# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email HOUHONGW@ZZU.EDU.CN _publ_contact_author_name 'Prof Hongwei Hou' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_address ; Department of Chemistry Zhengzhou University Zhengzhou Henan 450052 CHINA ; _publ_section_title ; Synthesis and crystal structures of novel compounds on the basis of a rigid angular ligand, and the magnetic properties of the Cu(II) polymer ; loop_ _publ_author_name 'Hongwei Hou' 'Yaoting Fan' 'Tie-Zhu Ge' 'Gang Li' 'Lixia Xie' 'Yu Zhu' data_Polymer_1 _database_code_depnum_ccdc_archive 'CCDC 213496' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H8 Ag N5 O4' _chemical_formula_weight 394.10 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.949(2) _cell_length_b 9.856(2) _cell_length_c 8.358(2) _cell_angle_alpha 102.12(3) _cell_angle_beta 110.50(3) _cell_angle_gamma 74.78(3) _cell_volume 660.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 210 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description PRISMATIC _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method ? _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 R-axis-IV _diffrn_measurement_method 'Osillation frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2263 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.53 _reflns_number_total 2263 _reflns_number_observed 2041 _reflns_observed_criterion >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics texsan _computing_publication_material texsan _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.8090P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0078(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2263 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_obs 0.0421 _refine_ls_wR_factor_all 0.0918 _refine_ls_wR_factor_obs 0.0884 _refine_ls_goodness_of_fit_all 1.101 _refine_ls_goodness_of_fit_obs 1.122 _refine_ls_restrained_S_all 1.101 _refine_ls_restrained_S_obs 1.122 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.30053(6) 0.45945(4) 0.41837(6) 0.0559(2) Uani 1 d . . N1 N 0.2408(5) 0.6666(4) 0.3136(5) 0.0400(9) Uani 1 d . . N2 N 0.0950(5) 1.1877(4) 0.2107(5) 0.0422(10) Uani 1 d . . N3 N 0.1035(5) 1.2862(4) 0.1174(5) 0.0433(10) Uani 1 d . . N4 N 0.2630(5) 1.3700(4) -0.3800(5) 0.0440(10) Uani 1 d . . N5 N 0.5536(6) 0.2432(5) 0.2756(5) 0.0485(11) Uani 1 d . . O1 O 0.2222(4) 1.0735(3) 0.0230(4) 0.0376(7) Uani 1 d . . O2 O 0.5126(6) 0.3724(4) 0.2664(6) 0.0776(13) Uani 1 d . . O3 O 0.4836(5) 0.1882(5) 0.3418(6) 0.0746(12) Uani 1 d . . O4 O 0.6645(7) 0.1702(5) 0.2227(6) 0.090(2) Uani 1 d . . C1 C 0.1533(6) 0.7822(5) 0.3769(6) 0.0445(12) Uani 1 d . . H1A H 0.1081(6) 0.7737(5) 0.4581(6) 0.053 Uiso 1 calc R . C2 C 0.1257(6) 0.9151(5) 0.3281(6) 0.0449(12) Uani 1 d . . H2B H 0.0644(6) 0.9938(5) 0.3765(6) 0.054 Uiso 1 calc R . C3 C 0.1913(6) 0.9282(4) 0.2060(5) 0.0337(10) Uani 1 d . . C4 C 0.2809(6) 0.8070(5) 0.1363(6) 0.0400(11) Uani 1 d . . H4B H 0.3249(6) 0.8115(5) 0.0523(6) 0.048 Uiso 1 calc R . C5 C 0.3030(6) 0.6795(5) 0.1951(6) 0.0416(11) Uani 1 d . . H5A H 0.3641(6) 0.5989(5) 0.1497(6) 0.050 Uiso 1 calc R . C6 C 0.1652(6) 1.0656(4) 0.1497(5) 0.0330(10) Uani 1 d . . C7 C 0.1797(6) 1.2147(4) 0.0093(6) 0.0358(10) Uani 1 d . . C8 C 0.1924(7) 1.4564(5) -0.2685(7) 0.0501(13) Uani 1 d . . H8A H 0.1595(7) 1.5526(5) -0.2791(7) 0.060 Uiso 1 calc R . C9 C 0.1665(7) 1.4096(5) -0.1395(7) 0.0467(12) Uani 1 d . . H9A H 0.1170(7) 1.4732(5) -0.0646(7) 0.056 Uiso 1 calc R . C10 C 0.2147(6) 1.2664(4) -0.1214(6) 0.0357(10) Uani 1 d . . C11 C 0.2895(6) 1.1757(5) -0.2343(6) 0.0386(11) Uani 1 d . . H11A H 0.3248(6) 1.0793(5) -0.2249(6) 0.046 Uiso 1 calc R . C12 C 0.3104(6) 1.2319(5) -0.3615(6) 0.0425(11) Uani 1 d . . H12A H 0.3598(6) 1.1707(5) -0.4380(6) 0.051 Uiso 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 Ag1 0.0798(4) 0.0392(2) 0.0646(3) 0.0248(2) 0.0356(2) -0.0070(2) N1 0.053(3) 0.032(2) 0.040(2) 0.014(2) 0.013(2) -0.011(2) N2 0.056(3) 0.034(2) 0.048(2) 0.014(2) 0.024(2) -0.008(2) N3 0.056(3) 0.031(2) 0.054(2) 0.014(2) 0.029(2) -0.005(2) N4 0.059(3) 0.033(2) 0.049(2) 0.015(2) 0.023(2) -0.009(2) N5 0.058(3) 0.043(2) 0.047(3) 0.009(2) 0.017(2) -0.011(2) O1 0.053(2) 0.0236(15) 0.042(2) 0.0124(13) 0.020(2) -0.0045(14) O2 0.096(3) 0.037(2) 0.096(3) 0.019(2) 0.028(3) -0.001(2) O3 0.077(3) 0.089(3) 0.075(3) 0.019(2) 0.031(2) -0.031(3) O4 0.127(4) 0.066(3) 0.097(4) 0.025(3) 0.082(3) 0.021(3) C1 0.062(3) 0.040(3) 0.044(3) 0.016(2) 0.027(2) -0.009(2) C2 0.056(3) 0.037(3) 0.050(3) 0.013(2) 0.023(2) -0.010(2) C3 0.040(3) 0.030(2) 0.032(2) 0.009(2) 0.010(2) -0.008(2) C4 0.049(3) 0.038(3) 0.042(3) 0.014(2) 0.021(2) -0.009(2) C5 0.053(3) 0.036(2) 0.040(3) 0.012(2) 0.017(2) -0.006(2) C6 0.043(3) 0.030(2) 0.030(2) 0.007(2) 0.014(2) -0.008(2) C7 0.041(3) 0.023(2) 0.048(3) 0.009(2) 0.016(2) -0.006(2) C8 0.071(4) 0.029(2) 0.064(3) 0.019(2) 0.035(3) -0.002(2) C9 0.065(4) 0.026(2) 0.061(3) 0.010(2) 0.036(3) -0.005(2) C10 0.041(3) 0.025(2) 0.045(3) 0.013(2) 0.012(2) -0.009(2) C11 0.050(3) 0.024(2) 0.049(3) 0.012(2) 0.023(2) -0.004(2) C12 0.052(3) 0.029(2) 0.051(3) 0.012(2) 0.020(2) -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 Ag1 N4 2.215(4) 1_546 ? Ag1 N1 2.251(4) . ? Ag1 O2 2.515(5) . ? N1 C1 1.327(6) . ? N1 C5 1.335(6) . ? N2 C6 1.293(6) . ? N2 N3 1.399(5) . ? N3 C7 1.300(6) . ? N4 C8 1.337(6) . ? N4 C12 1.340(6) . ? N4 Ag1 2.215(4) 1_564 ? N5 O4 1.224(6) . ? N5 O2 1.240(5) . ? N5 O3 1.241(6) . ? O1 C6 1.350(5) . ? O1 C7 1.361(5) . ? C1 C2 1.389(6) . ? C2 C3 1.385(6) . ? C3 C4 1.394(6) . ? C3 C6 1.461(6) . ? C4 C5 1.386(6) . ? C7 C10 1.453(6) . ? C8 C9 1.366(6) . ? C9 C10 1.387(6) . ? C10 C11 1.382(6) . ? C11 C12 1.383(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 N4 Ag1 N1 140.06(15) 1_546 . ? N4 Ag1 O2 130.07(14) 1_546 . ? N1 Ag1 O2 87.83(14) . . ? C1 N1 C5 117.8(4) . . ? C1 N1 Ag1 121.1(3) . . ? C5 N1 Ag1 120.9(3) . . ? C6 N2 N3 105.9(4) . . ? C7 N3 N2 106.3(4) . . ? C8 N4 C12 117.5(4) . . ? C8 N4 Ag1 119.5(3) . 