Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_General #==================================================================== # SUBMISSION DETAILS _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Zhiqiang Xu' 'Laurence K. Thompson' 'Daniel A. Black' 'Corbin Ralph' 'David O. Miller' 'Michael J. Leech' 'Judith A.K. Howard' _publ_contact_author_name 'Laurie K. Thompson' _publ_contact_author_address ; Laurie K. Thompson University Research Professor, Dept. of Chemistry, Memorial University, St. John's, Newfoundland, A1B 3X7 CANADA ; _publ_contact_author_email 'lthomp@morgan.ucs.mun.ca' _audit_creation_date '1998-08-14' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #==================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997). teXsan for Windows version 1.0. Single Crystal Structure Analysis Software. Version 1.01. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #==================================================================== loop_ _publ_manuscript_incl_extra_item '_geom_extra_table_head_3' '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' # # #------------------------------------------------------------------------------ data__x607(1) _database_code_CSD 158599 #==================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 24.219(5) _cell_length_b 9.127(2) _cell_length_c 13.515(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2987.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.2 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 690.18 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H26 Cl4 N10 Mn2 O2 ' _chemical_formula_moiety 'C20 H26 Cl4 N10 Mn2 O2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1400.00 _exptl_absorpt_coefficient_mu 1.239 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.893 _exptl_special_details ; The scan width was (0.84+0.35tan\q)\% with an \w scan speed of 4\% per minute (up to 11 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #==================================================================== #========= # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.01 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 6 0 2 0 2 1 2 2 _diffrn_reflns_number 3904 _reflns_number_total 3904 _reflns_number_gt 3096 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.067 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02124 _diffrn_orient_matrix_UB_12 -0.00939 _diffrn_orient_matrix_UB_13 0.06315 _diffrn_orient_matrix_UB_21 0.03470 _diffrn_orient_matrix_UB_22 0.02722 _diffrn_orient_matrix_UB_23 -0.03561 _diffrn_orient_matrix_UB_31 -0.00704 _diffrn_orient_matrix_UB_32 0.10571 _diffrn_orient_matrix_UB_33 0.01478 #------------------------------------------------------------------------------ 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 C 0 80 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 104 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 40 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Mn 0 8 0.295 0.729 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #==================================================================== #========= # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy #_atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Mn(1) 0.19429(2) 0.24705(7) -0.0253(7) 0.0378(1) 1.000 Uani d ? Mn(2) 0.07700(2) 0.06464(6) 0.2353(7) 0.0347(1) 1.000 Uani d ? Cl(1) 0.24303(4) 0.1444(1) -0.1686(7) 0.0605(3) 1.000 Uani d ? Cl(2) 0.20331(4) 0.5114(1) -0.0516(7) 0.0515(3) 1.000 Uani d ? Cl(3) -0.01804(4) 0.1024(1) 0.2951(7) 0.0632(4) 1.000 Uani d ? Cl(4) 0.10211(4) -0.1521(1) 0.3317(7) 0.0530(3) 1.000 Uani d ? O(1) -0.0179(1) -0.1283(3) 0.1374(7) 0.0595(9) 1.000 Uani d ? O(2) 0.1298(1) 0.2454(4) -0.2295(7) 0.073(1) 1.000 Uani d ? N(1) 0.2701(1) 0.2556(4) 0.0750(7) 0.0442(9) 1.000 Uani d ? N(2) 0.2179(1) -0.0089(4) 0.2450(7) 0.053(1) 1.000 Uani d ? N(3) 0.1887(1) 0.0660(3) 0.0882(7) 0.0329(8) 1.000 Uani d ? N(4) 0.1393(1) -0.0087(3) 0.1108(7) 0.0339(8) 1.000 Uani d ? N(5) 0.0345(1) -0.0737(4) 0.1182(7) 0.0411(9) 1.000 Uani d ? N(6) 0.1108(1) 0.2191(3) 0.3525(7) 0.0391(9) 1.000 Uani d ? N(7) 0.1584(2) 0.4835(4) 0.1802(7) 0.054(1) 1.000 Uani d ? N(8) 0.0979(1) 0.2845(3) 0.1621(7) 0.0327(8) 1.000 Uani d ? N(9) 0.1066(1) 0.3013(3) 0.0597(7) 0.0336(8) 1.000 Uani d ? N(10) 0.1203(1) 0.2443(4) -0.1286(7) 0.046(1) 1.000 Uani d ? C(1) 0.3134(2) 0.3416(5) 0.0587(7) 0.062(1) 1.000 Uani d ? C(2) 0.3611(2) 0.3348(6) 0.1143(8) 0.064(2) 1.000 Uani d ? C(3) 0.3640(2) 0.2374(6) 0.1905(7) 0.056(1) 1.000 Uani d ? C(4) 0.3199(2) 0.1464(5) 0.2077(7) 0.045(1) 1.000 Uani d ? C(5) 0.2733(1) 0.1605(4) 0.1492(7) 0.0330(9) 1.000 Uani d ? C(6) 0.2235(1) 0.0666(4) 0.1629(7) 0.0341(9) 1.000 Uani d ? C(7) 0.1197(1) -0.0923(4) 0.0414(7) 0.0359(9) 1.000 Uani d ? C(8) 0.0637(2) -0.1535(4) 0.0623(7) 0.039(1) 1.000 Uani d ? C(9) 0.1477(2) -0.1266(5) -0.0534(8) 0.053(1) 1.000 Uani d ? C(10) 0.0461(2) -0.2951(5) 0.0200(7) 0.059(1) 1.000 Uani d ? C(11) 0.1078(2) 0.1918(5) 0.4489(7) 0.055(1) 1.000 Uani d ? C(12) 0.1175(2) 0.2964(6) 0.5199(7) 0.065(2) 1.000 Uani d ? C(13) 0.1300(2) 0.4355(6) 0.4893(7) 0.070(2) 1.000 Uani d ? C(14) 0.1341(2) 0.4662(5) 0.3899(7) 0.054(1) 1.000 Uani d ? C(15) 0.1242(1) 0.3526(4) 0.3246(7) 0.0371(9) 1.000 Uani d ? C(16) 0.1275(1) 0.3745(4) 0.2146(7) 0.036(1) 1.000 Uani d ? C(17) 0.0633(1) 0.2985(4) 0.0050(7) 0.0351(9) 1.000 Uani d ? C(18) 0.0738(2) 0.3000(4) -0.1046(7) 0.040(1) 1.000 Uani d ? C(19) 0.0053(2) 0.2939(5) 0.0423(7) 0.054(1) 1.000 Uani d ? C(20) 0.0319(2) 0.3656(5) -0.1733(7) 0.057(1) 1.000 Uani d ? H(1A) 0.3118 0.4119 0.0089 0.075 1.000 Uiso c ? H(1B) -0.0218 -0.0587 0.2070 0.099 1.000 Uiso c ? H(2A) 0.1908 -0.0636 0.2556 0.063 1.000 Uiso c ? H(2B) 0.2412 -0.0001 0.2966 0.063 1.000 Uiso c ? H(2C) 0.3916 0.3970 0.1019 0.078 1.000 Uiso c ? H(2D) 0.1683 0.2485 -0.2395 0.086 1.000 Uiso c ? H(3) 0.3959 0.2334 0.2337 0.068 1.000 Uiso c ? H(4) 0.3215 0.0747 0.2611 0.054 1.000 Uiso c ? H(7A) 0.1798 0.5199 0.2283 0.104 1.000 Uiso c ? H(7B) 0.1685 0.4924 0.1204 0.051 1.000 Uiso c ? H(9A) 0.1423 -0.2254 -0.0676 0.064 1.000 Uiso c ? H(9B) 0.1329 -0.0653 -0.1022 0.064 1.000 Uiso c ? H(9C) 0.1863 -0.1064 -0.0452 0.064 1.000 Uiso c ? H(10A) 0.0294 -0.3538 0.0714 0.075 1.000 Uiso c ? H(10B) 0.0210 -0.2791 -0.0306 0.075 1.000 Uiso c ? H(10C) 0.0779 -0.3459 -0.0033 0.075 1.000 Uiso c ? H(11) 0.0985 0.0956 0.4717 0.066 1.000 Uiso c ? H(12) 0.1155 0.2738 0.5905 0.079 1.000 Uiso c ? H(13) 0.1358 0.5114 0.5386 0.085 1.000 Uiso c ? H(14) 0.1435 0.5615 0.3692 0.064 1.000 Uiso c ? H(19A) -0.0137 0.3794 0.0259 0.066 1.000 Uiso c ? H(19B) -0.0130 0.2098 0.0183 0.066 1.000 Uiso c ? H(19C) 0.0057 0.2862 0.1153 0.066 1.000 Uiso c ? H(20A) 0.0497 0.3850 -0.2334 0.071 1.000 Uiso c ? H(20B) 0.0188 0.4543 -0.1445 0.071 1.000 Uiso c ? H(20C) 0.0030 0.2986 -0.1808 0.071 1.000 Uiso c ? 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 Mn(1) 0.0356(3) 0.0487(3) 0.0291(2) 0.0015(3) 0.0001(2) 0.0071(3) Mn(2) 0.0348(2) 0.0381(3) 0.0312(3) -0.0047(2) -0.0010(2) 0.0014(3) Cl(1) 0.0545(6) 0.0784(8) 0.0487(6) 0.0144(6) 0.0141(5) -0.0013(6) Cl(2) 0.0636(6) 0.0494(6) 0.0414(5) 0.0035(5) 0.0111(5) 0.0131(5) Cl(3) 0.0372(5) 0.0913(9) 0.0611(7) 0.0071(6) 0.0057(5) -0.0079(7) Cl(4) 0.0519(6) 0.0477(5) 0.0593(6) -0.0036(5) -0.0057(5) 0.0185(5) O(1) 0.041(2) 0.076(2) 0.061(2) -0.026(2) -0.004(1) -0.002(2) O(2) 0.068(2) 0.126(3) 0.024(1) 0.019(2) -0.001(1) -0.001(2) N(1) 0.036(2) 0.051(2) 0.045(2) -0.006(1) 0.002(2) 0.011(2) N(2) 0.041(2) 0.073(2) 0.046(2) -0.016(2) -0.014(2) 0.026(2) N(3) 0.032(1) 0.039(2) 0.028(1) -0.001(1) -0.001(1) 0.002(1) N(4) 0.033(1) 0.036(2) 0.032(2) -0.003(1) -0.002(1) 0.001(1) N(5) 0.037(2) 0.048(2) 0.038(2) -0.013(1) -0.005(1) 0.002(2) N(6) 0.044(2) 0.045(2) 0.028(2) -0.004(1) 0.001(1) 0.003(1) N(7) 0.079(3) 0.057(2) 0.026(2) -0.033(2) 0.003(2) -0.000(2) N(8) 0.039(2) 0.035(2) 0.024(1) -0.003(1) 0.000(1) -0.000(1) N(9) 0.037(2) 0.039(2) 0.024(1) -0.003(1) -0.002(1) 0.000(1) N(10) 0.052(2) 0.061(2) 0.025(2) 0.001(2) -0.006(1) -0.001(2) C(1) 0.049(2) 0.075(3) 0.061(3) -0.016(2) -0.005(2) 0.027(3) C(2) 0.043(2) 0.077(3) 0.072(3) -0.024(2) -0.003(2) 0.006(3) C(3) 0.040(2) 0.094(4) 0.035(2) -0.016(2) -0.006(2) -0.003(2) C(4) 0.041(2) 0.063(3) 0.030(2) -0.006(2) -0.005(2) 0.003(2) C(5) 0.029(2) 0.046(2) 0.025(2) -0.000(1) 0.004(1) -0.004(2) C(6) 0.035(2) 0.037(2) 0.031(2) -0.000(1) -0.003(2) 0.001(2) C(7) 0.040(2) 0.033(2) 0.034(2) 0.002(2) -0.009(2) 0.001(2) C(8) 0.044(2) 0.036(2) 0.038(2) -0.002(2) -0.011(2) 0.004(2) C(9) 0.059(3) 0.055(3) 0.045(2) -0.002(2) 0.001(2) -0.020(2) C(10) 0.065(3) 0.044(2) 0.069(3) -0.013(2) -0.009(2) -0.009(2) C(11) 0.068(3) 0.064(3) 0.033(2) -0.018(2) -0.003(2) 0.011(2) C(12) 0.075(3) 0.097(4) 0.025(2) -0.024(3) 0.001(2) 0.000(2) C(13) 0.084(3) 0.092(4) 0.035(2) -0.040(3) 0.000(2) -0.013(3) C(14) 0.069(3) 0.056(3) 0.036(2) -0.018(2) 0.003(2) -0.008(2) C(15) 0.035(2) 0.047(2) 0.030(2) -0.004(2) 0.002(2) -0.000(2) C(16) 0.040(2) 0.039(2) 0.030(2) -0.002(2) -0.000(1) -0.001(2) C(17) 0.034(2) 0.038(2) 0.033(2) 0.002(2) -0.003(2) 0.001(2) C(18) 0.042(2) 0.050(2) 0.027(2) -0.003(2) -0.006(2) 0.002(2) C(19) 0.033(2) 0.074(3) 0.057(3) -0.003(2) 0.003(2) 0.004(2) C(20) 0.056(3) 0.078(3) 0.037(2) 0.007(2) -0.018(2) -0.001(2) #==================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|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 3096 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_all 0.0295 _refine_ls_wR_factor_ref 0.0280 _refine_ls_goodness_of_fit_all 1.576 _refine_ls_goodness_of_fit_ref 1.620 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.28 _refine_diff_density_max 0.29 #==================================================================== # MOLECULAR GEOMETRY _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 Mn(1) Cl(1) 2.45(1) . . ? Mn(1) Cl(2) 2.449(2) . . ? Mn(1) N(1) 2.284(8) . . ? Mn(1) N(3) 2.259(9) . . ? Mn(1) N(10) 2.272(8) . . ? Mn(2) Cl(3) 2.464(4) . . ? Mn(2) Cl(4) 2.446(7) . . ? Mn(2) N(5) 2.271(9) . . ? Mn(2) N(6) 2.273(9) . . ? Mn(2) N(8) 2.294(6) . . ? O(1) N(5) 1.388(5) . . ? O(1) H(1O) 1.14 . . no O(2) N(10) 1.38(1) . . ? O(2) H(2O) 0.94 . . no N(1) C(1) 1.329(6) . . ? N(1) C(5) 1.33(1) . . ? N(2) C(6) 1.31(1) . . ? N(2) H(2NA) 0.84 . . no N(2) H(2NB) 0.90 . . no N(3) N(4) 1.411(5) . . ? N(3) C(6) 1.32(1) . . ? N(4) C(7) 1.30(1) . . ? N(5) C(8) 1.265(9) . . ? N(6) C(11) 1.33(1) . . ? N(6) C(15) 1.316(6) . . ? N(7) C(16) 1.329(7) . . ? N(7) H(7NA) 0.90 . . no N(7) H(7NB) 0.85 . . no N(8) N(9) 1.41(1) . . ? N(8) C(16) 1.301(8) . . ? N(9) C(17) 1.283(9) . . ? N(10) C(18) 1.277(6) . . ? C(1) C(2) 1.379(9) . . ? C(1) H(1) 0.93 . . no C(2) C(3) 1.36(1) . . ? C(2) H(2) 0.95 . . no C(3) C(4) 1.373(6) . . ? C(3) H(3) 0.97 . . no C(4) C(5) 1.382(9) . . ? C(4) H(4) 0.98 . . no C(5) C(6) 1.490(5) . . ? C(7) C(8) 1.494(6) . . ? C(7) C(9) 1.48(1) . . ? C(8) C(10) 1.476(7) . . ? C(9) H(9B) 0.93 . . no C(9) H(9C) 0.94 . . no C(9) H(9A) 0.96 . . no C(10) H(10B) 0.97 . . no C(10) H(10C) 0.93 . . no C(10) H(10A) 0.95 . . no C(11) C(12) 1.37(1) . . ? C(11) H(11) 0.96 . . no C(12) C(13) 1.369(8) . . ? C(12) H(12) 0.98 . . no C(13) C(14) 1.38(1) . . ? C(13) H(13) 0.97 . . no C(14) C(15) 1.38(1) . . ? C(14) H(14) 0.94 . . no C(15) C(16) 1.50(1) . . ? C(17) C(18) 