Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hongwei Hou' _publ_contact_author_address ; Department of Chemistry Zhengzhou University Zhengzhou, Henan 450052 CHINA ; _publ_contact_author_email HOUHONGW@ZZU.EDU.CN _publ_section_title ; A Series of Organic-Metal Polymers Assembled from MCl2 (M=Zn, Cd, Co, Cu): Structures, Third-Order Nonlinear Optical and Fluorescent properties ; loop_ _publ_author_name 'Hongwei Hou' 'Yaoting Fan' 'Huayun Han' 'Yinglin Song' 'Yu Zhu' #== == == end data_polymer_4 _database_code_depnum_ccdc_archive 'CCDC 262171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 Cl2 Cu F4 N12 O4' _chemical_formula_weight 811.10 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 22.782(5) _cell_length_b 9.3699(19) _cell_length_c 19.862(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.91(3) _cell_angle_gamma 90.00 _cell_volume 3599.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 320 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description Prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 0.8519 _exptl_absorpt_process_details ; R-AXIS Data Processing Software Version4.0(OCT 21.1996) ; _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 'Oscillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4375 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2643 _reflns_number_gt 1811 _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^)+(0.0491P)^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 0.0032(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2643 _refine_ls_number_parameters 239 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.011 _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 0.7500 0.7500 0.0000 0.0352(3) Uani 1 2 d S . . Cl1 Cl 0.81831(7) 0.99802(13) 0.00059(8) 0.0455(4) Uani 1 1 d . . . O1 O 0.71447(17) 1.2198(4) 0.1964(2) 0.0435(9) Uani 1 1 d . . . O2 O 0.7891(3) 1.3274(6) 0.1383(3) 0.0969(17) Uani 1 1 d D . . H2 H 0.7639 1.3724 0.0975 0.145 Uiso 1 1 calc RD . . F1 F 0.49724(15) 1.2870(3) 0.0666(2) 0.0667(10) Uani 1 1 d . . . F2 F 0.52998(19) 1.7669(3) 0.1395(2) 0.0797(11) Uani 1 1 d . . . N1 N 0.6937(2) 0.8678(4) 0.0323(2) 0.0346(10) Uani 1 1 d . . . N2 N 0.6084(2) 0.9225(5) 0.0523(3) 0.0490(12) Uani 1 1 d . . . N3 N 0.6428(2) 1.0424(4) 0.0532(2) 0.0349(10) Uani 1 1 d . . . N4 N 0.6299(2) 1.1612(4) 0.2602(2) 0.0362(10) Uani 1 1 d . . . N5 N 0.5772(2) 1.2139(5) 0.2659(3) 0.0584(14) Uani 1 1 d . . . N6 N 0.6775(2) 1.2203(4) 0.3836(2) 0.0347(10) Uani 1 1 d . . . C1 C 0.6925(3) 1.0066(6) 0.0413(3) 0.0384(12) Uani 1 1 d . . . H1B H 0.7227 1.0709 0.0396 0.046 Uiso 1 1 calc R . . C2 C 0.6407(3) 0.8211(6) 0.0389(3) 0.0424(14) Uani 1 1 d . . . H2B H 0.6283 0.7254 0.0344 0.051 Uiso 1 1 calc R . . C3 C 0.6186(3) 1.1831(5) 0.0601(3) 0.0374(13) Uani 1 1 d . . . H3A H 0.5685 1.1856 0.0273 0.045 Uiso 1 1 calc R . . H3B H 0.6364 1.2546 0.0401 0.045 Uiso 1 1 calc R . . C4 C 0.6415(2) 1.2217(5) 0.1467(3) 0.0326(12) Uani 1 1 d . . . C5 C 0.6167(3) 1.1116(5) 0.1828(3) 0.0396(13) Uani 1 1 d . . . H5B H 0.5675 1.0952 0.1470 0.048 Uiso 1 1 calc R . . H5C H 0.6406 1.0220 0.1898 0.048 Uiso 1 1 calc R . . C6 C 0.6883(3) 1.1670(5) 0.3302(3) 0.0372(12) Uani 1 1 d . . . H6B H 0.7311 1.1372 0.3400 0.045 Uiso 1 1 calc R . . C7 C 0.6088(3) 1.2481(6) 0.3417(3) 0.0544(15) Uani 1 1 d . . . H7A H 0.5858 1.2879 0.3644 0.065 Uiso 1 1 calc R . . C8 C 0.6116(2) 1.3710(5) 0.1440(3) 0.0316(12) Uani 1 1 d . . . C9 C 0.5421(3) 1.3966(5) 0.1053(3) 0.0394(13) Uani 1 1 d . . . C10 C 0.5121(3) 1.5274(6) 0.1020(3) 0.0501(15) Uani 1 1 d . . . H10A H 0.4644 1.5393 0.0749 0.060 Uiso 1 1 calc R . . C11 C 0.5565(3) 1.6374(6) 0.1409(3) 0.0497(15) Uani 1 1 d . . . C12 C 0.6270(3) 1.6207(6) 0.1811(3) 0.0516(16) Uani 1 1 d . . . H12A H 0.6561 1.6979 0.2065 0.062 Uiso 1 1 calc R . . C13 C 0.6541(3) 1.4876(6) 0.1834(3) 0.0431(13) Uani 1 1 d . . . H13A H 0.7019 1.4756 0.2119 0.052 Uiso 1 1 calc R . . C14 C 0.8551(4) 1.3039(7) 0.1464(4) 0.086(2) Uani 1 1 d . . . H14A H 0.8738 1.3936 0.1431 0.129 Uiso 1 1 calc R . . H14B H 0.8492 1.2422 0.1046 0.129 Uiso 1 1 calc R . . H14C H 0.8863 1.2603 0.1968 0.129 Uiso 1 1 calc R . . H1E H 0.737(3) 1.263(6) 0.174(4) 0.09(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 Cu1 0.0385(5) 0.0437(5) 0.0255(5) -0.0007(4) 0.0185(4) 0.0071(4) Cl1 0.0459(8) 0.0450(8) 0.0504(8) -0.0016(7) 0.0288(7) -0.0032(7) O1 0.033(2) 0.058(2) 0.038(2) 0.0019(17) 0.0179(19) 0.0067(17) O2 0.069(3) 0.112(4) 0.107(4) 0.059(3) 0.045(3) 0.012(3) F1 0.0349(18) 0.059(2) 0.083(2) -0.0246(18) 0.0152(18) -0.0083(15) F2 0.085(3) 0.046(2) 0.094(3) -0.0061(18) 0.038(2) 0.0163(18) N1 0.034(3) 0.038(3) 0.033(2) -0.0033(19) 0.018(2) 0.0006(19) N2 0.046(3) 0.050(3) 0.062(3) -0.015(2) 0.036(3) -0.009(2) N3 0.039(3) 0.037(2) 0.032(2) -0.0052(18) 0.021(2) -0.002(2) N4 0.036(3) 0.043(3) 0.028(3) -0.0011(19) 0.016(2) 0.000(2) N5 0.033(3) 0.107(4) 0.035(3) -0.007(3) 0.017(2) 0.009(3) N6 0.043(3) 0.043(3) 0.026(2) -0.0012(19) 0.023(2) 0.001(2) C1 0.044(3) 0.042(3) 0.039(3) 0.001(3) 0.029(3) 0.002(3) C2 0.045(3) 