# ja994050j.cif [Cu2(bdpi)(CH3CN)2](ClO4)3_CH3CN_3H2O #------------------------------------------------------------------------------ _chemical_formula_weight 1192.25 _chemical_formula_sum 'C35 H44 Cl3 Cu2 N11 O15 ' #------------------------------------------------------------------------------ _cell_length_a 14.475(2) _cell_length_b 14.554(2) _cell_length_c 12.270(1) _cell_angle_alpha 108.474(8) _cell_angle_beta 107.348(8) _cell_angle_gamma 89.14(1) _cell_volume 2331.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 30.0 _cell_measurement_theta_max 37.7 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_density_diffrn 1.684 _exptl_crystal_F_000 1208.00 _exptl_absorpt_coefficient_mu 3.464 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.856 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -15.50 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 2 0 -3 3 1 -3 2 1 _diffrn_reflns_number 6033 _reflns_number_total 5761 _reflns_number_observed 5761 _reflns_observed_criterion >0.0sigma(I) _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.114 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 60.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03457 _diffrn_orient_matrix_UB_12 -0.01222 _diffrn_orient_matrix_UB_13 0.05418 _diffrn_orient_matrix_UB_21 0.04497 _diffrn_orient_matrix_UB_22 0.05139 _diffrn_orient_matrix_UB_23 0.07048 _diffrn_orient_matrix_UB_31 -0.04540 _diffrn_orient_matrix_UB_32 0.04999 _diffrn_orient_matrix_UB_33 -0.01618 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 4 -1.965 0.589 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 34 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 80 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 84 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 22 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 6 0.364 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Cu(1) 0.0236(1) 0.2335(1) 0.9392(1) 0.0435(5) Uani d . 1.00 . Cu(2) 0.4546(1) 0.2419(1) 0.9513(1) 0.0421(5) Uani d . 1.00 . Cl(1) 0.1703(3) 0.4526(3) 0.7236(4) 0.077(1) Uani d . 1.00 . Cl(2) 0.3507(3) 0.3302(3) 1.3827(3) 0.065(1) Uani d . 1.00 . Cl(3) 0.8279(3) 0.1500(3) 0.3382(3) 0.074(1) Uani d . 1.00 . O(1) 0.112(2) 0.516(2) 0.721(4) 0.57(2) Uani d . 1.00 . O(2) 0.168(2) 0.430(3) 0.815(2) 0.37(2) Uani d . 1.00 . O(3) 0.140(1) 0.369(1) 0.627(1) 0.174(6) Uani d . 1.00 . O(4) 0.264(1) 0.490(1) 0.752(1) 0.164(6) Uani d . 1.00 . O(5) 0.275(1) 0.296(2) 1.288(2) 0.31(1) Uani d . 1.00 . O(6) 0.318(1) 0.359(2) 1.477(2) 0.29(1) Uani d . 1.00 . O(7) 0.391(3) 0.406(2) 1.389(5) 0.45(3) Uani d . 1.00 . O(8) 0.419(2) 0.272(2) 1.387(3) 0.33(2) Uani d . 1.00 . O(9) 0.835(1) 0.245(1) 0.399(2) 0.179(7) Uani d . 1.00 . O(10) 0.741(2) 0.121(2) 0.267(2) 0.30(1) Uani d . 1.00 . O(11) 0.848(1) 0.0960(9) 0.415(1) 0.149(6) Uani d . 1.00 . O(12) 0.884(2) 0.130(2) 0.264(2) 0.25(1) Uani d . 1.00 . O(13) 0.6437(8) 0.060(2) 0.5477(9) 0.159(6) Uani d . 1.00 . O(14) 0.638(1) 0.193(3) 0.543(2) 0.26(1) Uani d . 1.00 . O(15) 0.114(2) 0.164(1) 0.490(1) 0.198(9) Uani d . 1.00 . N(1) 0.1612(6) 0.2180(6) 0.9379(7) 0.039(2) Uani d . 1.00 . N(2) 0.3145(6) 0.2243(6) 0.9408(6) 0.039(2) Uani d . 1.00 . N(3) -0.0063(6) 0.1695(6) 0.7575(7) 0.041(2) Uani d . 1.00 . N(4) 0.4015(6) 0.1849(6) 0.7689(7) 0.039(2) Uani d . 1.00 . N(5) -0.0529(6) 0.3423(7) 0.8854(8) 0.046(3) Uani d . 1.00 . N(6) 0.5368(6) 0.1203(6) 0.9269(8) 0.043(3) Uani d . 1.00 . N(7) -0.0698(6) 0.1153(6) 0.9158(8) 0.046(3) Uani d . 1.00 . N(8) 0.5094(6) 0.3515(6) 0.9092(8) 0.044(3) Uani d . 1.00 . N(9) 0.0445(7) 0.2932(7) 1.1160(8) 0.054(3) Uani d . 1.00 . N(10) 0.5175(7) 0.2987(6) 1.1276(8) 0.049(3) Uani d . 1.00 . N(11) -0.284(1) 0.231(1) 0.844(1) 0.103(5) Uani d . 1.00 . C(1) 0.2534(7) 0.2529(7) 1.0045(8) 0.035(3) Uani d . 1.00 . C(2) 0.1666(7) 0.1623(7) 0.8257(8) 0.039(3) Uani d . 1.00 . C(3) 0.2603(7) 0.1672(7) 0.8275(8) 0.038(3) Uani d . 1.00 . C(4) 0.0729(7) 0.1104(8) 0.7329(9) 0.044(3) Uani d . 1.00 . C(5) 0.3109(8) 0.1221(8) 0.7366(9) 0.046(3) Uani d . 1.00 . C(6) -0.0150(9) 0.2517(9) 0.7077(9) 0.051(3) Uani d . 1.00 . C(7) 0.4751(7) 0.1267(8) 0.7258(9) 0.046(3) Uani d . 1.00 . C(8) -0.0651(8) 0.3299(8) 0.769(1) 0.045(3) Uani d . 1.00 . C(9) 0.5249(8) 0.0732(8) 0.813(1) 0.048(3) Uani d . 1.00 . C(10) -0.123(1) 0.390(1) 0.712(1) 0.065(4) Uani d . 1.00 . C(11) 0.555(1) -0.017(1) 0.772(1) 0.067(5) Uani d . 1.00 . C(12) -0.1620(9) 0.464(1) 0.778(2) 0.073(5) Uani d . 1.00 . C(13) 0.6043(9) -0.0608(10) 0.858(2) 0.078(5) Uani d . 1.00 . C(14) -0.147(1) 0.480(1) 0.899(1) 0.073(5) Uani d . 1.00 . C(15) 0.6214(9) -0.007(1) 0.979(1) 0.059(4) Uani d . 1.00 . C(16) -0.0921(10) 0.4163(9) 0.949(1) 0.055(4) Uani d . 1.00 . C(17) 0.5870(8) 0.0812(10) 1.011(1) 0.052(4) Uani d . 1.00 . C(18) -0.1011(8) 0.1102(8) 0.7111(9) 0.048(3) Uani d . 1.00 . C(19) 0.3847(8) 0.2705(9) 0.7237(10) 0.052(4) Uani d . 1.00 . C(20) -0.1105(8) 0.0624(8) 0.7991(10) 0.050(3) Uani d . 1.00 . C(21) 0.4694(8) 0.3442(8) 0.7924(10) 0.049(3) Uani d . 1.00 . C(22) -0.1592(8) -0.0280(9) 0.766(1) 0.062(4) Uani d . 1.00 . C(23) 0.4989(9) 0.4053(9) 0.742(1) 0.060(4) Uani d . 1.00 . C(24) -0.1713(9) -0.0609(10) 0.854(1) 0.071(5) Uani d . 1.00 . C(25) 0.5760(9) 0.4757(10) 0.814(1) 0.066(5) Uani d . 1.00 . C(26) -0.1318(8) -0.005(1) 0.973(1) 0.065(5) Uani d . 1.00 . C(27) 0.6160(8) 0.4846(8) 0.932(1) 0.052(3) Uani d . 1.00 . C(28) -0.0806(8) 0.0828(8) 1.0042(10) 0.048(3) Uani d . 1.00 . C(29) 0.5816(7) 0.4212(8) 0.9772(10) 0.049(3) Uani d . 1.00 . C(30) 0.0515(9) 0.3196(9) 1.213(1) 0.054(4) Uani d . 1.00 . C(31) 0.5612(8) 0.3327(8) 1.2241(10) 0.048(3) Uani d . 1.00 . C(32) 0.059(1) 0.357(1) 1.341(1) 0.084(5) Uani d . 1.00 . C(33) 0.620(1) 0.380(1) 1.3511(9) 0.074(4) Uani d . 1.00 . C(34) -0.2594(10) 0.246(1) 0.938(2) 0.073(5) Uani d . 1.00 . C(35) -0.231(1) 0.268(1) 1.072(1) 0.090(6) Uani d . