Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # SUBMISSION DETAILS loop_ _publ_author_name 'Chun-Hua Yan' 'Shi-Qiang Bai' 'En-Qing Gao' 'Zhe-Ming Wang' _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 # TITLE AND AUTHOR LIST _publ_section_title ; New one- and two-dimensional metal-dicyanamido complexes with a flexible bridging co-ligand: structural and magnetic properties ; ## Crystallographic Data of Complex 1 data_1 _database_code_CSD 200571 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Mn N8' _chemical_formula_weight 385.30 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 16.0806(5) _cell_length_b 10.4123(4) _cell_length_c 12.7979(5) _cell_angle_alpha 90.00 _cell_angle_beta 122.0554(12) _cell_angle_gamma 90.00 _cell_volume 1816.12(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8214 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.959 _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_% none _diffrn_reflns_number 14449 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2081 _reflns_number_gt 1281 _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)' _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^)+(0.0522P)^2^+1.6270P] 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 0.0023(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2081 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.2500 0.2500 0.0000 0.0329(3) Uani 1 2 d S . . N1 N 0.31804(15) 0.4446(2) 0.0752(2) 0.0422(6) Uani 1 1 d . . . N2 N 0.31859(17) 0.1756(3) 0.1906(2) 0.0493(7) Uani 1 1 d . . . N3 N 0.61824(17) 0.1911(3) 0.5021(2) 0.0446(7) Uani 1 1 d . . . N4 N 0.44682(18) 0.1238(3) 0.4009(3) 0.0679(10) Uani 1 1 d . . . C1 C 0.5000 0.8768(4) 0.2500 0.097(3) Uani 1 2 d S . . H1A H 0.4889 0.9341 0.3003 0.116 Uiso 1 1 d R . . C2 C 0.4074(3) 0.8404(3) 0.1672(6) 0.112(2) Uani 1 1 d . . . H2A H 0.3886 0.8819 0.0899 0.135 Uiso 1 1 calc R . . H2B H 0.3661 0.8763 0.1941 0.135 Uiso 1 1 calc R . . C3 C 0.3803(2) 0.6999(3) 0.1390(4) 0.0756(14) Uani 1 1 d . . . C4 C 0.3347(2) 0.6354(3) 0.1888(4) 0.0755(13) Uani 1 1 d . . . H4A H 0.3243 0.6759 0.2457 0.091 Uiso 1 1 calc R . . C5 C 0.3043(2) 0.5099(3) 0.1537(3) 0.0569(10) Uani 1 1 d . . . H5A H 0.2724 0.4690 0.1873 0.068 Uiso 1 1 calc R . . C6 C 0.3634(2) 0.5074(3) 0.0281(3) 0.0537(9) Uani 1 1 d . . . H6A H 0.3743 0.4642 -0.0271 0.064 Uiso 1 1 calc R . . C7 C 0.3949(2) 0.6327(3) 0.0571(4) 0.0684(12) Uani 1 1 d . . . H7A H 0.4260 0.6719 0.0216 0.082 Uiso 1 1 calc R . . C8 C 0.38179(19) 0.1543(3) 0.2887(3) 0.0377(7) Uani 1 1 d . . . C9 C 0.5373(2) 0.1612(3) 0.4497(3) 0.0373(7) 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 Mn1 0.0211(3) 0.0251(3) 0.0348(4) -0.0012(3) 0.0029(2) -0.0007(2) N1 0.0296(12) 0.0296(13) 0.0528(16) -0.0073(12) 0.0120(11) -0.0028(10) N2 0.0307(13) 0.0518(17) 0.0438(15) 0.0053(13) 0.0051(12) -0.0002(12) N3 0.0291(13) 0.0418(15) 0.0479(15) 0.0055(12) 0.0102(11) -0.0013(11) N4 0.0288(13) 0.084(2) 0.0536(17) 0.0325(16) -0.0033(12) -0.0156(13) C1 