0.037(3) 0.049(3) -0.010(2) 0.027(3) -0.002(3) C3 0.043(3) 0.035(3) 0.031(3) 0.004(2) 0.018(3) 0.011(2) C4 0.031(3) 0.035(3) 0.029(3) -0.006(2) 0.014(2) 0.001(2) C5 0.051(3) 0.039(3) 0.030(3) -0.006(2) 0.022(3) -0.004(3) C6 0.031(3) 0.042(3) 0.037(3) 0.002(2) 0.017(3) 0.004(2) C7 0.041(3) 0.087(4) 0.038(3) -0.003(3) 0.022(3) 0.011(3) C8 0.033(3) 0.037(3) 0.026(3) -0.003(2) 0.016(2) -0.001(2) C9 0.033(3) 0.044(3) 0.036(3) -0.014(2) 0.015(3) -0.007(3) C10 0.040(3) 0.053(4) 0.047(4) 0.001(3) 0.016(3) 0.008(3) C11 0.058(4) 0.038(3) 0.048(4) -0.002(3) 0.024(3) 0.008(3) C12 0.055(4) 0.040(4) 0.052(4) -0.013(3) 0.023(3) -0.013(3) C13 0.036(3) 0.053(3) 0.038(3) -0.006(3) 0.018(3) -0.007(3) C14 0.100(6) 0.081(5) 0.073(5) 0.010(4) 0.043(5) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 2.028(4) 4_645 ? Cu1 N6 2.028(4) 6_575 ? Cu1 N1 2.036(4) . ? Cu1 N1 2.036(4) 7_665 ? O1 C4 1.416(6) . ? O1 H1E 0.94(6) . ? O2 C14 1.442(7) . ? O2 H2 0.8200 . ? F1 C9 1.363(5) . ? F2 C11 1.349(6) . ? N1 C1 1.316(6) . ? N1 C2 1.355(6) . ? N2 C2 1.312(6) . ? N2 N3 1.363(5) . ? N3 C1 1.317(6) . ? N3 C3 1.463(6) . ? N4 C6 1.323(6) . ? N4 N5 1.356(5) . ? N4 C5 1.478(6) . ? N5 C7 1.320(6) . ? N6 C6 1.309(6) . ? N6 C7 1.353(6) . ? N6 Cu1 2.028(4) 4_655 ? C1 H1B 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.554(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.525(6) . ? C4 C8 1.544(6) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6B 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.367(6) . ? C8 C13 1.394(6) . ? C9 C10 1.388(7) . ? C10 C11 1.362(7) . ? C10 H10A 0.9300 . ? C11 C12 1.373(7) . ? C12 C13 1.381(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 N6 Cu1 N6 180.0(2) 4_645 6_575 ? N6 Cu1 N1 89.13(15) 4_645 . ? N6 Cu1 N1 90.87(15) 6_575 . ? N6 Cu1 N1 90.87(15) 4_645 7_665 ? N6 Cu1 N1 89.13(15) 6_575 7_665 ? N1 Cu1 N1 180.00(18) . 7_665 ? C4 O1 H1E 113(4) . . ? C14 O2 H2 109.5 . . ? C1 N1 C2 102.8(4) . . ? C1 N1 Cu1 129.9(4) . . ? C2 N1 Cu1 126.7(3) . . ? C2 N2 N3 102.8(4) . . ? C1 N3 N2 109.3(4) . . ? C1 N3 C3 130.4(4) . . ? N2 N3 C3 120.2(4) . . ? C6 N4 N5 109.9(4) . . ? C6 N4 C5 130.1(4) . . ? N5 N4 C5 119.9(4) . . ? C7 N5 N4 102.1(4) . . ? C6 N6 C7 103.0(4) . . ? C6 N6 Cu1 126.0(3) . 4_655 ? C7 N6 Cu1 131.0(3) . 4_655 ? N1 C1 N3 111.0(4) . . ? N1 C1 H1B 124.5 . . ? N3 C1 H1B 124.5 . . ? N2 C2 N1 114.2(5) . . ? N2 C2 H2B 122.9 . . ? N1 C2 H2B 122.9 . . ? N3 C3 C4 113.0(4) . . ? N3 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? N3 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? O1 C4 C5 104.7(4) . . ? O1 C4 C8 111.7(3) . . ? C5 C4 C8 111.3(4) . . ? O1 C4 C3 110.6(4) . . ? C5 C4 C3 111.8(4) . . ? C8 C4 C3 106.8(4) . . ? N4 C5 C4 110.7(4) . . ? N4 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? C4 C5 H5C 109.5 . . ? H5B C5 H5C 108.1 . . ? N6 C6 N4 110.6(4) . . ? N6 C6 H6B 124.7 . . ? N4 C6 H6B 124.7 . . ? N5 C7 N6 114.3(5) . . ? N5 C7 H7A 122.8 . . ? N6 C7 H7A 122.8 . . ? C9 C8 C13 115.7(5) . . ? C9 C8 C4 122.4(4) . . ? C13 C8 C4 121.9(4) . . ? F1 C9 C8 119.0(4) . . ? F1 C9 C10 115.8(4) . . ? C8 C9 C10 125.2(5) . . ? C11 C10 C9 116.3(5) . . ? C11 C10 H10A 121.9 . . ? C9 C10 H10A 121.9 . . ? F2 C11 C10 118.6(5) . . ? F2 C11 C12 119.2(5) . . ? C10 C11 C12 122.2(5) . . ? C11 C12 C13 119.2(5) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C12 C13 C8 121.5(5) . . ? C12 C13 H13A 119.2 . . ? C8 C13 H13A 119.2 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? 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 N6 Cu1 N1 C1 94.0(4) 4_645 . . . ? N6 Cu1 N1 C1 -86.0(4) 6_575 . . . ? N1 Cu1 N1 C1 154(100) 7_665 . . . ? N6 Cu1 N1 C2 -96.1(4) 4_645 . . . ? N6 Cu1 N1 C2 83.9(4) 6_575 . . . ? N1 Cu1 N1 C2 -36(100) 7_665 . . . ? C2 N2 N3 C1 -0.5(5) . . . . ? C2 N2 N3 C3 174.9(4) . . . . ? C6 N4 N5 C7 -0.4(6) . . . . ? C5 N4 N5 C7 -179.0(5) . . . . ? C2 N1 C1 N3 0.4(6) . . . . ? Cu1 N1 C1 N3 172.2(3) . . . . ? N2 N3 C1 N1 0.0(6) . . . . ? C3 N3 C1 N1 -174.7(4) . . . . ? N3 N2 C2 N1 0.8(6) . . . . ? C1 N1 C2 N2 -0.8(6) . . . . ? Cu1 N1 C2 N2 -172.9(3) . . . . ? C1 N3 C3 C4 -105.5(6) . . . . ? N2 N3 C3 C4 80.2(5) . . . . ? N3 C3 C4 O1 58.9(5) . . . . ? N3 C3 C4 C5 -57.4(6) . . . . ? N3 C3 C4 C8 -179.4(4) . . . . ? C6 N4 C5 C4 -75.5(6) . . . . ? N5 N4 C5 C4 102.8(5) . . . . ? O1 C4 C5 N4 68.7(5) . . . . ? C8 C4 C5 N4 -52.2(5) . . . . ? C3 C4 C5 N4 -171.6(4) . . . . ? C7 N6 C6 N4 -0.6(6) . . . . ? Cu1 N6 C6 N4 179.5(3) 4_655 . . . ? N5 N4 C6 N6 0.6(6) . . . . ? C5 N4 C6 N6 179.1(4) . . . . ? N4 N5 C7 N6 0.0(7) . . . . ? C6 N6 C7 N5 0.4(7) . . . . ? Cu1 N6 C7 N5 -179.8(4) 4_655 . . . ? O1 C4 C8 C9 -174.5(4) . . . . ? C5 C4 C8 C9 -57.9(6) . . . . ? C3 C4 C8 C9 64.5(6) . . . . ? O1 C4 C8 C13 3.3(6) . . . . ? C5 C4 C8 C13 120.0(5) . . . . ? C3 C4 C8 C13 -117.7(5) . . . . ? C13 C8 C9 F1 -178.9(5) . . . . ? C4 C8 C9 F1 -0.9(7) . . . . ? C13 C8 C9 C10 0.7(8) . . . . ? C4 C8 C9 C10 178.7(5) . . . . ? F1 C9 C10 C11 179.7(5) . . . . ? C8 C9 C10 C11 0.1(8) . . . . ? C9 C10 C11 F2 180.0(5) . . . . ? C9 C10 C11 C12 0.0(9) . . . . ? F2 