1.50(1) . . ? C(17) C(19) 1.492(7) . . ? C(18) C(20) 1.501(9) . . ? C(19) H(19B) 0.93 . . no C(19) H(19C) 0.94 . . no C(19) H(19A) 0.99 . . no C(20) H(20B) 0.94 . . no C(20) H(20C) 0.95 . . no C(20) H(20A) 0.93 . . no #------------------------------------------------------------------------------ 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 Cl(1) Mn(1) Cl(2) 102.6(3) . . . ? Cl(1) Mn(1) N(1) 95.4(2) . . . ? Cl(1) Mn(1) N(3) 106.6(2) . . . ? Cl(1) Mn(1) N(10) 83.7(3) . . . ? Cl(2) Mn(1) N(1) 88.9(2) . . . ? Cl(2) Mn(1) N(3) 145.6(5) . . . ? Cl(2) Mn(1) N(10) 89.6(2) . . . ? N(1) Mn(1) N(3) 70.7(3) . . . ? N(1) Mn(1) N(10) 178.0(3) . . . ? N(3) Mn(1) N(10) 111.2(2) . . . ? Cl(3) Mn(2) Cl(4) 99.8(3) . . . ? Cl(3) Mn(2) N(5) 83.3(2) . . . ? Cl(3) Mn(2) N(6) 91.2(3) . . . ? Cl(3) Mn(2) N(8) 103.0(1) . . . ? Cl(4) Mn(2) N(5) 92.0(2) . . . ? Cl(4) Mn(2) N(6) 92.3(3) . . . ? Cl(4) Mn(2) N(8) 152.0(1) . . . ? N(5) Mn(2) N(6) 173.5(1) . . . ? N(5) Mn(2) N(8) 106.6(4) . . . ? N(6) Mn(2) N(8) 71.3(3) . . . ? N(5) O(1) H(1O) 91.7 . . . no N(10) O(2) H(2O) 107.9 . . . no Mn(1) N(1) C(1) 123.8(6) . . . ? Mn(1) N(1) C(5) 118.2(3) . . . ? C(1) N(1) C(5) 117.7(6) . . . ? C(6) N(2) H(2NA) 122.6 . . . no C(6) N(2) H(2NB) 122.9 . . . no H(2NA) N(2) H(2NB) 114.2 . . . no Mn(1) N(3) N(4) 123.4(4) . . . ? Mn(1) N(3) C(6) 118.7(3) . . . ? N(4) N(3) C(6) 112.4(7) . . . ? N(3) N(4) C(7) 115.9(7) . . . ? Mn(2) N(5) O(1) 118.9(6) . . . ? Mn(2) N(5) C(8) 118.9(3) . . . ? O(1) N(5) C(8) 114.6(4) . . . ? Mn(2) N(6) C(11) 123.2(3) . . . ? Mn(2) N(6) C(15) 117.6(7) . . . ? C(11) N(6) C(15) 117.9(7) . . . ? C(16) N(7) H(7NA) 110.4 . . . no C(16) N(7) H(7NB) 124.7 . . . no H(7NA) N(7) H(7NB) 119.3 . . . no Mn(2) N(8) N(9) 123.5(4) . . . ? Mn(2) N(8) C(16) 116.0(6) . . . ? N(9) N(8) C(16) 112.7(5) . . . ? N(8) N(9) C(17) 116.2(5) . . . ? Mn(1) N(10) O(2) 118.3(3) . . . ? Mn(1) N(10) C(18) 122.4(7) . . . ? O(2) N(10) C(18) 113.2(7) . . . ? N(1) C(1) C(2) 123.0(7) . . . ? N(1) C(1) H(1) 119.5 . . . no C(2) C(1) H(1) 117.5 . . . no C(1) C(2) C(3) 118.9(5) . . . ? C(1) C(2) H(2) 122.0 . . . no C(3) C(2) H(2) 119.0 . . . no C(2) C(3) C(4) 118.9(6) . . . ? C(2) C(3) H(3) 121.3 . . . no C(4) C(3) H(3) 119.7 . . . no C(3) C(4) C(5) 118.8(7) . . . ? C(3) C(4) H(4) 120.0 . . . no C(5) C(4) H(4) 121.2 . . . no N(1) C(5) C(4) 122.7(4) . . . ? N(1) C(5) C(6) 114.9(5) . . . ? C(4) C(5) C(6) 122.4(6) . . . ? N(2) C(6) N(3) 125.4(4) . . . ? N(2) C(6) C(5) 119.3(6) . . . ? N(3) C(6) C(5) 115.2(7) . . . ? N(4) C(7) C(8) 114.4(7) . . . ? N(4) C(7) C(9) 125.5(4) . . . ? C(8) C(7) C(9) 120.0(6) . . . ? N(5) C(8) C(7) 113.9(4) . . . ? N(5) C(8) C(10) 125.0(4) . . . ? C(7) C(8) C(10) 121.1(5) . . . ? C(7) C(9) H(9B) 108.6 . . . no C(7) C(9) H(9C) 107.8 . . . no C(7) C(9) H(9A) 107.8 . . . no H(9B) C(9) H(9C) 112.3 . . . no H(9B) C(9) H(9A) 110.3 . . . no H(9C) C(9) H(9A) 109.9 . . . no C(8) C(10) H(10B) 109.2 . . . no C(8) C(10) H(10C) 109.7 . . . no C(8) C(10) H(10A) 108.7 . . . no H(10B) C(10) H(10C) 110.1 . . . no H(10B) C(10) H(10A) 107.9 . . . no H(10C) C(10) H(10A) 111.3 . . . no N(6) C(11) C(12) 123.1(5) . . . ? N(6) C(11) H(11) 120.1 . . . no C(12) C(11) H(11) 116.9 . . . no C(11) C(12) C(13) 118.1(8) . . . ? C(11) C(12) H(12) 121.7 . . . no C(13) C(12) H(12) 120.1 . . . no C(12) C(13) C(14) 120.0(7) . . . ? C(12) C(13) H(13) 119.1 . . . no C(14) C(13) H(13) 121.0 . . . no C(13) C(14) C(15) 117.3(5) . . . ? C(13) C(14) H(14) 119.7 . . . no C(15) C(14) H(14) 123.0 . . . no N(6) C(15) C(14) 123.7(9) . . . ? N(6) C(15) C(16) 114.8(6) . . . ? C(14) C(15) C(16) 121.5(5) . . . ? N(7) C(16) N(8) 126.2(9) . . . ? N(7) C(16) C(15) 118.4(6) . . . ? N(8) C(16) C(15) 115.3(5) . . . ? N(9) C(17) C(18) 115.4(5) . . . ? N(9) C(17) C(19) 125.1(9) . . . ? C(18) C(17) C(19) 119.5(6) . . . ? N(10) C(18) C(17) 113.3(7) . . . ? N(10) C(18) C(20) 126.8(9) . . . ? C(17) C(18) C(20) 119.9(5) . . . ? C(17) C(19) H(19B) 111.2 . . . no C(17) C(19) H(19C) 110.4 . . . no C(17) C(19) H(19A) 109.3 . . . no H(19B) C(19) H(19C) 111.5 . . . no H(19B) C(19) H(19A) 107.5 . . . no H(19C) C(19) H(19A) 106.8 . . . no C(18) C(20) H(20B) 107.4 . . . no C(18) C(20) H(20C) 108.1 . . . no C(18) C(20) H(20A) 108.3 . . . no H(20B) C(20) H(20C) 110.4 . . . no H(20B) C(20) H(20A) 112.0 . . . no H(20C) C(20) H(20A) 110.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Mn(1) N(1) C(1) C(2) . . . . -173.3(6) no Mn(1) N(1) C(5) C(4) . . . . 173.1(5) no Mn(1) N(1) C(5) C(6) . . . . -5.1(8) no Mn(1) N(3) N(4) C(7) . . . . 68.1(5) no Mn(1) N(3) C(6) N(2) . . . . 163.6(4) no Mn(1) N(3) C(6) C(5) . . . . -17.4(6) no Mn(1) N(10) C(18) C(17) . . . . -28.3(5) no Mn(1) N(10) C(18) C(20) . . . . 150.6(5) no Mn(2) N(5) C(8) C(7) . . . . -31.5(9) no Mn(2) N(5) C(8) C(10) . . . . 148.4(6) no Mn(2) N(6) C(11) C(12) . . . . -166.1(4) no Mn(2) N(6) C(15) C(14) . . . . 166.1(3) no Mn(2) N(6) C(15) C(16) . . . . -13.3(4) no Mn(2) N(8) N(9) C(17) . . . . 75.1(4) no Mn(2) N(8) C(16) N(7) . . . . 157.8(4) no Mn(2) N(8) C(16) C(15) . . . . -24.1(4) no Cl(1) Mn(1) N(1) C(1) . . . . 65.9(5) no Cl(1) Mn(1) N(1) C(5) . . . . -108.2(5) no Cl(1) Mn(1) N(3) N(4) . . . . -107.2(5) no Cl(1) Mn(1) N(3) C(6) . . . . 101.1(5) no Cl(1) Mn(1) N(10) O(2) . . . . -23.3(3) no Cl(1) Mn(1) N(10) C(18) . . . . -173.9(5) no Cl(2) Mn(1) N(1) C(1) . . . . -36.7(6) no Cl(2) Mn(1) N(1) C(5) . . . . 149.3(5) no Cl(2) Mn(1) N(3) N(4) . . . . 105.8(6) no Cl(2) Mn(1) N(3) C(6) . . . . -45.9(5) no Cl(2) Mn(1) N(10) O(2) . . . . 79.4(4) no Cl(2) Mn(1) N(10) C(18) . . . . -71.1(5) no Cl(3) Mn(2) N(5) O(1) . . . . -21.5(4) no Cl(3) Mn(2) N(5) C(8) . . . . -169.4(6) no Cl(3) Mn(2) N(6) C(11) . . . . 64.7(4) no Cl(3) Mn(2) N(6) C(15) . . . . -102.1(4) no Cl(3) Mn(2) N(8) N(9) . . . . -113.5(4) no Cl(3) Mn(2) N(8) C(16) . . . . 99.8(4) no Cl(4) Mn(2) N(5) O(1) . . . . 78.2(4) no Cl(4) Mn(2) N(5) C(8) . . . . -69.7(6) no Cl(4) Mn(2) N(6) C(11) . . . . -35.2(3) no Cl(4) Mn(2) N(6) C(15) . . . . 158.0(3) no Cl(4) Mn(2) N(8) N(9) . . . . 103(1) no Cl(4) Mn(2) N(8) C(16) . . . . -44(1) no O(1) N(5) Mn(2) N(6) . . . . -53(4) no O(1) N(5) Mn(2) N(8) . . . . -123.1(4) no O(1) N(5) C(8) C(7) . . . . 179.3(7) no O(1) N(5) C(8) C(10) . . . . -1(1) no O(2) N(10) Mn(1) N(1) . . . . 41(9) no O(2) N(10) Mn(1) N(3) . . . . -128.7(4) no O(2) N(10) C(18) C(17) . . . . 179.8(3) no O(2) N(10) C(18) C(20) . . . . -1.3(6) no N(1) Mn(1) N(3) N(4) . . . . 162.8(6) no N(1) Mn(1) N(3) C(6) . . . . 11.1(5) no N(1) Mn(1) N(10) C(18) . . . . -110(9) no N(1) C(1) C(2) C(3) . . . . -1(1) no N(1) C(5) C(4) C(3) . . . . 2(1) no N(1) C(5) C(6) N(2) . . . . -166.3(6) no N(1) C(5) C(6) N(3) . . . . 14.7(8) no N(2) C(6) N(3) N(4) . . . . 9.0(7) no N(2) C(6) C(5) C(4) . . . . 15.5(9) no N(3) Mn(1) N(1) C(1) . . . . 171.6(6) no N(3) Mn(1) N(1) C(5) . . . . -2.5(5) no N(3) Mn(1) N(10) C(18) . . . . 80.7(5) no N(3) N(4) C(7) C(8) . . . . -172.1(4) no N(3) N(4) C(7) C(9) . . . . 6.7(7) no N(3) C(6) C(5) C(4) . . . . -163.5(6) no N(4) N(3) Mn(1) N(10) . . . . -17.6(7) no N(4) N(3) C(6) C(5) . . . . -172.1(4) no N(4) C(7) C(8) N(5) . . . . 28.3(9) no N(4) C(7) C(8) C(10) . . . . -151.6(7) no N(5) Mn(2) N(6) C(11) . . . . 96(4) no N(5) Mn(2) N(6) C(15) . . . . -70(4) no N(5) Mn(2) N(8) N(9) . . . . -26.7(3) no N(5) Mn(2) N(8) C(16) . . . . -173.5(4) no N(5) C(8) C(7) C(9) . . . . -150.7(7) no N(6) Mn(2) N(5) C(8) . . . . 159(3) no N(6) Mn(2) N(8) N(9) . . . . 159.8(3) no N(6) Mn(2) N(8) C(16) . . . . 13.0(4) no N(6) C(11) C(12) C(13) . . . . 0.9(7) no N(6) C(15) C(14) C(13) . . . . 0.6(6) no N(6) C(15) C(16) N(7) . . . . -156.6(3) no N(6) C(15) C(16) N(8) . . . . 25.1(5) no N(7) C(16) N(8) N(9) . . . . 7.4(5) no N(7) C(16) C(15) C(14) . . . . 24.0(5) no N(8) Mn(2) N(5) C(8) . . . . 89.0(6) no N(8) Mn(2) N(6) C(11) . . . . 168.0(3) no N(8) Mn(2) N(6) C(15) . . . . 1.2(3) no N(8) N(9) C(17) C(18) . . . . -173.6(3) no N(8) N(9) C(17) C(19) . . . . 6.3(5) no N(8) C(16) C(15) C(14) . . . . -154.3(4) no N(9) N(8) C(16) C(15) . . . . -174.4(3) no N(9) C(17) C(18) N(10) . . . . 27.5(5) no N(9) C(17) C(18) C(20) . . . . -151.5(4) no N(10) Mn(1) N(1) C(1) . . . . 2(9) no N(10) Mn(1) N(1) C(5) . . . . -172(9) no N(10) Mn(1) N(3) C(6) . . . . -169.3(5) no N(10) C(18) C(17) C(19) . . . . -152.4(4) no C(1) N(1) C(5) C(4) . . . . -1(1) no C(1) N(1) C(5) C(6) . . . . -179.5(6) no C(1) C(2) C(3) C(4) . . . . 2(1) no C(2) C(1) N(1) C(5) . . . . 1(1) no C(2) C(3) C(4) C(5) . . . . -2(1) no C(3) C(4) C(5) C(6) . . . . -179.8(6) no C(6) N(3) N(4) C(7) . . . . -138.6(5) no C(9) C(7) C(8) C(10) . . . . 29.5(9) no C(11) N(6) C(15) C(14) . . . . -1.4(6) no C(11) N(6) C(15) C(16) . . . . 179.2(3) no C(11) C(12) C(13) C(14) . . . . -1.8(7) no C(12) C(11) N(6) C(15) . . . . 0.6(6) no C(12) C(13) C(14) C(15) . . . . 1.1(7) no C(13) C(14) C(15) C(16) . . . . 179.9(4) no C(16) N(8) N(9) C(17) . . . . -137.2(3) no C(19) C(17) C(18) C(20) . . . . 28.6(5) no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'O(1)' 'H(1O)' 'Cl(3)' '1.14' '1.89' '2.996(9)' '161.5' '.' 'O(2)' 'H(2O)' 'Cl(1)' '0.94' '2.26' '3.007(5)' '136.0' '.' 'N(2)' 'H(2NA)' 'Cl(4)' '0.84' '2.52' '3.310(5)' '158.7' '.' 'N(2)' 'H(2NB)' 'Cl(2)' '0.90' '2.45' '3.35(1)' '173.8' '3_545' 'N(7)' 'H(7NA)' 'Cl(1)' '0.90' '2.59' '3.470(8)' '165.9' '3' 'N(7)' 'H(7NB)' 'Cl(2)' '0.85' '2.48' '3.33(1)' '176.6' '.' #==================================================================== data__x608(2) _database_code_CSD 158600 #==================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 19.277(5) _cell_length_b 21.233(5) _cell_length_c 12.479(3) _cell_angle_alpha 90 _cell_angle_beta 98.20(2) _cell_angle_gamma 90 _cell_volume 5055(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 29.4 _cell_measurement_theta_max 29.9 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'irregular' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1238.69 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H46.30 Cl4 N15 O22.65 Ni2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2546.00 _exptl_absorpt_coefficient_mu 3.696 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.818 _exptl_special_details ; The scan width was (1.68+0.14tan\q)\% with an \w scan speed of 8\% per minute (up to 11 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #==================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.32 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 6 0 -5 2 0 -4 2 -2 _diffrn_reflns_number 8018 _reflns_number_total 7764 _reflns_number_gt 5487 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03570 _diffrn_reflns_av_sigmaI/netI 0.068 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 60.12 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02082 _diffrn_orient_matrix_UB_12 0.03627 _diffrn_orient_matrix_UB_13 0.03541 _diffrn_orient_matrix_UB_21 0.01295 _diffrn_orient_matrix_UB_22 0.02889 _diffrn_orient_matrix_UB_23 -0.05726 _diffrn_orient_matrix_UB_31 -0.04632 _diffrn_orient_matrix_UB_32 -0.00823 _diffrn_orient_matrix_UB_33 -0.04498 #------------------------------------------------------------------------------ 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 C 0 120 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 185 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 60 