0.051(3) 0.021(2) 0.121(5) 0.000 -0.021(3) 0.000 C2 0.043(2) 0.0233(19) 0.194(5) -0.027(3) 0.010(3) -0.0008(16) C3 0.0228(15) 0.0294(17) 0.124(4) -0.019(2) 0.0049(19) -0.0020(14) C4 0.0370(18) 0.050(2) 0.114(3) -0.044(2) 0.023(2) -0.0059(17) C5 0.0369(16) 0.047(2) 0.076(2) -0.0243(19) 0.0231(17) -0.0077(15) C6 0.0493(18) 0.0339(17) 0.068(2) -0.0025(16) 0.0239(17) -0.0071(15) C7 0.052(2) 0.031(2) 0.101(3) 0.004(2) 0.026(2) -0.0075(16) C8 0.0262(14) 0.0277(15) 0.0449(18) 0.0025(13) 0.0092(14) -0.0019(11) C9 0.0328(16) 0.0316(16) 0.0362(16) 0.0074(13) 0.0107(13) 0.0011(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 Mn1 N2 2.216(3) 7 ? Mn1 N2 2.216(3) . ? Mn1 N3 2.220(2) 8_455 ? Mn1 N3 2.220(2) 2_655 ? Mn1 N1 2.261(2) . ? Mn1 N1 2.261(2) 7 ? N1 C5 1.326(4) . ? N1 C6 1.338(4) . ? N2 C8 1.142(3) . ? N3 C9 1.147(3) . ? N3 Mn1 2.220(2) 2_655 ? N4 C8 1.290(4) . ? N4 C9 1.301(4) . ? C1 C2 1.345(4) . ? C1 C2 1.345(4) 2_655 ? C2 C3 1.514(5) . ? C3 C4 1.375(6) . ? C3 C7 1.380(6) . ? C4 C5 1.383(5) . ? C6 C7 1.377(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 N2 Mn1 N2 180.00(19) 7 . ? N2 Mn1 N3 89.79(10) 7 8_455 ? N2 Mn1 N3 90.21(10) . 8_455 ? N2 Mn1 N3 90.21(10) 7 2_655 ? N2 Mn1 N3 89.79(10) . 2_655 ? N3 Mn1 N3 180.00(17) 8_455 2_655 ? N2 Mn1 N1 90.05(9) 7 . ? N2 Mn1 N1 89.95(9) . . ? N3 Mn1 N1 89.81(9) 8_455 . ? N3 Mn1 N1 90.19(9) 2_655 . ? N2 Mn1 N1 89.95(9) 7 7 ? N2 Mn1 N1 90.05(9) . 7 ? N3 Mn1 N1 90.19(9) 8_455 7 ? N3 Mn1 N1 89.81(9) 2_655 7 ? N1 Mn1 N1 180.0 . 7 ? C5 N1 C6 116.1(3) . . ? C5 N1 Mn1 123.0(2) . . ? C6 N1 Mn1 120.2(2) . . ? C8 N2 Mn1 155.6(2) . . ? C9 N3 Mn1 149.6(2) . 2_655 ? C8 N4 C9 120.0(3) . . ? C2 C1 C2 147.2(5) . 2_655 ? C1 C2 C3 121.2(3) . . ? C4 C3 C7 116.9(3) . . ? C4 C3 C2 121.1(4) . . ? C7 C3 C2 121.9(5) . . ? C3 C4 C5 119.6(4) . . ? N1 C5 C4 123.9(4) . . ? N1 C6 C7 123.6(4) . . ? C6 C7 C3 119.9(4) . . ? N2 C8 N4 174.2(3) . . ? N3 C9 N4 174.2(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.500 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.066 #===END # Crystallographic Data of Complex 2 data_2 _database_code_CSD 200572 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Co N8' _chemical_formula_weight 389.29 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' Co Co 0.3494 0.9721 '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 15.9615(4) _cell_length_b 10.2737(3) _cell_length_c 12.7113(5) _cell_angle_alpha 90.00 _cell_angle_beta 122.4209(12) _cell_angle_gamma 90.00 _cell_volume 1759.55(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8177 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description flake _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.920 _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_% none _diffrn_reflns_number 13913 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2022 _reflns_number_gt 1262 _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)' _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^)+(0.0492P)^2^+1.8853P] 