Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_year 2004 _journal_volume 6 _journal_page_first 549 _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_contact_author_address ; College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China ; _publ_contact_author_email chyan@chem.pku.edu.cn _publ_contact_author_phone 86-(10)-62754179 _publ_contact_author_fax 86-(10)-62754179 _publ_requested_category FO _publ_contact_letter ; ? ; _publ_section_title ; High-dimensional azido-bridged cadmium(II) polymeric complexes with bis(bidentate) diazine ligands ; loop_ _publ_author_name 'Yan-Feng Yue' 'En-Qing Gao' 'Shi-Qiang Bai' 'Zheng He' 'Chun-Hua Yan' ## Crystallographic Data of Complex 1 data_1 _database_code_depnum_ccdc_archive 'CCDC 244388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cd2 N16' _chemical_formula_weight 603.16 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.62200(10) _cell_length_b 7.7322(2) _cell_length_c 9.8897(4) _cell_angle_alpha 80.5127(10) _cell_angle_beta 88.4579(11) _cell_angle_gamma 70.5583(18) _cell_volume 470.76(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6987 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 290 _exptl_absorpt_coefficient_mu 2.298 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.734 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9130 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2135 _reflns_number_gt 1882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press, London. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0396P)^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 SHELXL _refine_ls_extinction_coef 0.028(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2135 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Cd1 Cd 0.21316(3) 0.10236(3) 0.95263(2) 0.03343(12) Uani 1 1 d . . . C1 C 0.2965(5) 0.1889(5) 0.6254(4) 0.0442(8) Uani 1 1 d . . . H1A H 0.3312 0.0607 0.6335 0.053 Uiso 1 1 calc R . . C2 C 0.3189(6) 0.2885(5) 0.4998(4) 0.0471(8) Uani 1 1 d . . . H2A H 0.3658 0.2282 0.4251 0.057 Uiso 1 1 calc R . . C3 C 0.2715(5) 0.4761(5) 0.4865(3) 0.0426(7) Uani 1 1 d . . . H3A H 0.2883 0.5453 0.4033 0.051 Uiso 1 1 calc R . . C4 C 0.1977(5) 0.5618(5) 0.5992(3) 0.0401(7) Uani 1 1 d . . . H4A H 0.1641 0.6897 0.5929 0.048 Uiso 1 1 calc R . . C5 C 0.1750(4) 0.4548(4) 0.7206(3) 0.0335(6) Uani 1 1 d . . . C6 C 0.0855(5) 0.5409(4) 0.8410(3) 0.0344(6) Uani 1 1 d . . . H6A H 0.0584 0.6676 0.8375 0.041 Uiso 1 1 calc R . . N1 N 0.2272(4) 0.2685(3) 0.7354(3) 0.0350(5) Uani 1 1 d . . . N2 N 0.0444(4) 0.4472(3) 0.9489(3) 0.0314(5) Uani 1 1 d . . . N3 N -0.0474(5) 0.0033(4) 0.8614(3) 0.0427(6) Uani 1 1 d . . . N4 N -0.1155(5) 0.0334(4) 0.7461(3) 0.0417(6) Uani 1 1 d . . . N5 N -0.1770(6) 0.0580(6) 0.6343(4) 0.0701(10) Uani 1 1 d . . . N6 N 0.5160(4) -0.1432(4) 0.9212(3) 0.0457(7) Uani 1 1 d . . . N7 N 0.5250(4) -0.2805(4) 0.8772(3) 0.0393(6) Uani 1 1 d . . . N8 N 0.5369(6) -0.4123(5) 0.8344(4) 0.0679(10) Uani 1 1 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 Cd1 0.02843(15) 0.02773(15) 0.04350(17) -0.00147(9) 0.00014(9) -0.01054(9) C1 0.0428(17) 0.0348(17) 0.053(2) -0.0108(15) 0.0085(15) -0.0090(14) C2 0.0423(18) 0.053(2) 0.0443(19) -0.0141(16) 0.0068(14) -0.0104(16) C3 0.0361(16) 0.052(2) 0.0394(18) -0.0029(15) 0.0043(13) -0.0168(15) C4 0.0407(17) 0.0369(16) 0.0435(18) -0.0004(13) 0.0003(13) -0.0169(14) C5 0.0291(14) 0.0298(14) 0.0416(17) -0.0048(12) 0.0014(12) -0.0104(11) C6 0.0369(15) 0.0232(13) 0.0407(17) -0.0016(12) 0.0003(12) -0.0085(12) N1 0.0337(13) 0.0280(12) 0.0420(14) -0.0058(11) 0.0036(10) -0.0087(10) N2 0.0263(11) 0.0260(12) 0.0392(14) -0.0047(10) 0.0006(9) -0.0055(9) N3 0.0427(14) 0.0505(16) 0.0420(16) 0.0006(13) -0.0029(12) -0.0284(13) N4 0.0407(14) 0.0354(14) 0.0501(19) -0.0005(12) 0.0022(13) -0.0173(12) N5 0.077(3) 0.086(3) 0.049(2) 0.0046(18) -0.0126(18) -0.037(2) N6 0.0298(13) 0.0337(14) 0.072(2) -0.0119(14) -0.0080(13) -0.0056(11) N7 0.0335(13) 0.0429(16) 0.0424(15) -0.0095(13) -0.0006(11) -0.0125(12) N8 0.063(2) 0.072(2) 0.080(3) -0.042(2) 0.0016(18) -0.0236(19) _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 N3 2.290(3) 2_557 ? Cd1 N6 2.313(3) . ? Cd1 N1 2.331(3) . ? Cd1 N6 2.345(3) 2_657 ? Cd1 N3 2.360(3) . ? Cd1 N2 2.519(2) . ? C1 N1 1.334(4) . ? C1 C2 1.381(5) . ? C2 C3 1.362(5) . ? C3 C4 1.385(5) . ? C4 C5 1.377(4) . ? C5 N1 1.349(4) . ? C5 C6 1.474(4) . ? C6 N2 1.265(4) . ? N2 N2 1.398(5) 2_567 ? N3 N4 1.195(4) . ? N3 Cd1 2.290(3) 2_557 ? N4 N5 1.152(5) . ? N6 N7 1.195(4) . ? N6 Cd1 2.345(3) 2_657 ? N7 N8 1.145(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 N3 Cd1 N6 106.43(11) 2_557 . ? N3 Cd1 N1 155.29(10) 2_557 . ? N6 Cd1 N1 93.14(10) . . ? N3 Cd1 N6 95.94(11) 2_557 2_657 ? N6 Cd1 N6 75.78(11) . 2_657 ? N1 Cd1 N6 103.53(10) . 2_657 ? N3 Cd1 N3 74.54(11) 2_557 . ? N6 Cd1 N3 99.05(10) . . ? N1 Cd1 N3 87.82(9) . . ? N6 Cd1 N3 167.64(10) 2_657 . ? N3 Cd1 N2 99.28(10) 2_557 . ? N6 Cd1 N2 147.68(9) . . ? N1 Cd1 N2 68.87(8) . . ? N6 Cd1 N2 82.48(9) 2_657 . ? N3 Cd1 N2 106.53(9) . . ? N1 C1 C2 122.9(3) . . ? C3 C2 C1 119.3(3) . . ? C2 C3 C4 118.7(3) . . ? C5 C4 C3 119.0(3) . . ? N1 C5 C4 122.5(3) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 121.0(3) . . ? N2 C6 C5 121.8(3) . . ? C1 N1 C5 117.5(3) . . ? C1 N1 Cd1 123.7(2) . . ? C5 N1 Cd1 118.6(2) . . ? C6 N2 N2 113.8(3) . 2_567 ? C6 N2 Cd1 112.1(2) . . ? N2 N2 Cd1 132.6(2) 2_567 . ? N4 N3 Cd1 123.7(2) . 2_557 ? N4 N3 Cd1 129.2(2) . . ? Cd1 N3 Cd1 105.46(11) 2_557 . ? N5 N4 N3 178.2(4) . . ? N7 N6 Cd1 127.7(2) . . ? N7 N6 Cd1 126.3(2) . 2_657 ? Cd1 N6 Cd1 104.22(11) . 2_657 ? N8 N7 N6 178.9(4) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.583 _refine_diff_density_min -1.217 _refine_diff_density_rms 0.124 #===END # Crystallographic Data of Complex 2 data_2 _database_code_depnum_ccdc_archive 'CCDC 244389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 Cd2 Cl2 N16 O9' _chemical_formula_weight 1004.34 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' O O 0.0106 0.0060 '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 10.75430(10) _cell_length_b 15.5103(2) _cell_length_c 22.9109(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3821.59(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 46284 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58292 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8732 _reflns_number_gt 5504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press, London. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0704P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 8732 _refine_ls_number_parameters 473 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 Cd1 Cd 0.03816(4) 0.34175(3) 0.302451(17) 0.04049(17) Uani 1 1 d . . . Cd2 Cd 0.04851(4) 0.64883(3) 0.315498(19) 0.04122(17) Uani 1 1 d . . . C1 C 0.0975(8) 0.2517(5) 0.4257(5) 0.056(2) Uani 1 1 d . . . H1A H 0.0335 0.2146 0.4151 0.067 Uiso 1 1 calc R . . C2 C 0.1735(8) 0.2290(4) 0.4708(4) 0.052(2) Uani 1 1 d . . . H2A H 0.1621 0.1768 0.4900 0.062 Uiso 1 1 calc R . . C3 C 0.2678(7) 0.2844(5) 0.4878(4) 0.056(2) Uani 1 1 d . . . H3A H 0.3204 0.2700 0.5186 0.067 Uiso 1 1 calc R . . C4 C 0.2821(7) 0.3607(5) 0.4586(4) 0.047(2) Uani 1 1 d . . . H4A H 0.3435 0.3996 0.4695 0.057 Uiso 1 1 calc R . . C5 C 0.2023(6) 0.3789(4) 0.4120(3) 0.0385(18) Uani 1 1 d . . . C6 C 0.2132(6) 0.4600(5) 0.3783(4) 0.040(2) Uani 1 1 d . . . C7 C 0.2223(7) 0.5319(5) 0.2401(4) 0.037(2) Uani 1 1 d . . . C8 C 0.2730(9) 0.4551(5) 0.2095(4) 0.064(3) Uani 1 1 d . . . H8A H 0.2730 0.4066 0.2356 0.097 Uiso 1 1 calc R . . H8B H 0.3566 0.4667 0.1970 0.097 Uiso 1 1 calc R . . H8C H 0.2223 0.4423 0.1761 0.097 Uiso 1 1 calc R . . C9 C 0.2153(6) 0.6126(4) 0.2058(4) 0.0395(18) Uani 1 1 d . . . C10 C 0.2937(7) 0.6320(5) 0.1602(4) 0.054(2) Uani 1 1 d . . . H10A H 0.3533 0.5923 0.1482 0.064 Uiso 1 1 calc R . . C11 C 0.2836(8) 0.7100(5) 0.1325(4) 0.055(2) Uani 1 1 d . . . H11A H 0.3385 0.7238 0.1025 0.066 Uiso 1 1 calc R . . C12 C 0.1951(8) 0.7667(5) 0.1481(5) 0.060(2) Uani 1 1 d . . . H12A H 0.1861 0.8193 0.1291 0.072 Uiso 1 1 calc R . . C13 C 0.1174(7) 0.7431(4) 0.1942(4) 0.049(2) Uani 1 1 d . . . H13A H 0.0544 0.7809 0.2051 0.058 Uiso 1 1 calc R . . C14 C -0.0320(7) 0.2751(4) 0.1732(4) 0.055(2) Uani 1 1 d . . . H14A H 0.0198 0.2295 0.1832 0.066 Uiso 1 1 calc R . . C15 C -0.1015(10) 0.2709(5) 0.1241(5) 0.073(3) Uani 1 1 d . . . H15A H -0.0964 0.2217 0.1011 0.088 Uiso 1 1 calc R . . C16 C -0.1769(9) 0.3343(5) 0.1073(5) 0.070(3) Uani 1 1 d . . . H16A H -0.2210 0.3306 0.0725 0.084 Uiso 1 1 calc R . . C17 C -0.1881(7) 0.4054(5) 0.1428(4) 0.055(2) Uani 1 1 d . . . H17A H -0.2414 0.4505 0.1332 0.066 Uiso 1 1 calc R . . C18 C -0.1162(7) 0.4076(4) 0.1942(4) 0.0377(19) Uani 1 1 d . . . C19 C -0.1218(9) 0.4790(5) 0.2376(4) 0.043(2) Uani 1 1 d . . . C20 C -0.1558(9) 0.5591(5) 0.2168(4) 0.058(2) Uani 1 1 d . . . H20A H -0.1562 0.5998 0.2484 0.087 Uiso 1 1 calc R . . H20B H -0.2374 0.5559 0.2000 0.087 Uiso 1 1 calc R . . H20C H -0.0974 0.5774 0.1877 0.087 Uiso 1 1 calc R . . C21 C -0.1288(8) 0.5196(5) 0.3821(4) 0.036(2) Uani 1 1 d . . . C22 C -0.1139(6) 0.5916(5) 0.4221(4) 0.048(2) Uani 1 1 d . . . C23 C -0.1783(7) 0.5972(5) 0.4732(4) 0.055(2) Uani 1 1 d . . . H23A H -0.2315 0.5526 0.4838 0.065 Uiso 1 1 calc R . . C24 C -0.1664(9) 0.6659(5) 0.5085(5) 0.070(3) Uani 1 1 d . . . H24A H -0.2152 0.6701 0.5419 0.084 Uiso 1 1 calc R . . C25 C -0.0814(9) 0.7306(6) 0.4954(5) 0.074(3) Uani 1 1 d . . . H25A H -0.0695 0.7779 0.5197 0.089 Uiso 1 1 calc R . . C26 C -0.0145(7) 0.7199(5) 0.4428(5) 0.056(2) Uani 1 1 d . . . H26A H 0.0440 0.7615 0.4327 0.067 Uiso 1 1 calc R . . N1 N 0.1117(5) 0.3245(4) 0.3965(3) 0.0418(15) Uani 1 1 d . . . N2 N 0.1836(4) 0.4536(3) 0.3227(3) 0.0415(17) Uani 1 1 d . . . N3 N 0.1844(5) 0.5330(4) 0.2925(3) 0.0389(16) Uani 1 1 d . . . N4 N 0.1286(5) 0.6689(3) 0.2237(3) 0.0425(16) Uani 1 1 d . . . N5 N 0.2568(8) 0.5284(5) 0.4033(4) 0.073(2) Uani 1 1 d . . . H5A H 0.2686 0.5745 0.3833 0.088 Uiso 1 1 calc R . . H5B H 0.2740 0.5276 0.4400 0.088 Uiso 1 1 calc R . . N6 N -0.0377(5) 0.3444(3) 0.2075(4) 0.0436(19) Uani 1 1 d . . . N7 N -0.0977(4) 0.4614(3) 0.2907(3) 0.0349(15) Uani 1 1 d . . . N8 N -0.0926(4) 0.5331(3) 0.3289(3) 0.040(2) Uani 1 1 d . . . N9 N -0.0312(5) 0.6530(3) 0.4072(4) 0.045(2) Uani 1 1 d . . . N10 N -0.1811(11) 0.4406(5) 0.4010(4) 0.108(4) Uani 1 1 d . . . H10B H -0.1901 0.3987 0.3768 0.129 Uiso 1 1 calc R . . H10C H -0.2039 0.4345 0.4368 0.129 Uiso 1 1 calc R . . N11 N 0.1941(7) 0.2467(5) 0.2714(4) 0.089(3) Uani 1 1 d . . . N12 N 0.2867(7) 0.2503(4) 0.2971(4) 0.056(2) Uani 1 1 d . . . N13 N 0.3815(6) 0.2543(4) 0.3238(4) 0.078(3) Uani 1 1 d . . . N14 N -0.1164(6) 0.7392(5) 0.2900(4) 0.079(3) Uani 1 1 d . . . N15 N -0.1995(7) 0.7538(4) 0.3187(5) 0.061(2) Uani 1 1 d . . . N16 N -0.2868(7) 0.7681(6) 0.3485(4) 0.092(3) Uani 1 1 d . . . Cl1 Cl 0.0092(4) 0.01355(11) 0.05235(18) 0.0704(7) Uani 1 1 d . . . Cl2 Cl 0.5046(3) 0.06059(11) 0.56045(14) 0.0673(5) Uani 1 1 d . . . O1 O 0.1152(7) 0.0527(5) 0.0288(4) 0.110(2) Uiso 1 1 d . . . O2 O -0.0516(9) -0.0292(6) 0.0071(5) 0.145(3) Uiso 1 1 d . . . O3 O 0.0476(10) -0.0547(8) 0.0832(6) 0.179(4) Uiso 1 1 d . . . O4 O -0.0800(10) 0.0683(7) 0.0743(6) 0.176(4) Uiso 1 1 d . . . O51 O 0.5522(18) 0.0121(10) 0.5105(9) 0.074(5) Uiso 0.52(3) 1 d P A 1 O52 O 0.5877(19) -0.0008(9) 0.5262(9) 0.071(5) Uiso 0.48(3) 1 d P A 2 O61 O 0.4377(12) 0.0216(12) 0.6028(7) 0.063(4) Uiso 0.52(3) 1 d P A 1 O62 O 0.4478(15) -0.0082(14) 0.5945(8) 0.070(5) Uiso 0.48(3) 1 d P A 2 O71 O 0.625(2) 0.0933(11) 0.5901(8) 0.091(6) Uiso 0.52(3) 1 d P A 1 O72 O 0.5744(17) 0.1123(9) 0.5965(7) 0.065(5) Uiso 0.48(3) 1 d P A 2 O81 O 0.450(2) 0.1349(13) 0.5303(8) 0.106(6) Uiso 0.52(3) 1 d P A 1 O82 O 0.3962(18) 0.1058(11) 0.5312(7) 0.077(6) Uiso 0.48(3) 1 d P A 2 O91 O 0.5452(15) 0.5590(12) 0.3271(10) 0.218(10) Uiso 0.75(2) 1 d P B 2 O92 O 0.536(3) 0.459(2) 0.3282(17) 0.127(16) Uiso 0.25(2) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0323(2) 0.0450(2) 0.0442(5) 0.0001(2) -0.0068(2) 0.00153(19) Cd2 0.0366(2) 0.0464(2) 0.0407(4) 0.0001(2) 0.0087(3) -0.00382(19) C1 0.056(5) 0.051(4) 0.060(7) -0.006(4) -0.007(5) -0.010(4) C2 0.077(5) 0.042(4) 0.036(6) 0.006(3) -0.011(4) 0.005(4) C3 0.062(5) 0.070(5) 0.036(6) 0.007(4) -0.011(4) 0.014(4) C4 0.058(4) 0.050(4) 0.033(6) -0.002(4) -0.008(4) 0.001(4) C5 0.047(4) 0.036(3) 0.033(5) 0.002(3) 0.001(4) 0.005(3) C6 0.037(4) 0.054(5) 0.029(6) 0.002(4) -0.005(4) -0.003(3) C7 0.032(4) 0.037(4) 0.042(6) 0.005(4) 0.000(4) -0.005(3) C8 0.087(6) 0.064(5) 0.042(6) 0.004(4) 0.026(5) 0.000(5) C9 0.030(3) 0.051(4) 0.037(5) -0.004(3) 0.006(3) -0.003(3) C10 