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 90 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 8 -2.956 0.509 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #==================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(1) 0.34820(4) 0.23548(3) 0.20534(5) 0.0626(2) 1.000 . Uani d ? Ni(2) 0.39198(4) 0.24164(4) -0.06992(5) 0.0644(2) 1.000 . Uani d ? Cl(1) 0.61191(8) 0.08429(7) -0.0624(1) 0.0911(5) 1.000 . Uani d ? Cl(2) 0.56671(9) 0.12233(8) 0.4524(1) 0.1080(6) 1.000 . Uani d ? Cl(3) 0.1763(1) 0.0800(2) 0.6950(2) 0.180(1) 1.000 . Uani d ? Cl(4) 0.1409(1) 0.0457(1) 0.1899(2) 0.1307(8) 1.000 . Uani d ? O(1) 0.3083(2) 0.2798(2) -0.2981(3) 0.143(2) 1.000 . Uani d ? O(2) 0.5014(2) 0.3083(2) -0.1892(2) 0.088(1) 1.000 . Uani d ? O(3) 0.2282(2) 0.2805(2) 0.3257(2) 0.087(1) 1.000 . Uani d ? O(4) 0.6188(3) 0.1002(3) -0.1697(4) 0.167(2) 1.000 . Uani d ? O(5) 0.6758(2) 0.0597(2) -0.0130(4) 0.133(2) 1.000 . Uani d ? O(6) 0.5568(2) 0.0406(2) -0.0630(4) 0.129(2) 1.000 . Uani d ? O(7) 0.5953(3) 0.1360(2) -0.0087(5) 0.171(2) 1.000 . Uani d ? O(8) 0.6278(9) 0.1705(9) 0.424(1) 0.131(6) 0.250 S Uiso d ? O(9) 0.5832(5) 0.1060(4) 0.3570(7) 0.213(4) 0.750 S Uiso d ? O(10) 0.5346(4) 0.0596(4) 0.4550(6) 0.179(3) 0.750 S Uiso d ? O(11) 0.5179(3) 0.1662(3) 0.4391(5) 0.192(2) 1.000 . Uiso d ? O(12) 0.5778(8) 0.1107(7) 0.574(1) 0.093(4) 0.250 S Uiso d ? O(13) 0.6208(4) 0.1275(4) 0.5352(6) 0.236(3) 1.000 . Uiso d ? O(14) 0.1980(5) 0.0495(4) 0.6146(7) 0.235(4) 0.850 S Uiso d ? O(15) 0.118(1) 0.028(1) 0.625(2) 0.26(1) 0.300 S Uiso d ? O(16) 0.1106(5) 0.0949(5) 0.6771(8) 0.234(4) 0.800 S Uiso d ? O(17) 0.157(2) 0.105(2) 0.783(3) 0.24(1) 0.250 S Uiso d ? O(18) 0.1965(4) 0.0349(4) 0.7768(7) 0.251(3) 1.000 . Uiso d ? O(19) 0.2192(5) 0.1432(5) 0.7025(7) 0.242(4) 0.800 S Uiso d ? O(20) 0.176(1) -0.003(1) 0.152(2) 0.230(9) 0.350 S Uiso d ? O(21) 0.1658(5) -0.0137(5) 0.2399(8) 0.200(4) 0.700 S Uiso d ? O(22) 0.1333(5) 0.0650(5) 0.3009(9) 0.191(4) 0.600 S Uiso d ? O(23) 0.0704(8) 0.0533(7) 0.188(1) 0.226(6) 0.500 S Uiso d ? O(24) 0.0845(7) 0.0290(6) 0.113(1) 0.198(5) 0.550 S Uiso d ? O(25) 0.1866(3) 0.0885(3) 0.1626(5) 0.187(2) 1.000 . Uiso d ? O(26) 0.142(1) 0.021(1) 0.058(2) 0.22(1) 0.300 S Uiso d ? O(27) 0.0282(9) 0.0494(8) 0.439(1) 0.123(5) 0.250 S Uiso d ? O(28) 0.7613(8) 0.0989(7) 0.760(1) 0.194(6) 0.400 S Uiso d ? O(29) 0.9476(7) 0.0493(6) 0.423(1) 0.207(5) 0.500 S Uiso d ? O(30) 0.2964(6) 0.1778(6) 0.6191(9) 0.195(5) 0.500 S Uiso d ? O(31) 0.9367(4) 0.0946(4) 0.2420(6) 0.211(3) 0.750 S Uiso d ? O(32) 0.8724(6) 0.0268(6) 0.0967(9) 0.189(4) 0.500 S Uiso d ? O(33) 0.7944(4) 0.1190(3) 0.9164(6) 0.173(3) 0.750 S Uiso d ? N(1) 0.4048(2) 0.2869(2) 0.3278(3) 0.074(1) 1.000 . Uani d ? N(2) 0.4734(2) 0.0919(2) 0.1202(3) 0.081(1) 1.000 . Uani d ? N(3) 0.3687(2) 0.3183(2) 0.1272(3) 0.061(1) 1.000 . Uani d ? N(4) 0.3591(2) 0.3182(2) 0.0135(3) 0.060(1) 1.000 . Uani d ? N(5) 0.3246(2) 0.2906(2) -0.1861(3) 0.085(2) 1.000 . Uani d ? N(6) 0.3488(2) 0.1502(2) 0.2857(3) 0.069(1) 1.000 . Uani d ? N(7) 0.4559(3) 0.3968(2) 0.1305(4) 0.110(2) 1.000 . Uani d ? N(8) 0.4349(2) 0.1927(2) 0.1572(3) 0.060(1) 1.000 . Uani d ? N(9) 0.4616(2) 0.2149(2) 0.0675(3) 0.061(1) 1.000 . Uani d ? N(10) 0.4862(2) 0.2820(2) -0.0927(3) 0.068(1) 1.000 . Uani d ? N(11) 0.4033(2) 0.1607(2) -0.1568(3) 0.071(1) 1.000 . Uani d ? N(12) 0.2945(2) 0.0788(2) 0.0050(3) 0.078(1) 1.000 . Uani d ? N(13) 0.3156(2) 0.1848(2) -0.0247(3) 0.062(1) 1.000 . Uani d ? N(14) 0.2861(2) 0.2018(2) 0.0677(3) 0.058(1) 1.000 . Uani d ? N(15) 0.2477(2) 0.2600(2) 0.2301(3) 0.074(1) 1.000 . Uani d ? C(1) 0.4219(4) 0.2732(3) 0.4316(4) 0.106(2) 1.000 . Uani d ? C(2) 0.4536(5) 0.3098(5) 0.5055(7) 0.173(5) 1.000 . Uani d ? C(3) 0.4818(4) 0.3687(5) 0.4592(9) 0.170(4) 1.000 . Uani d ? C(4) 0.4734(4) 0.3826(3) 0.3627(5) 0.107(2) 1.000 . Uani d ? C(5) 0.4322(2) 0.3389(2) 0.2949(4) 0.069(2) 1.000 . Uani d ? C(6) 0.4160(2) 0.3532(2) 0.1778(4) 0.063(1) 1.000 . Uani d ? C(7) 0.3120(3) 0.3524(3) -0.0382(4) 0.076(2) 1.000 . Uani d ? C(8) 0.2754(3) 0.3982(4) 0.0135(5) 0.139(3) 1.000 . Uani d ? C(9) 0.2965(3) 0.3420(3) -0.1558(4) 0.084(2) 1.000 . Uani d ? C(10) 0.2519(3) 0.3807(3) -0.2300(5) 0.121(3) 1.000 . Uani d ? C(11) 0.3085(3) 0.1338(2) 0.3586(4) 0.086(2) 1.000 . Uani d ? C(12) 0.3132(3) 0.0737(3) 0.4052(5) 0.103(2) 1.000 . Uani d ? C(13) 0.3581(3) 0.0304(3) 0.3695(5) 0.106(2) 1.000 . Uani d ? C(14) 0.4004(3) 0.0478(3) 0.2963(5) 0.092(2) 1.000 . Uani d ? C(15) 0.3947(2) 0.1081(2) 0.2547(3) 0.069(2) 1.000 . Uani d ? C(16) 0.4374(2) 0.1324(2) 0.1728(4) 0.067(2) 1.000 . Uani d ? C(17) 0.5211(2) 0.2404(2) 0.0783(3) 0.064(1) 1.000 . Uani d ? C(18) 0.5721(3) 0.2418(2) 0.1804(4) 0.087(2) 1.000 . Uani d ? C(19) 0.5384(3) 0.2719(2) -0.0215(4) 0.074(2) 1.000 . Uani d ? C(21) 0.4441(3) 0.1504(3) -0.2323(4) 0.092(2) 1.000 . Uani d ? C(22) 0.4459(3) 0.0954(3) -0.2887(4) 0.100(2) 1.000 . Uani d ? C(23) 0.4062(3) 0.0455(3) -0.2609(5) 0.111(3) 1.000 . Uani d ? C(24) 0.3641(3) 0.0515(2) -0.1790(4) 0.081(2) 1.000 . Uani d ? C(25) 0.3634(2) 0.1100(2) -0.1296(4) 0.071(2) 1.000 . Uani d ? C(26) 0.3214(2) 0.1253(2) -0.0441(3) 0.063(1) 1.000 . Uani d ? C(27) 0.2186(3) 0.2142(2) 0.0585(4) 0.070(2) 1.000 . Uani d ? C(28) 0.1683(3) 0.2021(3) -0.0407(4) 0.105(2) 1.000 . Uani d ? C(29) 0.1965(3) 0.2402(2) 0.1600(4) 0.071(2) 1.000 . Uani d ? C(30) 0.1226(3) 0.2448(3) 0.1766(4) 0.091(2) 1.000 . Uani d ? C(31) 0.6130(3) 0.2911(3) -0.0298(4) 0.104(2) 1.000 . Uani d ? H(1) 0.1221 0.1926 -0.0247 0.100 1.000 . Uiso c ? H(1O) 0.2688 0.3079 -0.3753 0.168 1.000 . Uiso c ? H(2Na) 0.4716 0.0465 0.1377 0.094 1.000 . Uiso c ? H(2) 0.1628 0.2387 -0.0894 0.100 1.000 . Uiso c ? H(2Nb) 0.5003 0.1036 0.0666 0.094 1.000 . Uiso c ? H(3) 0.1822 0.1677 -0.0837 0.100 1.000 . Uiso c ? H(4) 0.2808 0.3950 0.0892 0.130 1.000 . Uiso c ? H(5) 0.2940 0.4415 -0.0016 0.130 1.000 . Uiso c ? H(6) 0.2264 0.4010 -0.0146 0.130 1.000 . Uiso c ? H(7Na) 0.4920 0.4215 0.1748 0.127 1.000 . Uiso c ? H(7Nb) 0.4510 0.4032 0.0540 0.127 1.000 . Uiso c ? H(7) 0.5499 0.2401 0.2422 0.094 1.000 . Uiso c ? H(8) 0.6040 0.2056 0.1821 0.094 1.000 . Uiso c ? H(9) 0.6013 0.2786 0.1830 0.094 1.000 . Uiso c ? H(10) 0.1178 0.2443 0.2515 0.096 1.000 . Uiso c ? H(11) 0.1006 0.2805 0.1430 0.096 1.000 . Uiso c ? H(12) 0.0972 0.2075 0.1443 0.096 1.000 . Uiso c ? H(12Na) 0.2677 0.0856 0.0635 0.093 1.000 . Uiso c ? H(12Nb) 0.3016 0.0351 -0.0147 0.093 1.000 . Uiso c ? H(13) 0.6400 0.2945 0.0407 0.106 1.000 . Uiso c ? H(14) 0.6363 0.2571 -0.0667 0.106 1.000 . Uiso c ? H(15) 0.6164 0.3279 -0.0690 0.106 1.000 . Uiso c ? H(16) 0.2235 0.4103 -0.1923 0.124 1.000 . Uiso c ? H(17) 0.2789 0.4095 -0.2711 0.124 1.000 . Uiso c ? H(18) 0.2196 0.3595 -0.2823 0.124 1.000 . Uiso c ? H(19) 0.4593 0.3033 0.5875 0.189 1.000 . Uiso c ? H(20) 0.3336 0.0179 -0.1601 0.095 1.000 . Uiso c ? H(21) 0.2749 0.1662 0.3814 0.093 1.000 . Uiso c ? H(22) 0.4062 0.2310 0.4537 0.095 1.000 . Uiso c ? H(23) 0.4908 0.4224 0.3366 0.104 1.000 . Uiso c ? H(24) 0.2833 0.0619 0.4577 0.119 1.000 . Uiso c ? H(25) 0.3547 -0.0114 0.3958 0.135 1.000 . Uiso c ? H(26) 0.4753 0.0893 -0.3447 0.112 1.000 . Uiso c ? H(27O) 0.0718 0.0291 0.4406 0.142 0.250 S Uiso d ? H(27) 0.4753 0.1855 -0.2501 0.109 1.000 . Uiso c ? H(28) 0.4070 0.0039 -0.3023 0.120 1.000 . Uiso c ? H(28O) 0.7468 0.0906 0.7097 0.204 0.400 S Uiso d ? H(29O) 0.9254 0.0327 0.4501 0.254 0.500 S Uiso d ? H(29) 0.4358 0.0177 0.2764 0.111 1.000 . Uiso c ? H(30) 0.5174 0.3921 0.5140 0.178 1.000 . Uiso c ? H(31O1) 0.9210 0.0943 0.2967 0.257 0.750 S Uiso d ? H(31Ob) 0.8974 0.1077 0.1734 0.257 0.750 S Uiso d ? H(32Oa) 0.8347 0.0390 0.0695 0.231 0.500 S Uiso d ? H(32Ob) 0.9154 0.0071 0.1035 0.231 0.500 S Uiso d ? H(33Oa) 0.7820 0.1075 0.8564 0.212 0.750 S Uiso d ? H(33Ob) 0.8044 0.1609 0.9781 0.212 0.750 S Uiso 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 Ni(1) 0.0762(5) 0.0604(5) 0.0537(4) -0.0031(4) 0.0180(4) 0.0029(4) Ni(2) 0.0722(5) 0.0693(5) 0.0544(4) 0.0010(4) 0.0184(4) 0.0043(4) Cl(1) 0.096(1) 0.0652(8) 0.118(1) -0.0048(8) 0.0348(9) 0.0011(8) Cl(2) 0.116(1) 0.114(1) 0.087(1) 0.019(1) -0.0066(9) 0.0058(9) Cl(3) 0.153(2) 0.249(3) 0.130(2) 0.082(2) -0.007(2) -0.021(2) Cl(4) 0.116(1) 0.108(1) 0.173(2) -0.010(1) 0.035(1) 0.009(1) O(1) 0.166(4) 0.171(5) 0.094(3) -0.012(4) 0.030(3) -0.014(3) O(2) 0.099(2) 0.106(3) 0.068(2) -0.006(2) 0.041(2) 0.011(2) O(3) 0.099(2) 0.100(3) 0.071(2) 0.007(2) 0.048(2) -0.006(2) O(4) 0.162(5) 0.211(6) 0.136(4) -0.047(4) 0.047(3) 0.040(4) O(5) 0.095(3) 0.116(3) 0.190(5) 0.017(3) 0.029(3) 0.024(3) O(6) 0.129(3) 0.099(3) 0.171(4) -0.034(3) 0.063(3) -0.021(3) O(7) 0.153(4) 0.099(3) 0.278(7) -0.004(3) 0.086(4) -0.065(4) N(1) 0.092(3) 0.058(2) 0.070(3) 0.007(2) 0.008(2) -0.011(2) N(2) 0.089(3) 0.054(2) 0.101(3) 0.010(2) 0.015(2) 0.006(2) N(3) 0.073(2) 0.050(2) 0.063(2) 0.002(2) 0.019(2) 0.004(2) N(4) 0.061(2) 0.063(2) 0.058(2) -0.002(2) 0.016(2) -0.000(2) N(5) 0.092(3) 0.105(4) 0.058(3) 0.000(3) 0.011(2) 0.017(2) N(6) 0.083(3) 0.062(2) 0.061(2) -0.011(2) 0.013(2) 0.012(2) N(7) 0.123(4) 0.111(4) 0.098(3) -0.046(3) 0.021(3) -0.011(3) N(8) 0.073(2) 0.057(2) 0.054(2) -0.004(2) 0.017(2) 0.004(2) N(9) 0.067(2) 0.064(2) 0.053(2) 0.003(2) 0.015(2) 0.003(2) N(10) 0.079(3) 0.071(3) 0.060(2) -0.000(2) 0.032(2) 0.006(2) N(11) 0.076(3) 0.079(3) 0.061(2) 0.008(2) 0.018(2) -0.002(2) N(12) 0.089(3) 0.071(3) 0.075(3) -0.006(2) 0.016(2) -0.010(2) N(13) 0.053(2) 0.081(3) 0.054(2) -0.001(2) 0.017(2) -0.008(2) N(14) 0.066(2) 0.049(2) 0.060(2) -0.009(2) 0.014(2) 0.002(2) N(15) 0.093(3) 0.072(3) 0.065(3) -0.003(2) 0.039(2) 0.003(2) C(1) 0.194(7) 0.072(4) 0.042(3) -0.021(4) -0.015(3) -0.010(3) C(2) 0.176(9) 0.22(1) 0.130(7) 0.057(8) 0.032(6) 0.019(8) C(3) 0.117(6) 0.17(1) 0.22(1) -0.017(6) 0.021(8) -0.105(9) C(4) 0.141(6) 0.107(5) 0.066(4) 0.005(4) -0.010(4) -0.008(4) C(5) 0.058(3) 0.063(3) 0.083(4) 0.002(2) 0.001(2) -0.019(3) C(6) 0.070(3) 0.045(3) 0.077(3) 0.002(2) 0.020(3) -0.003(2) C(7) 0.064(3) 0.090(4) 0.078(4) 0.011(3) 0.019(3) 0.008(3) C(8) 0.092(4) 0.220(8) 0.102(5) 0.071(5) 0.004(4) 0.011(5) C(9) 0.082(4) 0.092(4) 0.080(4) 0.011(3) 0.018(3) 0.019(3) C(10) 0.100(4) 0.112(5) 0.152(6) 0.008(4) 0.023(4) 0.054(5) C(11) 0.115(4) 0.073(3) 0.072(3) -0.007(3) 0.021(3) 0.021(3) C(12) 0.112(5) 0.099(5) 0.104(4) -0.022(4) 0.035(4) 0.033(4) C(13) 0.109(5) 0.087(4) 0.120(5) -0.010(4) 0.010(4) 0.036(4) C(14) 0.089(4) 0.077(4) 0.110(4) 0.000(3) 0.016(3) 0.020(3) C(15) 0.075(3) 0.072(3) 0.057(3) -0.006(3) 0.004(2) 0.018(2) C(16) 0.060(3) 0.078(3) 0.061(3) 0.000(3) 0.008(2) -0.007(3) C(17) 0.065(3) 0.073(3) 0.059(3) 0.003(3) 0.020(2) -0.005(2) C(18) 0.090(4) 0.090(4) 0.080(3) -0.006(3) 0.009(3) -0.005(3) C(19) 0.076(3) 0.075(3) 0.075(3) -0.002(3) 0.029(3) -0.008(3) C(21) 0.092(4) 0.120(5) 0.070(3) 0.001(4) 0.026(3) 0.004(3) C(22) 0.108(5) 0.121(5) 0.074(4) 0.028(4) 0.025(3) -0.029(4) C(23) 0.115(5) 0.102(5) 0.108(5) 0.032(4) -0.003(4) -0.045(4) C(24) 0.085(3) 0.079(4) 0.078(3) -0.003(3) 0.011(3) -0.030(3) C(25) 0.064(3) 0.084(4) 0.064(3) 0.007(3) 0.005(2) -0.002(3) C(26) 0.068(3) 0.067(3) 0.054(3) -0.004(3) 0.004(2) -0.003(2) C(27) 0.083(3) 0.072(3) 0.059(3) -0.001(3) 0.020(3) 0.008(2) C(28) 0.077(4) 0.171(6) 0.064(3) 0.018(4) 0.003(3) 0.000(4) C(29) 0.076(3) 0.064(3) 0.076(3) -0.001(3) 0.025(3) 0.014(3) C(30) 0.076(3) 