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 0.0016(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2022 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Co1 Co 0.2500 0.2500 0.0000 0.0352(2) Uani 1 2 d S . . N1 N 0.31358(17) 0.4383(2) 0.0694(2) 0.0431(7) Uani 1 1 d . . . N2 N 0.31690(17) 0.1825(3) 0.1857(2) 0.0470(7) Uani 1 1 d . . . N3 N 0.62028(17) 0.1935(2) 0.4968(2) 0.0440(7) Uani 1 1 d . . . N4 N 0.44693(19) 0.1272(3) 0.3991(3) 0.0680(10) Uani 1 1 d . . . C1 C 0.5000 0.8745(5) 0.2500 0.106(3) Uani 1 2 d S . . H1A H 0.4889 0.9317 0.3003 0.127 Uiso 1 1 d R . . C2 C 0.4059(3) 0.8386(3) 0.1654(6) 0.109(2) Uani 1 1 d . . . H2A H 0.3872 0.8806 0.0874 0.131 Uiso 1 1 calc R . . H2B H 0.3642 0.8754 0.1919 0.131 Uiso 1 1 calc R . . C3 C 0.3784(2) 0.6961(4) 0.1370(5) 0.0757(14) Uani 1 1 d . . . C4 C 0.3328(2) 0.6303(4) 0.1867(4) 0.0723(13) Uani 1 1 d . . . H4A H 0.3229 0.6711 0.2446 0.087 Uiso 1 1 calc R . . C5 C 0.3012(2) 0.5031(3) 0.1507(3) 0.0550(9) Uani 1 1 d . . . H5A H 0.2699 0.4610 0.1852 0.066 Uiso 1 1 calc R . . C6 C 0.3596(2) 0.5018(3) 0.0227(3) 0.0541(9) Uani 1 1 d . . . H6A H 0.3701 0.4581 -0.0333 0.065 Uiso 1 1 calc R . . C7 C 0.3924(2) 0.6290(3) 0.0532(4) 0.0674(12) Uani 1 1 d . . . H7A H 0.4236 0.6691 0.0176 0.081 Uiso 1 1 calc R . . C8 C 0.3807(2) 0.1597(3) 0.2854(3) 0.0389(7) Uani 1 1 d . . . C9 C 0.5384(2) 0.1639(3) 0.4465(3) 0.0391(7) 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 Co1 0.0211(3) 0.0260(3) 0.0364(3) -0.0008(2) 0.0006(2) -0.0009(2) N1 0.0255(12) 0.0297(13) 0.0508(16) -0.0042(12) 0.0050(11) -0.0029(11) N2 0.0281(13) 0.0449(16) 0.0442(16) 0.0023(13) 0.0036(12) -0.0015(11) N3 0.0279(13) 0.0388(13) 0.0442(15) 0.0039(12) 0.0053(11) -0.0007(11) N4 0.0293(14) 0.081(2) 0.0533(18) 0.0280(16) -0.0048(13) -0.0150(14) C1 0.057(3) 0.020(2) 0.126(5) 0.000 -0.027(3) 0.000 C2 0.040(2) 0.0259(19) 0.183(5) -0.024(2) 0.008(3) -0.0039(16) C3 0.0241(16) 0.0291(17) 0.118(4) -0.017(2) 0.0008(19) -0.0015(15) C4 0.0326(17) 0.048(2) 0.104(3) -0.035(2) 0.015(2) -0.0035(16) C5 0.0343(17) 0.0438(19) 0.067(2) -0.0170(18) 0.0143(16) -0.0046(14) C6 0.0428(18) 0.0336(17) 0.064(2) -0.0002(16) 0.0139(17) -0.0044(15) C7 0.043(2) 0.0334(19) 0.096(3) 0.006(2) 0.017(2) -0.0061(15) C8 0.0271(14) 0.0292(15) 0.0443(18) 0.0006(13) 0.0083(14) -0.0048(12) C9 0.0321(16) 0.0321(15) 0.0353(16) 0.0068(13) 0.0063(13) 0.0030(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 Co1 N2 2.119(3) 7 ? Co1 N2 2.119(3) . ? Co1 N3 2.130(3) 8_455 ? Co1 N3 2.130(3) 2_655 ? Co1 N1 2.143(2) . ? Co1 N1 2.143(2) 7 ? N1 C5 1.330(4) . ? N1 C6 1.336(4) . ? N2 C8 1.147(3) . ? N3 C9 1.146(3) . ? N3 Co1 2.130(3) 2_655 ? N4 C8 1.295(4) . ? N4 C9 1.301(4) . ? C1 C2 1.348(4) . ? C1 C2 1.348(4) 2_655 ? C2 C3 1.515(5) . ? C3 C4 1.372(6) . ? C3 C7 1.383(6) . ? C4 C5 1.387(5) . ? C6 C7 1.384(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 N2 Co1 N2 180.00(19) 7 . ? N2 Co1 N3 89.16(10) 7 8_455 ? N2 Co1 N3 90.84(10) . 