0.053(5) 0.061(4) 0.046(7) 0.001(5) 0.008(4) -0.008(4) C11 0.063(5) 0.063(5) 0.038(6) 0.010(4) 0.001(4) -0.014(4) C12 0.067(5) 0.062(5) 0.051(7) 0.003(4) -0.011(5) -0.019(4) C13 0.057(5) 0.044(4) 0.045(6) 0.010(4) -0.001(4) 0.002(3) C14 0.073(5) 0.047(4) 0.046(6) -0.010(4) -0.015(5) 0.002(4) C15 0.097(7) 0.061(5) 0.061(8) -0.031(5) -0.012(5) -0.009(5) C16 0.094(6) 0.064(5) 0.051(8) -0.015(5) -0.034(6) 0.007(5) C17 0.058(5) 0.049(4) 0.058(7) -0.005(4) -0.023(5) 0.006(4) C18 0.046(4) 0.035(4) 0.032(5) -0.004(3) -0.006(4) 0.003(3) C19 0.049(5) 0.043(4) 0.037(6) -0.001(4) -0.007(4) -0.012(4) C20 0.087(7) 0.046(5) 0.040(6) -0.002(4) 0.003(4) 0.008(4) C21 0.030(4) 0.040(4) 0.038(6) -0.002(4) 0.003(4) -0.009(4) C22 0.028(4) 0.070(5) 0.047(7) -0.001(4) -0.003(4) 0.007(4) C23 0.061(5) 0.057(4) 0.046(6) -0.002(4) 0.017(5) -0.003(4) C24 0.087(6) 0.068(5) 0.054(8) -0.013(5) 0.028(5) 0.001(5) C25 0.076(6) 0.080(6) 0.065(9) -0.018(5) 0.010(5) -0.022(5) C26 0.065(5) 0.046(4) 0.057(7) -0.012(4) -0.002(5) -0.004(4) N1 0.041(3) 0.041(3) 0.043(5) -0.005(3) -0.001(3) -0.001(3) N2 0.030(3) 0.050(3) 0.045(5) 0.013(3) 0.003(3) -0.001(2) N3 0.029(3) 0.051(3) 0.036(5) 0.003(3) 0.005(3) 0.003(2) N4 0.044(3) 0.043(3) 0.040(5) 0.011(3) 0.002(3) -0.009(3) N5 0.102(7) 0.062(4) 0.056(6) 0.006(4) -0.009(5) 0.008(4) N6 0.044(3) 0.051(4) 0.036(6) -0.008(3) 0.000(3) 0.002(3) N7 0.033(3) 0.051(3) 0.021(4) 0.003(3) 0.000(3) 0.005(2) N8 0.024(3) 0.037(3) 0.059(7) -0.006(3) 0.002(3) 0.004(2) N9 0.050(4) 0.046(3) 0.038(6) 0.005(3) 0.013(3) -0.004(3) N10 0.203(11) 0.071(6) 0.048(7) -0.005(4) 0.044(7) -0.009(6) N11 0.062(5) 0.125(6) 0.080(7) -0.046(5) -0.034(4) 0.049(4) N12 0.060(4) 0.058(3) 0.050(6) -0.017(4) 0.001(4) 0.019(3) N13 0.055(4) 0.089(4) 0.088(8) -0.031(5) -0.027(5) 0.034(3) N14 0.056(4) 0.112(6) 0.069(7) 0.029(5) 0.019(4) 0.037(4) N15 0.058(4) 0.070(3) 0.057(6) 0.017(4) 0.003(4) 0.021(3) N16 0.072(5) 0.142(7) 0.062(6) 0.039(5) 0.030(4) 0.049(5) Cl1 0.0629(14) 0.0476(10) 0.1008(19) -0.0074(14) -0.0019(13) 0.0013(13) Cl2 0.0820(11) 0.0687(10) 0.0511(10) -0.0006(14) -0.0044(8) -0.0025(13) _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 N13 2.302(6) 3_455 ? Cd1 N1 2.310(7) . ? Cd1 N6 2.325(8) . ? Cd1 N11 2.344(7) . ? Cd1 N7 2.378(5) . ? Cd1 N2 2.382(5) . ? Cd2 N9 2.269(8) . ? Cd2 N4 2.294(7) . ? Cd2 N16 2.318(7) 3_565 ? Cd2 N14 2.335(7) . ? Cd2 N8 2.370(5) . ? Cd2 N3 2.374(5) . ? C1 N1 1.321(10) . ? C1 C2 1.364(12) . ? C1 H1A 0.9300 . ? C2 C3 1.385(11) . ? C2 H2A 0.9300 . ? C3 C4 1.368(11) . ? C3 H3A 0.9300 . ? C4 C5 1.399(11) . ? C4 H4A 0.9300 . ? C5 N1 1.337(9) . ? C5 C6 1.481(10) . ? C6 N5 1.293(11) . ? C6 N2 1.318(10) . ? C7 N3 1.269(10) . ? C7 C9 1.480(11) . ? C7 C8 1.486(12) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N4 1.343(9) . ? C9 C10 1.376(11) . ? C10 C11 1.371(11) . ? C10 H10A 0.9300 . ? C11 C12 1.344(12) . ? C11 H11A 0.9300 . ? C12 C13 1.396(12) . ? C12 H12A 0.9300 . ? C13 N4 1.339(9) . ? C13 H13A 0.9300 . ? C14 N6 1.332(10) . ? C14 C15 1.353(13) . ? C14 H14A 0.9300 . ? C15 C16 1.331(12) . ? C15 H15A 0.9300 . ? C16 C17 1.375(12) . ? C16 H16A 0.9300 . ? C17 C18 1.410(11) . ? C17 H17A 0.9300 . ? C18 N6 1.328(9) . ? C18 C19 1.490(12) . ? C19 N7 1.272(10) . ? C19 C20 1.380(11) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N8 1.296(10) . ? C21 N10 1.417(11) . ? C21 C22 1.454(12) . ? C22 N9 1.347(9) . ? C22 C23 1.362(12) . ? C23 C24 1.344(12) . ? C23 H23A 0.9300 . ? C24 C25 1.391(12) . ? C24 H24A 0.9300 . ? C25 C26 1.413(13) . ? C25 H25A 0.9300 . ? C26 N9 1.333(11) . ? C26 H26A 0.9300 . ? N2 N3 1.412(6) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N7 N8 1.417(6) . ? N10 H10B 0.8600 . ? N10 H10C 0.8600 . ? N11 N12 1.158(9) . ? N12 N13 1.191(9) . ? N13 Cd1 2.302(6) 3 ? N14 N15 1.133(10) . ? N15 N16 1.182(11) . ? N16 Cd2 2.318(7) 3_465 ? Cl1 O3 1.339(13) . ? Cl1 O4 1.376(12) . ? Cl1 O2 1.393(12) . ? Cl1 O1 1.401(9) . ? Cl2 O61 1.351(15) . ? Cl2 O72 1.374(14) . ? Cl2 O62 1.457(17) . ? Cl2 O51 1.462(18) . ? Cl2 O81 1.466(16) . ? Cl2 O82 1.517(15) . ? Cl2 O52 1.523(16) . ? Cl2 O71 1.551(17) . ? O91 O92 1.55(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 N13 Cd1 N1 88.7(3) 3_455 . ? N13 Cd1 N6 87.4(3) 3_455 . ? N1 Cd1 N6 174.36(19) . . ? N13 Cd1 N11 100.4(3) 3_455 . ? N1 Cd1 N11 88.0(3) . . ? N6 Cd1 N11 88.8(3) . . ? N13 Cd1 N7 94.6(2) 3_455 . ? N1 Cd1 N7 114.0(2) . . ? N6 Cd1 N7 70.4(2) . . ? N11 Cd1 N7 153.7(3) . . ? N13 Cd1 N2 155.6(3) 3_455 . ? N1 Cd1 N2 71.2(2) . . ? N6 Cd1 N2 113.6(2) . . ? N11 Cd1 N2 92.7(2) . . ? N7 Cd1 N2 81.79(17) . . ? N9 Cd2 N4 170.54(18) . . ? N9 Cd2 N16 88.3(3) . 3_565 ? N4 Cd2 N16 86.4(3) . 3_565 ? N9 Cd2 N14 85.9(3) . . ? N4 Cd2 N14 88.5(3) . . ? N16 Cd2 N14 109.2(3) 3_565 . ? N9 Cd2 N8 70.1(2) . . ? N4 Cd2 N8 117.5(2) . . ? N16 Cd2 N8 150.2(3) 3_565 . ? N14 Cd2 N8 90.0(2) . . ? N9 Cd2 N3 117.3(2) . . ? N4 Cd2 N3 70.7(2) . . ? N16 Cd2 N3 91.3(3) 3_565 . ? N14 Cd2 N3 150.0(3) . . ? N8 Cd2 N3 81.36(17) . . ? N1 C1 C2 122.4(7) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 119.5(7) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 118.7(8) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 118.6(7) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? N1 C5 C4 121.5(6) . . ? N1 C5 C6 117.1(7) . . ? C4 C5 C6 121.3(7) . . ? N5 C6 N2 125.3(8) . . ? N5 C6 C5 119.7(9) . . ? N2 C6 C5 114.9(6) . . ? N3 C7 C9 118.3(7) . . ? N3 C7 C8 125.2(8) . . ? C9 C7 C8 116.5(8) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 121.0(7) . . ? N4 C9 C7 115.1(7) . . ? C10 C9 C7 123.9(7) . . ? C11 C10 C9 119.8(8) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 C10 120.6(9) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 117.0(8) . . ? C11 C12 H12A 121.5 . . ? C13 C12 H12A 121.5 . . ? N4 C13 C12 123.5(7) . . ? N4 C13 H13A 118.2 . . ? C12 C13 H13A 118.2 . . ? N6 C14 C15 120.2(8) . . ? N6 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C16 C15 C14 122.8(8) . . ? C16 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C15 C16 C17 118.4(9) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? C16 C17 C18 117.7(7) . . ? C16 C17 H17A 121.1 . . ? C18 C17 H17A 121.1 . . ? N6 C18 C17 121.5(7) . . ? N6 C18 C19 114.9(7) . . ? C17 C18 C19 123.6(7) . . ? N7 C19 C20 125.2(8) . . ? N7 C19 C18 118.0(8) . . ? C20 C19 C18 