0.124(5) 0.080(3) 0.010(3) 0.034(3) 0.024(3) C(31) 0.084(4) 0.141(6) 0.095(4) -0.018(4) 0.034(3) 0.011(4) #==================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|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 5487 _refine_ls_number_parameters 627 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1462 _refine_ls_R_factor_gt 0.1100 _refine_ls_wR_factor_all 0.1130 _refine_ls_wR_factor_ref 0.1120 _refine_ls_goodness_of_fit_all 4.734 _refine_ls_goodness_of_fit_ref 5.570 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.89 _refine_diff_density_max 0.89 #==================================================================== #========= # MOLECULAR GEOMETRY _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 Ni(1) N(1) 2.059(9) . . ? Ni(1) N(3) 2.075(8) . . ? Ni(1) N(6) 2.068(8) . . ? Ni(1) N(8) 2.066(8) . . ? Ni(1) N(14) 2.075(8) . . ? Ni(1) N(15) 2.072(9) . . ? Ni(2) N(4) 2.077(8) . . ? Ni(2) N(5) 2.08(1) . . ? Ni(2) N(9) 2.099(8) . . ? Ni(2) N(10) 2.064(9) . . ? Ni(2) N(11) 2.060(9) . . ? Ni(2) N(13) 2.044(8) . . ? Cl(1) O(4) 1.41(1) . . ? Cl(1) O(5) 1.40(1) . . ? Cl(1) O(6) 1.410(9) . . ? Cl(1) O(7) 1.35(1) . . ? Cl(2) O(8) 1.64(4) . . ? Cl(2) O(9) 1.32(2) . . ? Cl(2) O(10) 1.47(2) . . ? Cl(2) O(11) 1.32(1) . . ? Cl(2) O(12) 1.52(3) . . ? Cl(2) O(13) 1.36(2) . . ? Cl(3) O(14) 1.31(2) . . ? Cl(3) O(15) 1.72(7) . . ? Cl(3) O(16) 1.29(2) . . ? Cl(3) O(17) 1.32(8) . . ? Cl(3) O(18) 1.41(2) . . ? Cl(3) O(19) 1.57(2) . . ? Cl(4) O(20) 1.36(6) . . ? Cl(4) O(21) 1.46(2) . . ? Cl(4) O(22) 1.47(2) . . ? Cl(4) O(23) 1.36(4) . . ? Cl(4) O(24) 1.39(3) . . ? Cl(4) O(25) 1.34(1) . . ? Cl(4) O(26) 1.73(6) . . ? O(1) N(5) 1.41(1) . . ? O(1) H(1O) 1.28 . . no O(2) N(10) 1.395(9) . . ? O(3) N(15) 1.371(9) . . ? O(8) O(13) 1.68(4) . . ? O(12) O(13) 1.08(3) . . ? O(14) O(15) 1.64(6) . . ? O(15) O(16) 1.57(6) . . ? O(16) O(17) 1.50(7) . . ? O(17) O(18) 1.69(7) . . ? O(20) O(21) 1.17(6) . . ? O(20) O(26) 1.36(7) . . ? O(22) O(23) 1.74(4) . . ? O(23) O(24) 1.13(4) . . ? O(24) O(26) 1.39(5) . . ? O(27) O(29) 1.54(4) . . ? O(27) H(27O) 0.94 . . no O(28) H(28O) 0.67 . . no O(28) H(33Oa 1.23 . . no O(29) H(29O) 0.68 . . no O(31) H(31Oa 0.78 . . no O(31) H(31Ob 1.09 . . no O(32) H(32Oa 0.80 . . no O(32) H(32Ob 0.92 . . no O(33) H(33Oa 0.79 . . no O(33) H(33Ob 1.17 . . no N(1) C(1) 1.32(1) . . ? N(1) C(5) 1.31(1) . . ? N(2) C(16) 1.33(1) . . ? N(2) H(2Na) 0.99 . . no N(2) H(2Nb) 0.94 . . no N(3) N(4) 1.40(1) . . ? N(3) C(6) 1.27(1) . . ? N(4) C(7) 1.27(1) . . ? N(5) C(9) 1.30(1) . . ? N(6) C(11) 1.33(1) . . ? N(6) C(15) 1.35(1) . . ? N(7) C(6) 1.39(1) . . ? N(7) H(7Na) 0.98 . . no N(7) H(7Nb) 0.96 . . no N(8) N(9) 1.38(1) . . ? N(8) C(16) 1.29(1) . . ? N(9) C(17) 1.26(1) . . ? N(10) C(19) 1.26(1) . . ? N(11) C(21) 1.33(1) . . ? N(11) C(25) 1.39(1) . . ? N(12) C(26) 1.31(1) . . ? N(12) H(12Na 0.96 . . no N(12) H(12Nb 0.97 . . no N(13) N(14) 1.40(1) . . ? N(13) C(26) 1.29(1) . . ? N(14) C(27) 1.32(1) . . ? N(15) C(29) 1.29(1) . . ? C(1) C(2) 1.29(3) . . ? C(1) H(22) 1.00 . . no C(2) C(3) 1.51(3) . . ? C(2) H(19) 1.02 . . no C(3) C(4) 1.23(3) . . ? C(3) H(30) 1.03 . . no C(4) C(5) 1.42(2) . . ? C(4) H(23) 0.98 . . no C(5) C(6) 1.48(1) . . ? C(7) C(8) 1.41(2) . . ? C(7) C(9) 1.47(2) . . ? C(8) H(4) 0.94 . . no C(8) H(5) 1.02 . . no C(8) H(6) 0.96 . . no C(9) C(10) 1.43(2) . . ? C(10) H(16) 1.00 . . no C(10) H(17) 0.99 . . no C(10) H(18) 0.95 . . no C(11) C(12) 1.40(2) . . ? C(11) H(21) 1.01 . . no C(12) C(13) 1.38(2) . . ? C(12) H(24) 0.97 . . no C(13) C(14) 1.36(2) . . ? C(13) H(25) 0.95 . . no C(14) C(15) 1.38(1) . . ? C(14) H(29) 0.99 . . no C(15) C(16) 1.49(1) . . ? C(17) C(18) 1.49(1) . . ? C(17) C(19) 1.49(1) . . ? C(18) H(7) 0.93 . . no C(18) H(8) 0.98 . . no C(18) H(9) 0.96 . . no C(19) C(31) 1.51(1) . . ? C(21) C(22) 1.37(2) . . ? C(21) H(27) 1.00 . . no C(22) C(23) 1.38(2) . . ? C(22) H(26) 0.97 . . no C(23) C(24) 1.40(2) . . ? C(23) H(28) 1.02 . . no C(24) C(25) 1.39(1) . . ? C(24) H(20) 0.97 . . no C(25) C(26) 1.47(1) . . ? C(27) C(28) 1.48(1) . . ? C(27) C(29) 1.50(1) . . ? C(28) H(1) 0.96 . . no C(28) H(2) 0.98 . . no C(28) H(3) 0.97 . . no C(29) C(30) 1.47(1) . . ? C(30) H(10) 0.95 . . no C(30) H(11) 0.94 . . no C(30) H(12) 0.99 . . no C(31) H(13) 0.96 . . no C(31) H(14) 1.00 . . no C(31) H(15) 0.93 . . no #------------------------------------------------------------------------------ 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) Ni(1) N(3) 77.5(4) . . . ? N(1) Ni(1) N(6) 98.0(4) . . . ? N(1) Ni(1) N(8) 94.8(3) . . . ? N(1) Ni(1) N(14) 168.1(3) . . . ? N(1) Ni(1) N(15) 99.4(4) . . . ? N(3) Ni(1) N(6) 168.7(4) . . . ? N(3) Ni(1) N(8) 91.2(3) . . . ? N(3) Ni(1) N(14) 91.7(3) . . . ? N(3) Ni(1) N(15) 95.8(3) . . . ? N(6) Ni(1) N(8) 78.8(3) . . . ? N(6) Ni(1) N(14) 93.6(3) . . . ? N(6) Ni(1) N(15) 95.1(4) . . . ? N(8) Ni(1) N(14) 90.2(3) . . . ? N(8) Ni(1) N(15) 165.2(4) . . . ? N(14) Ni(1) N(15) 76.6(4) . . . ? N(4) Ni(2) N(5) 75.8(4) . . . ? N(4) Ni(2) N(9) 90.4(3) . . . ? N(4) Ni(2) N(10) 94.7(3) . . . ? N(4) Ni(2) N(11) 168.3(3) . . . ? N(4) Ni(2) N(13) 92.3(3) . . . ? N(5) Ni(2) N(9) 165.2(4) . . . ? N(5) Ni(2) N(10) 99.8(4) . . . ? N(5) Ni(2) N(11) 98.7(4) . . . ? N(5) Ni(2) N(13) 94.9(4) . . . ? N(9) Ni(2) N(10) 75.7(3) . . . ? N(9) Ni(2) N(11) 95.8(3) . . . ? N(9) Ni(2) N(13) 90.9(3) . . . ? N(10) Ni(2) N(11) 96.5(4) . . . ? N(10) Ni(2) N(13) 164.9(4) . . . ? N(11) Ni(2) N(13) 77.7(3) . . . ? O(4) Cl(1) O(5) 108.2(7) . . . ? O(4) Cl(1) O(6) 109.1(7) . . . ? O(4) Cl(1) O(7) 109.8(8) . . . ? O(5) Cl(1) O(6) 111.9(7) . . . ? O(5) Cl(1) O(7) 110.0(8) . . . ? O(6) Cl(1) O(7) 107.8(7) . . . ? O(8) Cl(2) O(9) 72(2) . . . ? O(8) Cl(2) O(10) 153(2) . . . ? O(8) Cl(2) O(11) 93(2) . . . ? O(8) Cl(2) O(12) 108(2) . . . ? O(8) Cl(2) O(13) 67(1) . . . ? O(9) Cl(2) O(10) 86(1) . . . ? O(9) Cl(2) O(11) 109(1) . . . ? O(9) Cl(2) O(12) 147(2) . . . ? O(9) Cl(2) O(13) 117(1) . . . ? O(10) Cl(2) O(11) 110.3(9) . . . ? O(10) Cl(2) O(12) 80(2) . . . ? O(10) Cl(2) O(13) 110(1) . . . ? O(11) Cl(2) O(12) 104(2) . . . ? O(11) Cl(2) O(13) 120(1) . . . ? O(12) Cl(2) O(13) 43(1) . . . ? O(14) Cl(3) O(15) 64(2) . . . ? O(14) Cl(3) O(16) 114(2) . . . ? O(14) Cl(3) O(17) 174(4) . . . ? O(14) Cl(3) O(18) 98(1) . . . ? O(14) Cl(3) O(19) 104(1) . . . ? O(15) Cl(3) O(16) 61(2) . . . ? O(15) Cl(3) O(17) 116(4) . . . ? O(15) Cl(3) O(18) 92(2) . . . ? O(15) Cl(3) O(19) 151(2) . . . ? O(16) Cl(3) O(17) 70(3) . . . ? O(16) Cl(3) O(18) 117(1) . . . ? O(16) Cl(3) O(19) 107(2) . . . ? O(17) Cl(3) O(18) 76(3) . . . ? O(17) Cl(3) O(19) 79(3) . . . ? O(18) Cl(3) O(19) 116(1) . . . ? O(20) Cl(4) O(21) 49(3) . . . ? O(20) Cl(4) O(22) 132(3) . . . ? O(20) Cl(4) O(23) 129(3) . . . ? O(20) Cl(4) O(24) 86(3) . . . ? O(20) Cl(4) O(25) 93(2) . . . ? O(20) Cl(4) O(26) 50(3) . . . ? O(21) Cl(4) O(22) 85(1) . . . ? O(21) Cl(4) O(23) 112(2) . . . ? O(21) Cl(4) O(24) 105(2) . . . ? O(21) Cl(4) O(25) 120(1) . . . ? O(21) Cl(4) O(26) 96(2) . . . ? O(22) Cl(4) O(23) 76(2) . . . ? O(22) Cl(4) O(24) 123(2) . . . ? O(22) Cl(4) O(25) 102(1) . . . ? O(22) Cl(4) O(26) 175(2) . . . ? O(23) Cl(4) O(24) 49(2) . . . ? O(23) Cl(4) O(25) 127(2) . . . ? O(23) Cl(4) O(26) 99(2) . . . ? O(24) Cl(4) O(25) 118(2) . . . ? O(24) Cl(4) O(26) 51(2) . . . ? O(25) Cl(4) O(26) 82(2) . . . ? N(5) O(1) H(1O) 133.9 . . . no Cl(2) O(8) O(13) 49(1) . . . ? Cl(2) O(12) O(13) 60(2) . . . ? Cl(2) O(13) O(8) 64(2) . . . ? Cl(2) O(13) O(12) 76(2) . . . ? O(8) O(13) O(12) 135(3) . . . ? Cl(3) O(14) O(15) 70(3) . . . ? Cl(3) O(15) O(14) 46(2) . . . ? Cl(3) O(15) O(16) 46(2) . . . ? O(14) O(15) O(16) 86(4) . . . ? Cl(3) O(16) O(15) 73(3) . . . ? Cl(3) O(16) O(17) 56(3) . . . ? O(15) O(16) O(17) 115(4) . . . ? Cl(3) O(17) O(16) 54(3) . . . ? Cl(3) O(17) O(18) 54(3) . . . ? O(16) O(17) O(18) 93(4) . . . ? Cl(3) O(18) O(17) 50(3) . . . ? Cl(4) O(20) O(21) 70(3) . . . ? Cl(4) O(20) O(26) 79(4) . . . ? O(21) O(20) O(26) 140(6) . . . ? Cl(4) O(21) O(20) 61(3) . . . ? Cl(4) O(22) O(23) 49(1) . . . ? Cl(4) O(23) O(22) 55(2) . . . ? Cl(4) O(23) O(24) 67(3) . . . ? O(22) O(23) O(24) 121(4) . . . ? Cl(4) O(24) O(23) 65(3) . . . ? Cl(4) O(24) O(26) 77(3) . . . ? O(23) O(24) O(26) 140(5) . . . ? Cl(4) O(26) O(20) 50(3) . . . ? Cl(4) O(26) O(24) 52(2) . . . ? O(20) O(26) O(24) 87(4) . . . ? O(29) O(27) H(27O) 152.1 1_455 1_455 1_455 no H(28O) O(28) H(33Oa 170.9 . . . no O(27) O(29) H(29O) 129.5 1_655 1_655 1_655 no H(31Oa O(31) H(31Ob 111.9 . . . no H(32Oa O(32) H(32Ob 159.5 . . . no H(33Oa O(33) H(33Ob 148.6 . . . no Ni(1) N(1) C(1) 129.9(9) . . . ? Ni(1) N(1) C(5) 114.1(8) . . . ? C(1) N(1) C(5) 116(1) . . . ? C(16) N(2) H(2Na) 118.8 . . . no C(16) N(2) H(2Nb) 124.1 . . . no H(2Na) N(2) H(2Nb) 117.1 . . . no Ni(1) N(3) N(4) 117.8(6) . . . ? Ni(1) N(3) C(6) 115.6(7) . . . ? N(4) N(3) C(6) 118.9(9) . . . ? Ni(2) N(4) N(3) 120.2(6) . . . ? Ni(2) N(4) C(7) 116.2(8) . . . ? N(3) N(4) C(7) 119.7(9) . . . ? Ni(2) N(5) O(1) 129.8(9) . . . ? Ni(2) N(5) C(9) 117.5(9) . . . ? O(1) N(5) C(9) 112(1) . . . ? Ni(1) N(6) C(11) 126.9(8) . . . ? Ni(1) N(6) C(15) 113.6(7) . . . ? C(11) N(6) C(15) 119(1) . . . ? C(6) N(7) H(7Na) 120.7 . . . no C(6) N(7) H(7Nb) 122.5 . . . no H(7Na) N(7) H(7Nb) 116.7 . . . no Ni(1) N(8) N(9) 119.7(6) . . . ? Ni(1) N(8) C(16) 114.0(7) . . . ? N(9) N(8) C(16) 116.7(9) . . . ? Ni(2) N(9) N(8) 119.1(6) . . . ? Ni(2) N(9) C(17) 115.9(7) . . . ? N(8) N(9) C(17) 120.0(9) . . . ? Ni(2) N(10) O(2) 125.5(7) . . . ? Ni(2) N(10) C(19) 117.4(8) . . . ? O(2) N(10) C(19) 115.6(9) . . . ? Ni(2) N(11) C(21) 129.0(9) . . . ? Ni(2) N(11) C(25) 114.5(7) . . . ? C(21) N(11) C(25) 117(1) . . . ? C(26) N(12) H(12Na 122.2 . . . no C(26) N(12) H(12Nb 121.5 . . . no H(12Na N(12) H(12Nb 116.4 . . . no Ni(2) N(13) N(14) 117.8(6) . . . ? Ni(2) N(13) C(26) 116.1(7) . . . ? N(14) N(13) C(26) 117.5(9) . . . ? Ni(1) N(14) N(13) 121.0(6) . . . ? Ni(1) N(14) C(27) 116.8(7) . . . ? N(13) N(14) C(27) 119.4(8) . . . ? Ni(1) N(15) O(3) 126.0(7) . . . ? Ni(1) N(15) C(29) 117.3(7) . . . ? O(3) N(15) C(29) 114.4(9) . . . ? N(1) C(1) C(2) 126(2) . . . ? N(1) C(1) H(22) 115.2 . . . no C(2) C(1) H(22) 118.4 . . . no C(1) C(2) C(3) 113(2) . . . ? C(1) C(2) H(19) 127.3 . . . no C(3) C(2) H(19) 120.1 . . . no C(2) C(3) C(4) 125(2) . . . ? C(2) C(3) H(30) 112.9 . . . no C(4) C(3) H(30) 121.3 . . . no C(3) C(4) C(5) 114(2) . . . ? C(3) C(4) H(23) 121.8 . . . no C(5) C(4) H(23) 123.6 . . . no N(1) C(5) C(4) 125(1) . . . ? N(1) C(5) C(6) 116(1) . . . ? C(4) C(5) C(6) 118(1) . . . ? N(3) C(6) N(7) 125(1) . . . ? N(3) C(6) C(5) 114(1) . . . ? N(7) C(6) C(5) 120(1) . . . ? N(4) C(7) C(8) 122(1) . . . ? N(4) C(7) C(9) 117(1) . . . ? C(8) C(7) C(9) 121(1) . . . ? C(7) C(8) H(4) 114.9 . . . no C(7) C(8) H(5) 109.0 . . . no C(7) C(8) H(6) 113.9 . . . no H(4) C(8) H(5) 105.1 . . . no H(4) C(8) H(6) 109.6 . . . no H(5) C(8) H(6) 103.4 . . . no N(5) C(9) C(7) 112(1) . . . ? N(5) C(9) C(10) 122(1) . . . ? C(7) C(9) C(10) 125(1) . . . ? C(9) C(10) H(16) 112.2 . . . no C(9) C(10) H(17) 112.1 . . . no C(9) C(10) H(18) 116.7 . . . no H(16) C(10) H(17) 102.6 . . . no H(16) C(10) H(18) 105.9 . . . no H(17) C(10) H(18) 106.2 . . . no N(6) C(11) C(12) 121(1) . . . ? N(6) C(11) H(21) 118.3 . . . no C(12) C(11) H(21) 120.6 . . . no C(11) C(12) C(13) 119(1) . . . ? C(11) C(12) H(24) 