5O 108(3) . . ? Cd1 O5 H5O 108(3) . . ? Cd3 O5 H5O 109(3) . . ? N2 N1 C1 104.14(19) . . ? N2 N1 Cd1 119.52(15) . . ? C1 N1 Cd1 135.52(16) . . ? N3 N2 N1 110.0(2) . . ? N3 N2 Cd2 125.16(16) . 4_545 ? N1 N2 Cd2 123.87(16) . 4_545 ? N2 N3 N4 109.7(2) . . ? N2 N3 Cd3 113.23(15) . 8_566 ? N4 N3 Cd3 137.10(17) . 8_566 ? N3 N4 C1 104.3(2) . . ? C4 N5 C3 116.8(2) . . ? C4 N5 Cd3 118.86(18) . 1_565 ? C3 N5 Cd3 123.66(18) . 1_565 ? C2 N6 C5 115.4(2) . . ? N1 C1 N4 111.9(2) . . ? N1 C1 C2 123.8(2) . . ? N4 C1 C2 124.3(2) . . ? N6 C2 C3 122.7(2) . . ? N6 C2 C1 116.6(2) . . ? C3 C2 C1 120.6(2) . . ? N5 C3 C2 121.1(2) . . ? N5 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? N5 C4 C5 121.6(3) . . ? N5 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? N6 C5 C4 122.4(3) . . ? N6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? 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 O2 S1 O1 Cd3 169.58(13) . . . 4_545 ? O3 S1 O1 Cd3 -68.40(17) . . . 4_545 ? O4 S1 O1 Cd3 48.70(17) . . . 4_545 ? O2 S1 O1 Cd1 -48.07(15) . . . . ? O3 S1 O1 Cd1 73.96(15) . . . . ? O4 S1 O1 Cd1 -168.94(11) . . . . ? O5 Cd1 O1 S1 -15.72(14) . . . . ? O5 Cd1 O1 S1 -175.54(16) 4_545 . . . ? N1 Cd1 O1 S1 -169.34(13) . . . . ? N1 Cd1 O1 S1 69.83(14) 4_545 . . . ? O1 Cd1 O1 S1 -85.00(14) 4_545 . . . ? O5 Cd1 O1 Cd3 135.30(7) . . . 4_545 ? O5 Cd1 O1 Cd3 -24.53(6) 4_545 . . 4_545 ? N1 Cd1 O1 Cd3 -18.3(2) . . . 4_545 ? N1 Cd1 O1 Cd3 -139.15(7) 4_545 . . 4_545 ? O1 Cd1 O1 Cd3 66.01(6) 4_545 . . 4_545 ? O3 S1 O2 Cd2 -43.23(18) . . . . ? O4 S1 O2 Cd2 -161.85(13) . . . . ? O1 S1 O2 Cd2 77.73(16) . . . . ? O5 Cd2 O2 S1 157.59(15) 5_565 . . . ? O5 Cd2 O2 S1 -22.41(15) . . . . ? N2 Cd2 O2 S1 69.53(15) 8_465 . . . ? N2 Cd2 O2 S1 -110.47(15) 4_545 . . . ? O2 Cd2 O2 S1 177(91) 5_565 . . . ? O2 S1 O3 Cd3 68.21(17) . . . . ? O4 S1 O3 Cd3 -171.21(13) . . . . ? O1 S1 O3 Cd3 -52.52(18) . . . . ? O4 Cd3 O3 S1 -134.9(4) 6_565 . . . ? O5 Cd3 O3 S1 -16.12(16) . . . . ? N5 Cd3 O3 S1 158.57(17) 1_545 . . . ? O1 Cd3 O3 S1 54.48(16) 4_545 . . . ? N3 Cd3 O3 S1 -106.36(16) 8_465 . . . ? O2 S1 O4 Cd3 -55.63(18) . . . 6_566 ? O3 S1 O4 Cd3 -176.82(14) . . . 6_566 ? O1 S1 O4 Cd3 64.51(18) . . . 