116.8(8) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N8 C21 N10 123.2(8) . . ? N8 C21 C22 115.8(8) . . ? N10 C21 C22 121.0(9) . . ? N9 C22 C23 120.6(8) . . ? N9 C22 C21 117.1(8) . . ? C23 C22 C21 122.3(8) . . ? C24 C23 C22 121.3(8) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 120.3(9) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C26 115.8(8) . . ? C24 C25 H25A 122.1 . . ? C26 C25 H25A 122.1 . . ? N9 C26 C25 123.0(8) . . ? N9 C26 H26A 118.5 . . ? C25 C26 H26A 118.5 . . ? C1 N1 C5 119.2(7) . . ? C1 N1 Cd1 122.1(5) . . ? C5 N1 Cd1 115.1(5) . . ? C6 N2 N3 114.0(5) . . ? C6 N2 Cd1 113.7(4) . . ? N3 N2 Cd1 122.9(4) . . ? C7 N3 N2 116.9(6) . . ? C7 N3 Cd2 114.7(5) . . ? N2 N3 Cd2 123.2(4) . . ? C13 N4 C9 117.9(7) . . ? C13 N4 Cd2 123.0(5) . . ? C9 N4 Cd2 116.9(5) . . ? C6 N5 H5A 120.0 . . ? C6 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C18 N6 C14 119.3(8) . . ? C18 N6 Cd1 116.8(5) . . ? C14 N6 Cd1 121.4(6) . . ? C19 N7 N8 115.5(6) . . ? C19 N7 Cd1 113.6(5) . . ? N8 N7 Cd1 121.2(4) . . ? C21 N8 N7 116.3(6) . . ? C21 N8 Cd2 115.9(5) . . ? N7 N8 Cd2 122.6(4) . . ? C26 N9 C22 118.9(8) . . ? C26 N9 Cd2 122.6(6) . . ? C22 N9 Cd2 117.7(6) . . ? C21 N10 H10B 120.0 . . ? C21 N10 H10C 120.0 . . ? H10B N10 H10C 120.0 . . ? N12 N11 Cd1 115.5(6) . . ? N11 N12 N13 179.6(10) . . ? N12 N13 Cd1 118.9(6) . 3 ? N15 N14 Cd2 125.0(7) . . ? N14 N15 N16 179.2(10) . . ? N15 N16 Cd2 121.5(7) . 3_465 ? O3 Cl1 O4 120.7(8) . . ? O3 Cl1 O2 99.3(7) . . ? O4 Cl1 O2 103.7(7) . . ? O3 Cl1 O1 107.2(7) . . ? O4 Cl1 O1 116.2(5) . . ? O2 Cl1 O1 107.5(6) . . ? O61 Cl2 O72 97.0(9) . . ? O61 Cl2 O62 20.5(8) . . ? O72 Cl2 O62 109.6(10) . . ? O61 Cl2 O51 121.2(10) . . ? O72 Cl2 O51 125.3(10) . . ? O62 Cl2 O51 100.9(13) . . ? O61 Cl2 O81 118.5(9) . . ? O72 Cl2 O81 92.5(9) . . ? O62 Cl2 O81 131.3(11) . . ? O51 Cl2 O81 100.2(11) . . ? O61 Cl2 O82 96.6(9) . . ? O72 Cl2 O82 114.5(8) . . ? O62 Cl2 O82 104.7(9) . . ? O51 Cl2 O82 99.3(11) . . ? O81 Cl2 O82 28.4(7) . . ? O61 Cl2 O52 113.7(12) . . ? O72 Cl2 O52 110.7(9) . . ? O62 Cl2 O52 93.7(11) . . ? O51 Cl2 O52 21.5(8) . . ? O81 Cl2 O52 118.9(12) . . ? O82 Cl2 O52 120.8(10) . . ? O61 Cl2 O71 106.1(9) . . ? O72 Cl2 O71 24.3(7) . . ? O62 Cl2 O71 110.8(10) . . ? O51 Cl2 O71 102.6(10) . . ? O81 Cl2 O71 106.6(10) . . ? O82 Cl2 O71 133.3(7) . . ? O52 Cl2 O71 86.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.3(14) . . . . ? C1 C2 C3 C4 -0.1(13) . . . . ? C2 C3 C4 C5 -1.2(12) . . . . ? C3 C4 C5 N1 1.4(12) . . . . ? C3 C4 C5 C6 -179.7(7) . . . . ? N1 C5 C6 N5 150.6(7) . . . . ? C4 C5 C6 N5 -28.3(11) . . . . ? N1 C5 C6 N2 -33.6(9) . . . . ? C4 C5 C6 N2 147.5(7) . . . . ? N3 C7 C9 N4 -25.0(10) . . . . ? C8 C7 C9 N4 154.5(7) . . . . ? N3 C7 C9 C10 152.6(8) . . . . ? C8 C7 C9 C10 -27.9(11) . . . . ? N4 C9 C10 C11 0.1(12) . . . . ? C7 C9 C10 C11 -177.3(8) . . . . ? C9 C10 C11 C12 -2.2(13) . . . . ? C10 C11 C12 C13 1.4(12) . . . . ? C11 C12 C13 N4 1.5(12) . . . . ? N6 C14 C15 C16 0.4(16) . . . . ? C14 C15 C16 C17 -2.7(16) . . . . ? C15 C16 C17 C18 1.6(15) . . . . ? C16 C17 C18 N6 1.7(13) . . . . ? C16 C17 C18 C19 -178.0(9) . . . . ? N6 C18 C19 N7 -28.4(11) . . . . ? C17 C18 C19 N7 151.2(8) . . . . ? N6 C18 C19 C20 153.0(8) . . . . ? C17 C18 C19 C20 -27.3(12) . . . . ? N8 C21 C22 N9 -20.6(11) . . . . ? N10 C21 C22 N9 159.9(9) . . . . ? N8 C21 C22 C23 160.5(8) . . . . ? N10 C21 C22 C23 -18.9(13) . . . . ? N9 C22 C23 C24 3.6(13) . . . . ? C21 C22 C23 C24 -177.6(8) . . . . ? C22 C23 C24 C25 -4.2(15) . . . . ? C23 C24 C25 C26 2.0(15) . . . . ? C24 C25 C26 N9 0.7(14) . . . . ? C2 C1 N1 C5 -1.1(12) . . . . ? C2 C1 N1 Cd1 156.7(7) . . . . ? C4 C5 N1 C1 -0.3(11) . . . . ? C6 C5 N1 C1 -179.2(7) . . . . ? C4 C5 N1 Cd1 -159.6(6) . . . . ? C6 C5 N1 Cd1 21.4(7) . . . . ? N13 Cd1 N1 C1 30.0(6) 3_455 . . . ? N6 Cd1 N1 C1 -16(2) . . . . ? N11 Cd1 N1 C1 -70.5(6) . . . . ? N7 Cd1 N1 C1 124.4(6) . . . . ? N2 Cd1 N1 C1 -164.1(6) . . . . ? N13 Cd1 N1 C5 -171.3(5) 3_455 . . . ? N6 Cd1 N1 C5 143.0(19) . . . . ? N11 Cd1 N1 C5 88.2(5) . . . . ? N7 Cd1 N1 C5 -76.9(5) . . . . ? N2 Cd1 N1 C5 -5.4(4) . . . . ? N5 C6 N2 N3 -9.6(11) . . . . ? C5 C6 N2 N3 174.9(5) . . . . ? N5 C6 N2 Cd1 -157.3(6) . . . . ? C5 C6 N2 Cd1 27.2(7) . . . . ? N13 Cd1 N2 C6 23.6(8) 3_455 . . . ? N1 Cd1 N2 C6 -12.4(4) . . . . ? N6 Cd1 N2 C6 170.8(4) . . . . ? N11 Cd1 N2 C6 -99.4(5) . . . . ? N7 Cd1 N2 C6 106.5(5) . . . . ? N13 Cd1 N2 N3 -120.8(6) 3_455 . . . ? N1 Cd1 N2 N3 -156.8(5) . . . . ? N6 Cd1 N2 N3 26.4(5) . . . . ? N11 Cd1 N2 N3 116.2(5) . . . . ? N7 Cd1 N2 N3 -37.9(4) . . . . ? C9 C7 N3 N2 175.4(5) . . . . ? C8 C7 N3 N2 -4.0(11) . . . . ? C9 C7 N3 Cd2 19.9(8) . . . . ? C8 C7 N3 Cd2 -159.6(6) . . . . ? C6 N2 N3 C7 143.5(5) . . . . ? Cd1 N2 N3 C7 -72.1(7) . . . . ? C6 N2 N3 Cd2 -63.1(7) . . . . ? Cd1 N2 N3 Cd2 81.2(4) . . . . ? N9 Cd2 N3 C7 177.3(5) . . . . ? N4 Cd2 N3 C7 -8.2(5) . . . . ? N16 Cd2 N3 C7 -93.9(6) 3_565 . . . ? N14 Cd2 N3 C7 40.3(8) . . . . ? N8 Cd2 N3 C7 115.1(5) . . . . ? N9 Cd2 N3 N2 23.5(5) . . . . ? N4 Cd2 N3 N2 -162.0(5) . . . . ? N16 Cd2 N3 N2 112.3(5) 3_565 . . . ? N14 Cd2 N3 N2 -113.6(5) . . . . ? N8 Cd2 N3 N2 -38.8(4) . . . . ? C12 C13 N4 C9 -3.5(11) . . . . ? C12 C13 N4 Cd2 159.2(6) . . . . ? C10 C9 N4 C13 2.7(11) . . . . ? C7 C9 N4 C13 -179.7(7) . . . . ? C10 C9 N4 Cd2 -161.1(6) . . . . ? C7 C9 N4 Cd2 16.5(8) . . . . ? N9 Cd2 N4 C13 -19.5(16) . . . . ? N16 Cd2 N4 C13 -75.5(6) 3_565 . . . ? N14 Cd2 N4 C13 33.8(6) . . . . ? N8 Cd2 N4 C13 123.1(5) . . . . ? N3 Cd2 N4 C13 -168.2(6) . . . . ? N9 Cd2 N4 C9 143.3(12) . . . . ? N16 Cd2 N4 C9 87.4(5) 3_565 . . . ? N14 Cd2 N4 C9 -163.3(5) . . . . ? N8 Cd2 N4 C9 -74.0(5) . . . . ? N3 Cd2 N4 C9 -5.3(4) . . . . ? C17 C18 N6 C14 -4.0(11) . . . . ? C19 C18 N6 C14 175.7(8) . . . . ? C17 C18 N6 Cd1 -166.1(6) . . . . ? C19 C18 N6 Cd1 13.6(8) . . . . ? C15 C14 N6 C18 3.0(13) . . . . ? C15 C14 N6 Cd1 164.2(7) . . . . ? N13 Cd1 N6 C18 95.2(5) 3_455 . . . ? N1 Cd1 N6 C18 141.0(19) . . . . ? N11 Cd1 N6 C18 -164.3(5) . . . . ? N7 Cd1 N6 C18 -0.6(5) . . . . ? N2 Cd1 N6 C18 -71.8(5) . . . . ? N13 Cd1 N6 C14 -66.5(6) 3_455 . . . ? N1 Cd1 N6 C14 -21(2) . . . . ? N11 Cd1 N6 C14 34.0(6) . . . . ? N7 Cd1 N6 C14 -162.3(6) . . . . ? N2 Cd1 N6 C14 126.4(6) . . . . ? C20 C19 N7 N8 -7.5(12) . . . . ? C18 C19 N7 N8 174.1(6) . . . . ? C20 C19 N7 Cd1 -154.2(8) . . . . ? C18 C19 N7 Cd1 