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0389(9) 0.051(1) 0.0371(8) -0.0009(8) 0.0143(7) 0.0064(7) Cu(2) 0.0352(9) 0.052(1) 0.0333(8) -0.0017(8) 0.0081(6) 0.0073(7) Cl(1) 0.065(2) 0.061(2) 0.090(3) -0.009(2) 0.025(2) 0.002(2) Cl(2) 0.064(2) 0.077(2) 0.044(2) 0.001(2) 0.011(1) 0.010(1) Cl(3) 0.097(3) 0.067(2) 0.048(2) 0.001(2) 0.016(2) 0.011(2) O(1) 0.25(3) 0.17(2) 0.97(8) 0.12(2) -0.17(4) 0.12(4) O(2) 0.38(4) 0.50(5) 0.13(1) -0.32(4) 0.15(2) -0.10(2) O(3) 0.24(2) 0.18(1) 0.074(8) -0.11(1) 0.056(9) -0.021(8) O(4) 0.11(1) 0.19(1) 0.16(1) -0.07(1) 0.048(9) 0.00(1) O(5) 0.15(2) 0.49(4) 0.12(1) 0.03(2) -0.01(1) -0.07(2) O(6) 0.14(2) 0.60(5) 0.13(1) 0.01(2) 0.05(1) 0.13(2) O(7) 0.48(6) 0.25(3) 0.75(8) -0.03(4) 0.38(6) 0.18(4) O(8) 0.17(2) 0.20(2) 0.58(5) 0.11(2) 0.10(3) 0.09(3) O(9) 0.23(2) 0.10(1) 0.17(1) 0.03(1) 0.07(1) -0.005(10) O(10) 0.25(2) 0.34(3) 0.21(2) -0.15(2) -0.15(2) 0.13(2) O(11) 0.25(2) 0.109(10) 0.096(9) 0.02(1) 0.06(1) 0.046(8) O(12) 0.39(3) 0.27(2) 0.23(2) 0.16(2) 0.25(3) 0.15(2) O(13) 0.064(7) 0.31(2) 0.046(6) 0.00(1) 0.004(5) -0.004(9) O(14) 0.12(1) 0.53(4) 0.12(1) 0.05(2) 0.05(1) 0.08(2) O(15) 0.27(2) 0.22(2) 0.14(1) 0.11(2) 0.11(1) 0.07(1) N(1) 0.037(5) 0.037(5) 0.043(5) -0.002(4) 0.013(4) 0.013(4) N(2) 0.033(5) 0.048(5) 0.026(4) -0.013(4) 0.004(4) 0.005(4) N(3) 0.033(5) 0.041(5) 0.035(4) -0.009(4) 0.004(4) -0.003(4) N(4) 0.034(5) 0.041(5) 0.038(4) 0.001(4) 0.017(4) 0.001(4) N(5) 0.035(5) 0.045(6) 0.060(6) 0.007(5) 0.018(4) 0.019(5) N(6) 0.035(5) 0.040(5) 0.046(5) 0.007(4) 0.013(4) 0.004(4) N(7) 0.038(5) 0.046(6) 0.060(6) 0.011(5) 0.022(4) 0.020(5) N(8) 0.038(5) 0.036(5) 0.051(5) 0.007(4) 0.013(4) 0.006(4) N(9) 0.051(6) 0.070(7) 0.041(5) 0.009(5) 0.022(4) 0.011(5) N(10) 0.046(6) 0.046(6) 0.039(5) -0.003(5) 0.004(4) 0.002(4) N(11) 0.058(9) 0.12(1) 0.10(1) -0.007(8) 0.007(8) 0.01(1) C(1) 0.036(6) 0.042(6) 0.024(4) -0.005(5) 0.005(4) 0.010(4) C(2) 0.039(6) 0.038(6) 0.032(5) -0.002(5) 0.009(5) 0.002(4) C(3) 0.036(6) 0.043(6) 0.032(5) -0.004(5) 0.011(4) 0.006(4) C(4) 0.037(6) 0.036(6) 0.053(6) 0.009(5) 0.022(5) 0.000(5) C(5) 0.044(6) 0.050(7) 0.035(5) -0.005(6) 0.010(5) 0.006(5) C(6) 0.061(8) 0.059(8) 0.038(6) -0.001(6) 0.018(5) 0.019(5) C(7) 0.036(6) 0.057(7) 0.041(6) -0.004(6) 0.013(5) 0.007(5) C(8) 0.034(6) 0.041(7) 0.064(7) 0.009(6) 0.017(6) 0.020(6) C(9) 0.039(7) 0.036(7) 0.066(8) 0.000(6) 0.028(6) 0.002(6) C(10) 0.054(8) 0.071(10) 0.078(9) 0.009(8) 0.023(7) 0.031(8) C(11) 0.059(9) 0.054(9) 0.088(10) -0.004(7) 0.031(8) 0.014(8) C(12) 0.043(8) 0.059(10) 0.12(1) 0.015(7) 0.015(8) 0.043(9) C(13) 0.037(7) 0.045(8) 0.13(1) -0.005(7) 0.030(8) 0.001(9) C(14) 0.052(8) 0.063(10) 0.10(1) -0.016(8) 0.025(8) 0.013(9) C(15) 0.041(7) 0.057(9) 0.090(10) 0.014(7) 0.019(7) 0.041(8) C(16) 0.062(8) 0.040(7) 0.065(8) 0.001(7) 0.025(7) 0.012(6) C(17) 0.029(6) 0.055(9) 0.077(8) 0.007(6) 0.012(6) 0.033(7) C(18) 0.044(7) 0.051(7) 0.046(6) 0.000(6) 0.016(5) 0.009(5) C(19) 0.047(7) 0.061(8) 0.051(6) 0.008(6) 0.010(5) 0.026(6) C(20) 0.041(6) 0.052(7) 0.050(6) 0.000(6) 0.016(5) 0.004(5) C(21) 0.051(7) 0.054(7) 0.050(6) 0.009(6) 0.024(6) 0.019(6) C(22) 0.045(7) 0.051(8) 0.079(8) -0.012(6) 0.020(6) 0.005(6) C(23) 0.062(8) 0.070(9) 0.055(7) 0.010(7) 0.016(6) 0.031(7) C(24) 0.040(7) 0.057(9) 0.12(1) -0.008(7) 0.025(8) 0.026(8) C(25) 0.056(8) 0.068(9) 0.092(10) 0.013(7) 0.036(8) 0.037(8) C(26) 0.038(7) 0.08(1) 0.10(1) 0.015(7) 0.029(7) 0.066(9) C(27) 0.044(7) 0.035(6) 0.063(7) -0.004(6) 0.012(6) 0.000(5) C(28) 0.038(6) 0.056(7) 0.059(7) 0.010(6) 0.024(5) 0.023(6) C(29) 0.030(6) 0.048(7) 0.057(7) 0.002(6) 0.012(5) 0.002(5) C(30) 0.055(8) 0.061(8) 0.047(7) 0.004(6) 0.022(6) 0.012(6) C(31) 0.041(6) 0.055(7) 0.043(6) 0.001(6) 0.011(5) 0.010(6) C(32) 0.09(1) 0.12(1) 0.032(6) 0.026(10) 0.020(7) 0.015(7) C(33) 0.086(10) 0.084(10) 0.026(6) 0.003(8) -0.002(6) 0.002(6) C(34) 0.034(8) 0.046(8) 0.12(1) 0.001(7) 0.017(9) 0.014(9) C(35) 0.057(9) 0.12(1) 0.09(1) 0.002(9) 0.017(8) 0.03(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00903|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5761 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1558 _refine_ls_R_factor_obs 0.073(>2.0sigma(I)) _refine_ls_wR_factor_all 0.1506 _refine_ls_wR_factor_obs 0.109(>2.0sigma(I)) _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.02(>2.0sigma(I)) _refine_ls_shift/esd_max 2.4290 _refine_ls_shift/esd_mean 0.1030 _refine_diff_density_min -1.12 _refine_diff_density_max 0.86 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 2.006(8) 1_555 1_555 yes Cu(1) N(3) 2.037(8) 1_555 1_555 yes Cu(1) N(5) 2.085(10) 1_555 1_555 yes Cu(1) N(7) 2.096(9) 1_555 1_555 yes Cu(1) N(9) 1.993(9) 1_555 1_555 yes Cu(2) N(2) 2.008(8) 1_555 1_555 yes Cu(2) N(4) 2.026(8) 1_555 1_555 yes Cu(2) N(6) 2.111(9) 1_555 1_555 yes Cu(2) N(8) 2.060(9) 1_555 1_555 yes Cu(2) N(10) 1.977(9) 1_555 1_555 yes Cl(1) O(1) 1.25(2) 1_555 1_555 yes Cl(1) O(2) 1.28(3) 1_555 1_555 yes Cl(1) O(3) 1.37(1) 1_555 1_555 yes Cl(1) O(4) 1.37(1) 1_555 1_555 yes Cl(2) O(5) 1.30(2) 1_555 1_555 yes Cl(2) O(6) 1.33(2) 1_555 1_555 yes Cl(2) O(7) 1.22(3) 1_555 1_555 yes Cl(2) O(8) 1.29(2) 1_555 1_555 yes Cl(3) O(9) 1.33(1) 1_555 1_555 yes Cl(3) O(10) 1.29(2) 1_555 1_555 yes Cl(3) O(11) 1.38(1) 1_555 1_555 yes Cl(3) O(12) 1.35(2) 1_555 1_555 yes N(1) C(1) 1.35(1) 1_555 1_555 yes N(1) C(2) 1.38(1) 1_555 1_555 yes N(2) C(1) 1.33(1) 1_555 1_555 yes N(2) C(3) 1.37(1) 1_555 1_555 yes N(3) C(4) 1.47(1) 1_555 1_555 yes N(3) C(6) 1.49(1) 1_555 1_555 yes N(3) C(18) 1.49(1) 1_555 1_555 yes N(4) C(5) 1.49(1) 1_555 1_555 yes N(4) C(7) 1.47(1) 1_555 1_555 yes N(4) C(19) 1.51(1) 1_555 1_555 yes N(5) C(8) 1.34(1) 1_555 1_555 yes N(5) C(16) 1.34(1) 1_555 1_555 yes N(6) C(9) 1.30(1) 1_555 1_555 yes N(6) C(17) 1.35(1) 1_555 1_555 yes N(7) C(20) 1.34(1) 1_555 1_555 yes N(7) C(28) 1.36(1) 1_555 1_555 yes N(8) C(21) 1.35(1) 1_555 1_555 yes N(8) C(29) 1.34(1) 1_555 1_555 yes N(9) C(30) 1.10(1) 1_555 1_555 yes N(10) C(31) 1.11(1) 1_555 1_555 yes N(11) C(34) 1.05(2) 1_555 1_555 yes C(2) C(3) 1.35(1) 1_555 1_555 yes C(2) C(4) 1.51(1) 1_555 1_555 yes C(3) C(5) 1.49(1) 1_555 1_555 yes C(6) C(8) 1.46(2) 1_555 1_555 yes C(7) C(9) 1.52(2) 1_555 1_555 yes C(8) C(10) 1.40(2) 1_555 1_555 yes C(9) C(11) 1.36(2) 1_555 1_555 yes C(10) C(12) 1.36(2) 1_555 1_555 yes C(11) C(13) 1.41(2) 1_555 1_555 yes C(12) C(14) 1.37(2) 1_555 1_555 yes C(13) C(15) 1.39(2) 1_555 1_555 yes C(14) C(16) 1.38(2) 1_555 1_555 yes C(15) C(17) 1.36(2) 1_555 1_555 yes C(18) C(20) 1.49(2) 1_555 1_555 yes C(19) C(21) 1.49(2) 1_555 1_555 yes C(20) C(22) 1.38(2) 1_555 1_555 yes C(21) C(23) 1.37(2) 1_555 1_555 yes C(22) C(24) 1.36(2) 1_555 1_555 yes C(23) C(25) 1.40(2) 1_555 1_555 yes C(24) C(26) 1.37(2) 1_555 1_555 yes C(25) C(27) 1.36(2) 1_555 1_555 yes C(26) C(28) 1.37(2) 1_555 1_555 yes C(27) C(29) 1.38(2) 1_555 1_555 yes C(30) C(32) 1.47(2) 1_555 1_555 yes C(31) C(33) 1.47(1) 1_555 1_555 yes C(34) C(35) 1.50(2) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(3) 82.7(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(5) 121.0(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(7) 121.7(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(9) 100.6(4) 1_555 1_555 1_555 yes N(3) Cu(1) N(5) 82.1(4) 1_555 1_555 1_555 yes N(3) Cu(1) N(7) 81.6(3) 1_555 1_555 1_555 yes N(3) Cu(1) N(9) 176.4(3) 1_555 1_555 1_555 yes N(5) Cu(1) N(7) 111.7(3) 1_555 1_555 1_555 yes N(5) Cu(1) N(9) 97.3(4) 1_555 1_555 1_555 yes N(7) Cu(1) N(9) 95.3(4) 1_555 1_555 1_555 yes N(2) Cu(2) N(4) 83.1(3) 1_555 1_555 1_555 yes N(2) Cu(2) N(6) 119.8(3) 1_555 1_555 1_555 yes N(2) Cu(2) N(8) 123.1(3) 1_555 1_555 1_555 yes N(2) Cu(2) N(10) 101.9(3) 1_555 1_555 1_555 yes N(4) Cu(2) N(6) 81.6(3) 1_555 1_555 1_555 yes N(4) Cu(2) N(8) 81.7(3) 1_555 1_555 1_555 yes N(4) Cu(2) N(10) 175.0(3) 1_555 1_555 1_555 yes N(6) Cu(2) N(8) 111.6(3) 1_555 1_555 1_555 yes