1_564 ? C12 N4 Ag1 123.0(3) . 1_564 ? O4 N5 O2 120.4(5) . . ? O4 N5 O3 119.8(5) . . ? O2 N5 O3 119.7(5) . . ? C6 O1 C7 102.7(3) . . ? N5 O2 Ag1 104.1(3) . . ? N1 C1 C2 123.4(4) . . ? C3 C2 C1 118.6(4) . . ? C2 C3 C4 118.5(4) . . ? C2 C3 C6 120.8(4) . . ? C4 C3 C6 120.7(4) . . ? C5 C4 C3 118.4(4) . . ? N1 C5 C4 123.3(4) . . ? N2 C6 O1 113.1(4) . . ? N2 C6 C3 127.5(4) . . ? O1 C6 C3 119.4(4) . . ? N3 C7 O1 112.0(4) . . ? N3 C7 C10 128.3(4) . . ? O1 C7 C10 119.6(4) . . ? N4 C8 C9 123.0(4) . . ? C8 C9 C10 119.4(5) . . ? C11 C10 C9 118.5(4) . . ? C11 C10 C7 121.7(4) . . ? C9 C10 C7 119.7(4) . . ? C10 C11 C12 118.3(4) . . ? N4 C12 C11 123.3(4) . . ? 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 N4 Ag1 N1 C1 -1.6(5) 1_546 . . . ? O2 Ag1 N1 C1 -165.0(4) . . . . ? N4 Ag1 N1 C5 173.1(3) 1_546 . . . ? O2 Ag1 N1 C5 9.7(4) . . . . ? C6 N2 N3 C7 -0.6(5) . . . . ? O4 N5 O2 Ag1 -175.2(5) . . . . ? O3 N5 O2 Ag1 3.6(6) . . . . ? N4 Ag1 O2 N5 25.2(4) 1_546 . . . ? N1 Ag1 O2 N5 -168.7(3) . . . . ? C5 N1 C1 C2 -1.0(8) . . . . ? Ag1 N1 C1 C2 173.9(4) . . . . ? N1 C1 C2 C3 0.6(8) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C1 C2 C3 C6 179.7(5) . . . . ? C2 C3 C4 C5 -1.3(7) . . . . ? C6 C3 C4 C5 179.6(4) . . . . ? C1 N1 C5 C4 0.2(7) . . . . ? Ag1 N1 C5 C4 -174.7(4) . . . . ? C3 C4 C5 N1 0.9(7) . . . . ? N3 N2 C6 O1 0.6(5) . . . . ? N3 N2 C6 C3 178.6(4) . . . . ? C7 O1 C6 N2 -0.3(5) . . . . ? C7 O1 C6 C3 -178.5(4) . . . . ? C2 C3 C6 N2 6.1(8) . . . . ? C4 C3 C6 N2 -174.8(5) . . . . ? C2 C3 C6 O1 -176.0(4) . . . . ? C4 C3 C6 O1 3.1(7) . . . . ? N2 N3 C7 O1 0.4(5) . . . . ? N2 N3 C7 C10 177.4(5) . . . . ? C6 O1 C7 N3 -0.1(5) . . . . ? C6 O1 C7 C10 -177.4(4) . . . . ? C12 N4 C8 C9 -0.4(8) . . . . ? Ag1 N4 C8 C9 -179.3(4) 1_564 . . . ? N4 C8 C9 C10 0.0(9) . . . . ? C8 C9 C10 C11 0.7(8) . . . . ? C8 C9 C10 C7 -176.7(5) . . . . ? N3 C7 C10 C11 -176.3(5) . . . . ? O1 C7 C10 C11 0.5(7) . . . . ? N3 C7 C10 C9 1.0(8) . . . . ? O1 C7 C10 C9 177.8(4) . . . . ? C9 C10 C11 C12 -0.9(7) . . . . ? C7 C10 C11 C12 176.4(5) . . . . ? C8 N4 C12 C11 0.1(8) . . . . ? Ag1 N4 C12 C11 179.0(4) 1_564 . . . ? C10 C11 C12 N4 0.5(8) . . . . ? _refine_diff_density_max 0.434 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.087 #==============================END========================= data_Polymer_2 _database_code_depnum_ccdc_archive 'CCDC 213497' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Cu2 N4 O11' _chemical_formula_weight 651.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 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 29.829(6) _cell_length_b 13.139(3) _cell_length_c 8.5558(17) _cell_angle_alpha 90.00 _cell_angle_beta 105.95(3) _cell_angle_gamma 90.00 _cell_volume 3224.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description PRISMATIC _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.373 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7708 _exptl_absorpt_correction_T_max 0.7902 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 R-AXIS-IV _diffrn_measurement_method 'Osillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3234 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.1338 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 23.49 _reflns_number_total 1922 _reflns_number_gt 1245 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _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^)+(0.0843P)^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 0.0019(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1922 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1342 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1490 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Cu1 Cu 0.21318(3) 0.78290(9) 0.04033(14) 0.0418(5) Uani 1 1 d . . . O1 O 0.0000 0.8951(7) 0.2500 0.055(3) Uani 1 2 d S . . O2 O 0.24385(19) 0.9155(5) 0.0562(9) 0.059(2) Uani 1 1 d . . . O3 O 0.3063(2) 0.8598(5) -0.0127(9) 0.058(2) Uani 1 1 d . . . O4 O 0.1860(2) 0.8066(5) -0.1947(8) 0.057(2) Uani 1 1 d . . . O5 O 0.2491(2) 0.7494(5) -0.2600(8) 0.052(2) Uani 1 1 d . . . O6 O 0.0632(5) 0.6326(17) -0.392(3) 0.278(10) Uani 1 1 d . . . H6 H 0.0828 0.6746 -0.3467 0.417 Uiso 1 1 calc R . . N1 N 0.1522(2) 0.8393(6) 0.1123(9) 0.044(2) Uani 1 1 d . . . N2 N 0.0214(3) 1.0545(7) 0.2300(14) 0.084(3) Uani 1 1 d . . . C1 C 0.1495(3) 0.9360(9) 0.1508(12) 0.054(3) Uani 1 1 d . . . H1B H 0.1747 0.9777 0.1518 0.064 Uiso 1 1 calc R . . C2 C 0.1115(3) 0.9801(7) 0.1900(12) 0.049(3) Uani 1 1 d . . . H2C H 0.1112 1.0487 0.2166 0.059 Uiso 1 1 calc R . . C3 C 0.0744(3) 0.9176(9) 0.1876(12) 0.047(3) Uani 1 1 d . . . C4 C 0.0770(3) 0.8164(9) 0.1513(13) 