27.4(9) . . . . ? N13 Cd1 N7 C19 -100.2(6) 3_455 . . . ? N1 Cd1 N7 C19 169.2(5) . . . . ? N6 Cd1 N7 C19 -14.6(5) . . . . ? N11 Cd1 N7 C19 24.7(8) . . . . ? N2 Cd1 N7 C19 104.1(6) . . . . ? N13 Cd1 N7 N8 115.3(5) 3_455 . . . ? N1 Cd1 N7 N8 24.7(4) . . . . ? N6 Cd1 N7 N8 -159.2(4) . . . . ? N11 Cd1 N7 N8 -119.9(6) . . . . ? N2 Cd1 N7 N8 -40.5(4) . . . . ? N10 C21 N8 N7 -5.3(12) . . . . ? C22 C21 N8 N7 175.3(6) . . . . ? N10 C21 N8 Cd2 -160.5(7) . . . . ? C22 C21 N8 Cd2 20.0(9) . . . . ? C19 N7 N8 C21 147.3(5) . . . . ? Cd1 N7 N8 C21 -68.8(7) . . . . ? C19 N7 N8 Cd2 -59.3(8) . . . . ? Cd1 N7 N8 Cd2 84.6(4) . . . . ? N9 Cd2 N8 C21 -11.0(5) . . . . ? N4 Cd2 N8 C21 175.1(5) . . . . ? N16 Cd2 N8 C21 34.9(8) 3_565 . . . ? N14 Cd2 N8 C21 -96.6(6) . . . . ? N3 Cd2 N8 C21 112.3(6) . . . . ? N9 Cd2 N8 N7 -164.6(5) . . . . ? N4 Cd2 N8 N7 21.5(5) . . . . ? N16 Cd2 N8 N7 -118.6(6) 3_565 . . . ? N14 Cd2 N8 N7 109.9(5) . . . . ? N3 Cd2 N8 N7 -41.3(4) . . . . ? C25 C26 N9 C22 -1.3(12) . . . . ? C25 C26 N9 Cd2 168.1(7) . . . . ? C23 C22 N9 C26 -0.9(11) . . . . ? C21 C22 N9 C26 -179.7(8) . . . . ? C23 C22 N9 Cd2 -170.7(6) . . . . ? C21 C22 N9 Cd2 10.4(9) . . . . ? N4 Cd2 N9 C26 -24.6(16) . . . . ? N16 Cd2 N9 C26 31.2(6) 3_565 . . . ? N14 Cd2 N9 C26 -78.2(6) . . . . ? N8 Cd2 N9 C26 -169.7(7) . . . . ? N3 Cd2 N9 C26 121.8(6) . . . . ? N4 Cd2 N9 C22 144.8(11) . . . . ? N16 Cd2 N9 C22 -159.4(6) 3_565 . . . ? N14 Cd2 N9 C22 91.3(6) . . . . ? N8 Cd2 N9 C22 -0.3(5) . . . . ? N3 Cd2 N9 C22 -68.8(6) . . . . ? N13 Cd1 N11 N12 -122.3(8) 3_455 . . . ? N1 Cd1 N11 N12 -34.1(8) . . . . ? N6 Cd1 N11 N12 150.6(8) . . . . ? N7 Cd1 N11 N12 113.9(9) . . . . ? N2 Cd1 N11 N12 37.0(8) . . . . ? Cd1 N11 N12 N13 25(100) . . . . ? N11 N12 N13 Cd1 151(100) . . . 3 ? N9 Cd2 N14 N15 -11.7(8) . . . . ? N4 Cd2 N14 N15 175.9(8) . . . . ? N16 Cd2 N14 N15 -98.4(8) 3_565 . . . ? N8 Cd2 N14 N15 58.4(8) . . . . ? N3 Cd2 N14 N15 131.0(8) . . . . ? Cd2 N14 N15 N16 -77(82) . . . . ? N14 N15 N16 Cd2 -99(82) . . . 3_465 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.732 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.095 #===END # Crystallographic Data of Complex 3 data_3 _database_code_depnum_ccdc_archive 'CCDC 244390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H11 Cd2 N17' _chemical_formula_weight 618.18 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' 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, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.3175(3) _cell_length_b 12.4223(4) _cell_length_c 13.3087(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.3830(16) _cell_angle_gamma 90.00 _cell_volume 1937.04(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11575 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.238 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.823 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18404 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2220 _reflns_number_gt 1579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press, London. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0326P)^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 SHELXL _refine_ls_extinction_coef 0.00184(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2220 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0570 _refine_ls_wR_factor_gt 0.0530 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 0.083026(17) 0.454492(17) 0.427384(17) 0.04359(11) Uani 1 1 d . . . N4 N -0.1814(3) 0.4300(2) 0.3270(3) 0.0691(9) Uani 1 1 d . . . N3 N -0.0968(2) 0.4555(3) 0.4108(3) 0.0665(8) Uani 1 1 d . . . N5 N -0.2621(3) 0.4040(4) 0.2465(3) 0.1081(14) Uani 1 1 d . . . N6 N 0.0000 0.3641(3) 0.2500 0.0509(9) Uani 1 2 d S . . N1 N 0.2558(2) 0.5407(2) 0.4690(2) 0.0564(7) Uani 1 1 d . . . C1 C 0.3546(3) 0.5203(4) 0.5604(3) 0.0731(11) Uani 1 1 d . . . H1A H 0.3574 0.4678 0.6115 0.088 Uiso 1 1 calc R . . N9 N 0.1846(2) 0.3003(2) 0.5165(2) 0.0536(7) Uani 1 1 d . . . N2 N 0.0505(3) 0.6032(2) 0.3018(3) 0.0718(9) Uani 1 1 d . . . C6 C 0.1395(4) 0.6370(3) 0.2967(3) 0.0763(11) Uani 1 1 d . . . C5 C 0.2516(3) 0.6182(3) 0.3968(3) 0.0718(10) Uani 1 1 d . . . C4 C 0.3488(4) 0.6725(4) 0.4129(4) 0.1070(17) Uani 1 1 d . . . H4A H 0.3453 0.7234 0.3600 0.128 Uiso 1 1 calc R . . C2 C 0.4545(4) 0.5750(4) 0.5828(4) 0.0986(16) Uani 1 1 d . . . H2B H 0.5226 0.5599 0.6481 0.118 Uiso 1 1 calc R . . N7 N 0.0000 0.2692(4) 0.2500 0.0569(10) Uani 1 2 d S . . N8 N 0.0000 0.1771(4) 0.2500 0.137(3) Uani 1 2 d S . . N10 N 0.2500 0.2500 0.5000 0.0441(8) Uani 1 2 d S . . N11 N 0.1251(6) 0.6895(5) 0.2152(5) 0.087(2) Uani 0.50 1 d P . . H11A H 0.0570 0.7035 0.1625 0.104 Uiso 0.50 1 calc PR . . H11B H 0.1829 0.7131 0.2094 0.104 Uiso 0.50 1 calc PR . . C3 C 0.4503(4) 0.6503(4) 0.5078(5) 0.1134(18) Uani 1 1 d . . . H3A H 0.5163 0.6869 0.5205 0.136 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 0.03523(14) 0.03991(15) 0.04287(14) -0.00288(10) 0.00818(9) 0.00204(10) N4 0.0454(17) 0.065(2) 0.073(2) -0.0195(15) 0.0089(16) 0.0080(14) N3 0.0356(15) 0.086(2) 0.0606(17) -0.0342(16) 0.0088(13) -0.0064(15) N5 0.055(2) 0.110(3) 0.095(3) -0.036(2) -0.016(2) 0.000(2) N6 0.064(2) 0.036(2) 0.0395(18) 0.000 0.0140(17) 0.000 N1 0.0438(15) 0.0528(16) 0.0535(15) 0.0034(13) 0.0076(12) -0.0102(13) C1 0.042(2) 0.083(3) 0.065(2) 0.0114(19) 0.0021(17) -0.0078(19) N9 0.0476(16) 0.0514(17) 0.0623(17) 0.0107(13) 0.0266(14) 0.0106(13) N2 0.0568(19) 0.0377(16) 0.0707(18) 0.0044(13) -0.0106(14) -0.0035(14) C6 0.077(3) 0.043(2) 0.064(2) 0.0080(18) -0.0024(19) -0.017(2) C5 0.059(2) 0.054(2) 0.073(2) 0.0075(19) 0.0073(18) -0.0213(18) C4 0.080(3) 0.086(3) 0.108(3) 0.028(3) 0.007(3) -0.041(3) C2 0.050(2) 0.105(4) 0.096(3) 0.011(3) -0.002(2) -0.026(2) N7 0.073(3) 0.050(3) 0.0362(19) 0.000 0.0165(19) 0.000 N8 0.237(8) 0.042(3) 0.065(3) 0.000 0.016(4) 0.000 N10 0.0363(19) 0.040(2) 0.0468(19) 0.0077(15) 0.0127(16) 0.0010(17) N11 0.084(5) 0.096(5) 0.053(3) 0.021(3) 0.011(3) -0.041(4) C3 0.066(3) 0.104(4) 0.126(4) 0.019(3) 0.009(3) -0.044(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 N3 2.299(3) . ? Cd1 N9 2.319(3) . ? Cd1 N1 2.353(3) . ? Cd1 N3 2.355(3) 5_566 ? Cd1 N6 2.3611(19) . ? Cd1 N2 2.388(3) . ? N4 N5 1.145(4) . ? N4 N3 1.192(4) . ? N3 Cd1 2.355(3) 5_566 ? N6 N7 1.179(5) . ? N6 Cd1 2.3611(19) 2 ? N1 C1 1.325(4) . ? N1 C5 1.342(4) . ? C1 C2 1.394(6) . ? N9 N10 1.175(3) . ? N2 C6 1.290(5) . ? N2 N2 1.395(5) 2 ? C6 N11 1.201(6) . ? C6 C5 1.472(5) . ? C5 C4 1.384(5) . ? C4 C3 1.370(6) . ? C2 C3 1.349(6) . ? N7 N8 1.145(6) . ? N10 N9 1.175(3) 7_556 ? 