N(6) Cu(2) N(10) 95.9(4) 1_555 1_555 1_555 yes N(8) Cu(2) N(10) 95.3(4) 1_555 1_555 1_555 yes O(1) Cl(1) O(2) 103(2) 1_555 1_555 1_555 yes O(1) Cl(1) O(3) 113(1) 1_555 1_555 1_555 yes O(1) Cl(1) O(4) 111(1) 1_555 1_555 1_555 yes O(2) Cl(1) O(3) 105(1) 1_555 1_555 1_555 yes O(2) Cl(1) O(4) 105(1) 1_555 1_555 1_555 yes O(3) Cl(1) O(4) 116.2(10) 1_555 1_555 1_555 yes O(5) Cl(2) O(6) 106(1) 1_555 1_555 1_555 yes O(5) Cl(2) O(7) 114(2) 1_555 1_555 1_555 yes O(5) Cl(2) O(8) 113(1) 1_555 1_555 1_555 yes O(6) Cl(2) O(7) 101(2) 1_555 1_555 1_555 yes O(6) Cl(2) O(8) 117(1) 1_555 1_555 1_555 yes O(7) Cl(2) O(8) 103(2) 1_555 1_555 1_555 yes O(9) Cl(3) O(10) 110(1) 1_555 1_555 1_555 yes O(9) Cl(3) O(11) 111.2(10) 1_555 1_555 1_555 yes O(9) Cl(3) O(12) 111(1) 1_555 1_555 1_555 yes O(10) Cl(3) O(11) 106(1) 1_555 1_555 1_555 yes O(10) Cl(3) O(12) 104(1) 1_555 1_555 1_555 yes O(11) Cl(3) O(12) 112(1) 1_555 1_555 1_555 yes Cu(1) N(1) C(1) 141.8(7) 1_555 1_555 1_555 yes Cu(1) N(1) C(2) 112.3(6) 1_555 1_555 1_555 yes C(1) N(1) C(2) 105.2(8) 1_555 1_555 1_555 yes Cu(2) N(2) C(1) 141.8(6) 1_555 1_555 1_555 yes Cu(2) N(2) C(3) 111.2(6) 1_555 1_555 1_555 yes C(1) N(2) C(3) 106.9(8) 1_555 1_555 1_555 yes Cu(1) N(3) C(4) 109.4(6) 1_555 1_555 1_555 yes Cu(1) N(3) C(6) 105.2(6) 1_555 1_555 1_555 yes Cu(1) N(3) C(18) 107.8(6) 1_555 1_555 1_555 yes C(4) N(3) C(6) 112.0(8) 1_555 1_555 1_555 yes C(4) N(3) C(18) 112.1(8) 1_555 1_555 1_555 yes C(6) N(3) C(18) 109.9(8) 1_555 1_555 1_555 yes Cu(2) N(4) C(5) 108.6(6) 1_555 1_555 1_555 yes Cu(2) N(4) C(7) 107.9(6) 1_555 1_555 1_555 yes Cu(2) N(4) C(19) 105.8(6) 1_555 1_555 1_555 yes C(5) N(4) C(7) 110.1(8) 1_555 1_555 1_555 yes C(5) N(4) C(19) 112.9(8) 1_555 1_555 1_555 yes C(7) N(4) C(19) 111.3(8) 1_555 1_555 1_555 yes Cu(1) N(5) C(8) 111.5(8) 1_555 1_555 1_555 yes Cu(1) N(5) C(16) 129.2(9) 1_555 1_555 1_555 yes C(8) N(5) C(16) 119(1) 1_555 1_555 1_555 yes Cu(2) N(6) C(9) 112.4(8) 1_555 1_555 1_555 yes Cu(2) N(6) C(17) 128.0(8) 1_555 1_555 1_555 yes C(9) N(6) C(17) 118(1) 1_555 1_555 1_555 yes Cu(1) N(7) C(20) 112.7(7) 1_555 1_555 1_555 yes Cu(1) N(7) C(28) 126.6(7) 1_555 1_555 1_555 yes C(20) N(7) C(28) 120.1(9) 1_555 1_555 1_555 yes Cu(2) N(8) C(21) 112.3(7) 1_555 1_555 1_555 yes Cu(2) N(8) C(29) 129.7(8) 1_555 1_555 1_555 yes C(21) N(8) C(29) 117.7(10) 1_555 1_555 1_555 yes Cu(1) N(9) C(30) 174(1) 1_555 1_555 1_555 yes Cu(2) N(10) C(31) 172.8(9) 1_555 1_555 1_555 yes N(1) C(1) N(2) 111.6(8) 1_555 1_555 1_555 yes N(1) C(2) C(3) 108.6(8) 1_555 1_555 1_555 yes N(1) C(2) C(4) 116.7(8) 1_555 1_555 1_555 yes C(3) C(2) C(4) 134.7(9) 1_555 1_555 1_555 yes N(2) C(3) C(2) 107.8(8) 1_555 1_555 1_555 yes N(2) C(3) C(5) 118.7(8) 1_555 1_555 1_555 yes C(2) C(3) C(5) 133.5(9) 1_555 1_555 1_555 yes N(3) C(4) C(2) 107.7(8) 1_555 1_555 1_555 yes N(4) C(5) C(3) 107.6(8) 1_555 1_555 1_555 yes N(3) C(6) C(8) 111.8(9) 1_555 1_555 1_555 yes N(4) C(7) C(9) 110.1(8) 1_555 1_555 1_555 yes N(5) C(8) C(6) 116(1) 1_555 1_555 1_555 yes N(5) C(8) C(10) 120(1) 1_555 1_555 1_555 yes C(6) C(8) C(10) 123(1) 1_555 1_555 1_555 yes N(6) C(9) C(7) 115(1) 1_555 1_555 1_555 yes N(6) C(9) C(11) 124(1) 1_555 1_555 1_555 yes C(7) C(9) C(11) 120(1) 1_555 1_555 1_555 yes C(8) C(10) C(12) 119(1) 1_555 1_555 1_555 yes C(9) C(11) C(13) 117(1) 1_555 1_555 1_555 yes C(10) C(12) C(14) 120(1) 1_555 1_555 1_555 yes C(11) C(13) C(15) 117(1) 1_555 1_555 1_555 yes C(12) C(14) C(16) 117(1) 1_555 1_555 1_555 yes C(13) C(15) C(17) 120(1) 1_555 1_555 1_555 yes N(5) C(16) C(14) 123(1) 1_555 1_555 1_555 yes N(6) C(17) C(15) 121(1) 1_555 1_555 1_555 yes N(3) C(18) C(20) 110.4(9) 1_555 1_555 1_555 yes N(4) C(19) C(21) 108.5(9) 1_555 1_555 1_555 yes N(7) C(20) C(18) 114.9(9) 1_555 1_555 1_555 yes N(7) C(20) C(22) 121(1) 1_555 1_555 1_555 yes C(18) C(20) C(22) 123(1) 1_555 1_555 1_555 yes N(8) C(21) C(19) 115.4(9) 1_555 1_555 1_555 yes N(8) C(21) C(23) 122(1) 1_555 1_555 1_555 yes C(19) C(21) C(23) 121(1) 1_555 1_555 1_555 yes C(20) C(22) C(24) 119(1) 1_555 1_555 1_555 yes C(21) C(23) C(25) 118(1) 1_555 1_555 1_555 yes C(22) C(24) C(26) 119(1) 1_555 1_555 1_555 yes C(23) C(25) C(27) 119(1) 1_555 1_555 1_555 yes C(24) C(26) C(28) 120(1) 1_555 1_555 1_555 yes C(25) C(27) C(29) 118(1) 1_555 1_555 1_555 yes N(7) C(28) C(26) 119(1) 1_555 1_555 1_555 yes N(8) C(29) C(27) 122(1) 1_555 1_555 1_555 yes N(9) C(30) C(32) 178(1) 1_555 1_555 1_555 yes N(10) C(31) C(33) 178(1) 1_555 1_555 1_555 yes N(11) C(34) C(35) 176(1) 1_555 1_555 1_555 yes #===END [Cu(Me4bdpi)(H2O)2](ClO4)3_4H2O #------------------------------------------------------------------------------ _chemical_formula_weight 1079.24 _chemical_formula_sum 'C33 H49 Cl3 Cu2 N8 O18 ' #------------------------------------------------------------------------------ _cell_length_a 9.843(2) _cell_length_b 18.361(2) _cell_length_c 25.111(3) _cell_angle_alpha 90 _cell_angle_beta 97.84(2) _cell_angle_gamma 90 _cell_volume 4495(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.1 _cell_measurement_theta_max 24.3 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_density_diffrn 1.486 _exptl_crystal_F_000 2004.00 _exptl_absorpt_coefficient_mu 3.442 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.870 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.95 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 2 1 -1 3 -3 -2 2 2 _diffrn_reflns_number 8603 _reflns_number_total 8059 _reflns_number_observed 7792 _reflns_observed_criterion >0.0sigma(I) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.144 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 68.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01469 _diffrn_orient_matrix_UB_12 0.04744 _diffrn_orient_matrix_UB_13 0.01950 _diffrn_orient_matrix_UB_21 0.04310 _diffrn_orient_matrix_UB_22 0.02049 _diffrn_orient_matrix_UB_23 -0.03058 _diffrn_orient_matrix_UB_31 -0.09189 _diffrn_orient_matrix_UB_32 0.01720 _diffrn_orient_matrix_UB_33 -0.01735 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 8 -1.965 0.589 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 60 0.049 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 136 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 12 0.364 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Cu(1) 0.3617(2) 0.21606(7) 0.89089(5) 0.0601(4) Uani d . 1.00 . Cu(2) 0.6117(2) 0.27847(7) 0.68642(5) 0.0630(4) Uani d . 1.00 . Cl(1) 0.6918(3) 0.0793(1) 0.8878(1) 0.0778(9) Uani d . 1.00 . Cl(2) 0.2394(4) 0.0308(2) 0.7295(2) 0.108(1) Uani d . 1.00 . Cl(3) -0.2226(6) 0.0239(2) 0.5655(2) 0.117(2) Uani d . 1.00 . O(1) 0.3414(8) 0.1118(3) 0.8689(3) 0.072(2) Uani d . 1.00 . O(2) 0.554(1) 0.1799(4) 0.6614(3) 0.092(3) Uani d . 1.00 . O(3) 0.695(1) 0.1481(5) 0.9120(4) 0.118(4) Uani d . 1.00 . O(4) 0.685(1) 0.0908(6) 0.8327(4) 0.137(4) Uani d . 1.00 . O(5) 0.808(1) 0.0380(5) 0.9065(4) 0.109(3) Uani d . 