0.059(3) Uani 1 1 d . . . H4A H 0.0527 0.7725 0.1526 0.071 Uiso 1 1 calc R . . C5 C 0.1162(3) 0.7806(8) 0.1128(12) 0.056(3) Uani 1 1 d . . . H5A H 0.1173 0.7122 0.0861 0.068 Uiso 1 1 calc R . . C6 C 0.0332(3) 0.9605(8) 0.2231(12) 0.052(3) Uani 1 1 d . . . C7 C 0.2820(4) 0.9269(9) 0.0265(13) 0.057(3) Uani 1 1 d . . . C8 C 0.3001(3) 1.0383(8) 0.0362(16) 0.077(4) Uani 1 1 d . . . H8A H 0.2783 1.0826 0.0664 0.116 Uiso 1 1 calc R . . H8B H 0.3035 1.0585 -0.0679 0.116 Uiso 1 1 calc R . . H8C H 0.3298 1.0427 0.1161 0.116 Uiso 1 1 calc R . . C9 C 0.2088(3) 0.7865(8) -0.2955(11) 0.045(2) Uani 1 1 d . . . C10 C 0.1847(4) 0.8074(8) -0.4733(12) 0.067(3) Uani 1 1 d . . . H10A H 0.1543 0.8356 -0.4831 0.101 Uiso 1 1 calc R . . H10B H 0.1816 0.7450 -0.5337 0.101 Uiso 1 1 calc R . . H10C H 0.2029 0.8549 -0.5155 0.101 Uiso 1 1 calc R . . C11 C 0.0861(10) 0.505(4) -0.339(3) 0.39(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 Cu1 0.0458(7) 0.0444(8) 0.0421(8) 0.0022(8) 0.0239(5) 0.0060(6) O1 0.048(5) 0.043(7) 0.084(8) 0.000 0.032(5) 0.000 O2 0.058(4) 0.051(5) 0.081(6) -0.001(4) 0.041(4) -0.004(3) O3 0.058(4) 0.045(5) 0.081(6) 0.001(4) 0.036(4) -0.006(4) O4 0.066(4) 0.074(6) 0.033(4) 0.009(4) 0.018(3) 0.018(3) O5 0.048(3) 0.068(5) 0.043(4) 0.005(3) 0.018(3) 0.020(3) O6 0.169(13) 0.45(3) 0.22(2) 0.06(2) 0.073(12) -0.012(17) N1 0.055(5) 0.043(5) 0.040(5) 0.005(4) 0.024(4) 0.011(4) N2 0.079(6) 0.047(7) 0.155(11) 0.002(7) 0.082(7) 0.000(5) C1 0.051(5) 0.059(8) 0.059(8) 0.008(6) 0.029(5) 0.002(5) C2 0.046(5) 0.035(6) 0.076(8) 0.003(6) 0.034(5) 0.004(4) C3 0.050(5) 0.051(8) 0.048(7) 0.002(6) 0.027(5) 0.005(5) C4 0.049(6) 0.057(9) 0.080(9) -0.011(6) 0.034(6) -0.016(5) C5 0.055(5) 0.053(7) 0.074(8) -0.023(7) 0.039(5) -0.019(6) C6 0.051(6) 0.047(7) 0.071(8) 0.004(6) 0.040(5) -0.006(5) C7 0.068(7) 0.054(8) 0.050(8) 0.011(6) 0.017(6) 0.000(6) C8 0.077(7) 0.043(7) 0.119(11) 0.004(7) 0.037(7) -0.016(6) C9 0.064(6) 0.041(6) 0.035(6) -0.001(6) 0.020(5) 0.004(5) C10 0.081(7) 0.078(10) 0.042(7) -0.008(6) 0.015(5) 0.019(6) C11 0.31(3) 0.70(7) 0.20(3) 0.20(4) 0.14(3) 0.34(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O5 1.954(6) 7_565 ? Cu1 O2 1.955(6) . ? Cu1 O3 1.958(7) 7_565 ? Cu1 O4 1.975(6) . ? Cu1 N1 2.202(7) . ? Cu1 Cu1 2.623(2) 7_565 ? O1 C6 1.377(10) . ? O1 C6 1.377(10) 2 ? O2 C7 1.241(11) . ? O3 C7 1.245(12) . ? O3 Cu1 1.958(7) 7_565 ? O4 C9 1.264(10) . ? O5 C9 1.253(10) . ? O5 Cu1 1.954(6) 7_565 ? O6 C11 1.81(4) . ? N1 C5 1.324(11) . ? N1 C1 1.320(12) . ? N2 C6 1.291(12) . ? N2 N2 1.408(14) 2 ? C1 C2 1.394(11) . ? C2 C3 1.373(11) . ? C3 C4 1.372(13) . ? C3 C6 1.459(12) . ? C4 C5 1.380(12) . ? C7 C8 1.555(14) . ? C9 C10 1.518(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cu1 O2 89.5(3) 7_565 . ? O5 Cu1 O3 88.9(3) 7_565 7_565 ? O2 Cu1 O3 168.4(2) . 7_565 ? O5 Cu1 O4 168.6(2) 7_565 . ? O2 Cu1 O4 89.1(3) . . ? O3 Cu1 O4 90.2(3) 7_565 . ? O5 Cu1 N1 96.1(3) 7_565 . ? O2 Cu1 N1 95.0(3) . . ? O3 Cu1 N1 96.6(3) 7_565 . ? O4 Cu1 N1 95.3(3) . . ? O5 Cu1 Cu1 83.01(18) 7_565 7_565 ? O2 Cu1 Cu1 84.38(18) . 7_565 ? O3 Cu1 Cu1 83.97(19) 7_565 7_565 ? O4 Cu1 Cu1 85.58(18) . 7_565 ? N1 Cu1 Cu1 178.9(2) . 7_565 ? C6 O1 C6 102.8(10) . 2 ? C7 O2 Cu1 122.1(7) . . ? C7 O3 Cu1 122.3(6) . 7_565 ? C9 O4 Cu1 121.0(6) . . ? C9 O5 Cu1 125.3(6) . 7_565 ? C5 N1 C1 117.0(8) . . ? C5 N1 Cu1 122.6(7) . . ? C1 N1 Cu1 120.4(6) . . ? C6 N2 N2 106.7(5) . 2 ? N1 C1 C2 124.8(9) . . ? C3 C2 C1 116.9(9) . . ? C2 C3 C4 119.2(8) . . ? C2 C3 C6 119.2(10) . . ? C4 C3 C6 121.6(9) . . ? C3 C4 C5 119.3(9) . . ? N1 C5 C4 122.9(10) . . ? N2 C6 O1 111.8(8) . . ? N2 C6 C3 129.5(9) . . ? O1 C6 C3 118.7(9) . . ? O3 C7 O2 127.2(10) . . ? O3 C7 C8 117.4(9) . . ? O2 C7 C8 115.4(10) . . ? O5 C9 O4 125.1(9) . . ? O5 C9 C10 118.2(8) . . ? O4 C9 C10 116.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cu1 O2 C7 83.9(8) 7_565 . . . ? O3 Cu1 O2 C7 1(2) 7_565 . . . ? O4 Cu1 O2 C7 -84.8(8) . . . . ? N1 Cu1 O2 C7 180.0(8) . . . . ? Cu1 Cu1 O2 C7 0.8(8) 7_565 . . . ? O5 Cu1 O4 C9 1.2(19) 7_565 . . . ? O2 Cu1 O4 C9 84.1(8) . . . . ? O3 Cu1 O4 C9 -84.2(8) 7_565 . . . ? N1 Cu1 O4 C9 179.1(8) . . . . ? Cu1 Cu1 O4 C9 -0.3(7) 7_565 . . . ? O5 Cu1 N1 C5 -94.6(8) 7_565 . . . ? O2 Cu1 N1 C5 175.4(8) . . . . ? O3 Cu1 N1 C5 -4.9(8) 7_565 . . . ? O4 Cu1 N1 C5 85.9(8) . . . . ? Cu1 Cu1 N1 C5 -129(12) 7_565 . . . ? O5 Cu1 N1 C1 88.3(7) 7_565 . . . ? O2 Cu1 N1 C1 -1.8(8) . . . . ? O3 Cu1 N1 C1 177.9(7) 7_565 . . . ? O4 Cu1 N1 C1 -91.3(8) . . . . ? Cu1 Cu1 N1 C1 54(13) 7_565 . . . ? C5 N1 C1 C2 -0.6(15) . . . . ? Cu1 N1 C1 C2 176.7(7) . . . . ? N1 C1 C2 C3 -0.2(15) . . . . ? C1 C2 C3 C4 1.5(15) . . . . ? C1 C2 C3 C6 -178.2(9) . . . . ? C2 C3 C4 C5 -2.1(16) . . . . ? C6 C3 C4 C5 177.6(9) . . . . ? C1 N1 C5 C4 0.0(15) . . . . ? Cu1 N1 C5 C4 -177.3(8) . . . . ? C3 C4 C5 N1 1.4(17) . . . . ? N2 N2 C6 O1 2.4(16) 2 . . . ? N2 N2 C6 C3 -179.5(11) 2 . . . ? C6 O1 C6 N2 -1.0(7) 2 . . . ? C6 O1 C6 C3 -179.3(11) 2 . . . ? C2 C3 C6 N2 13.8(18) . . . . ? C4 C3 C6 N2 -165.9(12) . . . . ? C2 C3 C6 O1 -168.1(8) . . . . ? C4 C3 C6 O1 12.1(15) . . . . ? Cu1 O3 C7 O2 1.5(16) 7_565 . . . ? Cu1 O3 C7 C8 -177.0(8) 7_565 . . . ? Cu1 O2 C7 O3 -1.7(15) . . . . ? Cu1 O2 C7 C8 176.9(7) . . . . ? Cu1 O5 C9 O4 -1.7(14) 7_565 . . . ? Cu1 O5 C9 C10 179.6(7) 7_565 . . . ? Cu1 O4 C9 O5 1.2(14) . . . . ? Cu1 O4 C9 C10 179.