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 N3 Cd1 N9 112.40(11) . . ? N3 Cd1 N1 151.39(10) . . ? N9 Cd1 N1 89.34(9) . . ? N3 Cd1 N3 73.13(10) . 5_566 ? N9 Cd1 N3 98.72(11) . 5_566 ? N1 Cd1 N3 85.77(10) . 5_566 ? N3 Cd1 N6 86.29(7) . . ? N9 Cd1 N6 90.03(11) . . ? N1 Cd1 N6 113.11(7) . . ? N3 Cd1 N6 159.39(7) 5_566 . ? N3 Cd1 N2 95.43(12) . . ? N9 Cd1 N2 149.80(11) . . ? N1 Cd1 N2 69.17(10) . . ? N3 Cd1 N2 100.48(12) 5_566 . ? N6 Cd1 N2 79.93(11) . . ? N5 N4 N3 179.0(4) . . ? N4 N3 Cd1 124.5(3) . . ? N4 N3 Cd1 127.6(2) . 5_566 ? Cd1 N3 Cd1 106.87(10) . 5_566 ? N7 N6 Cd1 118.40(8) . . ? N7 N6 Cd1 118.40(8) . 2 ? Cd1 N6 Cd1 123.21(17) . 2 ? C1 N1 C5 118.7(3) . . ? C1 N1 Cd1 124.2(2) . . ? C5 N1 Cd1 117.1(2) . . ? N1 C1 C2 122.2(4) . . ? N10 N9 Cd1 130.37(17) . . ? C6 N2 N2 115.2(4) . 2 ? C6 N2 Cd1 115.0(2) . . ? N2 N2 Cd1 117.42(19) 2 . ? N11 C6 N2 117.9(5) . . ? N11 C6 C5 124.2(5) . . ? N2 C6 C5 117.6(3) . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.3(4) . . ? C3 C4 C5 119.0(4) . . ? C3 C2 C1 118.7(4) . . ? N8 N7 N6 180.000(1) . . ? N9 N10 N9 180.0(3) . 7_556 ? C2 C3 C4 119.8(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.731 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.163 #===END # Crystallographic Data of Complex 4 data_4 _database_code_depnum_ccdc_archive 'CCDC 244391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cd2 N18' _chemical_formula_weight 633.20 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.9875(3) _cell_length_b 12.8242(3) _cell_length_c 13.6191(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.9472(16) _cell_angle_gamma 90.00 _cell_volume 2022.03(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12256 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22313 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2318 _reflns_number_gt 1734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press, London. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data", University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _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^)+(0.0116P)^2^+10.8147P] 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 SHELXL _refine_ls_extinction_coef 0.00208(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2318 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.281 _refine_ls_restrained_S_all 1.281 _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 Cd1 Cd 0.07704(3) 0.44672(3) 0.42104(3) 0.03644(17) Uani 1 1 d . . . C1' C 0.354(3) 0.491(2) 0.553(3) 0.048(7) Uani 0.50 1 d P A 2 H11A H 0.3504 0.4334 0.5935 0.058 Uiso 0.50 1 calc PR A 2 C1 C 0.352(4) 0.5269(18) 0.551(4) 0.044(7) Uani 0.50 1 d P A 1 H12A H 0.3643 0.4681 0.5949 0.053 Uiso 0.50 1 calc PR A 1 C2' C 0.4552(19) 0.5417(19) 0.578(2) 0.075(7) Uani 0.50 1 d P A 2 H22A H 0.5226 0.5184 0.6376 0.090 Uiso 0.50 1 calc PR A 2 C2 C 0.4390(19) 0.5969(19) 0.5887(19) 0.064(5) Uani 0.50 1 d P A 1 H21A H 0.5060 0.5840 0.6533 0.077 Uiso 0.50 1 calc PR A 1 C3 C 0.4604(14) 0.6244(19) 0.5203(18) 0.076(6) Uani 0.50 1 d P A 2 H3A H 0.5299 0.6589 0.5396 0.091 Uiso 0.50 1 calc PR A 2 C4' C 0.3603(19) 0.6571(15) 0.431(2) 0.057(5) Uani 0.50 1 d P A 2 H42A H 0.3651 0.7105 0.3872 0.068 Uiso 0.50 1 calc PR A 2 C4 C 0.3311(17) 0.6968(15) 0.4373(17) 0.052(5) Uani 0.50 1 d P A 1 H41A H 0.3165 0.7571 0.3951 0.063 Uiso 0.50 1 calc PR A 1 C5 C 0.2517(6) 0.6135(5) 0.4040(5) 0.0499(15) Uani 1 1 d . . . C6 C 0.1407(6) 0.6324(4) 0.3022(5) 0.0465(15) Uani 1 1 d . A . C7 C 0.1416(6) 0.6939(5) 0.2157(5) 0.075(2) Uani 0.50 1 d P A 1 N1 N 0.2549(4) 0.5296(4) 0.4634(4) 0.0442(12) Uani 1 1 d . A . N2 N 0.0503(4) 0.5888(4) 0.3005(3) 0.0404(11) Uani 1 1 d . . . N3 N -0.0998(4) 0.4569(4) 0.4178(4) 0.0485(12) Uani 1 1 d . . . N4 N -0.1870(4) 0.4474(4) 0.3344(4) 0.0492(12) Uani 1 1 d . A . N5 N -0.2716(5) 0.4365(6) 0.2558(5) 0.087(2) Uani 1 1 d . . . N6 N 0.0000 0.3591(5) 0.2500 0.0457(17) Uani 1 2 d S . . N7 N 0.016(3) 0.2651(16) 0.249(3) 0.037(7) Uiso 0.32(3) 1 d P . 1 N7' N -0.038(5) 0.280(4) 0.254(5) 0.055(16) Uiso 0.18(3) 1 d P . 2 N8 N 0.023(2) 0.1748(13) 0.249(2) 0.057(7) Uiso 0.32(3) 1 d P . 1 N8' N -0.076(4) 0.192(3) 0.257(2) 0.047(12) Uiso 0.18(3) 1 d P . 2 N9 N 0.1759(5) 0.2984(5) 0.5050(5) 0.0624(16) Uani 1 1 d . . . N10 N 0.2500 0.2500 0.5000 0.0472(17) Uani 1 2 d S . . N11 N 0.4278(11) 0.6864(12) 0.5315(12) 0.067(4) Uani 0.50 1 d P A 1 N12 N 0.1416(6) 0.6939(5) 0.2157(5) 0.075(2) Uani 0.50 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0312(2) 0.0400(2) 0.0363(2) 0.0013(2) 0.01372(16) 0.0014(2) C1' 0.022(8) 0.058(19) 0.046(9) 0.008(14) -0.001(7) 0.007(13) C1 0.049(12) 0.031(15) 0.051(10) 0.011(11) 0.021(8) 0.005(12) C2' 0.038(10) 0.11(2) 0.069(12) -0.004(13) 0.017(8) 0.007(12) C2 0.039(10) 0.088(17) 0.056(10) -0.023(12) 0.013(8) -0.004(11) C3 0.031(9) 0.100(18) 0.095(14) -0.052(13) 0.028(9) -0.020(9) C4' 0.064(14) 0.039(12) 0.074(11) -0.019(10) 0.038(10) -0.014(9) C4 0.043(10) 0.041(12) 0.055(9) -0.011(8) 0.008(7) -0.014(8) C5 0.050(4) 0.057(4) 0.044(3) -0.012(3) 0.022(3) -0.019(3) C6 0.062(4) 0.037(3) 0.036(3) -0.006(2) 0.019(3) -0.012(3) C7 0.097(5) 0.063(4) 0.054(4) 0.017(3) 0.024(4) -0.021(4) N1 0.034(3) 0.055(3) 0.040(3) -0.003(2) 0.014(2) -0.002(2) N2 0.044(3) 0.038(3) 0.032(2) -0.0013(19) 0.011(2) -0.004(2) N3 0.031(3) 0.065(3) 0.045(3) -0.017(3) 0.014(2) -0.005(3) N4 0.038(3) 0.054(3) 0.050(3) -0.001(3) 0.015(2) -0.005(3) N5 0.045(4) 0.125(6) 0.061(4) -0.014(4) -0.002(3) -0.008(4) N6 0.059(5) 0.034(4) 0.039(4) 0.000 0.018(3) 0.000 N9 0.060(4) 0.062(4) 0.071(4) 0.023(3) 0.034(3) 0.027(3) N10 0.049(5) 0.043(4) 0.045(4) 0.010(3) 0.017(3) 0.006(4) N11 0.043(8) 0.077(10) 0.067(9) 0.004(8) 0.012(6) -0.016(7) N12 0.097(5) 0.063(4) 0.054(4) 0.017(3) 0.024(4) -0.021(4) _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 N3 2.280(5) . ? Cd1 N9 2.290(5) . ? Cd1 N6 2.362(3) . ? Cd1 N1 2.365(5) . ? Cd1 N2 2.370(4) . ? Cd1 N3 2.418(5) 5_566 ? C1' C2' 1.37(5) . ? C1' N1 1.40(3) . ? C1 N1 1.29(4) . ? C1 C2 1.35(5) . ? C2' C3 1.34(4) . ? C2 N11 1.36(3) . ? C3 C4' 1.38(3) . ? C4' C5 1.40(2) . ? C4 N11 1.33(2) . ? C4 C5 1.41(2) . ? C5 N1 1.335(8) . ? C5 C6 1.499(8) . ? C6 N2 1.292(7) . ? C6 C7 1.422(8) . ? N2 N2 1.403(8) 2 ? N3 N4 1.192(6) . ? N3 Cd1 2.418(5) 5_566 ? N4 N5 1.143(7) . ? N6 N7' 1.14(5) . ? N6 N7' 1.14(5) 2 ? N6 N7 1.22(2) . ? N6 N7 1.22(2) 2 ? N6 Cd1 2.362(3) 2 ? N7 N7 0.44(8) 2 ? N7 N8 1.16(2) . ? N7 N8 1.27(3) 2 ? N7' N7' 1.04(11) 2 ? N7' N8' 1.24(6) . ? N8 N8 0.60(6) 2 ? N8 N7 1.27(3) 2 ? N9 N10 1.174(6) . ? N10 N9 1.174(6) 7_556 ? 