1.00 . O(6) 0.576(1) 0.0402(5) 0.8957(7) 0.180(6) Uani d . 1.00 . O(7) 0.236(3) 0.1021(10) 0.719(2) 0.42(2) Uani d . 1.00 . O(8) 0.259(3) 0.027(3) 0.7787(10) 0.48(2) Uani d . 1.00 . O(9) 0.123(2) 0.002(1) 0.7155(7) 0.27(1) Uani d . 1.00 . O(10) 0.336(2) 0.002(1) 0.7034(8) 0.27(1) Uani d . 1.00 . O(11) -0.184(3) 0.0948(8) 0.5670(7) 0.26(1) Uani d . 1.00 . O(12) -0.349(3) 0.040(2) 0.544(1) 0.36(2) Uani d . 1.00 . O(13) -0.216(1) -0.0080(7) 0.6166(5) 0.149(5) Uani d . 1.00 . O(14) -0.143(3) -0.010(1) 0.5351(7) 0.27(1) Uani d . 1.00 . O(15) 0.363(9) 0.076(4) 0.520(6) 0.0(1) Uani d . 1.00 . O(16) 0.610(1) 0.0418(6) 0.6954(5) 0.142(5) Uani d . 1.00 . O(17) 0.346(3) 0.141(2) 0.600(2) 0.49(2) Uani d . 1.00 . O(18) 0.161(5) 0.065(2) 0.576(2) 0.48(3) Uani d . 1.00 . N(1) 0.4313(9) 0.2481(4) 0.8249(3) 0.056(2) Uani d . 1.00 . N(2) 0.5516(10) 0.2651(4) 0.7576(3) 0.065(2) Uani d . 1.00 . N(3) 0.4113(9) 0.3185(4) 0.9167(3) 0.062(2) Uani d . 1.00 . N(4) 0.6323(9) 0.3845(4) 0.7103(3) 0.062(2) Uani d . 1.00 . N(5) 0.156(1) 0.2608(5) 0.8937(3) 0.071(3) Uani d . 1.00 . N(6) 0.8351(10) 0.2876(5) 0.6965(4) 0.073(3) Uani d . 1.00 . N(7) 0.4315(9) 0.1949(4) 0.9717(3) 0.060(2) Uani d . 1.00 . N(8) 0.5456(10) 0.3307(4) 0.6140(3) 0.068(3) Uani d . 1.00 . C(1) 0.479(1) 0.2184(5) 0.7818(4) 0.064(3) Uani d . 1.00 . C(2) 0.478(1) 0.3181(4) 0.8279(3) 0.056(3) Uani d . 1.00 . C(3) 0.554(1) 0.3305(5) 0.7871(4) 0.059(3) Uani d . 1.00 . C(4) 0.429(1) 0.3661(5) 0.8695(4) 0.066(3) Uani d . 1.00 . C(5) 0.635(1) 0.3892(5) 0.7686(4) 0.064(3) Uani d . 1.00 . C(6) 0.298(1) 0.3485(5) 0.9435(4) 0.076(4) Uani d . 1.00 . C(7) 0.160(1) 0.3268(6) 0.9161(4) 0.073(4) Uani d . 1.00 . C(8) 0.045(2) 0.3701(8) 0.9153(6) 0.099(5) Uani d . 1.00 . C(9) -0.077(2) 0.343(1) 0.8922(8) 0.125(7) Uani d . 1.00 . C(10) -0.085(2) 0.278(1) 0.8704(7) 0.109(6) Uani d . 1.00 . C(11) 0.030(2) 0.2355(7) 0.8710(5) 0.087(4) Uani d . 1.00 . C(12) 0.028(2) 0.1624(9) 0.8461(6) 0.108(5) Uani d . 1.00 . C(13) 0.764(1) 0.4112(6) 0.6931(4) 0.072(3) Uani d . 1.00 . C(14) 0.873(1) 0.3576(6) 0.7035(4) 0.076(4) Uani d . 1.00 . C(15) 1.007(1) 0.3771(8) 0.7175(5) 0.090(5) Uani d . 1.00 . C(16) 1.106(2) 0.3250(9) 0.7272(6) 0.107(6) Uani d . 1.00 . C(17) 1.068(1) 0.2525(8) 0.7191(6) 0.100(5) Uani d . 1.00 . C(18) 0.932(2) 0.2366(7) 0.7050(6) 0.097(5) Uani d . 1.00 . C(19) 0.883(2) 0.1589(7) 0.6960(8) 0.125(6) Uani d . 1.00 . C(20) 0.539(1) 0.3096(6) 0.9523(4) 0.069(3) Uani d . 1.00 . C(21) 0.523(1) 0.2477(6) 0.9905(4) 0.072(3) Uani d . 1.00 . C(22) 0.595(1) 0.2428(7) 1.0407(4) 0.090(4) Uani d . 1.00 . C(23) 0.574(2) 0.1851(9) 1.0731(5) 0.109(5) Uani d . 1.00 . C(24) 0.480(2) 0.1350(7) 1.0558(4) 0.087(4) Uani d . 1.00 . C(25) 0.410(1) 0.1389(6) 1.0047(4) 0.074(3) Uani d . 1.00 . C(26) 0.304(2) 0.0843(6) 0.9853(5) 0.094(4) Uani d . 1.00 . C(27) 0.510(1) 0.4211(5) 0.6815(4) 0.074(3) Uani d . 1.00 . C(28) 0.486(1) 0.3945(5) 0.6249(4) 0.057(3) Uani d . 1.00 . C(29) 0.412(1) 0.4357(6) 0.5852(5) 0.088(4) Uani d . 1.00 . C(30) 0.392(2) 0.4082(8) 0.5336(5) 0.105(5) Uani d . 1.00 . C(31) 0.455(2) 0.3464(7) 0.5233(4) 0.091(4) Uani d . 1.00 . C(32) 0.531(1) 0.3078(6) 0.5641(4) 0.071(3) Uani d . 1.00 . C(33) 0.613(1) 0.2422(7) 0.5515(5) 0.090(4) Uani d . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.084(1) 0.0421(7) 0.0549(8) -0.0097(6) 0.0143(7) 0.0012(6) Cu(2) 0.096(1) 0.0437(7) 0.0499(8) -0.0001(7) 0.0131(7) 0.0014(6) Cl(1) 0.097(2) 0.058(1) 0.075(2) 0.012(1) 0.000(1) -0.003(1) Cl(2) 0.090(3) 0.091(2) 0.140(3) 0.004(2) 0.000(2) -0.030(2) Cl(3) 0.158(4) 0.097(3) 0.097(3) 0.029(3) 0.018(2) 0.030(2) O(1) 0.099(6) 0.050(3) 0.065(4) -0.021(3) 0.008(4) -0.006(3) O(2) 0.159(8) 0.049(4) 0.067(5) -0.010(4) 0.008(5) -0.009(3) O(3) 0.155(9) 0.074(5) 0.127(8) 0.011(6) 0.028(7) -0.035(5) O(4) 0.20(1) 0.129(8) 0.076(6) 0.046(8) -0.009(6) 0.005(6) O(5) 0.129(8) 0.099(6) 0.092(6) 0.040(6) -0.011(5) -0.019(5) O(6) 0.099(8) 0.081(7) 0.37(2) -0.010(6) 0.06(1) 0.071(10) O(7) 0.30(3) 0.10(1) 0.89(8) 0.04(1) 0.22(4) 0.03(2) O(8) 0.29(3) 0.93(10) 0.21(2) -0.12(4) -0.01(2) -0.34(4) O(9) 0.34(3) 0.29(2) 0.21(2) -0.22(2) 0.13(2) -0.11(2) O(10) 0.23(2) 0.35(3) 0.26(2) 0.15(2) 0.13(2) 0.15(2) O(11) 0.53(4) 0.11(1) 0.16(1) 0.06(2) 0.05(2) 0.049(9) O(12) 0.23(2) 0.35(4) 0.45(4) 0.06(2) -0.13(3) 0.06(3) O(13) 0.19(1) 0.140(10) 0.115(8) -0.006(9) 0.021(8) 0.045(7) O(14) 0.47(4) 0.19(2) 0.19(2) 0.17(2) 0.15(2) 0.03(1) O(15) 1.1(2) 1.0(2) 3.2(5) 0.7(1) 1.7(3) 1.5(2) O(16) 0.17(1) 0.099(7) 0.16(1) 0.000(7) 0.021(8) 0.027(7) O(17) 0.30(3) 0.27(3) 0.77(7) -0.13(2) -0.33(4) 0.29(4) O(18) 0.71(8) 0.36(4) 0.37(5) -0.02(5) 0.03(5) -0.04(4) N(1) 0.080(6) 0.041(3) 0.050(4) 0.000(4) 0.015(4) 0.009(3) N(2) 0.094(7) 0.043(4) 0.055(4) -0.003(4) 0.001(4) 0.002(3) N(3) 0.094(6) 0.043(4) 0.052(4) -0.013(4) 0.017(4) 0.002(3) N(4) 0.090(6) 0.051(4) 0.047(4) -0.001(4) 0.016(4) 0.015(3) N(5) 0.089(7) 0.067(5) 0.060(5) 0.003(5) 0.019(5) 0.007(4) N(6) 0.081(6) 0.062(5) 0.074(6) 0.011(5) 0.006(5) -0.001(4) N(7) 0.082(6) 0.049(4) 0.051(4) -0.011(4) 0.022(4) -0.001(3) N(8) 0.101(7) 0.060(5) 0.040(4) 0.014(4) 0.001(4) 0.009(3) C(1) 0.097(8) 0.039(4) 0.053(5) -0.012(5) 0.006(5) 0.000(4) C(2) 0.092(7) 0.042(4) 0.037(4) -0.005(4) 0.019(4) 0.005(3) C(3) 0.081(7) 0.044(5) 0.050(5) 0.002(4) -0.002(5) 0.000(4) C(4) 0.103(8) 0.039(4) 0.060(5) -0.003(5) 0.024(5) 0.000(4) C(5) 0.094(8) 0.050(5) 0.047(5) -0.017(5) 0.003(5) 0.007(4) C(6) 0.114(10) 0.047(5) 0.077(7) 0.003(6) 0.050(7) 0.002(5) C(7) 0.093(9) 0.067(6) 0.065(6) -0.008(6) 0.034(6) 0.016(5) C(8) 0.12(1) 0.089(9) 0.10(1) 0.041(9) 0.054(9) 0.018(8) C(9) 0.12(1) 0.12(1) 0.14(1) 0.02(1) 0.02(1) 0.04(1) C(10) 0.08(1) 0.13(1) 0.12(1) 0.021(10) 0.015(8) 0.04(1) C(11) 0.10(1) 0.077(8) 0.078(7) -0.018(7) 0.004(7) 0.015(6) C(12) 0.10(1) 0.12(1) 0.10(1) -0.014(9) -0.001(8) 0.015(9) C(13) 0.098(9) 0.062(6) 0.057(6) -0.005(6) 0.010(5) 0.012(5) C(14) 0.093(9) 0.076(7) 0.058(6) -0.018(6) 0.008(6) 0.004(5) C(15) 0.082(9) 0.094(9) 0.094(9) -0.014(8) 0.014(7) -0.007(7) C(16) 0.079(10) 0.12(1) 0.12(1) -0.033(9) 0.022(8) -0.002(10) C(17) 0.067(9) 0.104(10) 0.13(1) 0.003(7) 0.000(8) 0.002(9) C(18) 0.10(1) 0.076(8) 0.11(1) 0.001(7) -0.005(8) -0.006(7) C(19) 0.12(1) 0.071(8) 0.17(2) 0.024(8) -0.01(1) -0.005(9) C(20) 0.096(8) 0.060(5) 0.053(5) -0.012(5) 0.019(5) -0.004(4) C(21) 0.088(8) 0.072(6) 0.056(6) -0.015(6) 0.018(5) -0.010(5) C(22) 0.12(1) 0.095(8) 0.051(6) -0.017(8) -0.001(6) 0.003(6) C(23) 0.14(1) 0.12(1) 0.059(7) 0.01(1) 0.003(8) 0.009(8) C(24) 0.13(1) 0.081(8) 0.047(6) -0.007(8) 0.012(6) 0.010(5) C(25) 0.105(9) 0.058(6) 0.065(6) -0.001(6) 0.036(6) 0.012(5) C(26) 0.14(1) 0.068(7) 0.079(7) -0.029(7) 0.040(8) 0.008(6) C(27) 0.113(9) 0.049(5) 0.062(6) 0.001(6) 0.022(6) 0.010(5) C(28) 0.067(6) 0.051(5) 0.053(5) -0.004(4) 0.003(4) 0.014(4) C(29) 0.11(1) 0.071(7) 0.071(7) 0.011(7) -0.023(6) -0.007(6) C(30) 0.13(1) 0.11(1) 0.067(7) 0.041(9) -0.005(7) 