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.8805 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_full 0.8805 _refine_diff_density_max 0.693 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.114 #============================== END ========================= data_Polymer_3 _database_code_depnum_ccdc_archive 'CCDC 213498' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H22 Co N4 O10 S' _chemical_formula_weight 497.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 p2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.4061(15) _cell_length_b 10.725(2) _cell_length_c 26.453(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.11(3) _cell_angle_gamma 90.00 _cell_volume 2089.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 210 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.2 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7847 _exptl_absorpt_correction_T_max 0.8433 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 R-axis-IV _diffrn_measurement_method 'Osillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5345 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3237 _reflns_number_gt 2444 _reflns_threshold_expression >2sigma(I) _computing_data_collection RAXIS _computing_cell_refinement RAXIS _computing_data_reduction RAXIS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TEXSAN _computing_publication_material TEXSAN _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^)+(0.0688P)^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 0.0010(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3237 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Co1 Co 0.55901(8) 0.24880(6) 0.73098(2) 0.0269(2) Uani 1 1 d . . . S1 S 0.97458(15) 0.27260(11) 0.78803(5) 0.0328(3) Uani 1 1 d . . . O1 O 0.2818(4) 0.1180(3) 0.97789(12) 0.0352(8) Uani 1 1 d . . . O2 O 1.0259(5) 0.1671(3) 0.75638(16) 0.0511(10) Uani 1 1 d . . . O3 O 1.1160(4) 0.3693(3) 0.79126(13) 0.0396(9) Uani 1 1 d . . . O4 O 0.9426(5) 0.2274(4) 0.83829(15) 0.0560(11) Uani 1 1 d . . . O5 O 0.8056(4) 0.3291(3) 0.76246(12) 0.0333(8) Uani 1 1 d . . . O6 O 0.4219(5) 0.4109(4) 0.74902(16) 0.0394(9) Uani 1 1 d . . . O7 O 0.3138(7) 0.1777(5) 0.6984(2) 0.0545(14) Uani 1 1 d . . . O8 O 0.6966(6) 0.0852(4) 0.71277(15) 0.0412(10) Uani 1 1 d . . . O9 O 0.2203(17) 0.0476(10) 0.6105(4) 0.228(5) Uani 1 1 d . . . H9 H 0.2324 0.1103 0.6283 0.341 Uiso 1 1 calc R . . O10 O 0.5409(15) 0.1165(13) 0.4179(4) 0.201(4) Uani 1 1 d . . . H10 H 0.5251 0.1633 0.3934 0.302 Uiso 1 1 calc R . . N1 N 0.4991(5) 0.1770(4) 0.80393(14) 0.0286(9) Uani 1 1 d . . . N2 N 0.3002(6) -0.0772(4) 0.95249(16) 0.0443(12) Uani 1 1 d . . . N3 N 0.2445(6) -0.0767(4) 1.00147(16) 0.0419(11) Uani 1 1 d . . . N4 N 0.1108(5) 0.1810(4) 1.15645(15) 0.0328(10) Uani 1 1 d . . . C1 C 0.4452(6) 0.0589(5) 0.80857(17) 0.0292(11) Uani 1 1 d . . . H1A H 0.4482 0.0062 0.7807 0.035 Uiso 1 1 calc R . . C2 C 0.3864(6) 0.0112(5) 0.85161(18) 0.0319(11) Uani 1 1 d . . . H2C H 0.3501 -0.0716 0.8529 0.038 Uiso 1 1 calc R . . C3 C 0.3815(6) 0.0878(5) 0.89317(17) 0.0300(11) Uani 1 1 d . . . C4 C 0.4401(6) 0.2102(5) 0.89032(18) 0.0342(12) Uani 1 1 d . . . H4C H 0.4404 0.2641 0.9179 0.041 Uiso 1 1 calc R . . C5 C 0.4976(6) 0.2485(5) 0.84504(17) 0.0344(11) Uani 1 1 d . . . H5A H 0.5383 0.3302 0.8430 0.041 Uiso 1 1 calc R . . C6 C 0.3196(6) 0.0390(5) 0.94030(17) 0.0304(11) Uani 1 1 d . . . C7 C 0.2351(6) 0.0382(5) 1.01460(18) 0.0336(12) Uani 1 1 d . . . C8 C 0.1199(6) 0.0591(5) 1.14764(19) 0.0368(12) Uani 1 1 d . . . H8B H 0.1010 0.0044 1.1738 0.044 Uiso 1 1 calc R . . C9 C 0.1561(6) 0.0096(5) 1.10143(19) 0.0361(12) Uani 1 1 d . . . H9A H 0.1590 -0.0763 1.0966 0.043 Uiso 1 1 calc R . . C10 C 0.1876(6) 0.0901(5) 1.06263(18) 0.0319(11) Uani 1 1 d . . . C11 C 0.1770(8) 0.2163(5) 1.0712(2) 0.0532(16) Uani 1 1 d . . . H11A H 0.1968 0.2726 1.0456 0.064 Uiso 1 1 calc R . . C12 C 0.1365(8) 0.2592(6) 1.11830(19) 0.0502(14) Uani 1 1 d . . . H12A H 0.1270 0.3446 1.1235 0.060 Uiso 1 1 calc R . . C13 C 0.105(3) 0.078(3) 0.5607(9) 0.370(19) Uani 1 1 d . . . C14 C 0.3872(17) 0.1123(14) 0.4418(6) 0.190(7) Uani 1 1 d . . . H14A H 0.4137 0.0740 0.4746 0.284 Uiso 1 1 calc R . . H14B H 0.2964 0.0644 0.4218 0.284 Uiso 1 1 calc R . . H14C H 0.3432 0.1955 0.4460 0.284 Uiso 1 1 calc R . . H6F H 0.332(6) 0.393(5) 0.765(2) 0.037(14) Uiso 1 1 d . . . H6E H 0.428(7) 0.482(5) 0.740(2) 0.041(18) Uiso 1 1 d . . . H8F H 0.682(7) 0.004(7) 0.718(2) 0.06(2) Uiso 1 1 d . . . H8E H 0.802(8) 0.100(6) 0.721(3) 0.07(2) Uiso 1 1 d . . . H7F H 0.276(9) 0.150(7) 0.667(3) 0.08(2) Uiso 1 1 d . . . H7E H 0.258(7) 0.179(6) 0.711(2) 0.021(19) Uiso 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 0.0328(3) 0.0264(4) 0.0231(3) 0.0002(3) 0.0108(2) -0.0025(3) S1 0.0308(6) 0.0262(7) 0.0434(8) 0.0075(6) 0.0126(5) 0.0019(5) O1 0.0501(19) 0.036(2) 0.0224(18) 0.0027(16) 0.0167(15) 0.0018(16) O2 0.047(2) 0.033(2) 0.077(3) -0.005(2) 0.026(2) 0.0075(17) O3 0.0319(16) 0.038(2) 0.050(2) 0.0100(17) 0.0110(15) -0.0068(15) O4 0.064(2) 0.059(3) 0.046(2) 0.025(2) 0.0139(18) -0.008(2) O5 0.0264(15) 0.0284(19) 0.044(2) -0.0007(16) 0.0008(14) 0.0040(14) O6 0.040(2) 0.032(2) 0.051(2) 0.009(2) 0.0266(18) 0.0022(17) O7 0.050(3) 0.080(4) 0.035(3) -0.012(2) 0.012(2) -0.025(3) O8 0.052(2) 0.025(2) 0.049(3) -0.0004(18) 