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 N3 Cd1 N9 112.9(2) . . ? N3 Cd1 N6 92.02(12) . . ? N9 Cd1 N6 89.3(2) . . ? N3 Cd1 N1 147.45(18) . . ? N9 Cd1 N1 89.25(19) . . ? N6 Cd1 N1 112.64(12) . . ? N3 Cd1 N2 96.43(18) . . ? N9 Cd1 N2 149.07(19) . . ? N6 Cd1 N2 79.60(18) . . ? N1 Cd1 N2 69.14(16) . . ? N3 Cd1 N3 72.31(18) . 5_566 ? N9 Cd1 N3 99.3(2) . 5_566 ? N6 Cd1 N3 164.07(11) . 5_566 ? N1 Cd1 N3 81.08(16) . 5_566 ? N2 Cd1 N3 98.91(17) . 5_566 ? C2' C1' N1 116(3) . . ? N1 C1 C2 129(2) . . ? C3 C2' C1' 122(2) . . ? C1 C2 N11 119(2) . . ? C2' C3 C4' 118.6(19) . . ? C3 C4' C5 123(2) . . ? N11 C4 C5 117.8(17) . . ? N1 C5 C4' 114.2(11) . . ? N1 C5 C4 126.7(10) . . ? C4' C5 C4 27.3(8) . . ? N1 C5 C6 116.3(5) . . ? C4' C5 C6 127.6(11) . . ? C4 C5 C6 115.6(10) . . ? N2 C6 C7 125.0(6) . . ? N2 C6 C5 115.6(5) . . ? C7 C6 C5 119.4(6) . . ? C1 N1 C5 109.4(14) . . ? C1 N1 C1' 19(2) . . ? C5 N1 C1' 125.4(16) . . ? C1 N1 Cd1 130.8(17) . . ? C5 N1 Cd1 117.1(4) . . ? C1' N1 Cd1 117.4(16) . . ? C6 N2 N2 116.9(5) . 2 ? C6 N2 Cd1 118.2(4) . . ? N2 N2 Cd1 117.3(3) 2 . ? N4 N3 Cd1 121.8(4) . . ? N4 N3 Cd1 126.1(4) . 5_566 ? Cd1 N3 Cd1 107.69(18) . 5_566 ? N5 N4 N3 178.3(7) . . ? N7' N6 N7' 54(5) . 2 ? N7' N6 N7 38(3) . . ? N7' N6 N7 17(3) 2 . ? N7' N6 N7 17(3) . 2 ? N7' N6 N7 38(3) 2 2 ? N7 N6 N7 21(4) . 2 ? N7' N6 Cd1 112(3) . . ? N7' N6 Cd1 118(3) 2 . ? N7 N6 Cd1 118.9(19) . . ? N7 N6 Cd1 116.9(19) 2 . ? N7' N6 Cd1 118(3) . 2 ? N7' N6 Cd1 112(3) 2 2 ? N7 N6 Cd1 116.9(19) . 2 ? N7 N6 Cd1 118.9(19) 2 2 ? Cd1 N6 Cd1 123.2(3) . 2 ? N7 N7 N8 94(2) 2 . ? N7 N7 N6 79.6(18) 2 . ? N8 N7 N6 173(4) . . ? N7 N7 N8 66(2) 2 2 ? N8 N7 N8 28(3) . 2 ? N6 N7 N8 145(4) . 2 ? N7' N7' N6 63(3) 2 . ? N7' N7' N8' 114(3) 2 . ? N6 N7' N8' 177(5) . . ? N8 N8 N7 86(2) 2 . ? N8 N8 N7 66(2) 2 2 ? N7 N8 N7 20(4) . 2 ? N10 N9 Cd1 134.4(4) . . ? N9 N10 N9 180.0(6) . 7_556 ? C4 N11 C2 116.5(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.714 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.093 #===END # Crystallographic Data of Complex 5 data_5 _database_code_depnum_ccdc_archive 'CCDC 244392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Cd2 N16' _chemical_formula_weight 631.21 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)/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 12.733(3) _cell_length_b 12.911(3) _cell_length_c 13.920(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.79(3) _cell_angle_gamma 90.00 _cell_volume 2060.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11504 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.105 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.443 _exptl_absorpt_correction_T_max 0.666 _exptl_absorpt_process_details ? _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 11504 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4378 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Molecular Structure Corporation (1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_cell_refinement ; Molecular Structure Corporation (1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381 USA. ; _computing_data_reduction ; Sheldrick, G. M. (1998) SHELXS98, Program for the Solution of Crystal Structure, University of Gottingen, Germany. ; _computing_structure_solution ; Sheldrick, G. M. (1998) SHELXS98, Program for the Solution of Crystal Structure, University of Gottingen, Germany. ; _computing_structure_refinement ; Sheldrick, G. M. (1998) SHELXL98, Program for the Refinement of Crystal Structure, University of Gottingen, Germany. ; _computing_molecular_graphics ; Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _computing_publication_material ; Sheldrick, G. M. (1998) SHELXL98, Program for the refinement of Crystal Structure, University of Gottingen, Germany ; _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^)+(0.0294P)^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 0.00236(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4378 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0657 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 0.81708(2) 0.80509(3) 0.43303(2) 0.03215(10) Uani 1 1 d . . . Cd2 Cd 0.66252(2) 0.80288(3) 0.09615(2) 0.03483(10) Uani 1 1 d . . . C1 C 1.0822(4) 0.7179(4) 0.5521(4) 0.0492(13) Uani 1 1 d . . . H1A H 1.0889 0.7732 0.5974 0.059 Uiso 1 1 calc R . . C2 C 1.1775(4) 0.6533(5) 0.5776(4) 0.0656(16) Uani 1 1 d . . . H2A H 1.2466 0.6639 0.6386 0.079 Uiso 1 1 calc R . . C3 C 1.1652(4) 0.5723(5) 0.5082(5) 0.0710(17) Uani 1 1 d . . . H3A H 1.2274 0.5274 0.5227 0.085 Uiso 1 1 calc R . . C4 C 1.0627(4) 0.5572(4) 0.4184(4) 0.0613(15) Uani 1 1 d . . . H4A H 1.0552 0.5038 0.3711 0.074 Uiso 1 1 calc R . . C5 C 0.9707(4) 0.6237(4) 0.4001(4) 0.0447(12) Uani 1 1 d . . . C6 C 0.8564(4) 0.6132(3) 0.3071(3) 0.0468(11) Uani 1 1 d . . . C7 C 0.5699(4) 0.6355(4) 0.2066(4) 0.0512(12) Uani 1 1 d . . . C8 C 0.4644(4) 0.6611(4) 0.1059(4) 0.0500(12) Uani 1 1 d . . . C9 C 0.3606(4) 0.6052(4) 0.0750(4) 0.0629(15) Uani 1 1 d . . . H9A H 0.3552 0.5505 0.1161 0.075 Uiso 1 1 calc R . . C10 C 0.2671(4) 0.6335(5) -0.0175(4) 0.0698(16) Uani 1 1 d . . . H10A H 0.1969 0.5978 -0.0401 0.084 Uiso 1 1 calc R . . C11 C 0.2771(4) 0.7147(4) -0.0769(4) 0.0630(16) Uani 1 1 d . . . H11A H 0.2146 0.7351 -0.1400 0.076 Uiso 1 1 calc R . . C12 C 0.3833(4) 0.7647(4) -0.0394(4) 0.0532(13) Uani 1 1 d . . . H12A H 0.3910 0.8190 -0.0798 0.064 Uiso 1 1 calc R . . C13 C 0.8504(5) 0.5452(4) 0.2159(4) 0.0786(18) Uani 1 1 d . . . H13A H 0.7745 0.5510 0.1571 0.118 Uiso 1 1 calc R . . H13B H 0.8645 0.4744 0.2392 0.118 Uiso 1 1 calc R . . H13C H 0.9085 0.5672 0.1937 0.118 Uiso 1 1 calc R . . C14 C 0.5577(5) 0.5780(5) 0.2942(4) 0.0775(17) Uani 1 1 d . . . H14A H 0.6169 0.6006 0.3618 0.116 Uiso 1 1 calc R . . H14B H 0.5663 0.5051 0.2861 0.116 Uiso 1 1 calc R . . H14C H 0.4821 0.5913 0.2912 0.116 Uiso 1 1 calc R . . N1 N 0.9816(3) 0.7049(3) 