0.016(7) C(31) 0.12(1) 0.088(8) 0.054(6) 0.014(8) -0.009(6) -0.017(6) C(32) 0.078(8) 0.067(6) 0.068(6) -0.003(5) 0.009(5) 0.009(5) C(33) 0.11(1) 0.086(8) 0.078(7) -0.002(7) 0.034(7) -0.019(6) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00903|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7792 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1907 _refine_ls_R_factor_obs 0.0838(>2.0sigma(I)) _refine_ls_wR_factor_all 0.1865 _refine_ls_wR_factor_obs 0.1321(>2.0sigma(I)) _refine_ls_goodness_of_fit_all 1.135 _refine_ls_goodness_of_fit_obs 1.21(>2.0sigma(I)) _refine_ls_shift/esd_max 2.0700 _refine_ls_shift/esd_mean 0.1120 _refine_diff_density_min -0.81 _refine_diff_density_max 0.83 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) O(1) 1.995(6) 1_555 1_555 yes Cu(1) N(1) 1.968(7) 1_555 1_555 yes Cu(1) N(3) 2.027(7) 1_555 1_555 yes Cu(1) N(5) 2.089(8) 1_555 1_555 yes Cu(1) N(7) 2.197(10) 1_555 1_555 yes Cu(2) O(2) 1.973(7) 1_555 1_555 yes Cu(2) N(2) 1.973(8) 1_555 1_555 yes Cu(2) N(4) 2.039(8) 1_555 1_555 yes Cu(2) N(6) 2.186(10) 1_555 1_555 yes Cu(2) N(8) 2.080(7) 1_555 1_555 yes Cl(1) O(3) 1.400(8) 1_555 1_555 yes Cl(1) O(4) 1.394(10) 1_555 1_555 yes Cl(1) O(5) 1.400(9) 1_555 1_555 yes Cl(1) O(6) 1.38(1) 1_555 1_555 yes Cl(2) O(7) 1.33(2) 1_555 1_555 yes Cl(2) O(8) 1.23(3) 1_555 1_555 yes Cl(2) O(9) 1.26(2) 1_555 1_555 yes Cl(2) O(10) 1.33(2) 1_555 1_555 yes Cl(3) O(11) 1.36(2) 1_555 1_555 yes Cl(3) O(12) 1.32(2) 1_555 1_555 yes Cl(3) O(13) 1.40(1) 1_555 1_555 yes Cl(3) O(14) 1.32(2) 1_555 1_555 yes N(1) C(1) 1.35(1) 1_555 1_555 yes N(1) C(2) 1.36(1) 1_555 1_555 yes N(2) C(1) 1.32(1) 1_555 1_555 yes N(2) C(3) 1.41(1) 1_555 1_555 yes N(3) C(4) 1.50(1) 1_555 1_555 yes N(3) C(6) 1.48(1) 1_555 1_555 yes N(3) C(20) 1.45(1) 1_555 1_555 yes N(4) C(5) 1.46(1) 1_555 1_555 yes N(4) C(13) 1.50(1) 1_555 1_555 yes N(4) C(27) 1.48(1) 1_555 1_555 yes N(5) C(7) 1.34(1) 1_555 1_555 yes N(5) C(11) 1.37(2) 1_555 1_555 yes N(6) C(14) 1.34(1) 1_555 1_555 yes N(6) C(18) 1.33(2) 1_555 1_555 yes N(7) C(21) 1.36(1) 1_555 1_555 yes N(7) C(25) 1.36(1) 1_555 1_555 yes N(8) C(28) 1.35(1) 1_555 1_555 yes N(8) C(32) 1.31(1) 1_555 1_555 yes C(1) H(35) 0.942 1_555 1_555 no C(2) C(3) 1.37(1) 1_555 1_555 yes C(2) C(4) 1.50(1) 1_555 1_555 yes C(3) C(5) 1.45(1) 1_555 1_555 yes C(6) C(7) 1.49(2) 1_555 1_555 yes C(7) C(8) 1.38(2) 1_555 1_555 yes C(8) C(9) 1.35(2) 1_555 1_555 yes C(9) C(10) 1.31(2) 1_555 1_555 yes C(10) C(11) 1.37(2) 1_555 1_555 yes C(11) C(12) 1.48(2) 1_555 1_555 yes C(13) C(14) 1.46(2) 1_555 1_555 yes C(14) C(15) 1.36(2) 1_555 1_555 yes C(15) C(16) 1.36(2) 1_555 1_555 yes C(16) C(17) 1.39(2) 1_555 1_555 yes C(17) C(18) 1.37(2) 1_555 1_555 yes C(18) C(19) 1.51(2) 1_555 1_555 yes C(20) C(21) 1.51(1) 1_555 1_555 yes C(21) C(22) 1.36(2) 1_555 1_555 yes C(22) C(23) 1.37(2) 1_555 1_555 yes C(23) C(24) 1.34(2) 1_555 1_555 yes C(24) C(25) 1.37(2) 1_555 1_555 yes C(25) C(26) 1.48(2) 1_555 1_555 yes C(27) C(28) 1.49(1) 1_555 1_555 yes C(28) C(29) 1.38(1) 1_555 1_555 yes C(29) C(30) 1.38(2) 1_555 1_555 yes C(30) C(31) 1.33(2) 1_555 1_555 yes C(31) C(32) 1.38(2) 1_555 1_555 yes C(32) C(33) 1.51(2) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Cu(1) N(1) 95.0(3) 1_555 1_555 1_555 yes O(1) Cu(1) N(3) 171.7(4) 1_555 1_555 1_555 yes O(1) Cu(1) N(5) 108.0(3) 1_555 1_555 1_555 yes O(1) Cu(1) N(7) 95.6(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(3) 84.0(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(5) 110.1(3) 1_555 1_555 1_555 yes N(1) Cu(1) N(7) 140.2(3) 1_555 1_555 1_555 yes N(3) Cu(1) N(5) 80.0(4) 1_555 1_555 1_555 yes N(3) Cu(1) N(7) 80.1(3) 1_555 1_555 1_555 yes N(5) Cu(1) N(7) 102.8(3) 1_555 1_555 1_555 yes O(2) Cu(2) N(2) 93.8(3) 1_555 1_555 1_555 yes O(2) Cu(2) N(4) 169.2(4) 1_555 1_555 1_555 yes O(2) Cu(2) N(6) 110.3(4) 1_555 1_555 1_555 yes O(2) Cu(2) N(8) 96.0(3) 1_555 1_555 1_555 yes N(2) Cu(2) N(4) 83.2(3) 1_555 1_555 1_555 yes N(2) Cu(2) N(6) 109.0(4) 1_555 1_555 1_555 yes N(2) Cu(2) N(8) 138.8(4) 1_555 1_555 1_555 yes N(4) Cu(2) N(6) 80.5(3) 1_555 1_555 1_555 yes N(4) Cu(2) N(8) 79.8(3) 1_555 1_555 1_555 yes N(6) Cu(2) N(8) 104.8(3) 1_555 1_555 1_555 yes O(3) Cl(1) O(4) 106.8(6) 1_555 1_555 1_555 yes O(3) Cl(1) O(5) 112.0(6) 1_555 1_555 1_555 yes O(3) Cl(1) O(6) 112.1(8) 1_555 1_555 1_555 yes O(4) Cl(1) O(5) 109.8(6) 1_555 1_555 1_555 yes O(4) Cl(1) O(6) 107.1(9) 1_555 1_555 1_555 yes O(5) Cl(1) O(6) 108.7(7) 1_555 1_555 1_555 yes O(7) Cl(2) O(8) 104(2) 1_555 1_555 1_555 yes O(7) Cl(2) O(9) 110(1) 1_555 1_555 1_555 yes O(7) Cl(2) O(10) 106(1) 1_555 1_555 1_555 yes O(8) Cl(2) O(9) 105(1) 1_555 1_555 1_555 yes O(8) Cl(2) O(10) 116(1) 1_555 1_555 1_555 yes O(9) Cl(2) O(10) 112(1) 1_555 1_555 1_555 yes O(11) Cl(3) O(12) 92(1) 1_555 1_555 1_555 yes O(11) Cl(3) O(13) 113.4(10) 1_555 1_555 1_555 yes O(11) Cl(3) O(14) 106(1) 1_555 1_555 1_555 yes O(12) Cl(3) O(13) 113(1) 1_555 1_555 1_555 yes O(12) Cl(3) O(14) 117(2) 1_555 1_555 1_555 yes O(13) Cl(3) O(14) 112(1) 1_555 1_555 1_555 yes Cu(1) N(1) C(1) 138.8(6) 1_555 1_555 1_555 yes Cu(1) N(1) C(2) 112.9(6) 1_555 1_555 1_555 yes C(1) N(1) C(2) 105.8(7) 1_555 1_555 1_555 yes Cu(2) N(2) C(1) 138.3(6) 1_555 1_555 1_555 yes Cu(2) N(2) C(3) 112.7(6) 1_555 1_555 1_555 yes C(1) N(2) C(3) 106.4(8) 1_555 1_555 1_555 yes Cu(1) N(3) C(4) 109.6(5) 1_555 1_555 1_555 yes Cu(1) N(3) C(6) 109.1(6) 1_555 1_555 1_555 yes Cu(1) N(3) C(20) 104.1(6) 1_555 1_555 1_555 yes C(4) N(3) C(6) 108.4(7) 1_555 1_555 1_555 yes C(4) N(3) C(20) 111.6(8) 1_555 1_555 1_555 yes C(6) N(3) C(20) 113.9(8) 1_555 1_555 1_555 yes Cu(2) N(4) C(5) 109.7(5) 1_555 1_555 1_555 yes Cu(2) N(4) C(13) 106.4(6) 1_555 1_555 1_555 yes Cu(2) N(4) C(27) 104.4(6) 1_555 1_555 1_555 yes C(5) N(4) C(13) 111.9(8) 1_555 1_555 1_555 yes C(5) N(4) C(27) 111.4(8) 1_555 1_555 1_555 yes C(13) N(4) C(27) 112.7(7) 1_555 1_555 1_555 yes Cu(1) N(5) C(7) 111.9(8) 1_555 1_555 1_555 yes Cu(1) N(5) C(11) 130.2(8) 1_555 1_555 1_555 yes C(7) N(5) C(11) 117(1) 1_555 1_555 1_555 yes Cu(2) N(6) C(14) 110.4(8) 1_555 1_555 1_555 yes Cu(2) N(6) C(18) 130.5(9) 1_555 1_555 1_555 yes C(14) N(6) C(18) 118(1) 1_555 1_555 1_555 yes Cu(1) N(7) C(21) 108.5(6) 1_555 1_555 1_555 yes Cu(1) N(7) C(25) 132.5(7) 1_555 1_555 1_555 yes C(21) N(7) C(25) 118.8(9) 1_555 1_555 1_555 yes Cu(2) N(8) C(28) 108.3(6) 1_555 1_555 1_555 yes Cu(2) N(8) C(32) 131.9(7) 1_555 1_555 1_555 yes C(28) N(8) C(32) 118.4(8) 1_555 1_555 1_555 yes N(1) C(1) N(2) 112.1(7) 1_555 1_555 1_555 yes N(1) C(2) C(3) 109.3(7) 1_555 1_555 1_555 yes N(1) C(2) C(4) 117.0(7) 1_555 1_555 1_555 yes C(3) C(2) C(4) 133.4(8) 1_555 1_555 1_555 yes N(2) C(3) C(2) 106.3(8) 1_555 1_555 1_555 yes N(2) C(3) C(5) 115.7(8) 1_555 1_555 1_555 yes C(2) C(3) C(5) 137.9(8) 1_555 1_555 1_555 yes N(3) C(4) C(2) 106.9(7) 1_555 1_555 1_555 yes N(4) C(5) C(3) 110.0(8) 1_555 1_555 1_555 yes