0.019(2) -0.0013(18) O9 0.230(10) 0.225(12) 0.239(12) -0.137(10) 0.076(9) -0.036(9) O10 0.219(10) 0.237(12) 0.151(9) 0.068(8) 0.035(7) 0.089(9) N1 0.034(2) 0.029(2) 0.025(2) -0.0042(19) 0.0074(17) -0.0036(17) N2 0.064(3) 0.046(3) 0.027(3) -0.002(2) 0.021(2) -0.001(2) N3 0.066(3) 0.036(3) 0.028(2) 0.000(2) 0.023(2) -0.001(2) N4 0.042(2) 0.032(3) 0.027(2) -0.003(2) 0.0143(18) 0.0010(19) C1 0.036(2) 0.032(3) 0.020(3) -0.003(2) 0.008(2) -0.005(2) C2 0.044(3) 0.026(3) 0.028(3) 0.001(2) 0.010(2) -0.003(2) C3 0.030(2) 0.039(3) 0.021(3) 0.004(2) 0.0084(19) -0.001(2) C4 0.044(3) 0.036(3) 0.024(3) -0.004(2) 0.010(2) -0.004(2) C5 0.045(3) 0.031(3) 0.027(3) -0.004(3) 0.007(2) -0.011(2) C6 0.039(2) 0.036(3) 0.017(3) 0.001(2) 0.006(2) -0.002(2) C7 0.038(2) 0.044(3) 0.021(3) 0.008(2) 0.012(2) -0.001(2) C8 0.049(3) 0.035(3) 0.030(3) 0.010(2) 0.022(2) 0.007(2) C9 0.053(3) 0.029(3) 0.028(3) 0.001(2) 0.014(2) 0.006(2) C10 0.036(2) 0.038(3) 0.024(3) 0.005(2) 0.013(2) 0.004(2) C11 0.097(4) 0.038(4) 0.030(3) 0.006(3) 0.027(3) -0.006(3) C12 0.090(4) 0.034(3) 0.032(3) -0.001(3) 0.028(3) -0.009(3) C13 0.228(19) 0.55(5) 0.31(3) 0.27(3) -0.056(18) 0.07(2) C14 0.175(12) 0.170(14) 0.236(18) 0.081(12) 0.082(12) 0.032(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O7 2.071(5) . ? Co1 O6 2.094(4) . ? Co1 O5 2.109(3) . ? Co1 O8 2.111(4) . ? Co1 N1 2.167(4) . ? Co1 N4 2.182(4) 4_665 ? S1 O4 1.458(4) . ? S1 O3 1.470(3) . ? S1 O2 1.481(4) . ? S1 O5 1.487(3) . ? O1 C6 1.358(6) . ? O1 C7 1.366(6) . ? O9 C13 1.528(17) . ? O10 C14 1.360(12) . ? N1 C5 1.332(6) . ? N1 C1 1.338(6) . ? N2 C6 1.299(7) . ? N2 N3 1.401(5) . ? N3 C7 1.284(7) . ? N4 C8 1.330(6) . ? N4 C12 1.341(6) . ? N4 Co1 2.182(4) 4_566 ? C1 C2 1.361(6) . ? C2 C3 1.376(7) . ? C3 C4 1.387(7) . ? C3 C6 1.470(6) . ? C4 C5 1.376(6) . ? C7 C10 1.464(7) . ? C8 C9 1.385(7) . ? C9 C10 1.380(7) . ? C10 C11 1.376(7) . ? C11 C12 1.391(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 O7 Co1 O6 88.6(2) . . ? O7 Co1 O5 177.34(19) . . ? O6 Co1 O5 89.50(14) . . ? O7 Co1 O8 91.3(2) . . ? O6 Co1 O8 179.87(18) . . ? O5 Co1 O8 90.62(15) . . ? O7 Co1 N1 89.18(18) . . ? O6 Co1 N1 86.66(16) . . ? O5 Co1 N1 92.55(13) . . ? O8 Co1 N1 93.29(15) . . ? O7 Co1 N4 88.97(18) . 4_665 ? O6 Co1 N4 93.17(16) . 4_665 ? O5 Co1 N4 89.30(14) . 4_665 ? O8 Co1 N4 86.88(15) . 4_665 ? N1 Co1 N4 178.15(14) . 4_665 ? O4 S1 O3 111.4(2) . . ? O4 S1 O2 109.7(2) . . ? O3 S1 O2 110.4(2) . . ? O4 S1 O5 109.9(2) . . ? O3 S1 O5 107.4(2) . . ? O2 S1 O5 108.0(2) . . ? C6 O1 C7 102.6(4) . . ? S1 O5 Co1 131.7(2) . . ? C5 N1 C1 116.3(4) . . ? C5 N1 Co1 122.8(3) . . ? C1 N1 Co1 120.6(3) . . ? C6 N2 N3 106.1(4) . . ? C7 N3 N2 106.5(4) . . ? C8 N4 C12 117.9(4) . . ? C8 N4 Co1 121.0(3) . 4_566 ? C12 N4 Co1 121.1(3) . 4_566 ? N1 C1 C2 123.9(5) . . ? C1 C2 C3 118.8(5) . . ? C2 C3 C4 119.1(4) . . ? C2 C3 C6 120.1(4) . . ? C4 C3 C6 120.7(4) . . ? C5 C4 C3 117.2(5) . . ? N1 C5 C4 124.6(5) . . ? N2 C6 O1 112.3(4) . . ? N2 C6 C3 127.2(5) . . ? O1 C6 C3 120.4(4) . . ? N3 C7 O1 112.6(4) . . ? N3 C7 C10 128.6(5) . . ? O1 C7 C10 118.8(5) . . ? N4 C8 C9 123.3(5) . . ? C10 C9 C8 118.7(5) . . ? C11 C10 C9 118.4(5) . . ? C11 C10 C7 122.7(5) . . ? C9 C10 C7 118.9(5) . . ? C10 C11 C12 119.6(5) . . ? N4 C12 C11 121.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 S1 O5 Co1 -71.8(3) . . . . ? O3 S1 O5 Co1 166.9(2) . . . . ? O2 S1 O5 Co1 47.9(3) . . . . ? O7 Co1 O5 S1 -166(4) . . . . ? O6 Co1 O5 S1 149.8(3) . . . . ? O8 Co1 O5 S1 -30.2(3) . . . . ? N1 Co1 O5 S1 63.1(3) . . . . ? N4 Co1 O5 S1 -117.0(3) 4_665 . . . ? O7 Co1 N1 C5 -124.5(4) . . . . ? O6 Co1 N1 C5 -35.9(4) . . . . ? O5 Co1 N1 C5 53.4(3) . . . . ? O8 Co1 N1 C5 144.2(4) . . . . ? N4 Co1 N1 C5 -121(5) 4_665 . . . ? O7 Co1 N1 C1 49.4(4) . . . . ? O6 Co1 N1 C1 138.0(3) . . . . ? O5 Co1 N1 C1 -132.6(3) . . . . ? O8 Co1 N1 C1 -41.8(3) . . . . ? N4 Co1 N1 C1 53(5) 4_665 . . . ? C6 N2 N3 C7 0.0(6) . . . . ? C5 N1 C1 C2 1.8(6) . . . . ? Co1 N1 C1 C2 -172.5(3) . . . . ? N1 C1 C2 C3 -0.2(7) . . . . ? C1 C2 C3 C4 -1.3(7) . . . . ? C1 C2 C3 C6 -179.6(4) . . . . ? C2 C3 C4 C5 1.0(6) . . . . ? C6 C3 C4 C5 179.4(4) . . . . ? C1 N1 C5 C4 -2.1(7) . . . . ? Co1 N1 C5 C4 172.1(4) . . . . ? C3 C4 C5 N1 0.7(7) . . . . ? N3 N2 C6 O1 0.4(5) . . . . ? N3 N2 C6 C3 178.0(4) . . . . ? C7 O1 C6 N2 -0.5(5) . . . . ? C7 O1 C6 C3 -178.4(4) . . . . ? C2 C3 C6 N2 15.0(7) . . . . ? C4 C3 C6 N2 -163.4(5) . . . . ? C2 C3 C6 O1 -167.5(4) . . . . ? C4 C3 C6 O1 14.1(6) . . . . ? N2 N3 C7 O1 -0.3(6) . . . . ? N2 N3 C7 C10 -178.4(4) . . . . ? C6 O1 C7 N3 0.5(5) . . . . ? C6 O1 C7 C10 178.8(4) . . . . ? C12 N4 C8 C9 0.6(8) . . . . ? Co1 N4 C8 C9 -178.6(4) 4_566 . . . ? N4 C8 C9 C10 1.2(8) . . . . ? C8 C9 C10 C11 -1.7(7) . . . . ? C8 C9 C10 C7 176.9(4) . . . . ? N3 C7 C10 C11 -177.9(6) . . . . ? O1 C7 C10 C11 4.2(7) . . . . ? N3 C7 C10 C9 3.6(8) . . . . ? O1 C7 C10 C9 -174.3(4) . . . . ? C9 C10 C11 C12 0.5(8) . . . . ? C7 C10 C11 C12 -178.1(5) . . . . ? C8 N4 C12 C11 -1.9(8) . . . . ? Co1 N4 C12 C11 177.3(4) 4_566 . . . ? C10 C11 C12 N4 1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.582 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.086 #============================== END ========================= data_Polymer_4 _database_code_depnum_ccdc_archive 'CCDC 213499' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H16 Cd I2 N8 O2' _chemical_formula_weight 814.65 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 4.1122(8) _cell_length_b 13.463(3) _cell_length_c 23.674(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.69(3) _cell_angle_gamma 90.00 _cell_volume 1310.