C11 C12 C13 179.1(5) . . . . ? C10 C11 C12 C13 -0.9(9) . . . . ? C11 C12 C13 C8 1.8(8) . . . . ? C9 C8 C13 C12 -1.6(8) . . . . ? C4 C8 C13 C12 -179.6(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 Cl1 0.82 2.22 3.023(5) 167.1 7_675 O1 H1E O2 0.94(6) 1.77(6) 2.706(6) 172(6) . _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.836 _refine_diff_density_max 0.521 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.112 #== == ==end # Attachment 'corrected cif.CIF' data_Polymer_1 _database_code_depnum_ccdc_archive 'CCDC 286111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 Cl2 F2 N6 O2 Zn' _chemical_formula_weight 474.60 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 '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 8.1532(16) _cell_length_b 10.396(2) _cell_length_c 12.492(3) _cell_angle_alpha 99.87(3) _cell_angle_beta 106.06(3) _cell_angle_gamma 107.33(3) _cell_volume 933.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 278 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7137 _exptl_absorpt_correction_T_max 0.7345 _exptl_absorpt_process_details ; R-AXIS Data Processing Software Version4.0(OCT 21.1996) ; _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 2770 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2770 _reflns_number_gt 2314 _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^)+(0.0961P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2770 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 -1.17372(9) -0.33887(6) 1.07515(5) 0.0322(2) Uani 1 1 d . . . Cl1 Cl -1.3900(2) -0.24444(18) 1.05932(14) 0.0518(4) Uani 1 1 d . . . Cl2 Cl -1.1883(2) -0.45097(15) 0.90080(12) 0.0426(4) Uani 1 1 d . . . N1 N -0.9225(6) -0.1790(4) 1.1451(4) 0.0319(10) Uani 1 1 d . . . N2 N -0.6268(7) -0.0588(5) 1.1787(4) 0.0410(12) Uani 1 1 d . . . N3 N -0.7183(6) 0.0298(4) 1.1972(4) 0.0297(10) Uani 1 1 d . . . N4 N -0.3073(6) 0.4548(4) 1.3099(4) 0.0343(11) Uani 1 1 d . . . N5 N -0.0691(9) 0.5106(7) 1.2664(6) 0.0712(18) Uani 1 1 d . . . N6 N -0.1972(6) 0.5499(4) 1.1913(4) 0.0354(11) Uani 1 1 d . . . F1 F -0.8233(5) 0.3255(4) 1.3368(3) 0.0560(10) Uani 1 1 d . . . F2 F -0.9417(6) 0.1402(4) 1.6369(3) 0.0731(13) Uani 1 1 d . . . C1 C -0.7587(8) -0.1843(6) 1.1471(5) 0.0395(13) Uani 1 1 d . . . H1A H -0.7396 -0.2678 1.1282 0.047 Uiso 1 1 calc R . . C2 C -0.8906(7) -0.0438(5) 1.1782(4) 0.0312(12) Uani 1 1 d . . . H2B H -0.9776 -0.0059 1.1868 0.037 Uiso 1 1 calc R . . C3 C -0.6248(8) 0.1826(5) 1.2248(5) 0.0364(13) Uani 1 1 d . . . H3A H -0.7156 0.2252 1.2035 0.044 Uiso 1 1 calc R . . H3B H -0.5460 0.2023 1.1793 0.044 Uiso 1 1 calc R . . C4 C -0.5096(8) 0.2483(5) 1.3535(5) 0.0330(12) Uani 1 1 d . . . C5 C -0.6286(8) 0.2212(5) 1.4291(4) 0.0340(13) Uani 1 1 d . . . C6 C -0.7787(9) 0.2569(6) 1.4195(5) 0.0396(14) Uani 1 1 d . . . C7 C -0.8898(9) 0.2317(6) 1.4848(5) 0.0427(14) Uani 1 1 d . . . H7A H -0.9930 0.2561 1.4726 0.051 Uiso 1 1 calc R . . C8 C -0.8370(9) 0.1675(6) 1.5701(5) 0.0478(17) Uani 1 1 d . . . C9 C -0.6857(10) 0.1299(6) 1.5882(5) 0.0498(17) Uani 1 1 d . . . H9A H -0.6542 0.0864 1.6456 0.060 Uiso 1 1 calc R . . C10 C -0.5807(10) 0.1588(6) 1.5181(5) 0.0462(15) Uani 1 1 d . . . H10A H -0.4761 0.1362 1.5307 0.055 Uiso 1 1 calc R . . C11 C -0.4222(8) 0.4101(5) 1.3791(5) 0.0342(12) Uani 1 1 d . . . H11A H -0.5192 0.4477 1.3639 0.041 Uiso 1 1 calc R . . H11B H -0.3479 0.4496 1.4607 0.041 Uiso 1 1 calc R . . C12 C -0.1341(7) 0.4532(6) 1.3392(4) 0.0314(12) Uani 1 1 d . . . H12A H -0.0758 0.4195 1.3970 0.038 Uiso 1 1 calc R . . C13 C -0.3414(7) 0.5134(5) 1.2232(5) 0.0333(12) Uani 1 1 d . . . H13A H -0.4503 0.5265 1.1904 0.040 Uiso 1 1 calc R . . C14 C -0.7770(10) -0.1401(8) 0.8847(6) 0.0577(18) Uani 1 1 d . . . H14A H -0.6699 -0.1617 0.9155 0.087 Uiso 1 1 calc R . . H14B H -0.8848 -0.2218 0.8657 0.087 Uiso 1 1 calc R . . H14C H -0.7786 -0.0659 0.9414 0.087 Uiso 1 1 calc R . . O1 O -0.3708(6) 0.1920(4) 1.3868(4) 0.0442(10) Uani 1 1 d . . . H1B H -0.3415 0.1683 1.3310 0.066 Uiso 1 1 calc R . . O2 O -0.7734(7) -0.0973(5) 0.7844(4) 0.0576(12) Uani 1 1 d . . . H2 H -0.7036 -0.0155 0.8028 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0269(4) 0.0286(4) 0.0369(4) 0.0096(3) 0.0129(3) 0.0024(3) Cl1 0.0458(10) 0.0578(10) 0.0603(10) 0.0178(8) 0.0218(8) 0.0269(8) Cl2 0.0362(9) 0.0430(8) 0.0440(8) 0.0025(6) 0.0180(7) 0.0094(7) N1 0.029(3) 0.027(2) 0.037(2) 0.0075(19) 0.012(2) 0.005(2) N2 0.030(3) 0.027(2) 0.062(3) 0.002(2) 0.021(2) 0.004(2) N3 0.031(3) 0.023(2) 0.034(2) 0.0035(18) 0.013(2) 0.007(2) N4 0.034(3) 0.024(2) 0.037(3) 0.002(2) 0.018(2) -0.001(2) N5 0.065(4) 0.068(4) 0.085(5) 0.022(4) 0.023(4) 0.032(4) N6 0.026(3) 0.029(2) 0.044(3) 0.006(2) 0.013(2) 0.002(2) F1 0.056(3) 0.071(3) 0.061(2) 0.037(2) 0.027(2) 0.034(2) F2 0.083(3) 0.074(3) 0.060(2) 0.012(2) 0.053(2) 0.003(2) C1 0.039(4) 0.028(3) 0.051(4) 0.005(3) 0.019(3) 0.012(3) C2 0.030(3) 0.031(3) 0.036(3) 0.011(2) 0.016(2) 0.011(2) C3 0.044(4) 0.027(3) 0.038(3) 0.010(2) 0.020(3) 0.008(3) C4 0.037(3) 0.028(3) 0.034(3) 0.009(2) 0.014(2) 0.010(2) C5 