N(3) C(6) C(7) 112.6(9) 1_555 1_555 1_555 yes N(5) C(7) C(6) 114(1) 1_555 1_555 1_555 yes N(5) C(7) C(8) 122(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 123(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 118(1) 1_555 1_555 1_555 yes C(8) C(9) C(10) 120(1) 1_555 1_555 1_555 yes C(9) C(10) C(11) 120(1) 1_555 1_555 1_555 yes N(5) C(11) C(10) 120(1) 1_555 1_555 1_555 yes N(5) C(11) C(12) 116(1) 1_555 1_555 1_555 yes C(10) C(11) C(12) 123(1) 1_555 1_555 1_555 yes N(4) C(13) C(14) 112.0(8) 1_555 1_555 1_555 yes N(6) C(14) C(13) 115(1) 1_555 1_555 1_555 yes N(6) C(14) C(15) 121(1) 1_555 1_555 1_555 yes C(13) C(14) C(15) 122(1) 1_555 1_555 1_555 yes C(14) C(15) C(16) 120(1) 1_555 1_555 1_555 yes C(15) C(16) C(17) 118(1) 1_555 1_555 1_555 yes C(16) C(17) C(18) 118(1) 1_555 1_555 1_555 yes N(6) C(18) C(17) 122(1) 1_555 1_555 1_555 yes N(6) C(18) C(19) 115(1) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121(1) 1_555 1_555 1_555 yes N(3) C(20) C(21) 108.6(9) 1_555 1_555 1_555 yes N(7) C(21) C(20) 116.0(9) 1_555 1_555 1_555 yes N(7) C(21) C(22) 120(1) 1_555 1_555 1_555 yes C(20) C(21) C(22) 123(1) 1_555 1_555 1_555 yes C(21) C(22) C(23) 119(1) 1_555 1_555 1_555 yes C(22) C(23) C(24) 119(1) 1_555 1_555 1_555 yes C(23) C(24) C(25) 120(1) 1_555 1_555 1_555 yes N(7) C(25) C(24) 120(1) 1_555 1_555 1_555 yes N(7) C(25) C(26) 118(1) 1_555 1_555 1_555 yes C(24) C(25) C(26) 121.0(10) 1_555 1_555 1_555 yes N(4) C(27) C(28) 109.5(8) 1_555 1_555 1_555 yes N(8) C(28) C(27) 117.2(8) 1_555 1_555 1_555 yes N(8) C(28) C(29) 121.9(9) 1_555 1_555 1_555 yes C(27) C(28) C(29) 120.8(9) 1_555 1_555 1_555 yes C(28) C(29) C(30) 118(1) 1_555 1_555 1_555 yes C(29) C(30) C(31) 119(1) 1_555 1_555 1_555 yes C(30) C(31) C(32) 120(1) 1_555 1_555 1_555 yes N(8) C(32) C(31) 121(1) 1_555 1_555 1_555 yes N(8) C(32) C(33) 117.6(10) 1_555 1_555 1_555 yes C(31) C(32) C(33) 120(1) 1_555 1_555 1_555 yes #===END [Cu(MeIm(Py)2)(CH3CN)](ClO4)2_CH3CN #------------------------------------------------------------------------------ _chemical_formula_weight 637.92 _chemical_formula_sum 'C21 H25 Cl2 Cu N7 O8 ' #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 14.861(5) _cell_length_b 10.784(5) _cell_length_c 35.597(4) _cell_angle_alpha 90 _cell_angle_beta 90.57(2) _cell_angle_gamma 90 _cell_volume 5704(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.9 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 7925 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_theta_max 25.08 _diffrn_measured_fraction_theta_max 0.7676 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.7676 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.64 #------------------------------------------------------------------------------ _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7786 _reflns_number_gt 2857 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1053 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2857 _refine_ls_number_parameters 704 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00616|Fo|^2^]' _refine_ls_shift/su_max 0.2925 _refine_diff_density_max 1.40 _refine_diff_density_min -1.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.8762(1) -0.3120(1) 0.33464(5) 0.0606(5) Uani 1.00 d . . . Cu(2) Cu 0.6242(1) 0.1563(2) 0.58411(4) 0.0597(5) Uani 1.00 d . . . Cl(1) Cl 0.8678(4) 0.1852(5) 0.9552(2) 0.112(2) Uani 1.00 d . . . Cl(2) Cl 1.1227(3) -0.2723(5) 0.5510(2) 0.097(2) Uani 1.00 d . . . Cl(3) Cl 1.1220(2) 0.2557(4) 0.2918(1) 0.068(1) Uani 1.00 d . . . Cl(4) Cl 0.3887(4) -0.2632(5) 0.6998(2) 0.103(2) Uani 1.00 d . . . O(1) O 0.922(2) 0.157(3) 0.9274(9) 0.36(2) Uani 1.00 d . . . O(2) O 0.900(2) 0.167(2) 0.9903(8) 0.34(2) Uani 1.00 d . . . O(3) O 0.849(2) 0.302(2) 0.9579(5) 0.27(1) Uani 1.00 d . . . O(4) O 0.806(1) 0.109(3) 0.9475(8) 0.32(2) Uani 1.00 d . . . O(5) O 1.146(1) -0.315(2) 0.5164(5) 0.216(10) Uani 1.00 d . . . O(6) O 1.198(1) -0.313(2) 0.5750(5) 0.183(8) Uani 1.00 d . . . O(7) O 1.116(1) -0.149(2) 0.5533(7) 0.213(9) Uani 1.00 d . . . O(8) O 1.0481(8) -0.332(1) 0.5647(5) 0.162(7) Uani 1.00 d . . . O(9) O 1.2032(8) 0.188(1) 0.2968(4) 0.132(5) Uani 1.00 d . . . O(10) O 1.101(1) 0.319(2) 0.3251(4) 0.182(8) Uani 1.00 d . . . O(11) O 1.1267(8) 0.3405(9) 0.2621(3) 0.100(4) Uani 1.00 d . . . O(12) O 1.0506(9) 0.172(1) 0.2839(4) 0.139(6) Uani 1.00 d . . . O(13) O 0.415(2) -0.371(2) 0.7173(6) 0.25(1) Uani 1.00 d . . . O(14) O 0.457(1) -0.189(2) 0.6961(7) 0.27(1) Uani 1.00 d . . . O(15) O 0.360(2) -0.286(3) 0.6655(6) 0.30(1) Uani 1.00 d . . . O(16) O 0.328(2) -0.217(3) 0.7206(8) 0.29(1) Uani 1.00 d . . . N(1) N 0.8774(8) -0.285(2) 0.4521(3) 0.087(5) Uani 1.00 d . . . N(2) N 0.8710(7) -0.295(1) 0.3909(3) 0.064(4) Uani 1.00 d . . . N(3) N 0.8817(7) -0.1240(9) 0.3377(3) 0.054(3) Uani 1.00 d . . . N(4) N 0.9966(7) -0.288(1) 0.3081(3) 0.059(4) Uani 1.00 d . . . N(5) N 0.7596(7) -0.279(1) 0.3039(3) 0.062(4) Uani 1.00 d . . . N(6) N 0.8725(7) -0.498(1) 0.3333(3) 0.071(4) Uani 1.00 d . . . N(7) N 0.6323(8) 0.450(1) 0.6607(4) 0.074(4) Uani 1.00 d . . . N(8) N 0.6219(7) 0.296(1) 0.6211(3) 0.061(4) Uani 1.00 d . . . N(9) N 0.6168(8) 0.049(1) 0.6307(3) 0.064(4) Uani 1.00 d . . . N(10) N 0.5100(6) 0.065(1) 0.5703(3) 0.060(4) Uani 1.00 d . . . N(11) N 0.7445(7) 0.063(1) 0.5777(4) 0.065(4) Uani 1.00 d . . . N(12) N 0.6303(9) 0.257(1) 0.5387(4) 0.088(5) Uani 1.00 d . . . N(13) N 0.871(2) 0.263(2) 0.1221(8) 0.15(1) Uani 1.00 d . . . N(14) N 0.375(1) 0.225(2) 0.1159(6) 0.154(9) Uani 1.00 d . . . C(1) C 0.8765(9) -0.359(1) 0.4206(5) 0.070(5) Uani 1.00 d . . . C(2) C 0.8682(10) -0.167(1) 0.4383(5) 0.076(6) Uani 1.00 d . . . C(3) C 0.865(1) -0.174(1) 0.4031(4) 0.087(6) Uani 1.00 d . . . C(4) C 0.891(2) -0.327(2) 0.4915(6) 0.143(9) Uani 1.00 d . . . C(5) C 0.832(1) -0.084(1) 0.3715(6) 0.131(8) Uani 1.00 d . . . C(6) C 0.972(1) -0.086(1) 0.3359(7) 0.127(8) Uani 1.00 d . . . C(7) C 1.0242(9) -0.168(1) 0.3093(4) 0.077(5) Uani 1.00 d . . . C(8) C 1.104(1) -0.133(1) 0.2909(5) 0.084(6) Uani 1.00 d . . . C(9) C 1.154(1) -0.219(2) 0.2738(5) 0.094(6) Uani 1.00 d . . . C(10) C 1.125(1) -0.340(2) 0.2733(5) 0.096(7) Uani 1.00 d . . . C(11) C 1.044(1) -0.369(1) 0.2902(5) 0.084(6) Uani 1.00 d . . . C(12) C 0.829(1) -0.078(1) 0.3038(6) 0.117(7) Uani 1.00 d . . . C(13) C 0.747(1) -0.160(1) 0.2976(5) 0.086(6) Uani 1.00 d . . . C(14) C 0.669(1) -0.117(1) 0.2803(5) 0.089(6) Uani 1.00 d . . . C(15) C 0.6053(9) -0.200(2) 0.2697(4) 0.075(5) Uani 1.00 d . . . C(16) C 0.619(1) -0.322(2) 0.2754(4) 0.082(6) Uani 1.00 d . . . C(17) C 0.698(1) -0.357(1) 0.2934(4) 0.068(5) Uani 1.00 d . . . C(18) C 0.8716(9) -0.601(1) 0.3341(4) 0.061(5) Uani 1.00 d . . . C(19) C 0.8684(10) -0.732(1) 0.3386(5) 0.082(5) Uani 1.00 d . . . C(20) C 0.6313(9) 0.415(2) 0.6248(5) 0.075(6) Uani 1.00 d . . . C(21) C 0.617(1) 0.347(2) 0.6804(5) 0.096(7) Uani 1.00 d . . . C(22) C 0.608(1) 0.256(2) 0.6569(5) 