8_455 ? N2 Co1 N3 90.84(10) 7 2_655 ? N2 Co1 N3 89.16(10) . 2_655 ? N3 Co1 N3 180.00(18) 8_455 2_655 ? N2 Co1 N1 90.45(10) 7 . ? N2 Co1 N1 89.55(10) . . ? N3 Co1 N1 90.15(10) 8_455 . ? N3 Co1 N1 89.85(10) 2_655 . ? N2 Co1 N1 89.55(10) 7 7 ? N2 Co1 N1 90.45(10) . 7 ? N3 Co1 N1 89.85(10) 8_455 7 ? N3 Co1 N1 90.15(10) 2_655 7 ? N1 Co1 N1 180.0 . 7 ? C5 N1 C6 116.6(3) . . ? C5 N1 Co1 122.5(2) . . ? C6 N1 Co1 120.6(2) . . ? C8 N2 Co1 156.5(2) . . ? C9 N3 Co1 152.8(3) . 2_655 ? C8 N4 C9 118.9(3) . . ? C2 C1 C2 148.2(5) . 2_655 ? C1 C2 C3 120.7(3) . . ? C4 C3 C7 117.0(3) . . ? C4 C3 C2 121.6(4) . . ? C7 C3 C2 121.3(5) . . ? C3 C4 C5 120.1(4) . . ? N1 C5 C4 123.3(4) . . ? N1 C6 C7 123.5(4) . . ? C6 C7 C3 119.6(4) . . ? N2 C8 N4 174.6(3) . . ? N3 C9 N4 174.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.446 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.070 #===END # Crystallographic Data of Complex 3 data_3 _database_code_CSD 200573 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 N8 Zn' _chemical_formula_weight 395.73 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' 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 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 16.0448(3) _cell_length_b 10.3215(2) _cell_length_c 12.8434(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.3988(9) _cell_angle_gamma 90.00 _cell_volume 1795.87(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10717 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.386 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.583 _exptl_absorpt_correction_T_max 0.665 _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_% none _diffrn_reflns_number 16039 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2024 _reflns_number_gt 1615 _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)' _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^)+(0.0537P)^2^+2.2869P] 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 0.0070(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2024 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.2500 0.2500 0.0000 0.04520(19) Uani 1 2 d S . . N1 N 0.31294(15) 0.4378(2) 0.0687(2) 0.0520(5) Uani 1 1 d . . . N2 N 0.31742(16) 0.1804(3) 0.1871(2) 0.0609(6) Uani 1 1 d . . . N3 N 0.61901(16) 0.1929(3) 0.4983(2) 0.0598(6) Uani 1 1 d . . . N4 N 0.44693(18) 0.1292(4) 0.3973(2) 0.0877(10) Uani 1 1 d . . . C1 C 0.5000 0.8699(4) 0.2500 0.151(4) Uani 1 2 d S . . H1A H 0.4889 0.9272 0.3003 0.181 Uiso 1 1 d R . . C2 C 0.4068(3) 0.8340(3) 0.1660(5) 0.1029(16) Uani 1 1 d . . . H2A H 0.3887 0.8760 0.0891 0.123 Uiso 1 1 calc R . . H2B H 0.3651 0.8709 0.1919 0.123 Uiso 1 1 calc R . . C3 C 0.3784(2) 0.6928(3) 0.1368(3) 0.0729(10) Uani 1 1 d . . . C4 C 0.3325(2) 0.6269(3) 0.1857(3) 0.0749(9) Uani 1 1 d . . . H4A H 0.3229 0.6671 0.2433 0.090 Uiso 1 1 calc R . . C5 C 0.3008(2) 0.5013(3) 0.1494(3) 0.0642(7) Uani 1 1 d . . . H5A H 0.2694 0.4592 0.1831 0.077 Uiso 1 1 calc R . . C6 C 0.3586(2) 0.5006(3) 0.0228(3) 