0.044(4) 0.023(3) 0.032(3) 0.009(2) 0.015(3) 0.006(3) C6 0.053(4) 0.031(3) 0.030(3) 0.009(2) 0.011(3) 0.010(3) C7 0.042(4) 0.036(3) 0.043(3) 0.002(3) 0.015(3) 0.008(3) C8 0.053(4) 0.042(3) 0.035(3) 0.000(3) 0.026(3) -0.004(3) C9 0.071(5) 0.046(4) 0.043(4) 0.026(3) 0.028(3) 0.021(4) C10 0.052(4) 0.047(4) 0.040(3) 0.011(3) 0.019(3) 0.015(3) C11 0.040(3) 0.026(3) 0.036(3) 0.008(2) 0.018(3) 0.007(2) C12 0.038(3) 0.045(3) 0.035(3) 0.032(3) 0.022(2) 0.028(3) C13 0.024(3) 0.033(3) 0.039(3) 0.015(3) 0.009(2) 0.003(2) C14 0.063(5) 0.068(5) 0.052(4) 0.025(4) 0.027(4) 0.026(4) O1 0.040(3) 0.044(2) 0.049(2) 0.0079(19) 0.0168(19) 0.017(2) O2 0.053(3) 0.057(3) 0.046(3) 0.013(2) 0.015(2) 0.000(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 Zn1 N6 2.019(4) 1_445 ? Zn1 N1 2.051(5) . ? Zn1 Cl1 2.2396(17) . ? Zn1 Cl2 2.2404(17) . ? N1 C2 1.318(6) . ? N1 C1 1.346(7) . ? N2 C1 1.329(7) . ? N2 N3 1.375(6) . ? N3 C2 1.314(7) . ? N3 C3 1.473(6) . ? N4 C13 1.335(7) . ? N4 C12 1.363(7) . ? N4 C11 1.473(6) . ? N5 C12 1.315(8) . ? N5 N6 1.408(7) . ? N6 C13 1.315(7) . ? N6 Zn1 2.019(4) 1_665 ? F1 C6 1.381(6) . ? F2 C8 1.355(7) . ? C3 C4 1.529(8) . ? C4 O1 1.420(7) . ? C4 C5 1.532(7) . ? C4 C11 1.554(7) . ? C5 C6 1.362(8) . ? C5 C10 1.402(8) . ? C6 C7 1.377(8) . ? C7 C8 1.389(9) . ? C8 C9 1.374(10) . ? C9 C10 1.393(8) . ? C14 O2 1.404(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 N6 Zn1 N1 107.73(18) 1_445 . ? N6 Zn1 Cl1 105.66(14) 1_445 . ? N1 Zn1 Cl1 108.16(13) . . ? N6 Zn1 Cl2 117.77(14) 1_445 . ? N1 Zn1 Cl2 105.88(13) . . ? Cl1 Zn1 Cl2 111.30(7) . . ? C2 N1 C1 104.0(4) . . ? C2 N1 Zn1 126.8(4) . . ? C1 N1 Zn1 128.1(4) . . ? C1 N2 N3 102.1(5) . . ? C2 N3 N2 109.8(4) . . ? C2 N3 C3 129.7(4) . . ? N2 N3 C3 120.4(4) . . ? C13 N4 C12 110.8(4) . . ? C13 N4 C11 128.3(5) . . ? C12 N4 C11 120.5(4) . . ? C12 N5 N6 112.2(6) . . ? C13 N6 N5 103.9(5) . . ? C13 N6 Zn1 123.9(4) . 1_665 ? N5 N6 Zn1 131.6(4) . 1_665 ? N2 C1 N1 113.7(5) . . ? N3 C2 N1 110.3(5) . . ? N3 C3 C4 112.2(4) . . ? O1 C4 C3 110.7(4) . . ? O1 C4 C5 108.3(4) . . ? C3 C4 C5 111.1(5) . . ? O1 C4 C11 110.1(5) . . ? C3 C4 C11 110.1(4) . . ? C5 C4 C11 106.5(4) . . ? C6 C5 C10 115.7(5) . . ? C6 C5 C4 124.9(5) . . ? C10 C5 C4 119.4(5) . . ? C5 C6 F1 117.0(5) . . ? C5 C6 C7 126.2(5) . . ? F1 C6 C7 116.8(6) . . ? C6 C7 C8 115.3(6) . . ? F2 C8 C9 119.4(6) . . ? F2 C8 C7 117.7(6) . . ? C9 C8 C7 122.8(6) . . ? C8 C9 C10 118.2(6) . . ? C9 C10 C5 121.7(6) . . ? N4 C11 C4 113.6(4) . . ? N5 C12 N4 103.5(4) . . ? N6 C13 N4 109.5(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 N6 Zn1 N1 C2 -112.3(4) 1_445 . . . ? Cl1 Zn1 N1 C2 1.4(5) . . . . ? Cl2 Zn1 N1 C2 120.8(4) . . . . ? N6 Zn1 N1 C1 81.7(5) 1_445 . . . ? Cl1 Zn1 N1 C1 -164.5(4) . . . . ? Cl2 Zn1 N1 C1 -45.1(5) . . . . ? C1 N2 N3 C2 0.8(6) . . . . ? C1 N2 N3 C3 -174.9(5) . . . . ? C12 N5 N6 C13 0.1(7) . . . . ? C12 N5 N6 Zn1 171.8(4) . . . 1_665 ? N3 N2 C1 N1 -0.1(7) . . . . ? C2 N1 C1 N2 -0.6(6) . . . . ? Zn1 N1 C1 N2 167.8(4) . . . . ? N2 N3 C2 N1 -1.3(6) . . . . ? C3 N3 C2 N1 173.9(5) . . . . ? C1 N1 C2 N3 1.1(6) . . . . ? Zn1 N1 C2 N3 -167.5(3) . . . . ? C2 N3 C3 C4 102.6(6) . . . . ? N2 N3 C3 C4 -82.6(6) . . . . ? N3 C3 C4 O1 60.9(6) . . . . ? N3 C3 C4 C5 -59.4(6) . . . . ? N3 C3 C4 C11 -177.1(4) . . . . ? O1 C4 C5 C6 -177.9(5) . . . . ? C3 C4 C5 C6 -56.2(7) . . . . ? C11 C4 C5 C6 63.7(7) . . . . ? O1 C4 C5 C10 4.0(7) . . . . ? C3 C4 C5 C10 125.8(5) . . . . ? C11 C4 C5 C10 -114.3(6) . . . . ? C10 C5 C6 F1 176.5(5) . . . . ? C4 C5 C6 F1 -1.6(8) . . . . ? C10 C5 C6 C7 -3.1(9) . . . . ? C4 C5 C6 C7 178.8(5) . . . . ? C5 C6 C7 C8 2.0(9) . . . . ? F1 C6 C7 C8 -177.6(5) . . . . ? C6 C7 C8 F2 -180.0(5) . . . . ? C6 C7 C8 C9 -0.6(9) . . . . ? F2 C8 C9 C10 179.8(6) . . . . ? C7 C8 C9 C10 0.5(9) . . . . ? C8 C9 C10 C5 -1.6(10) . . . . ? C6 C5 C10 C9 2.8(9) . . . . ? C4 C5 C10 C9 -179.0(5) . . . . ? C13 N4 C11 C4 109.3(6) . . . . ? C12 N4 C11 C4 -78.3(6) . . . . ? O1 C4 C11 N4 64.8(6) . . . . ? C3 C4 C11 N4 -57.5(6) . . . . ? C5 C4 C11 N4 -178.0(5) . . . . ? N6 N5 C12 N4 0.4(7) . . . . ? C13 N4 C12 N5 -0.8(6) . . . . ? C11 N4 C12 N5 -174.5(5) . . . . ? N5 N6 C13 N4 -0.6(6) . . . . ? Zn1 N6 C13 N4 -173.2(3) 1_665 . . . ? C12 N4 C13 N6 1.0(6) . . . . ? C11 N4 C13 N6 174.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 0.755 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.116 #==end data_polymer_2 _database_code_depnum_ccdc_archive 'CCDC 286112' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 Cd Cl2 F4 N12 O5' _chemical_formula_weight 863.95 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 24.017(5) _cell_length_b 9.5929(19) _cell_length_c 20.662(4) _cell_angle_alpha 90.00 _cell_angle_beta 124.65(3) _cell_angle_gamma 90.00 _cell_volume 3916.