0.101(7) Uani 1.00 d . . . C(23) C 0.643(2) 0.575(2) 0.6734(6) 0.135(9) Uani 1.00 d . . . C(24) C 0.575(2) 0.122(2) 0.6605(6) 0.16(1) Uani 1.00 d . . . C(25) C 0.560(2) -0.053(2) 0.6214(6) 0.150(10) Uani 1.00 d . . . C(26) C 0.485(1) -0.025(2) 0.5949(5) 0.087(6) Uani 1.00 d . . . C(27) C 0.403(1) -0.089(2) 0.5916(6) 0.113(8) Uani 1.00 d . . . C(28) C 0.351(1) -0.062(2) 0.5620(7) 0.106(8) Uani 1.00 d . . . C(29) C 0.376(1) 0.023(2) 0.5369(5) 0.104(7) Uani 1.00 d . . . C(30) C 0.453(1) 0.082(1) 0.5427(4) 0.078(5) Uani 1.00 d . . . C(31) C 0.704(1) 0.021(3) 0.6418(7) 0.20(1) Uani 1.00 d . . . C(32) C 0.7631(10) -0.010(2) 0.6077(5) 0.094(6) Uani 1.00 d . . . C(33) C 0.841(1) -0.079(2) 0.6066(6) 0.110(7) Uani 1.00 d . . . C(34) C 0.898(1) -0.080(2) 0.5776(7) 0.117(8) Uani 1.00 d . . . C(35) C 0.8777(10) -0.002(2) 0.5489(6) 0.105(7) Uani 1.00 d . . . C(36) C 0.801(1) 0.061(2) 0.5491(4) 0.093(6) Uani 1.00 d . . . C(37) C 0.6295(9) 0.313(1) 0.5132(4) 0.066(5) Uani 1.00 d . . . C(38) C 0.629(1) 0.390(2) 0.4783(4) 0.087(6) Uani 1.00 d . . . C(39) C 0.881(2) 0.171(3) 0.1154(8) 0.114(9) Uani 1.00 d . . . C(40) C 0.888(2) 0.043(4) 0.1087(9) 0.22(2) Uani 1.00 d . . . C(41) C 0.377(1) 0.130(3) 0.1036(7) 0.132(10) Uani 1.00 d . . . C(42) C 0.377(1) 0.014(3) 0.089(1) 0.28(2) Uani 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.072(1) 0.0378(9) 0.072(1) -0.0023(8) 0.0032(9) -0.0041(8) Cu(2) 0.070(1) 0.060(1) 0.0489(10) -0.0046(8) 0.0012(8) 0.0083(8) Cl(1) 0.130(4) 0.080(4) 0.125(4) -0.011(3) -0.016(4) -0.004(3) Cl(2) 0.075(3) 0.098(4) 0.117(4) -0.012(3) 0.025(3) -0.004(3) Cl(3) 0.065(2) 0.072(3) 0.067(3) 0.002(2) 0.000(2) 0.002(2) Cl(4) 0.118(4) 0.102(4) 0.089(4) -0.015(3) 0.018(3) 0.015(3) O(1) 0.35(4) 0.37(4) 0.37(4) -0.04(3) 0.13(3) -0.24(3) O(2) 0.62(5) 0.19(2) 0.20(2) -0.05(3) -0.11(3) -0.01(2) O(3) 0.54(4) 0.12(2) 0.15(2) 0.06(2) 0.02(2) 0.01(1) O(4) 0.14(2) 0.43(4) 0.40(4) -0.05(2) -0.02(2) -0.26(3) O(5) 0.22(2) 0.31(3) 0.12(1) 0.05(2) 0.05(1) -0.02(2) O(6) 0.14(1) 0.26(2) 0.15(1) -0.01(1) 0.00(1) 0.03(1) O(7) 0.14(1) 0.09(1) 0.41(3) -0.01(1) 0.06(2) 0.01(1) O(8) 0.073(8) 0.16(1) 0.26(2) -0.024(9) 0.008(9) 0.05(1) O(9) 0.089(8) 0.13(1) 0.17(1) 0.026(8) 0.019(8) 0.056(10) O(10) 0.29(2) 0.17(2) 0.088(10) 0.02(1) 0.02(1) -0.02(1) O(11) 0.122(9) 0.070(7) 0.107(8) 0.018(6) 0.018(7) 0.030(6) O(12) 0.12(1) 0.11(1) 0.18(1) -0.028(9) -0.045(9) 0.043(10) O(13) 0.41(3) 0.11(1) 0.23(2) -0.04(2) 0.04(2) 0.04(2) O(14) 0.21(2) 0.27(3) 0.34(3) -0.12(2) -0.01(2) 0.15(2) O(15) 0.30(3) 0.49(5) 0.12(2) -0.11(3) -0.05(2) 0.07(2) O(16) 0.31(3) 0.29(3) 0.29(3) 0.05(2) 0.19(3) 0.02(2) N(1) 0.091(9) 0.12(1) 0.047(8) 0.004(9) -0.012(6) 0.015(9) N(2) 0.076(8) 0.060(8) 0.056(7) -0.007(6) 0.005(6) 0.017(7) N(3) 0.069(7) 0.031(6) 0.061(7) 0.004(5) 0.010(6) -0.002(5) N(4) 0.063(7) 0.048(7) 0.067(7) 0.008(6) 0.007(6) -0.001(6) N(5) 0.070(7) 0.045(7) 0.071(8) 0.000(6) 0.000(6) -0.016(6) N(6) 0.071(8) 0.053(8) 0.088(9) 0.014(7) -0.001(6) -0.001(7) N(7) 0.082(8) 0.066(9) 0.074(9) -0.016(7) -0.001(7) -0.034(8) N(8) 0.080(8) 0.053(8) 0.051(7) 0.000(6) -0.001(6) -0.005(6) N(9) 0.082(8) 0.048(7) 0.061(7) 0.007(6) -0.001(6) 0.013(6) N(10) 0.040(6) 0.065(8) 0.075(8) 0.000(5) 0.000(6) 0.004(7) N(11) 0.055(7) 0.065(8) 0.074(8) -0.006(6) -0.005(6) -0.004(7) N(12) 0.10(1) 0.09(1) 0.073(10) -0.001(8) 0.012(8) 0.024(8) N(13) 0.11(2) 0.19(2) 0.15(2) 0.00(2) 0.02(1) 0.04(2) N(14) 0.18(2) 0.13(2) 0.15(2) 0.03(2) -0.06(1) -0.01(1) C(1) 0.071(10) 0.065(10) 0.08(1) 0.008(8) 0.012(8) 0.004(9) C(2) 0.09(1) 0.06(1) 0.08(1) -0.005(8) -0.007(9) 0.010(9) C(3) 0.17(2) 0.037(9) 0.050(10) 0.009(9) -0.001(10) 0.025(8) C(4) 0.20(2) 0.11(2) 0.11(2) 0.00(2) -0.01(2) -0.02(1) C(5) 0.17(2) 0.04(1) 0.18(2) 0.00(1) 0.05(2) -0.03(1) C(6) 0.08(1) 0.034(9) 0.27(3) 0.005(8) 0.05(1) 0.01(1) C(7) 0.065(9) 0.06(1) 0.11(1) 0.009(8) -0.004(9) -0.002(9) C(8) 0.070(10) 0.07(1) 0.11(1) 0.006(9) 0.027(9) 0.036(10) C(9) 0.07(1) 0.11(2) 0.11(1) 0.01(1) 0.016(9) 0.03(1) C(10) 0.13(1) 0.08(1) 0.08(1) 0.00(1) 0.03(1) -0.001(10) C(11) 0.08(1) 0.056(10) 0.11(1) -0.009(9) 0.02(1) -0.003(9) C(12) 0.15(2) 0.044(10) 0.16(2) 0.01(1) -0.03(1) 0.03(1) C(13) 0.07(1) 0.05(1) 0.13(1) 0.002(9) -0.003(10) -0.018(10) C(14) 0.10(1) 0.055(10) 0.11(1) 0.023(10) 0.00(1) -0.007(9) C(15) 0.063(9) 0.09(1) 0.08(1) -0.009(10) -0.019(8) -0.010(9) C(16) 0.08(1) 0.09(1) 0.08(1) 0.005(10) -0.003(9) -0.014(10) C(17) 0.09(1) 0.044(8) 0.069(9) 0.005(8) -0.010(8) -0.009(7) C(18) 0.077(10) 0.042(9) 0.066(9) 0.018(8) 0.006(7) 0.004(7) C(19) 0.09(1) 0.032(8) 0.13(1) 0.000(8) 0.011(10) 0.010(8) C(20) 0.066(10) 0.06(1) 0.10(1) -0.013(8) 0.001(8) -0.004(9) C(21) 0.10(1) 0.11(2) 0.08(1) -0.02(1) -0.026(10) 0.01(1) C(22) 0.18(2) 0.07(1) 0.05(1) 0.02(1) 0.01(1) 0.002(9) C(23) 0.17(2) 0.11(2) 0.12(2) 0.03(1) -0.02(1) -0.04(1) C(24) 0.29(3) 0.08(2) 0.12(2) 0.02(2) 0.05(2) 0.02(1) C(25) 0.18(2) 0.14(2) 0.13(2) -0.09(2) -0.04(2) 0.09(2) C(26) 0.08(1) 0.09(1) 0.09(1) -0.02(1) -0.015(9) 0.00(1) C(27) 0.10(1) 0.08(1) 0.17(2) -0.04(1) 0.04(1) -0.01(1) C(28) 0.047(10) 0.12(2) 0.15(2) -0.02(1) -0.02(1) -0.06(2) C(29) 0.09(1) 0.12(2) 0.10(1) -0.04(1) 0.00(1) -0.03(1) C(30) 0.07(1) 0.09(1) 0.07(1) -0.028(9) -0.002(8) -0.013(9) C(31) 0.09(1) 0.32(4) 0.19(2) 0.05(2) 0.02(2) 0.19(2) C(32) 0.06(1) 0.14(2) 0.09(1) 0.00(1) -0.012(9) 0.03(1) C(33) 0.07(1) 0.13(2) 0.13(2) 0.03(1) -0.03(1) -0.01(1) C(34) 0.10(2) 0.12(2) 0.13(2) 0.05(1) -0.03(1) -0.07(1) C(35) 0.040(9) 0.14(2) 0.13(2) 0.02(1) -0.002(9) -0.06(1) C(36) 0.09(1) 0.12(2) 0.07(1) -0.01(1) -0.009(9) -0.01(1) C(37) 0.062(9) 0.07(1) 0.06(1) 0.011(8) -0.003(8) -0.013(9) C(38) 0.10(1) 0.09(1) 0.07(1) 0.009(10) 0.017(9) 0.023(9) C(39) 0.09(2) 0.15(3) 0.10(2) -0.01(2) 0.02(1) -0.02(2) C(40) 0.17(3) 0.25(4) 0.23(3) -0.08(3) 0.03(2) -0.13(3) C(41) 0.10(2) 0.14(2) 0.15(2) 0.04(2) -0.05(1) -0.06(2) C(42) 0.07(1) 0.29(4) 0.48(6) 0.06(2) -0.03(2) -0.24(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(2) 2.01(1) . . yes Cu(1) N(3) 2.032(10) . . yes Cu(1) N(4) 2.05(1) . . yes Cu(1) N(5) 2.07(1) . . yes Cu(1) N(6) 2.00(1) . . yes Cu(2) N(8) 2.00(1) . . yes Cu(2) N(9) 2.03(1) . . yes Cu(2) N(10) 2.02(1) . . yes Cu(2) N(11) 2.06(1) . . yes Cu(2) N(12) 1.95(1) . . yes Cl(1) O(1) 1.32(3) . . yes Cl(1) O(2) 1.35(2) . . yes Cl(1) O(3) 1.29(2) . . yes Cl(1) O(4) 1.26(2) . . yes Cl(2) O(5) 1.36(2) . . yes Cl(2) O(6) 1.47(2) . . yes Cl(2) O(7) 1.34(2) . . yes Cl(2) O(8) 1.38(1) . . yes Cl(3) O(9) 1.42(1) . . yes Cl(3) O(10) 1.40(1) . . yes Cl(3) O(11) 1.40(1) . . yes Cl(3) O(12) 1.42(1) . . yes Cl(4) O(13) 1.38(2) . . yes Cl(4) O(14) 1.30(2) . . yes Cl(4) O(15) 1.31(2) . . yes Cl(4) O(16) 1.28(2) . . yes N(1) C(1) 1.38(2) . . yes N(1) C(2) 1.37(2) . . yes N(1) C(4) 1.49(2) . . yes N(2) C(1) 1.27(2) . . yes N(2) C(3) 1.37(2) . . yes N(3) C(5) 1.49(2) . . yes N(3) C(6) 1.41(2) . . yes N(3) C(12) 1.51(2) . . yes