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 256 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.3 _exptl_crystal_description PRISMATIC _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.065 _exptl_crystal_density_method ? _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 3.229 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 R-AXIS-IV _diffrn_measurement_method 'Osillation frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3589 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2089 _reflns_number_observed 1880 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+8.5992P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2084 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_obs 0.0644 _refine_ls_wR_factor_all 0.1850 _refine_ls_wR_factor_obs 0.1569 _refine_ls_goodness_of_fit_all 1.127 _refine_ls_goodness_of_fit_obs 1.138 _refine_ls_restrained_S_all 1.272 _refine_ls_restrained_S_obs 1.138 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 0.0000 0.5000 0.5000 0.0418(4) Uani 1 d S . I1 I 0.4586(2) 0.45599(5) 0.41203(3) 0.0422(3) Uani 1 d . . O1 O -0.0533(18) 0.9958(6) 0.3594(3) 0.044(2) Uani 1 d . . C1 C -0.0988(30) 0.6988(9) 0.4190(5) 0.052(3) Uani 1 d . . H1A H -0.1977(30) 0.6496(9) 0.3969(5) 0.062 Uiso 1 calc R . C2 C -0.0873(27) 0.7912(9) 0.3962(5) 0.046(3) Uani 1 d . . H2A H -0.1816(27) 0.8049(9) 0.3609(5) 0.055 Uiso 1 calc R . C3 C 0.0713(26) 0.8645(8) 0.4280(5) 0.039(2) Uani 1 d . . C4 C 0.1960(27) 0.8395(8) 0.4810(5) 0.044(3) Uani 1 d . . H4A H 0.3010(27) 0.8870(8) 0.5035(5) 0.053 Uiso 1 calc R . C5 C 0.1631(28) 0.7436(8) 0.5002(5) 0.046(3) Uani 1 d . . H5A H 0.2456(28) 0.7277(8) 0.5360(5) 0.055 Uiso 1 calc R . C6 C 0.1165(28) 0.9662(8) 0.4070(5) 0.041(2) Uani 1 d . . C7 C 0.0343(26) 1.0926(8) 0.3553(4) 0.040(2) Uani 1 d . . C8 C -0.3738(36) 1.1742(13) 0.2207(6) 0.074(4) Uani 1 d . . H8A H -0.4735(36) 1.1451(13) 0.1891(6) 0.088 Uiso 1 calc R . C9 C -0.2518(33) 1.1102(10) 0.2628(5) 0.060(3) Uani 1 d . . H9A H -0.2727(33) 1.0416(10) 0.2596(5) 0.072 Uiso 1 calc R . C10 C -0.1006(28) 1.1531(9) 0.3088(5) 0.048(3) Uani 1 d . . C11 C -0.0769(35) 1.2545(9) 0.3113(5) 0.057(3) Uani 1 d . . H11A H 0.0265(35) 1.2853(9) 0.3421(5) 0.069 Uiso 1 calc R . C12 C -0.2099(38) 1.3106(11) 0.2672(6) 0.070(4) Uani 1 d . . H12A H -0.1928(38) 1.3794(11) 0.2693(6) 0.084 Uiso 1 calc R . N1 N 0.0159(23) 0.6722(7) 0.4690(4) 0.046(2) Uani 1 d . . N2 N 0.2856(27) 1.0349(7) 0.4301(5) 0.054(3) Uani 1 d . . N3 N 0.2380(26) 1.1204(7) 0.3954(5) 0.054(3) Uani 1 d . . N4 N -0.3603(34) 1.2715(11) 0.2219(5) 0.077(4) Uani 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 0.0370(6) 0.0306(6) 0.0575(8) 0.0036(5) -0.0013(5) -0.0015(5) I1 0.0376(4) 0.0354(4) 0.0533(5) -0.0027(3) -0.0045(3) -0.0029(3) O1 0.047(4) 0.033(4) 0.050(5) 0.000(3) -0.010(3) -0.007(4) C1 0.063(7) 0.033(6) 0.057(7) 0.005(5) -0.022(6) -0.016(6) C2 0.046(6) 0.040(6) 0.050(7) 0.001(5) -0.010(5) -0.009(5) C3 0.039(5) 0.026(5) 0.050(6) -0.005(5) -0.001(5) -0.004(4) C4 0.052(6) 0.024(5) 0.056(7) -0.006(5) -0.020(5) -0.005(5) C5 0.057(7) 0.032(6) 0.047(6) -0.001(5) -0.016(5) -0.005(5) C6 0.046(6) 0.032(6) 0.045(6) 0.000(5) -0.003(5) -0.006(5) C7 0.048(6) 0.025(5) 0.046(6) 0.002(5) -0.005(5) -0.009(5) C8 0.080(10) 0.085(12) 0.054(8) -0.006(8) -0.024(7) -0.001(9) C9 0.072(8) 0.048(7) 0.059(8) -0.004(6) -0.018(6) 0.007(7) C10 0.050(6) 0.042(6) 0.051(7) 0.004(5) 0.002(5) 0.001(6) C11 0.074(8) 0.042(7) 0.055(7) 0.007(6) -0.008(7) 0.004(6) C12 0.095(11) 0.042(7) 0.073(10) 0.011(7) 0.004(8) 0.017(8) N1 0.049(5) 0.031(5) 0.060(6) 0.003(5) 0.007(5) -0.001(4) N2 0.065(6) 0.027(5) 0.068(7) 0.010(5) -0.022(5) -0.007(5) N3 0.068(7) 0.029(5) 0.065(7) 0.006(5) -0.016(5) -0.010(5) N4 0.097(10) 0.069(9) 0.064(8) 0.010(7) -0.005(7) 0.011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.433(9) 3_566 ? Cd1 N1 2.433(9) . ? Cd1 I1 2.9117(11) . ? Cd1 I1 2.9117(11) 3_566 ? Cd1 I1 3.0612(11) 1_455 ? Cd1 I1 3.0612(11) 3_666 ? I1 Cd1 3.0612(11) 1_655 ? O1 C7 1.357(13) . ? O1 C6 1.367(14) . ? C1 N1 1.312(15) . ? C1 C2 1.36(2) . ? C2 C3 1.39(2) . ? C3 C4 1.38(2) . ? C3 C6 1.47(2) . ? C4 C5 1.38(2) . ? C5 N1 1.346(14) . ? C6 N2 1.271(14) . ? C7 N3 1.301(14) . ? C7 C10 1.47(2) . ? C8 N4 1.31(2) . ? C8 C9 1.40(2) . ? C9 C10 1.37(2) . ? C10 C11 1.37(2) . ? C11 C12 1.39(2) . ? C12 N4 1.33(2) . ? N2 N3 1.424(14) . ? 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 180.000(4) 3_566 . ? N1 Cd1 I1 92.6(2) 3_566 . ? N1 Cd1 I1 87.4(2) . . ? N1 Cd1 I1 87.4(2) 3_566 3_566 ? N1 Cd1 I1 92.6(2) . 3_566 ? I1 Cd1 I1 180.0 . 3_566 ? N1 Cd1 I1 89.7(2) 3_566 1_455 ? N1 Cd1 I1 90.3(2) . 1_455 ? I1 Cd1 I1 86.98(2) . 1_455 ? I1 Cd1 I1 93.02(2) 3_566 1_455 ? N1 Cd1 I1 90.3(2) 3_566 3_666 ? N1 Cd1 I1 89.7(2) . 3_666 ? I1 Cd1 I1 93.02(2) . 3_666 ? I1 Cd1 I1 86.98(2) 3_566 3_666 ? I1 Cd1 I1 180.0 1_455 3_666 ? Cd1 I1 Cd1 86.98(2) . 