0.4662(3) 0.0389(8) Uani 1 1 d . . . N2 N 0.7701(3) 0.6609(3) 0.3082(3) 0.0399(9) Uani 1 1 d . . . N3 N 0.6681(3) 0.6671(3) 0.2125(3) 0.0437(9) Uani 1 1 d . . . N4 N 0.4746(3) 0.7405(3) 0.0501(3) 0.0440(9) Uani 1 1 d . . . N5 N 0.8387(3) 0.7158(3) 0.5978(3) 0.0460(10) Uani 1 1 d . . . N6 N 0.9247(3) 0.6990(3) 0.6778(3) 0.0423(9) Uani 1 1 d . . . N7 N 1.0081(3) 0.6820(4) 0.7537(3) 0.0719(14) Uani 1 1 d . . . N8 N 0.9294(3) 0.9496(3) 0.5103(3) 0.0463(10) Uani 1 1 d . . . N9 N 1.0000 1.0000 0.5000 0.0357(12) Uani 1 2 d S . . N10 N 0.7443(3) 0.8889(3) 0.2667(3) 0.0438(9) Uani 1 1 d . . . N11 N 0.7655(3) 0.9784(3) 0.2630(3) 0.0462(10) Uani 1 1 d . . . N12 N 0.7839(4) 1.0649(4) 0.2604(3) 0.0830(16) Uani 1 1 d . . . N13 N 0.5898(3) 0.9598(3) 0.0232(3) 0.0521(11) Uani 1 1 d . . . N14 N 0.5000 1.0000 0.0000 0.0410(13) Uani 1 2 d S . . N15 N 0.6421(3) 0.6981(3) -0.0602(3) 0.0493(10) Uani 1 1 d . . . N16 N 0.5522(3) 0.6756(4) -0.1315(3) 0.0649(13) Uani 1 1 d . . . N17 N 0.4622(4) 0.6582(5) -0.2010(5) 0.126(3) Uani 1 1 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 Cd1 0.03117(17) 0.03266(19) 0.03249(17) -0.00212(14) 0.01374(13) -0.00126(13) Cd2 0.02782(17) 0.0393(2) 0.03533(18) 0.00057(15) 0.01179(13) 0.00083(14) C1 0.043(3) 0.061(4) 0.046(3) 0.009(2) 0.021(2) 0.001(2) C2 0.049(3) 0.083(5) 0.066(4) 0.024(3) 0.026(3) 0.011(3) C3 0.053(4) 0.082(5) 0.088(5) 0.033(4) 0.040(3) 0.029(3) C4 0.072(4) 0.057(4) 0.070(4) 0.018(3) 0.045(3) 0.022(3) C5 0.058(3) 0.044(3) 0.043(3) 0.017(2) 0.033(2) 0.017(2) C6 0.073(3) 0.032(3) 0.036(3) 0.010(2) 0.024(2) 0.008(2) C7 0.069(3) 0.045(3) 0.040(3) 0.002(2) 0.024(2) -0.005(2) C8 0.055(3) 0.054(3) 0.043(3) -0.008(2) 0.023(2) -0.012(2) C9 0.067(4) 0.059(4) 0.062(4) -0.007(3) 0.028(3) -0.026(3) C10 0.052(3) 0.087(5) 0.071(4) -0.029(3) 0.026(3) -0.023(3) C11 0.042(3) 0.079(5) 0.061(4) -0.017(3) 0.016(2) -0.008(3) C12 0.043(3) 0.065(4) 0.052(3) -0.006(3) 0.021(3) -0.004(2) C13 0.126(5) 0.058(4) 0.048(3) -0.001(3) 0.035(3) 0.033(3) C14 0.096(4) 0.089(5) 0.057(3) 0.010(3) 0.042(3) -0.013(4) N1 0.039(2) 0.047(2) 0.034(2) 0.0085(18) 0.0192(16) 0.0089(17) N2 0.053(2) 0.036(2) 0.031(2) 0.0014(16) 0.0186(17) 0.0029(17) N3 0.050(2) 0.043(3) 0.039(2) -0.0049(17) 0.0202(18) -0.0060(18) N4 0.037(2) 0.054(3) 0.039(2) 0.0007(19) 0.0146(18) -0.0046(17) N5 0.0265(19) 0.070(3) 0.039(2) 0.0150(19) 0.0127(16) 0.0082(18) N6 0.034(2) 0.045(2) 0.047(2) -0.002(2) 0.0173(18) 0.0045(18) N7 0.034(2) 0.102(4) 0.057(3) -0.007(3) -0.0013(19) 0.009(2) N8 0.051(3) 0.044(3) 0.050(2) -0.0057(19) 0.028(2) -0.0165(19) N9 0.043(3) 0.028(3) 0.033(3) -0.004(2) 0.015(2) 0.006(2) N10 0.054(2) 0.038(2) 0.039(2) -0.0011(18) 0.0191(17) -0.0062(19) N11 0.061(3) 0.044(3) 0.029(2) -0.0005(18) 0.0156(19) 0.000(2) N12 0.129(4) 0.044(3) 0.062(3) -0.001(2) 0.029(3) -0.019(3) N13 0.045(2) 0.045(3) 0.062(3) 0.014(2) 0.020(2) 0.0169(19) N14 0.050(4) 0.035(3) 0.032(3) 0.006(2) 0.013(2) 0.001(3) N15 0.032(2) 0.067(3) 0.045(2) -0.021(2) 0.0132(17) -0.006(2) N16 0.041(3) 0.084(4) 0.064(3) -0.033(3) 0.018(2) -0.006(2) N17 0.057(3) 0.174(7) 0.119(5) -0.087(5) 0.013(3) -0.023(4) _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 N15 2.271(3) 4_576 ? Cd1 N8 2.312(4) . ? Cd1 N1 2.331(3) . ? Cd1 N10 2.350(4) . ? Cd1 N2 2.437(4) . ? Cd1 N5 2.473(3) . ? Cd2 N5 2.246(3) 4_575 ? Cd2 N13 2.275(4) . ? Cd2 N4 2.335(3) . ? Cd2 N3 2.366(4) . ? Cd2 N10 2.410(4) . ? Cd2 N15 2.479(4) . ? C1 N1 1.329(5) . ? C1 C2 1.385(7) . ? C2 C3 1.386(8) . ? C3 C4 1.373(6) . ? C4 C5 1.383(6) . ? C5 N1 1.362(6) . ? C5 C6 1.474(6) . ? C6 N2 1.265(5) . ? C6 C13 1.518(6) . ? C7 N3 1.284(6) . ? C7 C14 1.493(6) . ? C7 C8 1.497(6) . ? C8 N4 1.327(6) . ? C8 C9 1.399(6) . ? C9 C10 1.369(7) . ? C10 C11 1.375(7) . ? C11 C12 1.380(6) . ? C12 N4 1.320(5) . ? N2 N3 1.401(5) . ? N5 N6 1.193(4) . ? N5 Cd2 2.246(3) 4_576 ? N6 N7 1.147(5) . ? N8 N9 1.168(3) . ? N9 N8 1.168(3) 3_776 ? N10 N11 1.193(5) . ? N11 N12 1.145(5) . ? N13 N14 1.166(3) . ? N14 N13 1.166(3) 3_675 ? N15 N16 1.179(5) . ? N15 Cd1 2.271(3) 4_575 ? N16 N17 1.156(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 N15 Cd1 N8 114.52(14) 4_576 . ? N15 Cd1 N1 142.65(13) 4_576 . ? N8 Cd1 N1 92.01(13) . . ? N15 Cd1 N10 94.32(12) 4_576 . ? N8 Cd1 N10 89.17(13) . . ? N1 Cd1 N10 112.73(12) . . ? N15 Cd1 N2 94.28(13) 4_576 . ? N8 Cd1 N2 149.14(12) . . ? N1 Cd1 N2 68.76(13) . . ? N10 Cd1 N2 77.32(12) . . ? N15 Cd1 N5 70.64(12) 4_576 . ? N8 Cd1 N5 98.52(13) . . ? N1 Cd1 N5 80.19(11) . . ? N10 Cd1 N5 164.87(11) . . ? N2 Cd1 N5 101.47(12) . . ? N5 Cd2 N13 108.11(14) 4_575 . ? N5 Cd2 N4 149.94(13) 4_575 . ? N13 Cd2 N4 90.89(13) . . ? N5 Cd2 N3 100.41(14) 4_575 . ? N13 Cd2 N3 148.25(14) . . ? N4 Cd2 N3 69.78(13) . . ? N5 Cd2 N10 92.18(12) 4_575 . ? N13 Cd2 N10 86.92(13) . . ? N4 Cd2 N10 112.40(12) . . ? N3 Cd2 N10 78.20(12) . . ? N5 Cd2 N15 70.93(12) 4_575 . ? N13 Cd2 N15 103.14(14) . . ? N4 Cd2 N15 82.38(12) . . ? N3 Cd2 N15 99.05(13) . . ? N10 Cd2 N15 162.26(11) . . ? N1 C1 C2 123.2(5) . . ? C1 C2 C3 117.1(5) . . ? C4 C3 C2 121.1(5) . . ? C3 C4 C5 118.2(5) . . ? N1 C5 C4 121.6(5) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.5(5) . . ? N2 C6 C5 118.4(4) . . ? N2 C6 C13 124.3(4) . . ? C5 C6 C13 117.3(4) . . ? N3 C7 C14 123.4(4) . . ? N3 C7 C8 116.3(4) . . ? C14 C7 C8 120.3(4) . . ? N4 C8 C9 122.6(5) . . ? N4 C8 C7 116.2(4) . . ? C9 C8 C7 121.2(5) . . ? C10 C9 C8 118.1(5) . . ? C9 C10 C11 119.9(5) . . ? C10 C11 C12 117.5(5) . . ? N4 C12 C11 124.2(5) . . ? C1 N1 C5 118.7(4) . . ? C1 N1 Cd1 122.6(3) . . ? C5 N1 Cd1 118.4(3) . . ? C6 N2 N3 117.8(4) . . ? C6 N2 Cd1 115.9(3) . . ? N3 N2 Cd1 118.2(3) . . ? C7 N3 N2 121.1(4) . . ? C7 N3 Cd2 116.9(3) . . ? N2 N3 Cd2 115.7(2) . . ? C12 N4 C8 117.8(4) . . ? C12 N4 Cd2 123.6(3) . . ? C8 N4 Cd2 117.2(3) . . ? N6 N5 Cd2 119.8(3) . 4_576 ? N6 N5 Cd1 129.6(3) . . ? Cd2 N5 Cd1 109.43(13) 4_576 . ? N7 N6 N5 178.8(5) . . ? N9 N8 Cd1 138.2(3) . . ? N8 N9 N8 180.0(3) . 3_776 ? N11 N10 Cd1 119.3(3) . . ? N11 N10 Cd2 114.3(3) . . ? Cd1 N10 Cd2 125.06(16) . . ? N12 N11 N10 178.2(5) . . ? N14 N13 Cd2 132.8(3) . . ? N13 N14 N13 180.000(1) 3_675 . ? N16 N15 Cd1 124.9(3) . 4_575 ? N16 N15 Cd2 124.4(3) . . ? Cd1 N15 Cd2 108.44(14) 4_575 . ? N17 N16 N15 176.8(6) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.779 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.141