0.0634(7) Uani 1 1 d . . . H6A H 0.3687 0.4575 -0.0332 0.076 Uiso 1 1 calc R . . C7 C 0.3917(2) 0.6265(3) 0.0541(3) 0.0732(9) Uani 1 1 d . . . H7A H 0.4229 0.6664 0.0191 0.088 Uiso 1 1 calc R . . C8 C 0.38138(17) 0.1601(2) 0.2849(2) 0.0481(6) Uani 1 1 d . . . C9 C 0.53801(17) 0.1652(2) 0.4460(2) 0.0479(6) 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 Zn1 0.0281(2) 0.0415(3) 0.0429(3) -0.00080(15) 0.00368(16) -0.00264(14) N1 0.0383(10) 0.0440(11) 0.0542(12) -0.0042(9) 0.0119(9) -0.0044(9) N2 0.0416(11) 0.0680(16) 0.0478(12) 0.0060(11) 0.0072(10) -0.0010(11) N3 0.0350(11) 0.0642(14) 0.0594(13) 0.0068(12) 0.0114(10) -0.0014(10) N4 0.0387(12) 0.137(3) 0.0547(14) 0.0327(16) 0.0033(11) -0.0175(15) C1 0.073(3) 0.031(2) 0.192(7) 0.000 -0.033(4) 0.000 C2 0.0595(19) 0.0387(15) 0.147(4) -0.017(2) 0.014(2) 0.0005(14) C3 0.0388(14) 0.0416(15) 0.094(2) -0.0118(16) 0.0064(14) -0.0023(12) C4 0.0523(16) 0.0626(18) 0.089(2) -0.0281(17) 0.0241(16) -0.0040(14) C5 0.0506(15) 0.0601(17) 0.0710(18) -0.0167(15) 0.0253(14) -0.0092(13) C6 0.0619(17) 0.0512(15) 0.0669(18) -0.0063(14) 0.0277(15) -0.0124(13) C7 0.0645(18) 0.0504(16) 0.087(2) -0.0007(16) 0.0291(17) -0.0138(14) C8 0.0345(11) 0.0497(13) 0.0468(13) 0.0002(11) 0.0130(10) -0.0038(10) C9 0.0374(12) 0.0527(14) 0.0407(12) 0.0051(10) 0.0123(10) 0.0038(10) _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 N1 2.145(2) . ? Zn1 N1 2.145(2) 7 ? Zn1 N2 2.162(2) 7 ? Zn1 N2 2.162(2) . ? Zn1 N3 2.171(2) 8_455 ? Zn1 N3 2.171(2) 2_655 ? N1 C5 1.325(4) . ? N1 C6 1.329(4) . ? N2 C8 1.137(3) . ? N3 C9 1.134(3) . ? N3 Zn1 2.171(2) 2_655 ? N4 C8 1.291(3) . ? N4 C9 1.298(3) . ? C1 C2 1.345(4) 2_655 ? C1 C2 1.345(4) . ? C2 C3 1.513(4) . ? C3 C7 1.373(5) . ? C3 C4 1.376(5) . ? C4 C5 1.380(4) . ? C6 C7 1.380(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 N1 Zn1 N1 180.0 . 7 ? N1 Zn1 N2 90.11(9) . 7 ? N1 Zn1 N2 89.89(9) 7 7 ? N1 Zn1 N2 89.89(9) . . ? N1 Zn1 N2 90.11(9) 7 . ? N2 Zn1 N2 180.00(18) 7 . ? N1 Zn1 N3 89.92(9) . 8_455 ? N1 Zn1 N3 90.08(9) 7 8_455 ? N2 Zn1 N3 89.61(10) 7 8_455 ? N2 Zn1 N3 90.39(10) . 8_455 ? N1 Zn1 N3 90.08(9) . 2_655 ? N1 Zn1 N3 89.92(9) 7 2_655 ? N2 Zn1 N3 90.39(10) 7 2_655 ? N2 Zn1 N3 89.61(10) . 2_655 ? N3 Zn1 N3 180.00(17) 8_455 2_655 ? C5 N1 C6 116.9(3) . . ? C5 N1 Zn1 122.3(2) . . ? C6 N1 Zn1 120.49(19) . . ? C8 N2 Zn1 155.1(2) . . ? C9 N3 Zn1 150.5(2) . 2_655 ? C8 N4 C9 120.0(3) . . ? C2 C1 C2 148.0(5) 2_655 . ? C1 C2 C3 121.5(3) . . ? C7 C3 C4 116.7(3) . . ? C7 C3 C2 121.4(4) . . ? C4 C3 C2 121.8(4) . . ? C3 C4 C5 120.0(3) . . ? N1 C5 C4 123.2(3) . . ? N1 C6 C7 123.2(3) . . ? C3 C7 C6 120.0(3) . . ? N2 C8 N4 173.4(3) . . ? N3 C9 N4 174.0(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.456 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.054 #===END # Crystallographic Data of Complex 4a data_CCDC185726 _database_code_CSD 185726 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Cd N8' _chemical_formula_weight 442.76 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 