1_655 ? C7 O1 C6 102.0(8) . . ? N1 C1 C2 126.4(11) . . ? C1 C2 C3 117.2(11) . . ? C4 C3 C2 118.2(10) . . ? C4 C3 C6 119.1(10) . . ? C2 C3 C6 122.7(11) . . ? C5 C4 C3 119.3(10) . . ? N1 C5 C4 122.4(11) . . ? N2 C6 O1 113.7(10) . . ? N2 C6 C3 127.3(11) . . ? O1 C6 C3 118.9(10) . . ? N3 C7 O1 113.0(9) . . ? N3 C7 C10 127.5(11) . . ? O1 C7 C10 119.4(9) . . ? N4 C8 C9 125.9(14) . . ? C10 C9 C8 116.9(13) . . ? C9 C10 C11 119.0(12) . . ? C9 C10 C7 121.2(11) . . ? C11 C10 C7 119.8(12) . . ? C10 C11 C12 118.9(13) . . ? N4 C12 C11 123.6(14) . . ? C1 N1 C5 116.3(10) . . ? C1 N1 Cd1 121.4(8) . . ? C5 N1 Cd1 122.1(8) . . ? C6 N2 N3 106.0(10) . . ? C7 N3 N2 105.2(9) . . ? C8 N4 C12 115.6(13) . . ? 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 Cd1 I1 Cd1 -90.4(2) 3_566 . . 1_655 ? N1 Cd1 I1 Cd1 89.6(2) . . . 1_655 ? I1 Cd1 I1 Cd1 163.6(979) 3_566 . . 1_655 ? I1 Cd1 I1 Cd1 180.0 1_455 . . 1_655 ? I1 Cd1 I1 Cd1 0.0 3_666 . . 1_655 ? N1 C1 C2 C3 2.5(21) . . . . ? C1 C2 C3 C4 -2.2(17) . . . . ? C1 C2 C3 C6 176.6(11) . . . . ? C2 C3 C4 C5 0.8(17) . . . . ? C6 C3 C4 C5 -178.1(11) . . . . ? C3 C4 C5 N1 0.7(19) . . . . ? C7 O1 C6 N2 0.5(13) . . . . ? C7 O1 C6 C3 176.5(10) . . . . ? C4 C3 C6 N2 6.7(19) . . . . ? C2 C3 C6 N2 -172.1(12) . . . . ? C4 C3 C6 O1 -168.7(10) . . . . ? C2 C3 C6 O1 12.4(17) . . . . ? C6 O1 C7 N3 0.6(12) . . . . ? C6 O1 C7 C10 -179.5(10) . . . . ? N4 C8 C9 C10 -1.1(25) . . . . ? C8 C9 C10 C11 0.0(20) . . . . ? C8 C9 C10 C7 179.7(12) . . . . ? N3 C7 C10 C9 164.9(13) . . . . ? O1 C7 C10 C9 -15.0(17) . . . . ? N3 C7 C10 C11 -15.4(19) . . . . ? O1 C7 C10 C11 164.7(11) . . . . ? C9 C10 C11 C12 0.5(21) . . . . ? C7 C10 C11 C12 -179.2(12) . . . . ? C10 C11 C12 N4 -0.1(23) . . . . ? C2 C1 N1 C5 -1.0(20) . . . . ? C2 C1 N1 Cd1 -176.3(10) . . . . ? C4 C5 N1 C1 -0.6(18) . . . . ? C4 C5 N1 Cd1 174.7(9) . . . . ? N1 Cd1 N1 C1 -123.7(954) 3_566 . . . ? I1 Cd1 N1 C1 66.3(9) . . . . ? I1 Cd1 N1 C1 -113.7(9) 3_566 . . . ? I1 Cd1 N1 C1 -20.7(9) 1_455 . . . ? I1 Cd1 N1 C1 159.3(9) 3_666 . . . ? N1 Cd1 N1 C5 61.2(934) 3_566 . . . ? I1 Cd1 N1 C5 -108.8(9) . . . . ? I1 Cd1 N1 C5 71.2(9) 3_566 . . . ? I1 Cd1 N1 C5 164.3(9) 1_455 . . . ? I1 Cd1 N1 C5 -15.7(9) 3_666 . . . ? O1 C6 N2 N3 -1.2(14) . . . . ? C3 C6 N2 N3 -176.9(11) . . . . ? O1 C7 N3 N2 -1.3(14) . . . . ? C10 C7 N3 N2 178.8(11) . . . . ? C6 N2 N3 C7 1.5(14) . . . . ? C9 C8 N4 C12 1.5(26) . . . . ? C11 C12 N4 C8 -0.8(24) . . . . ? _refine_diff_density_max 2.003 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.204 #==============================END================ #======= data_Complex_5 _database_code_depnum_ccdc_archive 'CCDC 213500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Mn N10 O4 S2' _chemical_formula_weight 655.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 7.9571(16) _cell_length_b 8.6740(17) _cell_length_c 11.326(2) _cell_angle_alpha 94.31(3) _cell_angle_beta 110.17(3) _cell_angle_gamma 94.66(3) _cell_volume 726.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 254 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.2 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 335 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8597 _exptl_absorpt_correction_T_max 0.8811 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 R-axis-IV _diffrn_measurement_method 'Osillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2127 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2127 _reflns_number_gt 1765 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _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^)+(0.1399P)^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 0.026(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2127 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1821 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.0000 0.0000 0.0000 0.0400(3) Uani 1 2 d S . . S1 S 0.1331(2) -0.22597(16) -0.35919(14) 0.0803(5) Uani 1 1 d . . . O1 O 0.2773(4) -0.5461(3) 0.4811(2) 0.0426(7) Uani 1 1 d . . . O2 O -0.2650(5) -0.1425(4) -0.0865(3) 0.0541(8) Uani 1 1 d . . . C1 C 0.1458(6) -0.3245(4) 0.0879(4) 0.0465(10) Uani 1 1 d . . . H1A H 0.1408 -0.3336 0.0044 0.056 Uiso 1 1 calc R . . C2 C 0.1978(6) -0.4465(4) 0.1580(4) 0.0480(10) Uani 1 1 d . . . H2A H 0.2228 -0.5369 0.1209 0.058 Uiso 1 1 calc R . . C3 C 0.2125(5) -0.4341(4) 0.2831(4) 0.0391(8) Uani 1 1 d . . . C4 C 0.1720(7) -0.2972(5) 0.3329(4) 0.0535(11) Uani 1 1 d . . . H4A H 0.1813 -0.2837 0.4173 0.064 Uiso 1 1 calc R . . C5 C 0.1177(7) -0.1812(5) 0.2561(4) 0.0535(11) Uani 1 1 d . . . H5A H 0.0908 -0.0902 0.2911 0.064 Uiso 1 1 calc R . . C6 C 0.2737(5) -0.5599(4) 0.3611(4) 0.0411(9) Uani 1 1 d . . . C7 C 0.3359(6) -0.6837(4) 0.5232(4) 0.0437(9) Uani 1 1 d . . . C8 C 0.3364(7) -0.6262(6) 0.8511(5) 0.0637(13) Uani 1 1 d . . . H8A H 0.3117 -0.5500 0.9031 0.076 Uiso 1 1 calc R . . C9 C 0.3161(7) -0.5968(6) 0.7299(5) 0.0568(11) Uani 1 1 d . . . H9A H 0.2790 -0.5033 0.7008 0.068 Uiso 1 1 calc R . . C10 C 0.3523(5) -0.7095(5) 0.6524(4) 0.0448(10) Uani 1 1 d . . . C11 C 0.4088(6) -0.8465(5) 0.7010(4) 0.0500(10) Uani 1 1 d . . . H11A H 0.4350 -0.9245 0.6513 0.060 Uiso 1 1 calc R . . C12 C 0.4251(7) -0.8645(6) 0.8241(5) 0.0579(12) Uani 1 1 d . . . H12A H 0.4630 -0.9564 0.8561 0.069 Uiso 1 1 calc R . . C13 C 0.1090(6) -0.1617(4) -0.2298(4) 0.0455(10) Uani 1 1 d . . . N1 N 0.1017(5) -0.1919(4) 0.1345(3) 0.0426(8) Uani 1 1 d . . . N2 N 0.3257(5) -0.6904(4) 0.3310(3) 0.0461(8) Uani 1 1 d . . . N3 N 0.3669(5) -0.7720(4) 0.4371(3) 