120.5 . . . no C(13) C(12) H(24) 120.6 . . . no C(12) C(13) C(14) 120(1) . . . ? C(12) C(13) H(25) 115.7 . . . no C(14) C(13) H(25) 124.3 . . . no C(13) C(14) C(15) 119(1) . . . ? C(13) C(14) H(29) 119.4 . . . no C(15) C(14) H(29) 121.6 . . . no N(6) C(15) C(14) 122(1) . . . ? N(6) C(15) C(16) 114(1) . . . ? C(14) C(15) C(16) 124(1) . . . ? N(2) C(16) N(8) 125(1) . . . ? N(2) C(16) C(15) 119(1) . . . ? N(8) C(16) C(15) 116(1) . . . ? N(9) C(17) C(18) 125(1) . . . ? N(9) C(17) C(19) 114(1) . . . ? C(18) C(17) C(19) 120(1) . . . ? C(17) C(18) H(7) 112.4 . . . no C(17) C(18) H(8) 109.7 . . . no C(17) C(18) H(9) 110.8 . . . no H(7) C(18) H(8) 108.1 . . . no H(7) C(18) H(9) 109.9 . . . no H(8) C(18) H(9) 105.8 . . . no N(10) C(19) C(17) 114(1) . . . ? N(10) C(19) C(31) 125(1) . . . ? C(17) C(19) C(31) 120(1) . . . ? N(11) C(21) C(22) 125(1) . . . ? N(11) C(21) H(27) 118.0 . . . no C(22) C(21) H(27) 117.4 . . . no C(21) C(22) C(23) 118(1) . . . ? C(21) C(22) H(26) 123.1 . . . no C(23) C(22) H(26) 118.8 . . . no C(22) C(23) C(24) 121(1) . . . ? C(22) C(23) H(28) 119.0 . . . no C(24) C(23) H(28) 120.0 . . . no C(23) C(24) C(25) 117(1) . . . ? C(23) C(24) H(20) 122.9 . . . no C(25) C(24) H(20) 120.2 . . . no N(11) C(25) C(24) 123(1) . . . ? N(11) C(25) C(26) 113(1) . . . ? C(24) C(25) C(26) 124(1) . . . ? N(12) C(26) N(13) 127(1) . . . ? N(12) C(26) C(25) 118(1) . . . ? N(13) C(26) C(25) 115(1) . . . ? N(14) C(27) C(28) 124(1) . . . ? N(14) C(27) C(29) 113(1) . . . ? C(28) C(27) C(29) 123(1) . . . ? C(27) C(28) H(1) 112.2 . . . no C(27) C(28) H(2) 112.3 . . . no C(27) C(28) H(3) 113.2 . . . no H(1) C(28) H(2) 105.9 . . . no H(1) C(28) H(3) 107.2 . . . no H(2) C(28) H(3) 105.5 . . . no N(15) C(29) C(27) 114(1) . . . ? N(15) C(29) C(30) 123(1) . . . ? C(27) C(29) C(30) 123(1) . . . ? C(29) C(30) H(10) 111.6 . . . no C(29) C(30) H(11) 112.0 . . . no C(29) C(30) H(12) 108.8 . . . no H(10) C(30) H(11) 110.4 . . . no H(10) C(30) H(12) 106.3 . . . no H(11) C(30) H(12) 107.5 . . . no C(19) C(31) H(13) 110.7 . . . no C(19) C(31) H(14) 109.4 . . . no C(19) C(31) H(15) 113.7 . . . no H(13) C(31) H(14) 104.9 . . . no H(13) C(31) H(15) 110.4 . . . no H(14) C(31) H(15) 107.3 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(3) O(30) 3.35(3) . . no O(1) O(30) 2.40(3) . 1_554 no O(1) O(19) 3.37(3) . 1_554 no O(2) O(31) 2.50(2) . 4_454 no O(2) C(30) 3.26(1) . 4_554 no O(2) O(27) 3.42(4) . 4_554 no O(2) O(29) 3.55(3) . 4_454 no O(3) O(33) 2.65(2) . 4_454 no O(3) O(28) 2.79(4) . 4_454 no O(3) O(4) 3.30(1) . 4_455 no O(3) C(31) 3.41(1) . 4_455 no O(4) O(28) 3.00(4) . 1_554 no O(4) O(12) 3.19(4) . 1_554 no O(4) O(33) 3.42(2) . 1_554 no O(4) C(22) 3.45(2) . . no O(4) C(21) 3.51(2) . . no O(4) C(14) 3.51(2) . 3_655 no O(5) O(33) 2.86(2) . 1_554 no O(5) N(12) 2.99(1) . 3_655 no O(5) C(24) 3.53(2) . 3_655 no O(5) O(28) 3.58(3) . 1_554 no O(6) N(2) 2.94(1) . 3_655 no O(6) N(2) 3.17(1) . . no O(6) O(6) 3.35(2) . 3_655 no O(6) C(22) 3.48(2) . . no O(6) C(23) 3.54(2) . . no O(7) C(17) 2.93(1) . . no O(7) C(19) 3.08(2) . . no O(7) N(2) 3.17(1) . . no O(7) C(31) 3.32(2) . . no O(7) N(9) 3.33(1) . . no O(7) C(18) 3.33(2) . . no O(8) C(28) 2.83(5) . 4 no O(8) C(8) 3.25(4) . 4 no O(8) C(27) 3.32(4) . 4 no O(8) C(18) 3.43(4) . . no O(8) C(10) 3.45(4) . 4 no O(8) C(9) 3.55(4) . 4 no O(8) C(7) 3.55(4) . 4 no O(8) C(29) 3.59(4) . 4 no O(9) N(2) 3.39(2) . . no O(9) C(16) 3.41(2) . . no O(9) C(23) 3.45(3) . 3_655 no O(9) C(10) 3.58(2) . 4 no O(10) C(14) 3.04(2) . . no O(10) O(10) 3.14(4) . 3_656 no O(10) C(13) 3.38(2) . 3_656 no O(10) C(13) 3.47(2) . . no O(10) C(15) 3.56(2) . . no O(10) C(23) 3.60(2) . 3_655 no O(11) C(1) 2.92(2) . . no O(11) C(15) 3.30(2) . . no O(11) C(2) 3.44(3) . . no O(11) N(1) 3.52(2) . . no O(11) C(16) 3.53(2) . . no O(11) N(6) 3.55(2) . . no O(12) C(13) 3.28(4) . 3_656 no O(12) C(22) 3.28(4) . 1_556 no O(12) C(30) 3.39(4) . 4 no O(13) C(8) 3.08(2) . 4 no O(13) C(30) 3.23(2) . 4 no O(13) C(29) 3.43(2) . 4 no O(13) C(13) 3.56(2) . 3_656 no O(14) O(30) 3.31(3) . . no O(14) O(29) 3.48(4) . 3_656 no O(15) O(29) 2.11(7) . 3_656 no O(15) O(27) 2.72(7) . . no O(15) O(27) 3.26(8) . 3_556 no O(15) O(31) 3.34(7) . 3_656 no O(15) N(7) 3.51(7) . 4_455 no O(16) N(7) 2.96(3) . 4_455 no O(16) O(27) 3.31(5) . . no O(16) O(29) 3.44(4) . 3_656 no O(16) C(31) 3.55(3) . 4_455 no O(16) C(18) 3.55(3) . 4_455 no O(17) C(28) 2.99(8) . 1_556 no O(17) O(32) 3.27(8) . 3_656 no O(17) C(26) 3.60(8) . 1_556 no O(17) N(12) 3.60(8) . 1_556 no O(18) O(32) 2.56(3) . 3_656 no O(18) C(24) 3.22(2) . 1_556 no O(18) N(12) 3.32(2) . 1_556 no O(18) C(10) 3.50(2) . 2_545 no O(18) C(26) 3.60(2) . 1_556 no O(19) O(30) 2.07(3) . . no O(19) C(25) 3.31(2) . 1_556 no O(19) C(26) 3.50(2) . 1_556 no O(19) C(24) 3.55(2) . 1_556 no O(19) C(31) 3.59(3) . 4_455 no O(20) O(28) 2.54(7) . 3_656 no O(20) O(33) 2.69(6) . 3_656 no O(20) O(32) 3.15(7) . 3_655 no O(20) N(12) 3.58(6) . . no O(21) O(28) 2.29(4) . 3_656 no O(21) O(33) 3.13(3) . 3_656 no O(21) C(6) 3.46(3) . 2_545 no O(21) C(4) 3.57(3) . 2_545 no O(21) N(7) 3.58(3) . 2_545 no O(22) O(27) 2.86(4) . . no O(22) C(12) 3.53(3) . . no O(23) O(31) 2.89(4) . 1_455 no O(23) O(27) 3.35(5) . . no O(23) C(3) 3.52(4) . 4_454 no O(24) O(32) 3.09(4) . 3_655 no O(24) C(4) 3.33(3) . 2_545 no O(24) C(3) 3.35(4) . 4_454 no O(25) N(12) 3.07(2) . . no O(25) C(27) 3.07(2) . . no O(25) C(29) 3.23(2) . . no O(25) C(11) 3.29(2) . . no O(25) N(14) 3.39(2) . . no O(25) C(28) 3.48(2) . . no O(25) N(6) 3.53(2) . . no O(25) C(30) 3.55(2) . . no O(26) O(32) 2.16(6) . 3_655 no O(26) O(33) 3.22(6) . 3_656 no O(26) N(12) 3.34(6) . . no O(27) O(29) 1.54(4) . 1_455 no O(27) O(29) 2.71(4) . 3_656 no O(27) O(27) 2.90(8) . 3_556 no O(27) O(31) 2.97(4) . 1_455 no O(27) N(7) 3.15(4) . 4_455 no O(27) N(7) 3.38(4) . 2_545 no O(28) N(15) 3.03(4) . 4 no O(28) C(8) 3.12(4) . 4 no O(28) N(3) 3.33(3) . 4 no O(28) C(6) 3.44(3) . 4 no O(28) C(5) 3.52(4) . 4 no O(29) O(31) 2.44(3) . . no O(29) N(7) 2.81(3) . 4 no O(29) O(29) 3.32(6) . 3_756 no O(29) C(7) 3.43(3) . 4 no O(29) N(4) 3.56(3) . 4 no O(30) C(21) 3.22(3) . 1_556 no O(30) N(11) 3.25(3) . 1_556 no O(30) N(5) 3.40(3) . 1_556 no O(30) C(11) 3.42(3) . . no O(30) C(22) 3.43(3) . 1_556 no O(30) C(12) 3.52(3) . . no O(30) C(25) 3.52(3) . 1_556 no O(31) O(32) 2.50(3) . . no O(31) N(10) 3.39(2) . 4 no O(31) C(9) 3.42(2) . 4 no O(31) N(5) 3.46(2) . 4 no O(32) O(33) 3.19(3) . 1_554 no O(33) N(1) 3.23(2) . 4 no O(33) C(1) 3.35(2) . 4 no O(33) C(5) 3.36(2) . 4 no O(33) C(2) 3.46(3) . 4 no O(33) N(15) 3.49(2) . 4 no O(33) C(3) 3.59(3) . 4 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ni(1) N(1) C(1) C(2) . . . . -175(2) no Ni(1) N(1) C(5) C(4) . . . . -180(1) no Ni(1) N(1) C(5) C(6) . . . . 2(1) no Ni(1) N(3) N(4) Ni(2) . . . . -41.8(9) no Ni(1) N(3) N(4) C(7) . . . . 115.0(9) no Ni(1) N(3) C(6) N(7) . . . . 155.5(9) no Ni(1) N(3) C(6) C(5) . . . . -18(1) no Ni(1) N(6) C(11) C(12) . . . . 179(1) no Ni(1) N(6) C(15) C(14) . . . . -177.3(9) no Ni(1) N(6) C(15) C(16) . . . . 2(1) no Ni(1) N(8) N(9) Ni(2) . . . . -41.1(9) no Ni(1) N(8) N(9) C(17) . . . . 113.1(9) no Ni(1) N(8) C(16) N(2) . . . . 157.7(9) no Ni(1) N(8) C(16) C(15) . . . . -21(1) no Ni(1) N(14) N(13) Ni(2) . . . . -41.5(9) no Ni(1) N(14) N(13) C(26) . . . . 105.2(9) no Ni(1) N(14) C(27) C(28) . . . . 171(1) no Ni(1) N(14) C(27) C(29) . . . . -11(1) no Ni(1) N(15) C(29) C(27) . . . . -13(1) no Ni(1) N(15) C(29) C(30) . . . . 169.4(8) no Ni(2) N(4) N(3) C(6) . . . . 106.3(9) no Ni(2) N(4) C(7) C(8) . . . . 168(1) no Ni(2) N(4) C(7) C(9) . . . . -12(1) no Ni(2) N(5) C(9) C(7) . . . . -7(1) no Ni(2) N(5) C(9) C(10) . . . . 177(1) no Ni(2) N(9) N(8) C(16) . . . . 103.1(9) no Ni(2) N(9) C(17) C(18) . . . . 163.8(9) no Ni(2) N(9) C(17) C(19) . . . . -15(1) no Ni(2) N(10) C(19) C(17) . . . . -10(1) no Ni(2) N(10) C(19) C(31) . . . . 172.7(9) no Ni(2) N(11) C(21) C(22) . . . . -177(1) no Ni(2) N(11) C(25) C(24) . . . . -179.8(9) no Ni(2) N(11) C(25) C(26) . . . . 0(1) no Ni(2) N(13) N(14) C(27) . . . . 118.8(8) no Ni(2) N(13) C(26) N(12) . . . . 156.7(9) no Ni(2) N(13) C(26) C(25) . . . . -22(1) no Cl(2) O(8) O(13) O(12) . . . . -30(4) no Cl(2) O(12) O(13) O(8) . . . . 28(4) no Cl(3) O(14) O(15) O(16) . . . . 26(2) no Cl(3) O(15) O(16) O(17) . . . . -38(4) no Cl(3) O(16) O(15) O(14) . . . . -26(2) no Cl(3) O(16) O(17) O(18) . . . . -41(2) no Cl(3) O(17) O(16) O(15) . . . . 45(4) no Cl(3) O(18) O(17) O(16) . . . . 41(2) no Cl(4) O(20) O(26) O(24) . . . . -41(3) no Cl(4) O(21) O(20) O(26) . . . . -43(8) no Cl(4) O(22) O(23) O(24) . . . . 12(3) no Cl(4) O(23) O(24) O(26) . . . . -19(7) no Cl(4) O(24) O(23) O(22) . . . . -11(3) no Cl(4) O(24) O(26) O(20) . . . . 40(4) no Cl(4) O(26) O(20) O(21) . . . . 40(8) no Cl(4) O(26) O(24) O(23) . . . . 17(6) no O(1) N(5) Ni(2) N(4) . . . . 175(1) no O(1) N(5) Ni(2) N(9) . . . . 153(1) no O(1) N(5) Ni(2) N(10) . . . . 82(1) no O(1) N(5) Ni(2) N(11) . . . . -16(1) no O(1) N(5) Ni(2) N(13) . . . . -94(1) no O(1) N(5) C(9) C(7) . . . . 178(1) no O(1) N(5) C(9) C(10) . . . . 2(2) no O(2) N(10) Ni(2) N(4) . . . . -103.5(8) no O(2) N(10) Ni(2) N(5) . . . . -27.2(8) no O(2) N(10) Ni(2) N(9) . . . . 167.2(8) no O(2) N(10) Ni(2) N(11) . . . . 72.9(8) no O(2) N(10) Ni(2) N(13) . . . . 139(1) no O(2) N(10) C(19) C(17) . . . . -176.6(8) no O(2) N(10) C(19) C(31) . . . . 6(2) no O(3) N(15) Ni(1) N(1) . . . . -24.3(8) no O(3) N(15) Ni(1) N(3) . . . . -102.5(8) no O(3) N(15) Ni(1) N(6) . . . . 74.7(8) no O(3) N(15) Ni(1) N(8) . . . . 140(1) no O(3) N(15) Ni(1) N(14) . . . . 167.1(8) no O(3) N(15) C(29) C(27) . . . . -176.3(8) no O(3) N(15) C(29) C(30) . . . . 6(2) no O(8) Cl(2) O(12) O(13) . . . . -21(3) no O(8) Cl(2) O(13) O(12) . . . . 159(3) no O(8) O(13) Cl(2) O(9) . . . . 55(2) no O(8) O(13) Cl(2) O(10) . . . . 151(2) no O(8) O(13) Cl(2) O(11) . . . . -80(2) no O(8) O(13) Cl(2) O(12) . . . . -159(3) no O(9) Cl(2) O(8) O(13) . . . . -130(2) no O(9) Cl(2) O(12) O(13) . . . . 65(4) no O(9) Cl(2) O(13) O(12) . . . . -146(2) no O(10) Cl(2) O(8) O(13) . . . . -89(3) no O(10) Cl(2) O(12) O(13) . . . . 133(2) no O(10) Cl(2) O(13) O(12) . . . . -50(2) no O(11) Cl(2) O(8) O(13) . . . . 121(1) no O(11) Cl(2) O(12) O(13) . . . . -119(2) no O(11) Cl(2) O(13) O(12) . . . . 78(2) no O(12) Cl(2) O(8) O(13) . . . . 15(2) no O(14) Cl(3) O(15) O(16) . . . . -142(3) no O(14) Cl(3) O(16) O(15) . . . . 37(3) no O(14) Cl(3) O(16) O(17) . . . . 175(4) no O(14) Cl(3) O(17) O(16) . . . . -126(31) no O(14) Cl(3) O(17) O(18) . . . . 0(32) no O(14) Cl(3) O(18) O(17) . . . . -179.9992 no O(14) O(15) Cl(3) O(16) . . . . 142(3) no O(14) O(15) Cl(3) O(17) . . . . -173(4) no O(14) O(15) Cl(3) O(18) . . . . -98(2) no O(14) O(15) Cl(3) O(19) . . . . 71(5) no O(14) O(15) O(16) O(17) . . . . -64(5) no O(15) Cl(3) O(16) O(17) . . . . 138(4) no O(15) Cl(3) O(17) O(16) . . . . -41(4) no O(15) Cl(3) O(17) O(18) . . . . 85(3) no O(15) Cl(3) O(18) O(17) . . . . -116(4) no O(15) O(14) Cl(3) O(16) . . . . -36(3) no O(15) O(14) Cl(3) O(17) . . . . 88(32) no O(15) O(14) Cl(3) O(18) . . . . 88(3) no O(15) O(14) Cl(3) O(19) . . . . -152(3) no O(15) O(16) Cl(3) O(17) . . . . -138(4) no O(15) O(16) Cl(3) O(18) . . . . -76(3) no O(15) O(16) Cl(3) O(19) . . . . 151(3) no O(15) O(16) O(17) O(18) . . . . 4(5) no O(16) Cl(3) O(17) O(18) . . . . 