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 267 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description Prismatic _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8501 _exptl_absorpt_correction_T_max 0.8624 _exptl_absorpt_process_details ; R-AXIS Data Processing Software Version4.0(OCT 21.1996) ; _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 'Oscillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4319 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.1061 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.00 _reflns_number_total 2590 _reflns_number_gt 1899 _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^)+(0.0760P)^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 0.0013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2590 _refine_ls_number_parameters 250 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.041 _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 0.7500 0.7500 0.0000 0.0430(3) Uani 1 2 d S . . Cl1 Cl 0.68052(10) 0.9733(2) -0.00737(13) 0.0647(6) Uani 1 1 d . . . O1 O 0.7932(2) 0.7915(5) 0.3096(3) 0.0523(14) Uani 1 1 d . . . H1A H 0.7758 0.7355 0.3230 0.078 Uiso 1 1 calc R . . O2 O 0.8541(8) 1.2636(19) 0.1143(12) 0.147(7) Uani 0.50 1 d PD . . O3 O 0.7726(4) 1.1633(9) 0.1366(5) 0.102(2) Uani 1 1 d D . . F1 F 1.00344(19) 0.6981(5) 0.4401(3) 0.0813(17) Uani 1 1 d . . . F2 F 0.9558(3) 0.2345(5) 0.3598(3) 0.0942(17) Uani 1 1 d . . . N1 N 0.8325(3) 0.7906(7) 0.1326(3) 0.0507(17) Uani 1 1 d . . . N2 N 0.9307(3) 0.8052(12) 0.2506(4) 0.106(4) Uani 1 1 d . . . N3 N 0.8800(3) 0.8460(7) 0.2559(3) 0.0479(15) Uani 1 1 d . . . N4 N 0.8664(3) 0.9479(6) 0.4548(3) 0.0476(16) Uani 1 1 d . . . N5 N 0.8985(3) 1.0646(7) 0.4585(4) 0.071(2) Uani 1 1 d . . . N6 N 0.8123(3) 1.1157(7) 0.4673(3) 0.0496(16) Uani 1 1 d . . . C1 C 0.8224(3) 0.8342(8) 0.1846(4) 0.0507(19) Uani 1 1 d . . . H1B H 0.7800 0.8548 0.1734 0.061 Uiso 1 1 calc R . . C2 C 0.8994(4) 0.7710(13) 0.1752(5) 0.103(4) Uani 1 1 d . . . H2B H 0.9220 0.7365 0.1541 0.124 Uiso 1 1 calc R . . C3 C 0.8913(4) 0.8898(8) 0.3296(4) 0.0509(19) Uani 1 1 d . . . H3A H 0.8684 0.9777 0.3220 0.061 Uiso 1 1 calc R . . H3B H 0.9393 0.9042 0.3683 0.061 Uiso 1 1 calc R . . C4 C 0.8649(3) 0.7801(7) 0.3609(4) 0.0445(19) Uani 1 1 d . . . C5 C 0.8884(3) 0.6311(8) 0.3596(4) 0.0408(17) Uani 1 1 d . . . C6 C 0.9569(3) 0.5972(8) 0.3987(4) 0.0494(19) Uani 1 1 d . . . C7 C 0.9802(4) 0.4657(9) 0.3990(5) 0.058(2) Uani 1 1 d . . . H7A H 1.0262 0.4467 0.4261 0.070 Uiso 1 1 calc R . . C8 C 0.9334(4) 0.3662(9) 0.3584(5) 0.061(2) Uani 1 1 d . . . C9 C 0.8656(4) 0.3897(9) 0.3189(5) 0.065(2) Uani 1 1 d . . . H9A H 0.8348 0.3175 0.2925 0.078 Uiso 1 1 calc R . . C10 C 0.8435(4) 0.5229(9) 0.3186(4) 0.056(2) Uani 1 1 d . . . H10A H 0.7973 0.5402 0.2902 0.067 Uiso 1 1 calc R . . C11 C 0.8887(4) 0.8125(8) 0.4468(4) 0.052(2) Uani 1 1 d . . . H11A H 0.8714 0.7412 0.4642 0.062 Uiso 1 1 calc R . . H11B H 0.9377 0.8089 0.4808 0.062 Uiso 1 1 calc R . . C12 C 0.8637(4) 1.1636(9) 0.4646(5) 0.066(2) Uani 1 1 d . . . H12A H 0.8736 1.2578 0.4669 0.080 Uiso 1 1 calc R . . C13 C 0.8150(4) 0.9814(9) 0.4604(5) 0.052(2) Uani 1 1 d . . . H13A H 0.7855 0.9175 0.4595 0.063 Uiso 1 1 calc R . . C14 C 0.9208(11) 1.228(3) 0.1670(14) 0.148(13) Uani 0.50 1 d PD . . H3F H 0.8142(19) 1.185(7) 0.139(4) 0.037(18) Uiso 1 1 d D . . H3E H 0.748(4) 1.103(8) 0.095(4) 0.09(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0441(4) 0.0518(5) 0.0365(4) 0.0020(5) 0.0249(3) -0.0040(4) Cl1 0.0677(13) 0.0586(13) 0.0740(14) 0.0020(11) 0.0440(11) 0.0076(10) O1 0.040(3) 0.066(4) 0.042(3) 0.008(2) 0.018(2) 0.009(2) O2 0.100(12) 0.136(16) 0.173(19) 0.039(13) 0.059(12) 0.023(11) O3 0.086(5) 0.109(6) 0.120(7) -0.045(5) 0.063(5) -0.010(5) F1 0.040(2) 0.067(3) 0.099(4) -0.032(3) 0.016(3) -0.007(2) F2 0.105(4) 0.055(4) 0.107(4) -0.007(3) 0.051(3) 0.016(3) N1 0.047(3) 0.073(5) 0.036(3) 0.002(3) 0.026(3) 0.000(3) N2 0.047(4) 0.221(11) 0.056(5) -0.017(6) 0.033(4) 0.004(5) N3 0.046(3) 0.061(4) 0.039(4) -0.003(3) 0.026(3) -0.001(3) N4 0.049(3) 0.050(4) 0.045(4) -0.007(3) 0.027(3) 0.002(3) N5 0.063(4) 0.059(5) 0.110(6) -0.031(4) 0.061(4) -0.018(4) N6 0.045(3) 0.060(5) 0.051(4) -0.013(3) 0.032(3) -0.010(3) C1 0.043(4) 0.053(5) 0.047(5) 0.011(4) 0.020(4) 0.009(4) C2 0.047(5) 0.217(14) 0.043(5) -0.017(7) 0.025(4) 0.013(7) C3 0.056(4) 0.051(5) 0.040(4) -0.003(4) 0.024(4) -0.004(4) C4 0.041(4) 0.052(6) 0.032(4) -0.001(3) 0.015(3) 0.005(3) C5 0.038(4) 0.046(4) 0.031(4) -0.006(3) 0.016(3) 0.004(3) C6 0.042(4) 0.051(5) 0.047(4) -0.018(4) 0.020(4) -0.006(4) C7 0.046(4) 0.058(5) 0.060(5) -0.003(4) 0.023(4) 0.012(4) C8 0.076(6) 0.041(5) 0.059(5) -0.005(4) 0.034(5) 0.007(5) C9 0.065(5) 0.049(6) 0.065(6) -0.017(4) 0.027(5) -0.016(4) C10 0.044(4) 0.059(5) 0.054(5) -0.009(4) 0.021(4) -0.012(4) C11 0.051(4) 0.057(5) 0.036(4) -0.002(4) 0.018(4) 0.014(4) C12 0.062(5) 0.048(5) 0.098(7) -0.026(5) 0.051(5) -0.001(4) C13 0.055(5) 0.053(5) 0.067(5) 0.005(4) 0.045(4) -0.002(4) C14 0.13(2) 0.23(4) 0.105(19) 0.07(2) 0.075(17) 0.04(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 2.327(6) . ? Cd1 N1 2.327(6) 7_665 ? Cd1 N6 2.345(6) 6_575 ? Cd1 N6 2.345(6) 4_645 ? Cd1 Cl1 2.666(2) 7_665 ? Cd1 Cl1 2.666(2) . ? O1 C4 1.423(7) . ? O1 H1A 0.8200 . ? O2 C14 1.373(17) . ? O3 H3F 0.99(2) . ? O3 H3E 0.91(2) . ? F1 C6 1.353(8) . ? F2 C8 1.367(9) . ? N1 C1 1.297(9) . ? N1 C2 1.335(9) . ? N2 C2 1.330(11) . ? N2 N3 1.341(8) . ? N3 C1 1.333(8) . ? N3 C3 1.450(9) . ? N4 N5 1.337(9) . ? N4 C13 1.342(8) . ? N4 C11 1.450(9) . ? N5 C12 1.319(9) . ? N6 C13 1.303(10) . ? N6 C12 1.347(9) . ? N6 Cd1 2.345(6) 4_655 ? C1 H1B 0.9300 . ? C2 H2B 0.9300 . ? C3 C4 1.545(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.542(10) . ? C4 C11 1.557(10) . ? C5 C10 1.385(10) . ? C5 C6 1.397(9) . ? C6 C7 1.379(11) . ? C7 C8 1.344(11) . ? C7 H7A 0.9300 . ? C8 C9 1.361(10) . ? C9 C10 1.382(11) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0(3) . 