0.0485(9) Uani 1 1 d . . . N4 N 0.3895(6) -0.7575(5) 0.8993(4) 0.0614(10) Uani 1 1 d . . . N5 N 0.0894(5) -0.1141(4) -0.1383(4) 0.0541(9) Uani 1 1 d . . . H2F H -0.264(10) -0.204(8) -0.149(8) 0.11(2) Uiso 1 1 d . . . H2E H -0.292(9) -0.189(7) -0.026(7) 0.10(2) Uiso 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 0.0576(6) 0.0411(5) 0.0263(5) 0.0085(3) 0.0180(4) 0.0148(4) S1 0.1179(12) 0.0802(9) 0.0576(9) -0.0100(7) 0.0539(9) 0.0082(8) O1 0.0544(15) 0.0475(14) 0.0274(14) 0.0106(11) 0.0144(12) 0.0091(12) O2 0.072(2) 0.0575(18) 0.0336(16) 0.0046(14) 0.0214(16) 0.0018(15) C1 0.069(3) 0.044(2) 0.0228(19) 0.0081(15) 0.0108(19) 0.0096(18) C2 0.070(3) 0.040(2) 0.034(2) 0.0066(16) 0.015(2) 0.0129(18) C3 0.0435(19) 0.0432(19) 0.0287(19) 0.0103(15) 0.0088(16) 0.0065(15) C4 0.078(3) 0.061(2) 0.031(2) 0.0149(18) 0.025(2) 0.024(2) C5 0.080(3) 0.054(2) 0.034(2) 0.0119(18) 0.023(2) 0.029(2) C6 0.049(2) 0.046(2) 0.0265(19) 0.0103(15) 0.0094(17) 0.0035(17) C7 0.051(2) 0.045(2) 0.035(2) 0.0147(16) 0.0138(19) 0.0052(17) C8 0.072(3) 0.086(3) 0.044(3) 0.016(2) 0.030(3) 0.019(3) C9 0.070(3) 0.066(3) 0.040(3) 0.021(2) 0.021(2) 0.021(2) C10 0.048(2) 0.053(2) 0.031(2) 0.0139(17) 0.0099(18) 0.0015(18) C11 0.058(2) 0.051(2) 0.039(2) 0.0140(18) 0.014(2) 0.0037(19) C12 0.060(3) 0.068(3) 0.045(3) 0.025(2) 0.015(2) 0.006(2) C13 0.062(2) 0.0377(19) 0.041(2) 0.0080(16) 0.021(2) 0.0129(17) N1 0.0520(18) 0.0440(17) 0.0336(18) 0.0113(14) 0.0138(16) 0.0150(15) N2 0.061(2) 0.0483(18) 0.0308(18) 0.0108(14) 0.0157(16) 0.0100(15) N3 0.067(2) 0.0491(18) 0.0283(18) 0.0132(14) 0.0116(17) 0.0134(16) N4 0.065(2) 0.082(3) 0.041(2) 0.025(2) 0.019(2) 0.011(2) N5 0.072(2) 0.057(2) 0.042(2) 0.0041(16) 0.030(2) 0.0155(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N5 2.142(3) . ? Mn1 N5 2.142(3) 2 ? Mn1 O2 2.214(3) . ? Mn1 O2 2.214(3) 2 ? Mn1 N1 2.345(3) 2 ? Mn1 N1 2.345(3) . ? S1 C13 1.607(4) . ? O1 C6 1.346(4) . ? O1 C7 1.376(5) . ? C1 N1 1.352(5) . ? C1 C2 1.375(6) . ? C2 C3 1.377(5) . ? C3 C4 1.385(6) . ? C3 C6 1.464(6) . ? C4 C5 1.378(6) . ? C5 N1 1.334(5) . ? C6 N2 1.297(5) . ? C7 N3 1.298(5) . ? C7 C10 1.459(5) . ? C8 N4 1.335(7) . ? C8 C9 1.373(7) . ? C9 C10 1.379(6) . ? C10 C11 1.390(6) . ? C11 C12 1.377(6) . ? C12 N4 1.326(6) . ? C13 N5 1.152(5) . ? N2 N3 1.395(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 N5 Mn1 N5 180.00(18) . 2 ? N5 Mn1 O2 89.48(13) . . ? N5 Mn1 O2 90.52(13) 2 . ? N5 Mn1 O2 90.52(13) . 2 ? N5 Mn1 O2 89.48(13) 2 2 ? O2 Mn1 O2 180.00(12) . 2 ? N5 Mn1 N1 89.74(14) . 2 ? N5 Mn1 N1 90.26(14) 2 2 ? O2 Mn1 N1 90.61(12) . 2 ? O2 Mn1 N1 89.39(12) 2 2 ? N5 Mn1 N1 90.26(14) . . ? N5 Mn1 N1 89.74(14) 2 . ? O2 Mn1 N1 89.39(12) . . ? O2 Mn1 N1 90.61(12) 2 . ? N1 Mn1 N1 180.00(9) 2 . ? C6 O1 C7 102.8(3) . . ? N1 C1 C2 123.2(4) . . ? C1 C2 C3 119.7(4) . . ? C2 C3 C4 117.6(4) . . ? C2 C3 C6 120.8(3) . . ? C4 C3 C6 121.5(4) . . ? C5 C4 C3 119.3(4) . . ? N1 C5 C4 123.8(4) . . ? N2 C6 O1 112.2(4) . . ? N2 C6 C3 129.0(4) . . ? O1 C6 C3 118.7(3) . . ? N3 C7 O1 112.2(3) . . ? N3 C7 C10 130.3(4) . . ? O1 C7 C10 117.6(3) . . ? N4 C8 C9 124.2(5) . . ? C8 C9 C10 118.2(5) . . ? C9 C10 C11 118.5(4) . . ? C9 C10 C7 120.6(4) . . ? C11 C10 C7 120.8(4) . . ? C12 C11 C10 118.7(4) . . ? N4 C12 C11 123.3(5) . . ? N5 C13 S1 178.7(4) . . ? C5 N1 C1 116.4(4) . . ? C5 N1 Mn1 124.4(3) . . ? C1 N1 Mn1 119.2(3) . . ? C6 N2 N3 107.1(3) . . ? C7 N3 N2 105.7(3) . . ? C12 N4 C8 117.1(4) . . ? C13 N5 Mn1 165.9(4) . . ? 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 -2.3(7) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C1 C2 C3 C6 -177.8(4) . . . . ? C2 C3 C4 C5 0.6(7) . . . . ? C6 C3 C4 C5 178.9(4) . . . . ? C3 C4 C5 N1 -0.2(7) . . . . ? C7 O1 C6 N2 -0.5(4) . . . . ? C7 O1 C6 C3 178.6(3) . . . . ? C2 C3 C6 N2 2.3(7) . . . . ? C4 C3 C6 N2 -176.0(4) . . . . ? C2 C3 C6 O1 -176.6(3) . . . . ? C4 C3 C6 O1 5.0(6) . . . . ? C6 O1 C7 N3 0.6(4) . . . . ? C6 O1 C7 C10 -178.8(3) . . . . ? N4 C8 C9 C10 0.1(8) . . . . ? C8 C9 C10 C11 -0.5(7) . . . . ? C8 C9 C10 C7 -179.0(4) . . . . ? N3 C7 C10 C9 178.4(4) . . . . ? O1 C7 C10 C9 -2.3(6) . . . . ? N3 C7 C10 C11 0.0(6) . . . . ? O1 C7 C10 C11 179.3(3) . . . . ? C9 C10 C11 C12 0.4(6) . . . . ? C7 C10 C11 C12 178.9(4) . . . . ? C10 C11 C12 N4 0.1(7) . . . . ? C4 C5 N1 C1 -1.4(7) . . . . ? C4 C5 N1 Mn1 177.7(4) . . . . ? C2 C1 N1 C5 2.6(6) . . . . ? C2 C1 N1 Mn1 -176.6(3) . . . . ? N5 Mn1 N1 C5 167.7(3) . . . . ? N5 Mn1 N1 C5 -12.3(3) 2 . . . ? O2 Mn1 N1 C5 -102.9(3) . . . . ? O2 Mn1 N1 C5 77.1(3) 2 . . . ? N1 Mn1 N1 C5 105(100) 2 . . . ? N5 Mn1 N1 C1 -13.2(3) . . . . ? N5 Mn1 N1 C1 166.8(3) 2 . . . ? O2 Mn1 N1 C1 76.2(3) . . . . ? O2 Mn1 N1 C1 -103.8(3) 2 . . . ? N1 Mn1 N1 C1 -76(100) 2 . . . ? O1 C6 N2 N3 0.3(5) . . . . ? C3 C6 N2 N3 -178.8(4) . . . . ? O1 C7 N3 N2 -0.5(4) . . . . ? C10 C7 N3 N2 178.9(4) . . . . ? C6 N2 N3 C7 0.1(4) . . . . ? C11 C12 N4 C8 -0.5(7) . . . . ? C9 C8 N4 C12 0.4(7) . . . . ? S1 C13 N5 Mn1 4(20) . . . . ? N5 Mn1 N5 C13 167(100) 2 . . . ? O2 Mn1 N5 C13 62.2(14) . . . . ? O2 Mn1 N5 C13 -117.8(14) 2 . . . ? N1 Mn1 N5 C13 -28.4(14) 2 . . . ? N1 Mn1 N5 C13 151.6(14) . . . . ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.874 _refine_diff_density_max 0.537 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.084 #=======================END========================