126(2) no O(16) Cl(3) O(18) O(17) . . . . -58(3) no O(16) O(15) Cl(3) O(17) . . . . 45(4) no O(16) O(15) Cl(3) O(18) . . . . 120(2) no O(16) O(15) Cl(3) O(19) . . . . -72(5) no O(16) O(17) Cl(3) O(18) . . . . -126(2) no O(16) O(17) Cl(3) O(19) . . . . 113(2) no O(17) O(16) Cl(3) O(18) . . . . 62(4) no O(17) O(16) Cl(3) O(19) . . . . -71(4) no O(17) O(18) Cl(3) O(19) . . . . 70(3) no O(18) O(17) Cl(3) O(19) . . . . -121(2) no O(20) Cl(4) O(22) O(23) . . . . -129(4) no O(20) Cl(4) O(23) O(22) . . . . 132(4) no O(20) Cl(4) O(23) O(24) . . . . -36(5) no O(20) Cl(4) O(24) O(23) . . . . 153(4) no O(20) Cl(4) O(24) O(26) . . . . -40(4) no O(20) Cl(4) O(26) O(24) . . . . 124(5) no O(20) O(21) Cl(4) O(22) . . . . -165(3) no O(20) O(21) Cl(4) O(23) . . . . 123(4) no O(20) O(21) Cl(4) O(24) . . . . 72(4) no O(20) O(21) Cl(4) O(25) . . . . -64(3) no O(20) O(21) Cl(4) O(26) . . . . 20(4) no O(20) O(26) Cl(4) O(21) . . . . -20(4) no O(20) O(26) Cl(4) O(22) . . . . -113(24) no O(20) O(26) Cl(4) O(23) . . . . -133(4) no O(20) O(26) Cl(4) O(24) . . . . -124(5) no O(20) O(26) Cl(4) O(25) . . . . 100(4) no O(20) O(26) O(24) O(23) . . . . 57(8) no O(21) Cl(4) O(20) O(26) . . . . 154(5) no O(21) Cl(4) O(22) O(23) . . . . -114(2) no O(21) Cl(4) O(23) O(22) . . . . 78(2) no O(21) Cl(4) O(23) O(24) . . . . -90(3) no O(21) Cl(4) O(24) O(23) . . . . 107(3) no O(21) Cl(4) O(24) O(26) . . . . -85(3) no O(21) Cl(4) O(26) O(24) . . . . 104(3) no O(21) O(20) Cl(4) O(22) . . . . 20(4) no O(21) O(20) Cl(4) O(23) . . . . -87(4) no O(21) O(20) Cl(4) O(24) . . . . -113(3) no O(21) O(20) Cl(4) O(25) . . . . 129(3) no O(21) O(20) Cl(4) O(26) . . . . -154(5) no O(21) O(20) O(26) O(24) . . . . 0(10) no O(22) Cl(4) O(20) O(26) . . . . 173(3) no O(22) Cl(4) O(23) O(24) . . . . -168(3) no O(22) Cl(4) O(24) O(23) . . . . 13(3) no O(22) Cl(4) O(24) O(26) . . . . -179(3) no O(22) Cl(4) O(26) O(24) . . . . 11(25) no O(22) O(23) Cl(4) O(24) . . . . 168(3) no O(22) O(23) Cl(4) O(25) . . . . -95(2) no O(22) O(23) Cl(4) O(26) . . . . 178(2) no O(22) O(23) O(24) O(26) . . . . -30(9) no O(23) Cl(4) O(20) O(26) . . . . 67(5) no O(23) Cl(4) O(24) O(26) . . . . 168(4) no O(23) Cl(4) O(26) O(24) . . . . -9(3) no O(23) O(22) Cl(4) O(24) . . . . -10(3) no O(23) O(22) Cl(4) O(25) . . . . 126(2) no O(23) O(22) Cl(4) O(26) . . . . -21(24) no O(23) O(24) Cl(4) O(25) . . . . -116(3) no O(23) O(24) Cl(4) O(26) . . . . -168(4) no O(24) Cl(4) O(20) O(26) . . . . 41(3) no O(24) O(23) Cl(4) O(25) . . . . 97(3) no O(24) O(23) Cl(4) O(26) . . . . 10(3) no O(24) O(26) Cl(4) O(25) . . . . -136(3) no O(25) Cl(4) O(20) O(26) . . . . -78(4) no O(25) Cl(4) O(24) O(26) . . . . 52(3) no N(1) Ni(1) N(3) N(4) . . . . 164.2(7) no N(1) Ni(1) N(3) C(6) . . . . 15.0(7) no N(1) Ni(1) N(6) C(11) . . . . 79(1) no N(1) Ni(1) N(6) C(15) . . . . -103.3(8) no N(1) Ni(1) N(8) N(9) . . . . -100.6(7) no N(1) Ni(1) N(8) C(16) . . . . 114.3(8) no N(1) Ni(1) N(14) N(13) . . . . 93(2) no N(1) Ni(1) N(14) C(27) . . . . -68(2) no N(1) Ni(1) N(15) C(29) . . . . 174.0(8) no N(1) C(1) C(2) C(3) . . . . -10(3) no N(1) C(5) C(4) C(3) . . . . -1(3) no N(1) C(5) C(6) N(3) . . . . 10(1) no N(1) C(5) C(6) N(7) . . . . -163(1) no N(2) C(16) N(8) N(9) . . . . 11(2) no N(2) C(16) C(15) N(6) . . . . -166(1) no N(2) C(16) C(15) C(14) . . . . 14(2) no N(3) Ni(1) N(1) C(1) . . . . 177(1) no N(3) Ni(1) N(1) C(5) . . . . -8.6(8) no N(3) Ni(1) N(6) C(11) . . . . 144(2) no N(3) Ni(1) N(6) C(15) . . . . -38(2) no N(3) Ni(1) N(8) N(9) . . . . -23.1(7) no N(3) Ni(1) N(8) C(16) . . . . -168.2(8) no N(3) Ni(1) N(14) N(13) . . . . 68.9(7) no N(3) Ni(1) N(14) C(27) . . . . -91.9(8) no N(3) Ni(1) N(15) C(29) . . . . 95.8(8) no N(3) N(4) Ni(2) N(5) . . . . 164.0(7) no N(3) N(4) Ni(2) N(9) . . . . -21.4(7) no N(3) N(4) Ni(2) N(10) . . . . -97.1(7) no N(3) N(4) Ni(2) N(11) . . . . 101(2) no N(3) N(4) Ni(2) N(13) . . . . 69.5(7) no N(3) N(4) C(7) C(8) . . . . 10(2) no N(3) N(4) C(7) C(9) . . . . -169.7(9) no N(3) C(6) C(5) C(4) . . . . -167(1) no N(4) Ni(2) N(5) C(9) . . . . 0.9(9) no N(4) Ni(2) N(9) N(8) . . . . 68.7(7) no N(4) Ni(2) N(9) C(17) . . . . -86.5(8) no N(4) Ni(2) N(10) C(19) . . . . 90.8(9) no N(4) Ni(2) N(11) C(21) . . . . 141(2) no N(4) Ni(2) N(11) C(25) . . . . -41(2) no N(4) Ni(2) N(13) N(14) . . . . -21.8(7) no N(4) Ni(2) N(13) C(26) . . . . -168.9(8) no N(4) N(3) Ni(1) N(6) . . . . 97(2) no N(4) N(3) Ni(1) N(8) . . . . 69.6(7) no N(4) N(3) Ni(1) N(14) . . . . -20.7(7) no N(4) N(3) Ni(1) N(15) . . . . -97.4(7) no N(4) N(3) C(6) N(7) . . . . 7(2) no N(4) N(3) C(6) C(5) . . . . -166.8(8) no N(4) C(7) C(9) N(5) . . . . 12(2) no N(4) C(7) C(9) C(10) . . . . -172(1) no N(5) Ni(2) N(4) C(7) . . . . 6.3(8) no N(5) Ni(2) N(9) N(8) . . . . 89(2) no N(5) Ni(2) N(9) C(17) . . . . -66(2) no N(5) Ni(2) N(10) C(19) . . . . 167.2(9) no N(5) Ni(2) N(11) C(21) . . . . 80(1) no N(5) Ni(2) N(11) C(25) . . . . -101.6(8) no N(5) Ni(2) N(13) N(14) . . . . -97.7(7) no N(5) Ni(2) N(13) C(26) . . . . 115.2(8) no N(5) C(9) C(7) C(8) . . . . -167(1) no N(6) Ni(1) N(1) C(1) . . . . -13(1) no N(6) Ni(1) N(1) C(5) . . . . 161.0(8) no N(6) Ni(1) N(3) C(6) . . . . -52(2) no N(6) Ni(1) N(8) N(9) . . . . 162.2(7) no N(6) Ni(1) N(8) C(16) . . . . 17.1(7) no N(6) Ni(1) N(14) N(13) . . . . -101.2(7) no N(6) Ni(1) N(14) C(27) . . . . 98.1(8) no N(6) Ni(1) N(15) C(29) . . . . -87.0(8) no N(6) C(11) C(12) C(13) . . . . -4(2) no N(6) C(15) C(14) C(13) . . . . 1(2) no N(6) C(15) C(16) N(8) . . . . 12(1) no N(7) C(6) C(5) C(4) . . . . 19(2) no N(8) Ni(1) N(1) C(1) . . . . -93(1) no N(8) Ni(1) N(1) C(5) . . . . 81.6(8) no N(8) Ni(1) N(3) C(6) . . . . -79.7(8) no N(8) Ni(1) N(6) C(11) . . . . 172(1) no N(8) Ni(1) N(6) C(15) . . . . -9.9(7) no N(8) Ni(1) N(14) N(13) . . . . -22.3(7) no N(8) Ni(1) N(14) C(27) . . . . 176.9(8) no N(8) Ni(1) N(15) C(29) . . . . -22(2) no N(8) N(9) Ni(2) N(10) . . . . 163.4(7) no N(8) N(9) Ni(2) N(11) . . . . -101.4(7) no N(8) N(9) Ni(2) N(13) . . . . -23.7(7) no N(8) N(9) C(17) C(18) . . . . 9(2) no N(8) N(9) C(17) C(19) . . . . -170.2(8) no N(8) C(16) C(15) C(14) . . . . -168(1) no N(9) Ni(2) N(4) C(7) . . . . -179.1(8) no N(9) Ni(2) N(5) C(9) . . . . -21(2) no N(9) Ni(2) N(10) C(19) . . . . 1.6(8) no N(9) Ni(2) N(11) C(21) . . . . -97(1) no N(9) Ni(2) N(11) C(25) . . . . 81.2(7) no N(9) Ni(2) N(13) N(14) . . . . 68.6(7) no N(9) Ni(2) N(13) C(26) . . . . -78.5(8) no N(9) N(8) Ni(1) N(14) . . . . 68.6(7) no N(9) N(8) Ni(1) N(15) . . . . 95(1) no N(9) N(8) C(16) C(15) . . . . -167.0(8) no N(9) C(17) C(19) N(10) . . . . 17(2) no N(9) C(17) C(19) C(31) . . . . -166(1) no N(10) Ni(2) N(4) C(7) . . . . 105.3(8) no N(10) Ni(2) N(5) C(9) . . . . -91(1) no N(10) Ni(2) N(9) C(17) . . . . 8.2(7) no N(10) Ni(2) N(11) C(21) . . . . -21(1) no N(10) Ni(2) N(11) C(25) . . . . 157.3(7) no N(10) Ni(2) N(13) N(14) . . . . 96(1) no N(10) Ni(2) N(13) C(26) . . . . -51(2) no N(10) C(19) C(17) C(18) . . . . -162(1) no N(11) Ni(2) N(4) C(7) . . . . -57(2) no N(11) Ni(2) N(5) C(9) . . . . 170.3(9) no N(11) Ni(2) N(9) C(17) . . . . 103.5(8) no N(11) Ni(2) N(10) C(19) . . . . -92.8(9) no N(11) Ni(2) N(13) N(14) . . . . 164.4(7) no N(11) Ni(2) N(13) C(26) . . . . 17.3(7) no N(11) C(21) C(22) C(23) . . . . -4(2) no N(11) C(25) C(24) C(23) . . . . -2(2) no N(11) C(25) C(26) N(12) . . . . -165(1) no N(11) C(25) C(26) N(13) . . . . 14(1) no N(12) C(26) N(13) N(14) . . . . 10(2) no N(12) C(26) C(25) C(24) . . . . 15(2) no N(13) Ni(2) N(4) C(7) . . . . -88.1(8) no N(13) Ni(2) N(5) C(9) . . . . 92(1) no N(13) Ni(2) N(9) C(17) . . . . -178.8(8) no N(13) Ni(2) N(10) C(19) . . . . -26(2) no N(13) Ni(2) N(11) C(21) . . . . 173(1) no N(13) Ni(2) N(11) C(25) . . . . -8.5(7) no N(13) N(14) Ni(1) N(15) . . . . 164.4(7) no N(13) N(14) C(27) C(28) . . . . 10(2) no N(13) N(14) C(27) C(29) . . . . -172.0(8) no N(13) C(26) C(25) C(24) . . . . -166(1) no N(14) Ni(1) N(1) C(1) . . . . 153(2) no N(14) Ni(1) N(1) C(5) . . . . -33(2) no N(14) Ni(1) N(3) C(6) . . . . -169.9(8) no N(14) Ni(1) N(6) C(11) . . . . -98(1) no N(14) Ni(1) N(6) C(15) . . . . 79.6(8) no N(14) Ni(1) N(8) C(16) . . . . -76.5(8) no N(14) Ni(1) N(15) C(29) . . . . 5.5(8) no N(14) N(13) C(26) C(25) . . . . -169.7(8) no N(14) C(27) C(29) N(15) . . . . 15(1) no N(14) C(27) C(29) C(30) . . . . -167(1) no N(15) Ni(1) N(1) C(1) . . . . 83(1) no N(15) Ni(1) N(1) C(5) . . . . -102.5(8) no N(15) Ni(1) N(3) C(6) . . . . 113.4(8) no N(15) Ni(1) N(6) C(11) . . . . -21(1) no N(15) Ni(1) N(6) C(15) . . . . 156.4(8) no N(15) Ni(1) N(8) C(16) . . . . -50(2) no N(15) Ni(1) N(14) C(27) . . . . 3.7(7) no N(15) C(29) C(27) C(28) . . . . -166(1) no C(1) N(1) C(5) C(4) . . . . -5(2) no C(1) N(1) C(5) C(6) . . . . 177(1) no C(1) C(2) C(3) C(4) . . . . 3(3) no C(2) C(1) N(1) C(5) . . . . 11(3) no C(2) C(3) C(4) C(5) . . . . 2(3) no C(3) C(4) C(5) C(6) . . . . 177(2) no C(6) N(3) N(4) C(7) . . . . -97(1) no C(8) C(7) C(9) C(10) . . . . 9(2) no C(11) N(6) C(15) C(14) . . . . 1(2) no C(11) N(6) C(15) C(16) . . . . -180(1) no C(11) C(12) C(13) C(14) . . . . 5(2) no C(12) C(11) N(6) C(15) . . . . 1(2) no C(12) C(13) C(14) C(15) . . . . -3(2) no C(13) C(14) C(15) C(16) . . . . -179(1) no C(16) N(8) N(9) C(17) . . . . -103(1) no C(18) C(17) C(19) C(31) . . . . 15(2) no C(21) N(11) C(25) C(24) . . . . -1(2) no C(21) N(11) C(25) C(26) . . . . 179(1) no C(21) C(22) C(23) C(24) . . . . 1(2) no C(22) C(21) N(11) C(25) . . . . 4(2) no C(22) C(23) C(24) C(25) . . . . 1(2) no C(23) C(24) C(25) C(26) . . . . 179(1) no C(26) N(13) N(14) C(27) . . . . -95(1) no C(28) C(27) C(29) C(30) . . . . 12(2) no #------------------------------------------------------------------------------ #===END data_shelxl(3) _database_code_CSD 158601 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H41.50 Cl4 N24 Ni2 O21.75' _chemical_formula_weight 1345.59 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6681(11) _cell_length_b 13.3204(8) _cell_length_c 22.0456(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.3430(10) _cell_angle_gamma 90.00 _cell_volume 5188.