7_665 ? N1 Cd1 N6 89.5(2) . 6_575 ? N1 Cd1 N6 90.5(2) 7_665 6_575 ? N1 Cd1 N6 90.5(2) . 4_645 ? N1 Cd1 N6 89.5(2) 7_665 4_645 ? N6 Cd1 N6 180.0(2) 6_575 4_645 ? N1 Cd1 Cl1 88.91(16) . 7_665 ? N1 Cd1 Cl1 91.09(16) 7_665 7_665 ? N6 Cd1 Cl1 88.67(16) 6_575 7_665 ? N6 Cd1 Cl1 91.33(16) 4_645 7_665 ? N1 Cd1 Cl1 91.09(16) . . ? N1 Cd1 Cl1 88.91(16) 7_665 . ? N6 Cd1 Cl1 91.33(16) 6_575 . ? N6 Cd1 Cl1 88.67(16) 4_645 . ? Cl1 Cd1 Cl1 180.00(9) 7_665 . ? C4 O1 H1A 109.5 . . ? H3F O3 H3E 106(7) . . ? C1 N1 C2 102.8(6) . . ? C1 N1 Cd1 126.4(5) . . ? C2 N1 Cd1 130.7(5) . . ? C2 N2 N3 103.4(6) . . ? C1 N3 N2 107.7(6) . . ? C1 N3 C3 130.0(6) . . ? N2 N3 C3 122.3(6) . . ? N5 N4 C13 108.9(6) . . ? N5 N4 C11 121.1(6) . . ? C13 N4 C11 129.9(7) . . ? C12 N5 N4 103.3(6) . . ? C13 N6 C12 103.2(6) . . ? C13 N6 Cd1 130.9(5) . 4_655 ? C12 N6 Cd1 125.0(5) . 4_655 ? N1 C1 N3 112.2(6) . . ? N1 C1 H1B 123.9 . . ? N3 C1 H1B 123.9 . . ? N2 C2 N1 113.9(7) . . ? N2 C2 H2B 123.1 . . ? N1 C2 H2B 123.1 . . ? N3 C3 C4 111.5(6) . . ? N3 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N3 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O1 C4 C5 111.0(5) . . ? O1 C4 C3 104.3(5) . . ? C5 C4 C3 112.5(6) . . ? O1 C4 C11 109.7(5) . . ? C5 C4 C11 107.7(5) . . ? C3 C4 C11 111.6(6) . . ? C10 C5 C6 115.4(7) . . ? C10 C5 C4 122.7(6) . . ? C6 C5 C4 121.8(6) . . ? F1 C6 C7 117.6(6) . . ? F1 C6 C5 118.5(6) . . ? C7 C6 C5 123.8(7) . . ? C8 C7 C6 117.0(7) . . ? C8 C7 H7A 121.5 . . ? C6 C7 H7A 121.5 . . ? C7 C8 C9 123.2(8) . . ? C7 C8 F2 117.6(7) . . ? C9 C8 F2 119.2(7) . . ? C8 C9 C10 118.7(7) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C9 C10 C5 121.8(7) . . ? C9 C10 H10A 119.1 . . ? C5 C10 H10A 119.1 . . ? N4 C11 C4 112.9(6) . . ? N4 C11 H11A 109.0 . . ? C4 C11 H11A 109.0 . . ? N4 C11 H11B 109.0 . . ? C4 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N5 C12 N6 113.9(8) . . ? N5 C12 H12A 123.0 . . ? N6 C12 H12A 123.0 . . ? N6 C13 N4 110.6(7) . . ? N6 C13 H13A 124.7 . . ? N4 C13 H13A 124.7 . . ? 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 N1 C1 167(100) 7_665 . . . ? N6 Cd1 N1 C1 130.0(7) 6_575 . . . ? N6 Cd1 N1 C1 -50.0(7) 4_645 . . . ? Cl1 Cd1 N1 C1 -141.4(6) 7_665 . . . ? Cl1 Cd1 N1 C1 38.6(6) . . . . ? N1 Cd1 N1 C2 -16(100) 7_665 . . . ? N6 Cd1 N1 C2 -53.4(9) 6_575 . . . ? N6 Cd1 N1 C2 126.6(9) 4_645 . . . ? Cl1 Cd1 N1 C2 35.3(9) 7_665 . . . ? Cl1 Cd1 N1 C2 -144.7(9) . . . . ? C2 N2 N3 C1 -0.1(11) . . . . ? C2 N2 N3 C3 178.4(9) . . . . ? C13 N4 N5 C12 -1.3(9) . . . . ? C11 N4 N5 C12 179.4(7) . . . . ? C2 N1 C1 N3 2.0(10) . . . . ? Cd1 N1 C1 N3 179.4(5) . . . . ? N2 N3 C1 N1 -1.2(10) . . . . ? C3 N3 C1 N1 -179.6(7) . . . . ? N3 N2 C2 N1 1.4(14) . . . . ? C1 N1 C2 N2 -2.1(13) . . . . ? Cd1 N1 C2 N2 -179.4(7) . . . . ? C1 N3 C3 C4 69.9(10) . . . . ? N2 N3 C3 C4 -108.2(9) . . . . ? N3 C3 C4 O1 -72.3(7) . . . . ? N3 C3 C4 C5 48.1(8) . . . . ? N3 C3 C4 C11 169.3(6) . . . . ? O1 C4 C5 C10 -5.3(9) . . . . ? C3 C4 C5 C10 -121.7(7) . . . . ? C11 C4 C5 C10 114.8(8) . . . . ? O1 C4 C5 C6 173.2(6) . . . . ? C3 C4 C5 C6 56.8(9) . . . . ? C11 C4 C5 C6 -66.6(8) . . . . ? C10 C5 C6 F1 -179.8(7) . . . . ? C4 C5 C6 F1 1.6(10) . . . . ? C10 C5 C6 C7 -1.2(11) . . . . ? C4 C5 C6 C7 -179.8(7) . . . . ? F1 C6 C7 C8 179.3(7) . . . . ? C5 C6 C7 C8 0.6(12) . . . . ? C6 C7 C8 C9 -0.9(13) . . . . ? C6 C7 C8 F2 -178.4(7) . . . . ? C7 C8 C9 C10 1.7(14) . . . . ? F2 C8 C9 C10 179.2(8) . . . . ? C8 C9 C10 C5 -2.3(13) . . . . ? C6 C5 C10 C9 2.0(11) . . . . ? C4 C5 C10 C9 -179.4(7) . . . . ? N5 N4 C11 C4 -79.5(8) . . . . ? C13 N4 C11 C4 101.3(9) . . . . ? O1 C4 C11 N4 -56.0(8) . . . . ? C5 C4 C11 N4 -176.9(6) . . . . ? C3 C4 C11 N4 59.1(8) . . . . ? N4 N5 C12 N6 1.9(10) . . . . ? C13 N6 C12 N5 -1.7(10) . . . . ? Cd1 N6 C12 N5 168.7(6) 4_655 . . . ? C12 N6 C13 N4 0.8(9) . . . . ? Cd1 N6 C13 N4 -168.8(4) 4_655 . . . ? N5 N4 C13 N6 0.3(9) . . . . ? C11 N4 C13 N6 179.6(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O3 0.82 1.91 2.693(9) 160.3 4_645 O3 H3F O2 0.99(2) 1.52(4) 2.45(2) 154(6) . _diffrn_measured_fraction_theta_max 0.842 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.842 _refine_diff_density_max 0.699 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.100 #== == == end data_polymer_3 _database_code_depnum_ccdc_archive 'CCDC 286113' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 Cl2 Co F4 N12 O4' _chemical_formula_weight 806.49 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 22.876(5) _cell_length_b 9.3066(19) _cell_length_c 20.258(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.26(3) _cell_angle_gamma 90.00 _cell_volume 3646.