6_566 ? O5 Cd2 O5 Cd1 17.9(13) 5_565 . . . ? N2 Cd2 O5 Cd1 -151.93(9) 8_465 . . . ? N2 Cd2 O5 Cd1 28.07(9) 4_545 . . . ? O2 Cd2 O5 Cd1 125.02(8) 5_565 . . . ? O2 Cd2 O5 Cd1 -54.98(8) . . . . ? O5 Cd2 O5 Cd3 139.9(11) 5_565 . . . ? N2 Cd2 O5 Cd3 -29.91(8) 8_465 . . . ? N2 Cd2 O5 Cd3 150.09(8) 4_545 . . . ? O2 Cd2 O5 Cd3 -112.96(8) 5_565 . . . ? O2 Cd2 O5 Cd3 67.04(8) . . . . ? O5 Cd1 O5 Cd2 106.53(7) 4_545 . . . ? N1 Cd1 O5 Cd2 -124.48(8) . . . . ? N1 Cd1 O5 Cd2 -28.57(9) 4_545 . . . ? O1 Cd1 O5 Cd2 148.78(10) 4_545 . . . ? O1 Cd1 O5 Cd2 67.55(8) . . . . ? O5 Cd1 O5 Cd3 -15.30(5) 4_545 . . . ? N1 Cd1 O5 Cd3 113.69(8) . . . . ? N1 Cd1 O5 Cd3 -150.41(8) 4_545 . . . ? O1 Cd1 O5 Cd3 26.95(7) 4_545 . . . ? O1 Cd1 O5 Cd3 -54.28(8) . . . . ? O4 Cd3 O5 Cd2 116.42(8) 6_565 . . . ? O3 Cd3 O5 Cd2 -55.48(8) . . . . ? N5 Cd3 O5 Cd2 -90.4(4) 1_545 . . . ? O1 Cd3 O5 Cd2 -152.60(9) 4_545 . . . ? N3 Cd3 O5 Cd2 25.59(9) 8_465 . . . ? O4 Cd3 O5 Cd1 -118.70(8) 6_565 . . . ? O3 Cd3 O5 Cd1 69.40(8) . . . . ? N5 Cd3 O5 Cd1 34.5(5) 1_545 . . . ? O1 Cd3 O5 Cd1 -27.72(7) 4_545 . . . ? N3 Cd3 O5 Cd1 150.48(9) 8_465 . . . ? O5 Cd1 N1 N2 -137.10(17) . . . . ? O5 Cd1 N1 N2 19.37(18) 4_545 . . . ? N1 Cd1 N1 N2 134.2(2) 4_545 . . . ? O1 Cd1 N1 N2 -67.42(18) 4_545 . . . ? O1 Cd1 N1 N2 13.6(3) . . . . ? O5 Cd1 N1 C1 55.1(3) . . . . ? O5 Cd1 N1 C1 -148.4(3) 4_545 . . . ? N1 Cd1 N1 C1 -33.6(2) 4_545 . . . ? O1 Cd1 N1 C1 124.8(3) 4_545 . . . ? O1 Cd1 N1 C1 -154.2(2) . . . . ? C1 N1 N2 N3 -0.7(3) . . . . ? Cd1 N1 N2 N3 -171.91(16) . . . . ? C1 N1 N2 Cd2 168.45(17) . . . 4_545 ? Cd1 N1 N2 Cd2 -2.7(3) . . . 4_545 ? N1 N2 N3 N4 0.7(3) . . . . ? Cd2 N2 N3 N4 -168.25(18) 4_545 . . . ? N1 N2 N3 Cd3 -178.64(15) . . . 8_566 ? Cd2 N2 N3 Cd3 12.4(3) 4_545 . . 8_566 ? N2 N3 N4 C1 -0.4(3) . . . . ? Cd3 N3 N4 C1 178.7(2) 8_566 . . . ? N2 N1 C1 N4 0.4(3) . . . . ? Cd1 N1 C1 N4 169.49(18) . . . . ? N2 N1 C1 C2 -178.1(2) . . . . ? Cd1 N1 C1 C2 -9.1(4) . . . . ? N3 N4 C1 N1 0.0(3) . . . . ? N3 N4 C1 C2 178.6(2) . . . . ? C5 N6 C2 C3 1.5(4) . . . . ? C5 N6 C2 C1 179.2(3) . . . . ? N1 C1 C2 N6 -23.4(4) . . . . ? N4 C1 C2 N6 158.2(3) . . . . ? N1 C1 C2 C3 154.4(3) . . . . ? N4 C1 C2 C3 -24.0(4) . . . . ? C4 N5 C3 C2 -0.4(4) . . . . ? Cd3 N5 C3 C2 169.86(19) 1_565 . . . ? N6 C2 C3 N5 -0.6(4) . . . . ? C1 C2 C3 N5 -178.3(2) . . . . ? C3 N5 C4 C5 0.6(4) . . . . ? Cd3 N5 C4 C5 -170.2(2) 1_565 . . . ? C2 N6 C5 C4 -1.3(5) . . . . ? N5 C4 C5 N6 0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.566 _refine_diff_density_min -1.300 _refine_diff_density_rms 0.194