16.3548(5) _cell_length_b 10.4935(4) _cell_length_c 13.0115(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.0231(19) _cell_angle_gamma 90.00 _cell_volume 1893.23(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8226 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.893 _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_% none _diffrn_reflns_number 16206 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2132 _reflns_number_gt 1255 _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)' _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^)+(0.0334P)^2^+0.9242P] 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 0.0027(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2132 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.2500 0.2500 0.0000 0.05122(18) Uani 1 2 d S . . N1 N 0.3179(2) 0.4482(3) 0.0758(3) 0.0595(8) Uani 1 1 d . . . N2 N 0.3198(2) 0.1706(4) 0.1959(3) 0.0745(10) Uani 1 1 d . . . N3 N 0.6147(2) 0.1908(4) 0.5049(3) 0.0716(9) Uani 1 1 d . . . N4 N 0.4477(2) 0.1255(5) 0.4009(3) 0.1032(15) Uani 1 1 d . . . C1 C 0.5000 0.8748(6) 0.2500 0.153(5) Uani 1 2 d S . . H1A H 0.4893 0.9310 0.3000 0.184 Uiso 1 1 d R . . C2 C 0.4089(3) 0.8383(4) 0.1701(6) 0.116(2) Uani 1 1 d . . . H2A H 0.3896 0.8796 0.0938 0.139 Uiso 1 1 calc R . . H2B H 0.3691 0.8743 0.1977 0.139 Uiso 1 1 calc R . . C3 C 0.3811(3) 0.6999(5) 0.1419(5) 0.0797(14) Uani 1 1 d . . . C4 C 0.3350(3) 0.6359(5) 0.1878(4) 0.0883(15) Uani 1 1 d . . . H4A H 0.3241 0.6761 0.2431 0.106 Uiso 1 1 calc R . . C5 C 0.3044(3) 0.5124(5) 0.1532(4) 0.0796(13) Uani 1 1 d . . . H5A H 0.2726 0.4720 0.1859 0.096 Uiso 1 1 calc R . . C6 C 0.3640(3) 0.5103(4) 0.0317(4) 0.0766(12) Uani 1 1 d . . . H6A H 0.3756 0.4677 -0.0220 0.092 Uiso 1 1 calc R . . C7 C 0.3951(3) 0.6337(4) 0.0617(4) 0.0854(14) Uani 1 1 d . . . H7A H 0.4260 0.6729 0.0273 0.102 Uiso 1 1 calc R . . C8 C 0.3828(2) 0.1548(4) 0.2913(3) 0.0556(9) Uani 1 1 d . . . C9 C 0.5364(3) 0.1638(4) 0.4507(3) 0.0583(9) 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 0.0349(2) 0.0465(2) 0.0490(2) -0.00179(18) 0.00646(15) -0.00208(19) N1 0.0495(17) 0.0523(19) 0.0613(19) -0.0107(15) 0.0190(16) -0.0075(15) N2 0.0543(19) 0.087(3) 0.054(2) 0.0092(18) 0.0102(17) 0.0000(19) N3 0.0452(18) 0.081(2) 0.070(2) 0.0076(18) 0.0174(17) -0.0075(17) N4 0.052(2) 0.161(4) 0.062(2) 0.036(2) 0.0064(18) -0.023(2) C1 0.078(5) 0.028(4) 0.214(9) 0.000 -0.016(5) 0.000 C2 0.078(3) 0.045(3) 0.171(5) -0.021(3) 0.029(3) 0.001(3) C3 0.051(2) 0.049(2) 0.104(4) -0.016(3) 0.017(2) -0.003(2) C4 0.068(3) 0.079(3) 0.112(4) -0.042(3) 0.043(3) -0.012(3) C5 0.071(3) 0.075(3) 0.096(3) -0.026(3) 0.046(3) -0.019(2) C6 0.086(3) 0.063(3) 0.084(3) -0.016(2) 0.047(3) -0.018(2) C7 0.092(3) 0.057(3) 0.105(3) -0.008(3) 0.051(3) -0.024(2) C8 0.0438(19) 0.059(3) 0.054(2) 0.0010(17) 0.0189(19) -0.0029(17) C9 0.054(2) 0.063(3) 0.049(2) 0.0030(18) 0.0207(18) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.317(3) . ? Cd1 N1 2.317(3) 7 ? Cd1 N2 2.325(3) 7 ? Cd1 N2 2.325(3) . ? Cd1 N3 2.331(3) 8_455 ? Cd1 N3 2.331(3) 2_655 ? N1 C5 1.323(5) . ? N1 C6 1.335(5) . ? N2 C8 1.129(4) . ? N3 C9 1.123(4) . ? N3 Cd1 2.331(3) 2_655 ? N4 C8 1.284(4) . ? N4 C9 1.300(5) . ? C1 C2 1.343(5) . ? C1 C2 1.343(5) 2_655 ? C2 C3 1.509(7) . ? C3 C4 1.361(7) . ? C3 C7 1.370(7) . ? C4 C5 1.376(6) . ? C6 C7 1.370(6) . ? 