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 289 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description prismatic _exptl_crystal_colour res _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8632 _exptl_absorpt_correction_T_max 0.8745 _exptl_absorpt_process_details ; R-AXIS Data Processing Software Version4.0(OCT 21.1996) ; _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 'Oscillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4494 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2710 _reflns_number_gt 1903 _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^)+(0.0727P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2710 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.7500 0.7500 0.0000 0.0368(3) Uani 1 2 d S . . Cl1 Cl 0.68638(6) 0.52690(14) -0.00080(7) 0.0495(4) Uani 1 1 d . . . O1 O 0.78585(16) 0.2663(5) -0.1941(2) 0.0542(10) Uani 1 1 d . . . O2 O 0.8516(5) 0.3032(11) 0.1427(4) 0.194(3) Uani 1 1 d . . . H2 H 0.8482 0.2577 0.1061 0.291 Uiso 1 1 calc R . . F1 F 1.00281(14) 0.2029(3) -0.0686(2) 0.0783(11) Uani 1 1 d . . . F2 F 0.9703(2) -0.2796(4) -0.1428(3) 0.0975(13) Uani 1 1 d . . . N1 N 0.80961(18) 0.6228(4) -0.0327(2) 0.0426(10) Uani 1 1 d . . . N2 N 0.8961(2) 0.5628(5) -0.0487(3) 0.0579(12) Uani 1 1 d . . . N3 N 0.85990(19) 0.4448(4) -0.0516(2) 0.0442(10) Uani 1 1 d . . . N4 N 0.9248(2) 0.2889(6) -0.2616(3) 0.0676(15) Uani 1 1 d . . . N5 N 0.87085(18) 0.3342(4) -0.2560(2) 0.0417(10) Uani 1 1 d . . . N6 N 0.82543(19) 0.2799(4) -0.3790(2) 0.0433(10) Uani 1 1 d . . . C1 C 0.8643(2) 0.6668(6) -0.0366(3) 0.0516(13) Uani 1 1 d . . . H1A H 0.8780 0.7624 -0.0312 0.062 Uiso 1 1 calc R . . C2 C 0.8084(2) 0.4838(6) -0.0428(3) 0.0461(12) Uani 1 1 d . . . H2A H 0.7763 0.4213 -0.0437 0.055 Uiso 1 1 calc R . . C3 C 0.8817(3) 0.3025(6) -0.0607(3) 0.0483(13) Uani 1 1 d . . . H3A H 0.8630 0.2310 -0.0422 0.058 Uiso 1 1 calc R . . H3B H 0.9317 0.2969 -0.0281 0.058 Uiso 1 1 calc R . . C4 C 0.8591(2) 0.2656(5) -0.1449(3) 0.0439(12) Uani 1 1 d . . . C5 C 0.8892(2) 0.1163(5) -0.1442(3) 0.0404(12) Uani 1 1 d . . . C6 C 0.9592(2) 0.0912(6) -0.1064(3) 0.0486(13) Uani 1 1 d . . . C7 C 0.9874(3) -0.0377(6) -0.1051(3) 0.0578(15) Uani 1 1 d . . . H7A H 1.0350 -0.0491 -0.0792 0.069 Uiso 1 1 calc R . . C8 C 0.9442(3) -0.1493(6) -0.1426(3) 0.0598(15) Uani 1 1 d . . . C9 C 0.8730(3) -0.1334(6) -0.1821(3) 0.0635(16) Uani 1 1 d . . . H9A H 0.8436 -0.2107 -0.2075 0.076 Uiso 1 1 calc R . . C10 C 0.8475(2) -0.0006(6) -0.1824(3) 0.0531(14) Uani 1 1 d . . . H10A H 0.7998 0.0117 -0.2096 0.064 Uiso 1 1 calc R . . C11 C 0.8826(2) 0.3795(5) -0.1811(3) 0.0463(13) Uani 1 1 d . . . H11A H 0.8576 0.4681 -0.1881 0.056 Uiso 1 1 calc R . . H11B H 0.9314 0.3986 -0.1454 0.056 Uiso 1 1 calc R . . C12 C 0.8128(2) 0.3271(5) -0.3268(3) 0.0435(12) Uani 1 1 d . . . H12A H 0.7692 0.3522 -0.3375 0.052 Uiso 1 1 calc R . . C13 C 0.8952(3) 0.2574(7) -0.3356(3) 0.0664(17) Uani 1 1 d . . . H13A H 0.9196 0.2226 -0.3570 0.080 Uiso 1 1 calc R . . C14 C 0.7859(2) 0.3275(6) 0.1292(3) 0.0509(15) Uani 1 1 d . . . H14A H 0.7886 0.4005 0.1642 0.076 Uiso 1 1 calc R . . H14B H 0.7686 0.2402 0.1379 0.076 Uiso 1 1 calc R . . H14C H 0.7554 0.3586 0.0763 0.076 Uiso 1 1 calc R . . H1E H 0.769(4) 0.194(10) -0.180(6) 0.18(4) 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 0.0404(5) 0.0412(6) 0.0329(5) -0.0022(5) 0.0225(4) 0.0006(4) Cl1 0.0504(7) 0.0470(8) 0.0549(8) -0.0014(6) 0.0307(6) -0.0040(6) O1 0.0387(18) 0.072(3) 0.046(2) 0.005(2) 0.0191(17) 0.0106(18) O2 0.282(10) 0.157(8) 0.130(6) 0.013(5) 0.101(7) -0.004(7) F1 0.0404(16) 0.070(2) 0.098(3) -0.0284(19) 0.0189(16) -0.0054(15) F2 0.111(3) 0.056(2) 0.113(3) -0.007(2) 0.051(3) 0.0279(19) N1 0.046(2) 0.048(3) 0.044(2) -0.008(2) 0.030(2) -0.0014(19) N2 0.052(2) 0.055(3) 0.073(3) -0.022(3) 0.037(2) -0.007(2) N3 0.053(2) 0.047(3) 0.040(2) -0.005(2) 0.029(2) 0.003(2) N4 0.043(2) 0.118(5) 0.043(3) -0.007(3) 0.024(2) 0.005(2) N5 0.043(2) 0.050(3) 0.035(2) -0.002(2) 0.0226(19) 0.0008(19) N6 0.050(2) 0.052(3) 0.036(2) 0.000(2) 0.028(2) 0.0021(18) C1 0.051(3) 0.049(3) 0.060(3) -0.013(3) 0.033(3) -0.004(3) C2 0.059(3) 0.049(3) 0.048(3) 0.000(3) 0.040(3) 0.007(2) C3 0.054(3) 0.052(3) 0.036(3) 0.000(2) 0.022(2) 0.016(2) C4 0.042(3) 0.053(3) 0.036(3) -0.004(3) 0.020(2) 0.006(2) C5 0.039(3) 0.047(3) 0.032(3) -0.002(2) 0.017(2) 0.004(2) C6 0.041(3) 0.048(3) 0.046(3) -0.013(3) 0.015(2) -0.011(2) C7 0.046(3) 0.056(4) 0.059(4) -0.002(3) 0.020(3) 0.009(3) C8 0.063(3) 0.051(4) 0.062(4) -0.002(3) 0.031(3) 0.013(3) C9 0.061(3) 0.049(4) 0.067(4) -0.013(3) 0.025(3) -0.007(3) C10 0.049(3) 0.060(4) 0.046(3) -0.005(3) 0.022(2) -0.007(3) C11 0.054(3) 0.047(3) 0.037(3) -0.006(2) 0.023(2) 0.000(2) C12 0.035(2) 0.054(3) 0.039(3) 0.005(2) 0.019(2) 0.012(2) C13 0.051(3) 0.108(5) 0.043(3) -0.006(4) 0.027(3) 0.017(3) C14 0.039(3) 0.056(3) 0.063(4) 0.034(3) 