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2750 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6261 _exptl_absorpt_correction_T_max 0.7822 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27406 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 26.40 _reflns_number_total 10621 _reflns_number_gt 8668 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0629P)^2^+7.5709P] 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 10621 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.132314(18) 0.22499(3) 0.139567(15) 0.01837(9) Uani 1 1 d . . . Ni2 Ni 0.312719(19) 0.37132(3) 0.146875(16) 0.01950(10) Uani 1 1 d . . . Cl1A Cl 0.59215(11) 0.31105(13) 0.29456(11) 0.0604(5) Uani 0.75 1 d P . . Cl1B Cl 0.5731(3) 0.3006(4) 0.3286(3) 0.0585(14) Uani 0.25 1 d P . . Cl2 Cl 0.39294(5) 0.08495(8) 0.43164(4) 0.0452(2) Uani 1 1 d . . . Cl3 Cl 0.10282(5) -0.00400(7) 0.33715(4) 0.03885(19) Uani 1 1 d . . . Cl4 Cl 0.12942(4) 0.05887(6) -0.06494(3) 0.03344(18) Uani 1 1 d . . . O1 O 0.5194(3) 0.3175(3) 0.2759(2) 0.1077(16) Uani 1 1 d . . . O2 O 0.6189(3) 0.2164(3) 0.3093(3) 0.1203(18) Uani 1 1 d . . . O3 O 0.5994(2) 0.3743(3) 0.3519(2) 0.0921(13) Uani 1 1 d . . . O4B O 0.5235(10) 0.2445(13) 0.3628(8) 0.104(6) Uani 0.25 1 d P . . O4A O 0.6376(5) 0.3546(6) 0.2493(3) 0.142(3) Uani 0.75 1 d P . . O5 O 0.3563(2) 0.1779(3) 0.41949(17) 0.0807(11) Uani 1 1 d . . . O6 O 0.42983(18) 0.0446(3) 0.37947(14) 0.0675(9) Uani 1 1 d . . . O7 O 0.33435(17) 0.0164(3) 0.45095(16) 0.0715(9) Uani 1 1 d . . . O8 O 0.44643(16) 0.0959(3) 0.48014(13) 0.0587(8) Uani 1 1 d . . . O9 O 0.11028(19) 0.1041(2) 0.33797(17) 0.0691(9) Uani 1 1 d . . . O10 O 0.1287(3) -0.0362(3) 0.39549(18) 0.0967(14) Uani 1 1 d . . . O11 O 0.1458(3) -0.0431(4) 0.2911(2) 0.1197(18) Uani 1 1 d . . . O12 O 0.02557(16) -0.0297(3) 0.32970(18) 0.0703(9) Uani 1 1 d . . . O13 O 0.18240(14) 0.0120(2) -0.02386(12) 0.0478(6) Uani 1 1 d . . . O14 O 0.1647(2) 0.1409(3) -0.09447(15) 0.0704(9) Uani 1 1 d . . . O15 O 0.06595(15) 0.0935(2) -0.03084(12) 0.0514(7) Uani 1 1 d . . . O16 O 0.10368(14) -0.0129(2) -0.10948(11) 0.0427(6) Uani 1 1 d . . . O17 O 0.2541(2) -0.1830(3) -0.05662(16) 0.0713(9) Uani 1 1 d . . . O18 O 0.3927(3) -0.0165(5) -0.0200(4) 0.142(2) Uani 1 1 d . . . O19 O 0.1811(2) -0.2601(3) 0.33526(18) 0.0777(10) Uani 1 1 d . . . O20 O 0.43681(16) 0.1366(2) 0.26222(13) 0.0576(8) Uani 1 1 d . . . O21 O 0.76293(17) 0.1291(2) 0.25876(14) 0.0572(8) Uani 1 1 d . . . O22 O 0.6074(6) 0.4449(7) 0.4768(4) 0.088(3) Uani 0.50 1 d P . . O24 O 0.5209(13) 0.412(2) 0.4320(11) 0.148(9) Uani 0.25 1 d P . . N1 N 0.05769(13) 0.22670(18) 0.21333(10) 0.0223(5) Uani 1 1 d . . . N2 N -0.03700(17) 0.2590(2) 0.31260(14) 0.0420(7) Uani 1 1 d . . . N3 N 0.14654(15) 0.4556(2) 0.26535(12) 0.0314(6) Uani 1 1 d . . . N4 N 0.14432(12) 0.36984(17) 0.17290(10) 0.0189(5) Uani 1 1 d . . . N5 N 0.20581(12) 0.43052(17) 0.15481(10) 0.0194(5) Uani 1 1 d . . . N6 N 0.11872(13) 0.53804(19) 0.10763(12) 0.0277(5) Uani 1 1 d . . . N7 N 0.31337(16) 0.6948(2) 0.04210(14) 0.0392(7) Uani 1 1 d . . . N8 N 0.32240(13) 0.51018(17) 0.10188(11) 0.0218(5) Uani 1 1 d . . . N9 N 0.04930(13) 0.26188(17) 0.07528(10) 0.0205(5) Uani 1 1 d . . . N10 N -0.04667(14) 0.3230(2) -0.01837(12) 0.0282(5) Uani 1 1 d . . . N11 N 0.19145(14) 0.3785(2) -0.01734(12) 0.0326(6) Uani 1 1 d . . . N12 N 0.19713(12) 0.26542(17) 0.06439(10) 0.0205(5) Uani 1 1 d . . . N13 N 0.27528(13) 0.28860(18) 0.07175(11) 0.0213(5) Uani 1 1 d . . . N14 N 0.30393(15) 0.1362(2) 0.02402(14) 0.0359(6) Uani 1 1 d . . . N15 N 0.53449(16) 0.2050(2) 0.06350(16) 0.0446(7) Uani 1 1 d . . . N16 N 0.41308(13) 0.30656(18) 0.11589(11) 0.0246(5) Uani 1 1 d . . . N17 N 0.13528(13) 0.06967(17) 0.12466(10) 0.0215(5) Uani 1 1 d . . . N18 N 0.16442(16) -0.1330(2) 0.10092(14) 0.0366(6) Uani 1 1 d . . . N19 N 0.32689(16) 0.0651(2) 0.18172(16) 0.0436(8) Uani 1 1 d . . . N20 N 0.22846(13) 0.18183(17) 0.18583(11) 0.0223(5) Uani 1 1 d . . . N21 N 0.28199(13) 0.25486(17) 0.20489(11) 0.0214(5) Uani 1 1 d . . . N22 N 0.24714(19) 0.2234(2) 0.30498(13) 0.0441(8) Uani 1 1 d . . . N23 N 0.39460(19) 0.4671(3) 0.35105(14) 0.0476(8) Uani 1 1 d . . . N24 N 0.35500(13) 0.41881(18) 0.23197(11) 0.0254(5) Uani 1 1 d . . . C1 C 0.00282(17) 0.1622(2) 0.22764(14) 0.0286(6) Uani 1 1 d . . . C2 C -0.04482(19) 0.1799(3) 0.27641(16) 0.0364(7) Uani 1 1 d . . . C3 C 0.01822(19) 0.3232(3) 0.29807(15) 0.0351(7) Uani 1 1 d . . . C4 C 0.06466(16) 0.3095(2) 0.24875(13) 0.0230(6) Uani 1 1 d . . . C5 C 0.12256(15) 0.3831(2) 0.22878(13) 0.0217(6) Uani 1 1 d . . . C6 C 0.18891(15) 0.5067(2) 0.12075(12) 0.0200(5) Uani 1 1 d . . . C7 C 0.25587(16) 0.5596(2) 0.09519(12) 0.0218(6) Uani 1 1 d . . . C8 C 0.25212(17) 0.6513(2) 0.06635(15) 0.0319(7) Uani 1 1 d . . . C9 C 0.37802(19) 0.6462(3) 0.04897(17) 0.0371(8) Uani 1 1 d . . . C10 C 0.38346(16) 0.5544(2) 0.07876(14) 0.0283(6) Uani 1 1 d . . . C11 C -0.02531(16) 0.2495(2) 0.07870(13) 0.0252(6) Uani 1 1 d . . . C12 C -0.07317(16) 0.2807(2) 0.03166(14) 0.0281(6) Uani 1 1 d . . . C13 C 0.02882(17) 0.3341(2) -0.02218(14) 0.0277(6) Uani 1 1 d . . . C14 C 0.07705(15) 0.3044(2) 0.02443(12) 0.0207(5) Uani 1 1 d . . . C15 C 0.16087(15) 0.3170(2) 0.02302(12) 0.0217(6) Uani 1 1 d . . . C16 C 0.32210(16) 0.2186(2) 0.05449(13) 0.0244(6) Uani 1 1 d . . . C17 C 0.40228(16) 0.2368(2) 0.07275(14) 0.0268(6) Uani 1 1 d . . . C18 C 0.46292(18) 0.1865(3) 0.04700(17) 0.0384(8) Uani 1 1 d . . . C19 C 0.54452(18) 0.2751(3) 0.10570(18) 0.0417(8) Uani 1 1 d . . . C20 C 0.48466(17) 0.3260(3) 0.13226(15) 0.0325(7) Uani 1 1 d . . . C21 C 0.08426(16) 0.0111(2) 0.09783(13) 0.0245(6) Uani 1 1 d . . . C22 C 0.09963(18) -0.0902(2) 0.08658(15) 0.0313(7) Uani 1 1 d . . . C23 C 0.21514(19) -0.0742(2) 0.12926(17) 0.0364(8) Uani 1 1 d . . . C24 C 0.20099(16) 0.0258(2) 0.14165(14) 0.0266(6) Uani 1 1 d . . . C25 C 0.25613(16) 0.0946(2) 0.17241(14) 0.0264(6) Uani 1 1 d . . . C26 C 0.28411(17) 0.2738(2) 0.26255(13) 0.0259(6) Uani 1 1 d . . . C27 C 0.33194(17) 0.3620(2) 0.27918(14) 0.0271(6) Uani 1 1 d . . . C28 C 0.3517(2) 0.3866(3) 0.33827(15) 0.0389(8) Uani 1 1 d . . . C29 C 0.4181(2) 0.5209(3) 0.30413(17) 0.0440(9) Uani 1 1 d . . . C30 C 0.39860(19) 0.4976(2) 0.24462(15) 0.0334(7) Uani 1 1 d . . . H1 H -0.0044 0.1037 0.2041 0.034 Uiso 1 1 d . . . H2 H -0.0845 0.1346 0.2842 0.044 Uiso 1 1 d . . . H3 H 0.0251 0.3812 0.3228 0.043 Uiso 1 1 d . . . H4 H 0.2047 0.6839 0.0630 0.038 Uiso 1 1 d . . . H5 H 0.4228 0.6753 0.0330 0.045 Uiso 1 1 d . . . H6 H 0.4311 0.5225 0.0824 0.034 Uiso 1 1 d . . . H7 H -0.0466 0.2187 0.1137 0.030 Uiso 1 1 d . . . H8 H -0.1265 0.2722 0.0358 0.034 Uiso 1 1 d . . . H9 H 0.0497 0.3640 -0.0576 0.033 Uiso 1 1 d . . . H10 H 0.4527 0.1363 0.0175 0.046 Uiso 1 1 d . . . H11 H 0.5945 0.2917 0.1183 0.050 Uiso 1 1 d . . . H12 H 0.4945 0.3751 0.1629 0.040 Uiso 1 1 d . . . H13 H 0.0370 0.0387 0.0860 0.030 Uiso 1 1 d . . . H14 H 0.0614 -0.1301 0.0681 0.037 Uiso 1 1 d . . . H15 H 0.2619 -0.1029 0.1407 0.043 Uiso 1 1 d . . . H16 H 0.3337 0.3464 0.3706 0.047 Uiso 1 1 d . . . H17 H 0.4501 0.5762 0.3120 0.053 Uiso 1 1 d . . . H18 H 0.4171 0.5385 0.2129 0.041 Uiso 1 1 d . . . H19 H 0.1323 0.4532 0.2990 0.076 Uiso 1 1 d . . . H20 H 0.1802 0.4954 0.2534 0.076 Uiso 1 1 d . . . H21 H 0.0844 0.5051 0.1222 0.076 Uiso 1 1 d . . . H22 H 0.1107 0.5833 0.0843 0.076 Uiso 1 1 d . . . H23 H 0.2363 0.3845 -0.0206 0.076 Uiso 1 1 d . . . H24 H 0.1624 0.4243 -0.0422 0.076 Uiso 1 1 d . . . H25 H 0.2531 0.1259 0.0039 0.076 Uiso 1 1 d . . . H26 H 0.3255 0.0954 0.0165 0.076 Uiso 1 1 d . . . H27 H 0.3370 0.0129 0.1701 0.076 Uiso 1 1 d . . . H28 H 0.3485 0.0976 0.1988 0.076 Uiso 1 1 d . . . H29 H 0.2146 0.1804 0.2938 0.076 Uiso 1 1 d . . . H30 H 0.2535 0.2390 0.3317 0.076 Uiso 1 1 d . . . H31 H 0.2864 -0.1348 -0.0370 0.076 Uiso 1 1 d . . . H32 H 0.2775 -0.2086 -0.0929 0.076 Uiso 1 1 d . . . H33 H 0.3619 -0.0714 -0.0354 0.076 Uiso 1 1 d . . . H34 H 0.4437 -0.0303 -0.0297 0.076 Uiso 1 1 d . . . H35 H 0.2340 -0.2549 0.3456 0.076 Uiso 1 1 d . . . H36 H 0.1668 -0.3294 0.3405 0.076 Uiso 1 1 d . . . H37 H 0.4567 0.1973 0.2655 0.076 Uiso 1 1 d . . . H38 H 0.4238 0.1121 0.3080 0.076 Uiso 1 1 d . . . H39 H 0.7166 0.1637 0.2745 0.076 Uiso 1 1 d . . . H40 H 0.7620 0.1092 0.2168 0.076 Uiso 1 1 d . . . H41 H 0.5808 0.5053 0.4662 0.076 Uiso 0.50 1 d P . . H42 H 0.6582 0.4656 0.4895 0.076 Uiso 0.50 1 d P . . H43 H 0.5676 0.4179 0.4119 0.076 Uiso 0.25 1 d P . . H44 H 0.5068 0.3373 0.4260 0.076 Uiso 0.25 1 d P . . 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 Ni1 0.01713(17) 0.01784(18) 0.02013(18) 0.00034(13) -0.00043(12) 0.00029(13) Ni2 0.01686(17) 0.01734(18) 0.02429(19) 0.00120(13) -0.00150(13) 0.00067(13) Cl1A 0.0522(10) 0.0347(8) 0.0941(14) 0.0015(9) -0.0199(10) -0.0101(7) Cl1B 0.045(3) 0.040(2) 0.091(4) 0.010(3) -0.022(3) -0.0142(19) Cl2 0.0362(4) 0.0571(6) 0.0422(5) 0.0021(4) 0.0038(3) 0.0152(4) Cl3 0.0305(4) 0.0432(5) 0.0429(5) 0.0004(4) 0.0011(3) -0.0027(3) Cl4 0.0335(4) 0.0369(4) 0.0298(4) -0.0001(3) -0.0041(3) -0.0050(3) O1 0.106(3) 0.086(3) 0.131(4) 0.000(3) -0.064(3) 0.014(2) O2 0.120(4) 0.081(3) 0.160(5) 0.027(3) 0.013(3) 0.046(3) O3 0.095(3) 0.073(3) 0.108(3) 0.011(2) -0.028(2) -0.037(2) O4B 0.103(12) 0.090(11) 0.120(14) 0.040(10) -0.040(10) -0.069(10) O4A 0.190(8) 0.124(6) 0.112(5) -0.007(4) 0.044(5) -0.072(6) O5 0.103(3) 0.066(2) 0.073(2) 0.0079(18) -0.008(2) 0.041(2) O6 0.064(2) 0.088(2) 0.0512(18) -0.0074(16) 0.0114(15) 0.0195(17) O7 0.0459(17) 0.088(3) 0.081(2) 0.0105(19) 0.0014(16) -0.0086(16) O8 0.0431(15) 0.078(2) 0.0556(17) 0.0036(15) -0.0052(13) -0.0005(14) O9 0.068(2) 0.0443(17) 0.095(3) 0.0071(17) -0.0095(18) -0.0199(15) O10 0.141(4) 0.070(2) 0.079(3) 0.027(2) -0.047(3) -0.032(2) O11 0.094(3) 0.161(5) 0.105(3) -0.054(3) 0.047(3) 0.002(3) O12 0.0375(15) 0.061(2) 0.112(3) -0.0157(19) 0.0031(16) -0.0149(14) O13 0.0399(14) 0.0565(17) 0.0469(15) 0.0011(13) -0.0133(11) 0.0045(12) O14 0.086(2) 0.062(2) 0.063(2) 0.0187(16) -0.0035(17) -0.0333(18) O15 0.0470(15) 0.0629(18) 0.0441(15) -0.0126(13) -0.0030(12) 0.0120(13) O16 0.0438(14) 0.0507(15) 0.0337(13) -0.0095(11) -0.0020(10) -0.0093(12) O17 0.084(2) 0.0550(19) 0.075(2) 0.0081(17) -0.0190(18) 0.0031(17) O18 0.116(4) 0.124(5) 0.186(7) -0.071(5) -0.014(5) 0.039(4) O19 0.076(2) 0.074(2) 0.084(2) -0.0129(19) 0.0161(19) 0.0065(19) O20 0.0446(16) 0.074(2) 0.0535(17) -0.0022(15) -0.0153(13) -0.0041(14) O21 0.0589(18) 0.0455(17) 0.0673(19) 0.0161(14) 0.0150(14) 0.0161(13) O22 0.124(7) 0.073(5) 0.067(5) -0.008(4) 0.005(5) -0.021(5) O24 0.122(18) 0.20(3) 0.120(17) -0.038(18) -0.020(14) -0.004(17) N1 0.0235(12) 0.0219(12) 0.0215(11) 0.0028(9) -0.0006(9) -0.0007(9) N2 0.0431(17) 0.0435(18) 0.0397(16) -0.0044(13) 0.0176(13) -0.0103(14) N3 0.0386(15) 0.0280(14) 0.0278(13) -0.0066(11) 0.0069(11) -0.0072(11) N4 0.0174(11) 0.0176(11) 0.0217(11) 0.0027(9) 0.0016(8) 0.0001(8) N5 0.0182(11) 0.0169(11) 0.0233(11) 0.0005(9) 0.0024(9) -0.0009(9) N6 0.0203(12) 0.0271(13) 0.0357(14) 0.0099(11) 0.0023(10) 0.0052(10) N7 0.0355(15) 0.0287(15) 0.0535(18) 0.0157(13) 0.0027(13) -0.0030(12) N8 0.0211(11) 0.0202(12) 0.0243(12) 0.0005(9) 0.0010(9) -0.0008(9) N9 0.0194(11) 0.0195(12) 0.0226(12) -0.0023(9) 0.0003(9) 0.0005(9) N10 0.0230(12) 0.0304(14) 0.0312(13) 0.0027(11) -0.0046(10) 0.0011(10) N11 0.0208(12) 0.0427(16) 0.0344(14) 0.0137(12) 0.0007(10) -0.0011(11) N12 0.0147(11) 0.0233(12) 0.0236(12) -0.0024(9) -0.0011(9) 0.0000(9) N13 0.0159(11) 0.0232(12) 0.0247(12) -0.0006(9) 0.0002(9) 0.0002(9) N14 0.0268(13) 0.0312(15) 0.0498(17) -0.0170(13) -0.0016(12) 0.0056(11) N15 0.0224(14) 0.0457(18) 0.066(2) -0.0021(16) 0.0040(13) 0.0070(12) N16 0.0184(11) 0.0238(12) 0.0316(13) 0.0048(10) -0.0017(9) 0.0012(9) N17 0.0230(12) 0.0182(12) 0.0233(12) 0.0005(9) 0.0006(9) -0.0015(9) N18 0.0335(15) 0.0220(13) 0.0543(18) -0.0082(12) -0.0010(13) -0.0022(11) N19 0.0294(14) 0.0232(14) 0.078(2) -0.0126(14) -0.0221(14) 0.0082(11) N20 0.0227(12) 0.0168(11) 0.0273(12) 0.0017(9) -0.0054(9) -0.0018(9) N21 0.0194(11) 0.0174(11) 0.0272(12) 0.0016(9) -0.0055(9) -0.0010(9) N22 0.059(2) 0.0472(18) 0.0264(14) 0.0026(13) -0.0024(13) -0.0260(15) N23 0.057(2) 0.0465(19) 0.0389(17) -0.0057(14) -0.0118(14) -0.0162(15) N24 0.0240(12) 0.0226(12) 0.0297(13) 0.0002(10) -0.0036(10) -0.0012(10) C1 0.0305(16) 0.0277(16) 0.0276(15) 0.0038(12) 0.0007(12) -0.0049(12) C2 0.0323(17) 0.0404(19) 0.0365(18) 0.0046(15) 0.0072(13) -0.0101(14) C3 0.0350(17) 0.0335(18) 0.0370(18) -0.0066(14) 0.0114(14) -0.0076(14) C4 0.0228(14) 0.0224(14) 0.0239(14) 0.0003(11) 0.0012(11) 0.0009(11) C5 0.0203(13) 0.0194(13) 