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 Cd1 N1 180.0 . 7 ? N1 Cd1 N2 89.50(12) . 7 ? N1 Cd1 N2 90.50(12) 7 7 ? N1 Cd1 N2 90.50(12) . . ? N1 Cd1 N2 89.50(12) 7 . ? N2 Cd1 N2 180.0(2) 7 . ? N1 Cd1 N3 89.78(12) . 8_455 ? N1 Cd1 N3 90.22(12) 7 8_455 ? N2 Cd1 N3 90.73(12) 7 8_455 ? N2 Cd1 N3 89.27(12) . 8_455 ? N1 Cd1 N3 90.22(12) . 2_655 ? N1 Cd1 N3 89.78(12) 7 2_655 ? N2 Cd1 N3 89.27(12) 7 2_655 ? N2 Cd1 N3 90.73(12) . 2_655 ? N3 Cd1 N3 180.00(14) 8_455 2_655 ? C5 N1 C6 116.0(4) . . ? C5 N1 Cd1 123.1(3) . . ? C6 N1 Cd1 120.5(3) . . ? C8 N2 Cd1 152.9(3) . . ? C9 N3 Cd1 146.5(3) . 2_655 ? C8 N4 C9 121.7(4) . . ? C2 C1 C2 146.9(6) . 2_655 ? C1 C2 C3 122.0(5) . . ? C4 C3 C7 116.1(4) . . ? C4 C3 C2 122.3(5) . . ? C7 C3 C2 121.5(5) . . ? C3 C4 C5 120.7(5) . . ? N1 C5 C4 123.4(4) . . ? N1 C6 C7 123.3(4) . . ? C6 C7 C3 120.6(5) . . ? N2 C8 N4 172.5(4) . . ? N3 C9 N4 172.5(4) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.510 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.071 #===END # Crystallographic Data of Complex 4b data_CCDC185727 _database_code_CSD 185727 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H14 Cd N8' _chemical_formula_weight 442.76 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 orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 13.2140(2) _cell_length_b 21.7332(4) _cell_length_c 28.7125(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8245.7(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20254 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.908 _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_% none _diffrn_reflns_number 36198 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2346 _reflns_number_gt 1692 _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)' _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^)+(0.0925P)^2^+10.3993P] 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 0.00037(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2346 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.3750 0.3750 0.074184(15) 0.0630(2) Uani 1 2 d S . . N1 N 0.4278(3) 0.30524(15) 0.13099(12) 0.0636(8) Uani 1 1 d . . . N2 N 0.2166(3) 0.32710(19) 0.07226(15) 0.0817(10) Uani 1 1 d . . . N3 N 0.0693(4) 0.1942(2) -0.01741(18) 0.1041(15) Uani 1 1 d . . . N4 N 0.0766(5) 0.2833(4) 0.0309(4) 0.186(4) Uani 1 1 d . . . C1 C 0.6250 0.1250 0.1895(2) 0.0797(18) Uani 1 2 d S . . H1A H 0.6713 0.1471 0.1699 0.096 Uiso 1 1 d R . . C2 C 0.5660(4) 0.1709(2) 0.22038(15) 0.0777(12) Uani 1 1 d . . . H2A H 0.5154 0.1490 0.2384 0.093 Uiso 1 1 calc R . . H2B H 0.6121 0.1908 0.2419 0.093 Uiso 1 1 calc R . . C3 C 0.5157(3) 0.21834(18) 0.19075(15) 0.0660(10) Uani 1 1 d . . . C4 C 0.5584(3) 0.2749(2) 0.18328(15) 0.0736(11) Uani 1 1 d . . . H4A H 0.6189 0.2851 0.1980 0.088 Uiso 1 1 calc R . . C5 C 0.5131(3) 0.31660(19) 0.15442(14) 0.0684(10) Uani 1 1 d . . . H5A H 0.5433 0.3550 0.1509 0.082 Uiso 1 1 calc R . . C6 C 0.3851(4) 0.2510(2) 0.1383(2) 0.0852(15) Uani 1 1 d . . . H6A H 0.3248 0.2419 0.1231 0.102 Uiso 1 1 calc R . . C7 C 0.4266(4) 0.2072(2) 0.1678(2) 0.0920(15) Uani 1 1 d . . . H7A H 0.3937 0.1698 0.1721 0.110 Uiso 1 1 calc R . . C8 C 0.0805(4) 0.2346(3) 0.0057(2) 0.0941(16) Uani 1 1 d . . . C9 C 0.1561(4) 0.3030(2) 0.0527(2) 0.0881(15) 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 0.0660(3) 0.0506(3) 0.0723(4) 0.000 0.000 -0.00096(15) N1 0.0633(19) 0.0502(17) 0.077(2) 0.0016(14) 0.0025(15) 0.0000(14) N2 0.074(2) 0.072(2) 0.099(3) -0.0094(19) -0.005(2) -0.0038(19) N3 0.098(3) 0.108(3) 0.106(3) -0.044(3) 0.000(3) -0.003(3) N4 0.090(4) 0.181(6) 0.287(10) -0.143(7) -0.042(5) 0.024(4) C1 0.098(5) 0.079(4) 0.062(4) 0.000 0.000 0.027(3) C2 0.093(3) 0.071(2) 0.069(3) 0.002(2) 0.009(2) 0.024(2) C3 0.067(2) 0.060(2) 0.071(2) -0.0017(18) 0.0122(18) 0.0147(17) C4 0.071(2) 0.078(3) 0.071(3) 0.003(2) 0.0011(19) 0.002(2) C5 0.076(2) 0.062(2) 0.067(3) 0.0021(18) -0.0014(19) -0.0116(18) C6 0.075(3) 0.054(2) 0.127(4) 0.017(3) -0.020(3) -0.0103(19) C7 0.094(3) 0.052(2) 0.131(4) 0.018(2) -0.014(3) -0.008(2) C8 0.064(3) 0.107(4) 0.110(4) -0.042(3) -0.008(3) 0.005(3) C9 0.058(2) 0.087(3) 0.120(4) -0.040(3) -0.003(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.333(3) 2 ? Cd1 N1 2.333(3) . ? Cd1 N3 2.337(4) 29 ? Cd1 N3 2.337(4) 18_665 ? Cd1 N2 2.339(4) 2 ? Cd1 N2 2.339(4) . ? N1 C6 1.324(5) . ? N1 C5 1.336(5) . ? N2 C9 1.109(6) . ? N3 C8 1.110(6) . ? N3 Cd1 2.337(4) 29 ? N4 C8 1.283(7) . ? N4 C9 1.295(8) . ? C1 C2 1.546(6) 14_545 ? C1 C2 1.546(6) . ? C2 C3 1.492(6) . ? C3 C7 1.370(7) . ? C3 C4 1.371(6) . ? C4 C5 1.366(6) . ? C6 C7 1.388(7) . ? 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 Cd1 N1 91.31(16) 2 . ? N1 Cd1 N3 179.01(14) 2 29 ? N1 Cd1 N3 88.58(17) . 29 ? N1 Cd1 N3 88.58(17) 2 18_665 ? N1 Cd1 N3 179.01(14) . 18_665 ? N3 Cd1 N3 91.5(3) 29 18_665 ? N1 Cd1 N2 89.70(13) 2 2 ? N1 Cd1 N2 92.19(13) . 2 ? N3 Cd1 N2 89.33(16) 29 2 ? N3 Cd1 N2 88.79(16) 18_665 2 ? N1 Cd1 N2 92.19(13) 2 . ? N1 Cd1 N2 89.70(13) . . ? N3 Cd1 N2 88.79(16) 29 . ? N3 Cd1 N2 89.33(16) 18_665 . ? N2 Cd1 N2 177.3(2) 2 . ? C6 N1 C5 116.4(4) . . ? C6 N1 Cd1 124.2(3) . . ? C5 N1 Cd1 118.9(3) . . ? C9 N2 Cd1 150.2(4) . . ? C8 N3 Cd1 152.2(5) . 29 ? C8 N4 C9 120.8(6) . . ? C2 C1 C2 110.1(5) 14_545 . ? C3 C2 C1 110.1(4) . . ? C7 C3 C4 116.0(4) . . ? C7 C3 C2 122.3(4) . . ? C4 C3 C2 121.7(4) . . ? C5 C4 C3 120.6(4) . . ? N1 C5 C4 123.6(4) . . ? N1 C6 C7 122.6(4) . . ? C3 C7 C6 120.8(4) . . ? N3 C8 N4 169.7(6) . . ? N2 C9 N4 170.2(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.884 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.091 #===END