0.030(3) 0.010(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 Co1 N6 2.133(4) 6_566 ? Co1 N6 2.133(4) 4_654 ? Co1 N1 2.159(4) 7_665 ? Co1 N1 2.159(4) . ? Co1 Cl1 2.5307(13) . ? Co1 Cl1 2.5307(13) 7_665 ? O1 C4 1.421(5) . ? O1 H1E 0.89(9) . ? O2 C14 1.395(9) . ? O2 H2 0.8200 . ? F1 C6 1.359(5) . ? F2 C8 1.352(6) . ? N1 C2 1.308(6) . ? N1 C1 1.359(6) . ? N2 C1 1.310(6) . ? N2 N3 1.357(6) . ? N3 C2 1.333(5) . ? N3 C3 1.461(6) . ? N4 C13 1.308(7) . ? N4 N5 1.365(5) . ? N5 C12 1.338(5) . ? N5 C11 1.456(6) . ? N6 C12 1.313(6) . ? N6 C13 1.366(6) . ? N6 Co1 2.133(4) 4_644 ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.534(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C11 1.538(7) . ? C4 C5 1.547(7) . ? C5 C6 1.377(6) . ? C5 C10 1.380(7) . ? C6 C7 1.356(7) . ? C7 C8 1.352(7) . ? C7 H7A 0.9300 . ? C8 C9 1.388(7) . ? C9 C10 1.365(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 N6 Co1 N6 180.000(2) 6_566 4_654 ? N6 Co1 N1 88.57(14) 6_566 7_665 ? N6 Co1 N1 91.43(14) 4_654 7_665 ? N6 Co1 N1 91.43(14) 6_566 . ? N6 Co1 N1 88.57(14) 4_654 . ? N1 Co1 N1 180.00(18) 7_665 . ? N6 Co1 Cl1 90.57(11) 6_566 . ? N6 Co1 Cl1 89.43(11) 4_654 . ? N1 Co1 Cl1 89.80(11) 7_665 . ? N1 Co1 Cl1 90.20(11) . . ? N6 Co1 Cl1 89.43(11) 6_566 7_665 ? N6 Co1 Cl1 90.57(11) 4_654 7_665 ? N1 Co1 Cl1 90.20(11) 7_665 7_665 ? N1 Co1 Cl1 89.80(11) . 7_665 ? Cl1 Co1 Cl1 180.000(1) . 7_665 ? C4 O1 H1E 108(6) . . ? C14 O2 H2 109.5 . . ? C2 N1 C1 103.4(4) . . ? C2 N1 Co1 128.8(3) . . ? C1 N1 Co1 127.2(3) . . ? C1 N2 N3 102.7(4) . . ? C2 N3 N2 109.7(4) . . ? C2 N3 C3 130.5(4) . . ? N2 N3 C3 119.8(4) . . ? C13 N4 N5 103.0(4) . . ? C12 N5 N4 108.8(4) . . ? C12 N5 C11 131.0(4) . . ? N4 N5 C11 120.3(4) . . ? C12 N6 C13 102.6(4) . . ? C12 N6 Co1 125.4(3) . 4_644 ? C13 N6 Co1 132.0(3) . 4_644 ? N2 C1 N1 114.1(5) . . ? N2 C1 H1A 122.9 . . ? N1 C1 H1A 122.9 . . ? N1 C2 N3 110.1(5) . . ? N1 C2 H2A 124.9 . . ? N3 C2 H2A 124.9 . . ? N3 C3 C4 114.1(4) . . ? N3 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N3 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? O1 C4 C3 110.5(4) . . ? O1 C4 C11 104.1(4) . . ? C3 C4 C11 112.3(4) . . ? O1 C4 C5 111.3(4) . . ? C3 C4 C5 107.8(4) . . ? C11 C4 C5 110.9(4) . . ? C6 C5 C10 115.4(5) . . ? C6 C5 C4 122.5(4) . . ? C10 C5 C4 122.1(4) . . ? C7 C6 F1 117.9(4) . . ? C7 C6 C5 124.1(5) . . ? F1 C6 C5 118.0(5) . . ? C8 C7 C6 118.1(5) . . ? C8 C7 H7A 120.9 . . ? C6 C7 H7A 120.9 . . ? C7 C8 F2 119.9(5) . . ? C7 C8 C9 121.5(5) . . ? F2 C8 C9 118.6(5) . . ? C10 C9 C8 117.8(5) . . ? C10 C9 H9A 121.1 . . ? C8 C9 H9A 121.1 . . ? C9 C10 C5 123.1(4) . . ? C9 C10 H10A 118.5 . . ? C5 C10 H10A 118.5 . . ? N5 C11 C4 112.3(4) . . ? N5 C11 H11A 109.1 . . ? C4 C11 H11A 109.1 . . ? N5 C11 H11B 109.1 . . ? C4 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N6 C12 N5 111.0(4) . . ? N6 C12 H12A 124.5 . . ? N5 C12 H12A 124.5 . . ? N4 C13 N6 114.6(5) . . ? N4 C13 H13A 122.7 . . ? N6 C13 H13A 122.7 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? 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 N6 Co1 N1 C2 87.9(4) 6_566 . . . ? N6 Co1 N1 C2 -92.1(4) 4_654 . . . ? N1 Co1 N1 C2 -160(100) 7_665 . . . ? Cl1 Co1 N1 C2 -2.7(4) . . . . ? Cl1 Co1 N1 C2 177.3(4) 7_665 . . . ? N6 Co1 N1 C1 -81.8(4) 6_566 . . . ? N6 Co1 N1 C1 98.2(4) 4_654 . . . ? N1 Co1 N1 C1 30(100) 7_665 . . . ? Cl1 Co1 N1 C1 -172.4(4) . . . . ? Cl1 Co1 N1 C1 7.6(4) 7_665 . . . ? C1 N2 N3 C2 1.2(5) . . . . ? C1 N2 N3 C3 -177.0(4) . . . . ? C13 N4 N5 C12 -0.1(6) . . . . ? C13 N4 N5 C11 179.8(5) . . . . ? N3 N2 C1 N1 -0.8(6) . . . . ? C2 N1 C1 N2 0.2(6) . . . . ? Co1 N1 C1 N2 171.9(3) . . . . ? C1 N1 C2 N3 0.6(6) . . . . ? Co1 N1 C2 N3 -171.0(3) . . . . ? N2 N3 C2 N1 -1.1(6) . . . . ? C3 N3 C2 N1 176.8(4) . . . . ? C2 N3 C3 C4 102.3(6) . . . . ? N2 N3 C3 C4 -80.0(5) . . . . ? N3 C3 C4 O1 -61.1(6) . . . . ? N3 C3 C4 C11 54.6(5) . . . . ? N3 C3 C4 C5 177.1(4) . . . . ? O1 C4 C5 C6 174.2(4) . . . . ? C3 C4 C5 C6 -64.5(6) . . . . ? C11 C4 C5 C6 58.8(6) . . . . ? O1 C4 C5 C10 -4.8(7) . . . . ? C3 C4 C5 C10 116.5(5) . . . . ? C11 C4 C5 C10 -120.2(5) . . . . ? C10 C5 C6 C7 -0.2(8) . . . . ? C4 C5 C6 C7 -179.3(5) . . . . ? C10 C5 C6 F1 179.1(5) . . . . ? C4 C5 C6 F1 0.0(7) . . . . ? F1 C6 C7 C8 180.0(5) . . . . ? C5 C6 C7 C8 -0.7(9) . . . . ? C6 C7 C8 F2 179.8(5) . . . . ? C6 C7 C8 C9 0.6(9) . . . . ? C7 C8 C9 C10 0.4(9) . . . . ? F2 C8 C9 C10 -178.9(5) . . . . ? C8 C9 C10 C5 -1.4(9) . . . . ? C6 C5 C10 C9 1.3(8) . . . . ? C4 C5 C10 C9 -179.6(5) . . . . ? C12 N5 C11 C4 75.7(6) . . . . ? N4 N5 C11 C4 -104.2(5) . . . . ? O1 C4 C11 N5 -69.5(5) . . . . ? C3 C4 C11 N5 171.0(4) . . . . ? C5 C4 C11 N5 50.3(5) . . . . ? C13 N6 C12 N5 0.4(6) . . . . ? Co1 N6 C12 N5 -179.9(3) 4_644 . . . ? N4 N5 C12 N6 -0.2(6) . . . . ? C11 N5 C12 N6 179.9(5) . . . . ? N5 N4 C13 N6 0.4(7) . . . . ? C12 N6 C13 N4 -0.5(7) . . . . ? Co1 N6 C13 N4 179.9(4) 4_644 . . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.844 _refine_diff_density_max 0.416 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.071