N(4) C(7) 1.36(2) . . yes N(4) C(11) 1.30(2) . . yes N(5) C(13) 1.32(2) . . yes N(5) C(17) 1.30(2) . . yes N(6) C(18) 1.11(1) . . yes N(7) C(20) 1.33(2) . . yes N(7) C(21) 1.33(2) . . yes N(7) C(23) 1.43(2) . . yes N(8) C(20) 1.29(2) . . yes N(8) C(22) 1.36(2) . . yes N(9) C(24) 1.47(2) . . yes N(9) C(25) 1.42(2) . . yes N(9) C(31) 1.38(2) . . yes N(10) C(26) 1.36(2) . . yes N(10) C(30) 1.31(2) . . yes N(11) C(32) 1.35(2) . . yes N(11) C(36) 1.33(2) . . yes N(12) C(37) 1.09(2) . . yes N(13) C(39) 1.03(3) . . yes N(14) C(41) 1.12(2) . . yes C(2) C(3) 1.26(2) . . yes C(3) C(5) 1.56(2) . . yes C(6) C(7) 1.51(2) . . yes C(7) C(8) 1.41(2) . . yes C(8) C(9) 1.34(2) . . yes C(9) C(10) 1.38(2) . . yes C(10) C(11) 1.38(2) . . yes C(12) C(13) 1.52(2) . . yes C(13) C(14) 1.39(2) . . yes C(14) C(15) 1.35(2) . . yes C(15) C(16) 1.34(2) . . yes C(16) C(17) 1.38(2) . . yes C(18) C(19) 1.43(2) . . yes C(21) C(22) 1.30(2) . . yes C(22) C(24) 1.54(3) . . yes C(25) C(26) 1.49(2) . . yes C(26) C(27) 1.39(2) . . yes C(27) C(28) 1.33(3) . . yes C(28) C(29) 1.33(3) . . yes C(29) C(30) 1.31(2) . . yes C(31) C(32) 1.55(3) . . yes C(32) C(33) 1.38(2) . . yes C(33) C(34) 1.34(3) . . yes C(34) C(35) 1.36(3) . . yes C(35) C(36) 1.33(2) . . yes C(37) C(38) 1.49(2) . . yes C(39) C(40) 1.41(4) . . yes C(41) C(42) 1.34(3) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(2) Cu(1) N(3) 81.4(7) . 1_555 1_555 yes N(2) Cu(1) N(4) 119.8(6) . 1_555 1_555 yes N(2) Cu(1) N(5) 117.2(6) . 1_555 1_555 yes N(2) Cu(1) N(6) 96.3(8) . 1_555 1_555 yes N(3) Cu(1) N(4) 82.3(6) . 1_555 1_555 yes N(3) Cu(1) N(5) 83.3(6) . 1_555 1_555 yes N(3) Cu(1) N(6) 177.6(7) . 1_555 1_555 yes N(4) Cu(1) N(5) 117.7(6) . 1_555 1_555 yes N(4) Cu(1) N(6) 98.6(7) . 1_555 1_555 yes N(5) Cu(1) N(6) 98.3(7) . 1_555 1_555 yes N(8) Cu(2) N(9) 83.3(7) . 1_555 1_555 yes N(8) Cu(2) N(10) 120.4(6) . 1_555 1_555 yes N(8) Cu(2) N(11) 117.1(7) . 1_555 1_555 yes N(8) Cu(2) N(12) 97.4(8) . 1_555 1_555 yes N(9) Cu(2) N(10) 82.7(7) . 1_555 1_555 yes N(9) Cu(2) N(11) 81.5(7) . 1_555 1_555 yes N(9) Cu(2) N(12) 179.2(8) . 1_555 1_555 yes N(10) Cu(2) N(11) 117.5(6) . 1_555 1_555 yes N(10) Cu(2) N(12) 96.6(8) . 1_555 1_555 yes N(11) Cu(2) N(12) 98.5(8) . 1_555 1_555 yes O(1) Cl(1) O(2) 112(2) . 1_555 1_555 yes O(1) Cl(1) O(3) 103(2) . 1_555 1_555 yes O(1) Cl(1) O(4) 104(2) . 1_555 1_555 yes O(2) Cl(1) O(3) 102(2) . 1_555 1_555 yes O(2) Cl(1) O(4) 116(2) . 1_555 1_555 yes O(3) Cl(1) O(4) 116(2) . 1_555 1_555 yes O(5) Cl(2) O(6) 104(1) . 1_555 1_555 yes O(5) Cl(2) O(7) 109(2) . 1_555 1_555 yes O(5) Cl(2) O(8) 116(1) . 1_555 1_555 yes O(6) Cl(2) O(7) 108(1) . 1_555 1_555 yes O(6) Cl(2) O(8) 105(1) . 1_555 1_555 yes O(7) Cl(2) O(8) 111(1) . 1_555 1_555 yes O(9) Cl(3) O(10) 110(1) . 1_555 1_555 yes O(9) Cl(3) O(11) 110(1) . 1_555 1_555 yes O(9) Cl(3) O(12) 110(1) . 1_555 1_555 yes O(10) Cl(3) O(11) 110(1) . 1_555 1_555 yes O(10) Cl(3) O(12) 104(1) . 1_555 1_555 yes O(11) Cl(3) O(12) 110(1) . 1_555 1_555 yes O(13) Cl(4) O(14) 111(2) . 1_555 1_555 yes O(13) Cl(4) O(15) 109(2) . 1_555 1_555 yes O(13) Cl(4) O(16) 102(2) . 1_555 1_555 yes O(14) Cl(4) O(15) 102(2) . 1_555 1_555 yes O(14) Cl(4) O(16) 114(2) . 1_555 1_555 yes O(15) Cl(4) O(16) 116(2) . 1_555 1_555 yes C(1) N(1) C(2) 107(1) . 1_555 1_555 yes C(1) N(1) C(4) 128(2) . 1_555 1_555 yes C(2) N(1) C(4) 123(2) . 1_555 1_555 yes Cu(1) N(2) C(1) 139(1) . 1_555 1_555 yes Cu(1) N(2) C(3) 113(1) . 1_555 1_555 yes C(1) N(2) C(3) 106(1) . 1_555 1_555 yes Cu(1) N(3) C(5) 110(1) . 1_555 1_555 yes Cu(1) N(3) C(6) 106(1) . 1_555 1_555 yes Cu(1) N(3) C(12) 105(1) . 1_555 1_555 yes C(5) N(3) C(6) 115(1) . 1_555 1_555 yes C(5) N(3) C(12) 109(1) . 1_555 1_555 yes C(6) N(3) C(12) 108(1) . 1_555 1_555 yes Cu(1) N(4) C(7) 111(1) . 1_555 1_555 yes Cu(1) N(4) C(11) 127(1) . 1_555 1_555 yes C(7) N(4) C(11) 120(1) . 1_555 1_555 yes Cu(1) N(5) C(13) 114(1) . 1_555 1_555 yes Cu(1) N(5) C(17) 131(1) . 1_555 1_555 yes C(13) N(5) C(17) 113(1) . 1_555 1_555 yes Cu(1) N(6) C(18) 177(2) . 1_555 1_555 yes C(20) N(7) C(21) 102(2) . 1_555 1_555 yes C(20) N(7) C(23) 127(2) . 1_555 1_555 yes C(21) N(7) C(23) 130(2) . 1_555 1_555 yes Cu(2) N(8) C(20) 144(1) . 1_555 1_555 yes Cu(2) N(8) C(22) 111(1) . 1_555 1_555 yes C(20) N(8) C(22) 103(1) . 1_555 1_555 yes Cu(2) N(9) C(24) 105(1) . 1_555 1_555 yes Cu(2) N(9) C(25) 105(1) . 1_555 1_555 yes Cu(2) N(9) C(31) 107(1) . 1_555 1_555 yes C(24) N(9) C(25) 106(2) . 1_555 1_555 yes C(24) N(9) C(31) 110(2) . 1_555 1_555 yes C(25) N(9) C(31) 119(2) . 1_555 1_555 yes Cu(2) N(10) C(26) 114(1) . 1_555 1_555 yes Cu(2) N(10) C(30) 129(1) . 1_555 1_555 yes C(26) N(10) C(30) 116(2) . 1_555 1_555 yes Cu(2) N(11) C(32) 110(1) . 1_555 1_555 yes Cu(2) N(11) C(36) 129(1) . 1_555 1_555 yes C(32) N(11) C(36) 119(1) . 1_555 1_555 yes Cu(2) N(12) C(37) 177(2) . 1_555 1_555 yes N(1) C(1) N(2) 109(2) . 1_555 1_555 yes N(1) C(2) C(3) 106(2) . 1_555 1_555 yes N(2) C(3) C(2) 110(1) . 1_555 1_555 yes N(2) C(3) C(5) 114(2) . 1_555 1_555 yes C(2) C(3) C(5) 134(2) . 1_555 1_555 yes N(3) C(5) C(3) 105(1) . 1_555 1_555 yes N(3) C(6) C(7) 112(1) . 1_555 1_555 yes N(4) C(7) C(6) 115(1) . 1_555 1_555 yes N(4) C(7) C(8) 121(1) . 1_555 1_555 yes C(6) C(7) C(8) 122(2) . 1_555 1_555 yes C(7) C(8) C(9) 118(2) . 1_555 1_555 yes C(8) C(9) C(10) 117(2) . 1_555 1_555 yes C(9) C(10) C(11) 119(2) . 1_555 1_555 yes N(4) C(11) C(10) 122(2) . 1_555 1_555 yes N(3) C(12) C(13) 108(1) . 1_555 1_555 yes N(5) C(13) C(12) 112(2) . 1_555 1_555 yes N(5) C(13) C(14) 123(2) . 1_555 1_555 yes C(12) C(13) C(14) 123(2) . 1_555 1_555 yes C(13) C(14) C(15) 117(2) . 1_555 1_555 yes C(14) C(15) C(16) 120(2) . 1_555 1_555 yes C(15) C(16) C(17) 120(2) . 1_555 1_555 yes N(5) C(17) C(16) 123(1) . 1_555 1_555 yes N(6) C(18) C(19) 174(2) . 1_555 1_555 yes N(7) C(20) N(8) 114(2) . 1_555 1_555 yes N(7) C(21) C(22) 107(2) . 1_555 1_555 yes N(8) C(22) C(21) 113(2) . 1_555 1_555 yes N(8) C(22) C(24) 117(2) . 1_555 1_555 yes C(21) C(22) C(24) 127(2) . 1_555 1_555 yes N(9) C(24) C(22) 108(2) . 1_555 1_555 yes N(9) C(25) C(26) 119(2) . 1_555 1_555 yes N(10) C(26) C(25) 111(2) . 1_555 1_555 yes N(10) C(26) C(27) 120(2) . 1_555 1_555 yes C(25) C(26) C(27) 126(2) . 1_555 1_555 yes C(26) C(27) C(28) 124(2) . 1_555 1_555 yes C(27) C(28) C(29) 115(2) . 1_555 1_555 yes C(28) C(29) C(30) 117(2) . 1_555 1_555 yes N(10) C(30) C(29) 124(2) . 1_555 1_555 yes N(9) C(31) C(32) 113(2) . 1_555 1_555 yes N(11) C(32) C(31) 115(2) . 1_555 1_555 yes N(11) C(32) C(33) 115(2) . 1_555 1_555 yes C(31) C(32) C(33) 127(2) . 1_555 1_555 yes C(32) C(33) C(34) 125(2) . 1_555 1_555 yes C(33) C(34) C(35) 115(2) . 1_555 1_555 yes C(34) C(35) C(36) 119(2) . 1_555 1_555 yes N(11) C(36) C(35) 123(2) . 1_555 1_555 yes N(12) C(37) C(38) 176(2) . 1_555 1_555 yes N(13) C(39) C(40) 176(4) . 1_555 1_555 yes N(14) C(41) C(42) 175(4) . 1_555 1_555 yes #===END