0.0254(14) 0.0013(11) 0.0005(10) 0.0027(10) C6 0.0194(13) 0.0189(13) 0.0216(13) -0.0011(10) 0.0012(10) 0.0017(10) C7 0.0234(14) 0.0194(13) 0.0227(13) -0.0005(11) 0.0015(10) 0.0005(11) C8 0.0260(15) 0.0255(16) 0.0442(19) 0.0085(13) -0.0005(13) 0.0017(12) C9 0.0308(17) 0.0318(18) 0.049(2) 0.0106(15) 0.0068(14) -0.0059(13) C10 0.0219(14) 0.0279(16) 0.0352(16) 0.0008(13) 0.0017(12) -0.0014(12) C11 0.0207(14) 0.0275(15) 0.0276(15) 0.0015(12) 0.0011(11) -0.0002(11) C12 0.0188(13) 0.0329(17) 0.0326(16) -0.0013(13) -0.0023(11) 0.0000(12) C13 0.0248(14) 0.0312(16) 0.0270(15) 0.0046(12) -0.0016(11) 0.0004(12) C14 0.0198(13) 0.0193(13) 0.0231(13) -0.0014(11) 0.0016(10) 0.0020(10) C15 0.0200(13) 0.0233(14) 0.0219(13) -0.0031(11) 0.0015(10) 0.0012(11) C16 0.0197(13) 0.0262(15) 0.0273(14) -0.0009(12) 0.0016(11) 0.0014(11) C17 0.0201(14) 0.0253(15) 0.0351(16) 0.0027(12) 0.0006(12) 0.0021(11) C18 0.0235(15) 0.0366(19) 0.055(2) -0.0054(16) 0.0046(14) 0.0064(13) C19 0.0176(15) 0.049(2) 0.058(2) 0.0073(18) -0.0041(14) 0.0018(14) C20 0.0216(14) 0.0336(17) 0.0422(18) 0.0058(14) -0.0049(12) -0.0006(12) C21 0.0232(14) 0.0266(15) 0.0237(14) -0.0015(11) 0.0014(11) -0.0031(11) C22 0.0309(16) 0.0275(16) 0.0356(17) -0.0067(13) 0.0020(13) -0.0059(13) C23 0.0300(16) 0.0225(16) 0.057(2) -0.0032(14) -0.0055(14) 0.0027(13) C24 0.0256(14) 0.0205(14) 0.0337(16) 0.0004(12) -0.0051(12) -0.0008(11) C25 0.0259(14) 0.0200(14) 0.0333(16) 0.0044(12) -0.0063(12) -0.0009(11) C26 0.0268(14) 0.0231(15) 0.0277(15) 0.0029(12) -0.0053(11) -0.0014(11) C27 0.0270(15) 0.0251(15) 0.0292(15) 0.0006(12) -0.0045(12) -0.0022(12) C28 0.048(2) 0.0366(19) 0.0317(17) -0.0007(14) -0.0070(14) -0.0108(15) C29 0.051(2) 0.0369(19) 0.044(2) -0.0055(16) -0.0092(16) -0.0153(16) C30 0.0345(17) 0.0258(16) 0.0396(18) 0.0005(13) -0.0048(13) -0.0080(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N20 2.058(2) . ? Ni1 N4 2.075(2) . ? Ni1 N12 2.091(2) . ? Ni1 N9 2.092(2) . ? Ni1 N17 2.096(2) . ? Ni1 N1 2.100(2) . ? Ni2 N5 2.055(2) . ? Ni2 N21 2.085(2) . ? Ni2 N16 2.090(2) . ? Ni2 N13 2.093(2) . ? Ni2 N8 2.106(2) . ? Ni2 N24 2.112(2) . ? Cl1A Cl1B 0.836(6) . ? Cl1A O1 1.349(4) . ? Cl1A O2 1.385(4) . ? Cl1A O4A 1.409(7) . ? Cl1A O3 1.523(5) . ? Cl1A O4B 2.131(17) . ? Cl1B O3 1.199(6) . ? Cl1B O4B 1.379(16) . ? Cl1B O2 1.449(7) . ? Cl1B O1 1.511(6) . ? Cl2 O5 1.421(3) . ? Cl2 O6 1.430(3) . ? Cl2 O8 1.430(3) . ? Cl2 O7 1.446(3) . ? Cl3 O11 1.374(4) . ? Cl3 O12 1.416(3) . ? Cl3 O10 1.428(3) . ? Cl3 O9 1.446(3) . ? Cl4 O14 1.418(3) . ? Cl4 O15 1.430(3) . ? Cl4 O13 1.441(3) . ? Cl4 O16 1.442(2) . ? O17 H31 0.960(3) . ? O17 H32 0.965(4) . ? O18 O22 1.081(9) 2_645 ? O18 H33 0.973(6) . ? O18 H34 0.946(6) . ? O19 H35 0.964(4) . ? O19 H36 0.964(4) . ? O20 H37 0.884(3) . ? O20 H38 1.087(3) . ? O21 H39 1.003(3) . ? O21 H40 0.962(3) . ? O22 O18 1.081(9) 2_655 ? O22 H41 0.960(10) . ? O22 H42 0.978(10) . ? O24 H43 0.94(2) . ? O24 H44 1.03(3) . ? N1 C1 1.334(4) . ? N1 C4 1.356(4) . ? N2 C2 1.328(5) . ? N2 C3 1.338(4) . ? N3 C5 1.326(4) . ? N3 H19 0.784(3) . ? N3 H20 0.841(3) . ? N4 C5 1.305(4) . ? N4 N5 1.413(3) . ? N5 C6 1.296(4) . ? N6 C6 1.338(3) . ? N6 H21 0.816(2) . ? N6 H22 0.805(2) . ? N7 C9 1.321(4) . ? N7 C8 1.342(4) . ? N8 C10 1.333(4) . ? N8 C7 1.355(4) . ? N9 C11 1.331(4) . ? N9 C14 1.351(4) . ? N10 C12 1.327(4) . ? N10 C13 1.345(4) . ? N11 C15 1.327(4) . ? N11 H23 0.800(2) . ? N11 H24 0.966(3) . ? N12 C15 1.307(4) . ? N12 N13 1.423(3) . ? N13 C16 1.305(4) . ? N14 C16 1.325(4) . ? N14 H25 1.009(3) . ? N14 H26 0.684(3) . ? N15 C19 1.329(5) . ? N15 C18 1.337(4) . ? N16 C20 1.338(4) . ? N16 C17 1.342(4) . ? N17 C21 1.328(4) . ? N17 C24 1.351(4) . ? N18 C22 1.316(4) . ? N18 C23 1.342(4) . ? N19 C25 1.326(4) . ? N19 H27 0.762(3) . ? N19 H28 0.688(3) . ? N20 C25 1.295(4) . ? N20 N21 1.419(3) . ? N21 C26 1.296(4) . ? N22 C26 1.327(4) . ? N22 H29 0.846(3) . ? N22 H30 0.634(3) . ? N23 C29 1.327(5) . ? N23 C28 1.342(4) . ? N24 C30 1.330(4) . ? N24 C27 1.351(4) . ? C1 C2 1.390(5) . ? C1 H1 0.945(3) . ? C2 H2 0.942(3) . ? C3 C4 1.378(4) . ? C3 H3 0.952(3) . ? C4 C5 1.486(4) . ? C6 C7 1.491(4) . ? C7 C8 1.378(4) . ? C8 H4 0.946(3) . ? C9 C10 1.390(5) . ? C9 H5 0.952(3) . ? C10 H6 0.947(3) . ? C11 C12 1.397(4) . ? C11 H7 0.953(3) . ? C12 H8 0.954(3) . ? C13 C14 1.388(4) . ? C13 H9 0.952(3) . ? C14 C15 1.491(4) . ? C16 C17 1.490(4) . ? C17 C18 1.389(4) . ? C18 H10 0.950(4) . ? C19 C20 1.389(5) . ? C19 H11 0.950(3) . ? C20 H12 0.955(3) . ? C21 C22 1.399(4) . ? C21 H13 0.948(3) . ? C22 H14 0.949(3) . ? C23 C24 1.383(4) . ? C23 H15 0.943(3) . ? C24 C25 1.497(4) . ? C26 C27 1.492(4) . ? C27 C28 1.386(4) . ? C28 H16 0.947(4) . ? C29 C30 1.390(5) . ? C29 H17 0.943(3) . ? C30 H18 0.947(3) . ? 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 N20 Ni1 N4 90.11(9) . . ? N20 Ni1 N12 90.60(9) . . ? N4 Ni1 N12 89.19(9) . . ? N20 Ni1 N9 167.07(9) . . ? N4 Ni1 N9 95.24(9) . . ? N12 Ni1 N9 77.74(9) . . ? N20 Ni1 N17 77.33(9) . . ? N4 Ni1 N17 166.16(9) . . ? N12 Ni1 N17 96.64(9) . . ? N9 Ni1 N17 98.26(9) . . ? N20 Ni1 N1 98.02(9) . . ? N4 Ni1 N1 77.23(9) . . ? N12 Ni1 N1 163.86(9) . . ? N9 Ni1 N1 94.65(9) . . ? N17 Ni1 N1 98.54(9) . . ? N5 Ni2 N21 89.45(9) . . ? N5 Ni2 N16 165.46(9) . . ? N21 Ni2 N16 96.77(9) . . ? N5 Ni2 N13 89.03(9) . . ? N21 Ni2 N13 90.66(9) . . ? N16 Ni2 N13 77.81(9) . . ? N5 Ni2 N8 77.32(9) . . ? N21 Ni2 N8 164.72(9) . . ? N16 Ni2 N8 97.88(9) . . ? N13 Ni2 N8 96.65(9) . . ? N5 Ni2 N24 97.46(9) . . ? N21 Ni2 N24 76.70(9) . . ? N16 Ni2 N24 96.75(10) . . ? N13 Ni2 N24 165.66(9) . . ? N8 Ni2 N24 97.24(9) . . ? Cl1B Cl1A O1 84.0(5) . . ? Cl1B Cl1A O2 77.1(5) . . ? O1 Cl1A O2 116.9(3) . . ? Cl1B Cl1A O4A 159.8(5) . . ? O1 Cl1A O4A 107.7(5) . . ? O2 Cl1A O4A 110.2(5) . . ? Cl1B Cl1A O3 51.7(4) . . ? O1 Cl1A O3 107.0(3) . . ? O2 Cl1A O3 106.3(3) . . ? O4A Cl1A O3 108.3(3) . . ? Cl1B Cl1A O4B 20.4(6) . . ? O1 Cl1A O4B 72.4(5) . . ? O2 Cl1A O4B 69.5(6) . . ? O4A Cl1A O4B 179.7(7) . . ? O3 Cl1A O4B 71.9(5) . . ? Cl1A Cl1B O3 95.2(5) . . ? Cl1A Cl1B O4B 147.3(10) . . ? O3 Cl1B O4B 117.1(10) . . ? Cl1A Cl1B O2 68.7(5) . . ? O3 Cl1B O2 122.8(5) . . ? O4B Cl1B O2 95.7(10) . . ? Cl1A Cl1B O1 62.6(5) . . ? O3 Cl1B O1 116.6(5) . . ? O4B Cl1B O1 96.0(7) . . ? O2 Cl1B O1 103.8(5) . . ? O5 Cl2 O6 112.6(2) . . ? O5 Cl2 O8 110.5(2) . . ? O6 Cl2 O8 109.70(19) . . ? O5 Cl2 O7 106.2(2) . . ? O6 Cl2 O7 109.3(2) . . ? O8 Cl2 O7 108.4(2) . . ? O11 Cl3 O12 111.0(3) . . ? O11 Cl3 O10 112.1(3) . . ? O12 Cl3 O10 109.6(3) . . ? O11 Cl3 O9 109.6(3) . . ? O12 Cl3 O9 109.3(2) . . ? O10 Cl3 O9 105.0(2) . . ? O14 Cl4 O15 109.9(2) . . ? O14 Cl4 O13 109.69(19) . . ? O15 Cl4 O13 108.54(16) . . ? O14 Cl4 O16 109.63(18) . . ? O15 Cl4 O16 109.08(16) . . ? O13 Cl4 O16 109.99(16) . . ? Cl1A O1 Cl1B 33.4(2) . . ? Cl1A O2 Cl1B 34.2(2) . . ? Cl1B O3 Cl1A 33.1(3) . . ? Cl1B O4B Cl1A 12.2(4) . . ? H31 O17 H32 110.7(4) . . ? O22 O18 H33 86.9(9) 2_645 . ? O22 O18 H34 96.6(8) 2_645 . ? H33 O18 H34 107.9(5) . . ? H35 O19 H36 107.2(4) . . ? H37 O20 H38 106.6(3) . . ? H39 O21 H40 116.7(3) . . ? O18 O22 H41 79.2(8) 2_655 . ? O18 O22 H42 67.8(7) 2_655 . ? H41 O22 H42 106.3(8) . . ? H43 O24 H44 104(2) . . ? C1 N1 C4 116.8(3) . . ? C1 N1 Ni1 129.5(2) . . ? C4 N1 Ni1 113.55(18) . . ? C2 N2 C3 115.9(3) . . ? C5 N3 H19 116.3(3) . . ? C5 N3 H20 119.5(3) . . ? H19 N3 H20 123.6(3) . . ? C5 N4 N5 114.8(2) . . ? C5 N4 Ni1 115.48(18) . . ? N5 N4 Ni1 120.60(16) . . ? C6 N5 N4 115.9(2) . . ? C6 N5 Ni2 117.36(18) . . ? N4 N5 Ni2 120.86(16) . . ? C6 N6 H21 115.9(3) . . ? C6 N6 H22 122.0(3) . . ? H21 N6 H22 121.8(3) . . ? C9 N7 C8 116.2(3) . . ? C10 N8 C7 116.5(2) . . ? C10 N8 Ni2 129.5(2) . . ? C7 N8 Ni2 113.92(18) . . ? C11 N9 C14 117.6(2) . . ? C11 N9 Ni1 128.5(2) . . ? C14 N9 Ni1 113.84(17) . . ? C12 N10 C13 117.0(2) . . ? C15 N11 H23 121.9(3) . . ? C15 N11 H24 123.6(3) . . ? H23 N11 H24 114.1(3) . . ? C15 N12 N13 115.9(2) . . ? C15 N12 Ni1 114.85(18) . . ? N13 N12 Ni1 120.08(16) . . ? C16 N13 N12 115.3(2) . . ? C16 N13 Ni2 114.14(18) . . ? N12 N13 Ni2 120.40(17) . . ? C16 N14 H25 123.2(3) . . ? C16 N14 H26 130.3(3) . . ? H25 N14 H26 106.3(3) . . ? C19 N15 C18 116.2(3) . . ? C20 N16 C17 117.1(3) . . ? C20 N16 Ni2 129.4(2) . . ? C17 N16 Ni2 113.57(18) . . ? C21 N17 C24 116.7(2) . . ? C21 N17 Ni1 129.2(2) . . ? C24 N17 Ni1 113.93(18) . . ? C22 N18 C23 115.9(3) . . ? C25 N19 H27 116.2(3) . . ? C25 N19 H28 114.6(3) . . ? H27 N19 H28 128.9(4) . . ? C25 N20 N21 115.5(2) . . ? C25 N20 Ni1 116.67(19) . . ? N21 N20 Ni1 120.13(16) . . ? C26 N21 N20 116.1(2) . . ? C26 N21 Ni2 116.76(19) . . ? N20 N21 Ni2 120.28(16) . . ? C26 N22 H29 118.3(3) . . ? C26 N22 H30 113.8(3) . . ? H29 N22 H30 127.4(4) . . ? C29 N23 C28 116.5(3) . . ? C30 N24 C27 117.2(3) . . ? C30 N24 Ni2 128.6(2) . . ? C27 N24 Ni2 114.19(19) . . ? N1 C1 C2 121.2(3) . . ? N1 C1 H1 119.7(3) . . ? C2 C1 H1 119.1(3) . . ? N2 C2 C1 122.6(3) . . ? N2 C2 H2 118.3(3) . . ? C1 C2 H2 119.2(3) . . ? N2 C3 C4 122.8(3) . . ? N2 C3 H3 118.2(3) . . ? C4 C3 H3 119.0(3) . . ? N1 C4 C3 120.7(3) . . ? N1 C4 C5 115.2(2) . . ? C3 C4 C5 124.1(3) . . ? N4 C5 N3 125.3(3) . . ? N4 C5 C4 113.4(2) . . ? N3 C5 C4 121.2(3) . . ? N5 C6 N6 125.4(3) . . ? N5 C6 C7 114.1(2) . . ? N6 C6 C7 120.5(2) . . ? N8 C7 C8 121.4(3) . . ? N8 C7 C6 114.8(2) . . ? C8 C7 C6 123.9(3) . . ? N7 C8 C7 122.0(3) . . ? N7 C8 H4 119.1(3) . . ? C7 C8 H4 118.8(3) . . ? N7 C9 C10 122.8(3) . . ? N7 C9 H5 118.6(3) . . ? C10 C9 H5 118.6(3) . . ? N8 C10 C9 121.0(3) . . ? N8 C10 H6 119.4(3) . . ? C9 C10 H6 119.6(3) . . ? N9 C11 C12 121.1(3) . . ? N9 C11 H7 119.7(3) . . ? C12 C11 H7 119.3(3) . . ? N10 C12 C11 121.9(3) . . ? N10 C12 H8 119.0(3) . . ? C11 C12 H8 119.1(3) . . ? N10 C13 C14 121.8(3) . . ? N10 C13 H9 119.1(3) . . ? C14 C13 H9 119.1(3) . . ? N9 C14 C13 120.6(3) . . ? N9 C14 C15 115.5(2) . . ? C13 C14 C15 123.9(3) . . ? N12 C15 N11 126.4(3) . . ? N12 C15 C14 114.2(2) . . ? N11 C15 C14 119.5(2) . . ? N13 C16 N14 126.0(3) . . ? N13 C16 C17 114.1(3) . . ? N14 C16 C17 119.9(3) . . ? N16 C17 C18 121.2(3) . . ? N16 C17 C16 115.8(3) . . ? C18 C17 C16 123.1(3) . . ? N15 C18 C17 122.0(3) . . ? N15 C18 H10 119.5(3) . . ? C17 C18 H10 118.4(3) . . ? N15 C19 C20 122.6(3) . . ? N15 C19 H11 119.2(4) . . ? C20 C19 H11 118.2(4) . . ? N16 C20 C19 120.9(3) . . ? N16 C20 H12 119.4(3) . . ? C19 C20 H12 119.8(3) . . ? N17 C21 C22 120.9(3) . . ? N17 C21 H13 119.3(3) . . ? C22 C21 H13 119.8(3) . . ? N18 C22 C21 123.0(3) . . ? N18 C22 H14 118.4(3) . . ? C21 C22 H14 118.5(3) . . ? N18 C23 C24 122.2(3) . . ? N18 C23 H15 118.0(3) . . ? C24 C23 H15 119.8(3) . . ? N17 C24 C23 121.2(3) . . ? N17 C24 C25 114.6(3) . . ? C23 C24 C25 124.1(3) . . ? N20 C25 N19 126.0(3) . . ? N20 C25 C24 114.0(2) . . ? N19 C25 C24 119.9(3) . . ? N21 C26 N22 125.5(3) . . ? N21 C26 C27 114.1(3) . . ? N22 C26 C27 120.4(3) . . ? N24 C27 C28 121.1(3) . . ? N24 C27 C26 115.1(3) . . ? C28 C27 C26 123.8(3) . . ? N23 C28 C27 121.6(3) . . ? N23 C28 H16 119.0(3) . . ? C27 C28 H16 119.4(3) . . ? N23 C29 C30 122.5(3) . . ? N23 C29 H17 118.0(4) . . ? C30 C29 H17 119.5(4) . . ? N24 C30 C29 120.9(3) . . ? N24 C30 H18 120.2(3) . . ? C29 C30 H18 118.9(3) . . ? 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 O1 Cl1A Cl1B O3 -117.3(4) . . . . ? O2 Cl1A Cl1B O3 123.3(5) . . . . ? O4A Cl1A Cl1B O3 9(2) . . . . ? O4B Cl1A Cl1B O3 -171(2) . . . . ? O1 Cl1A Cl1B O4B 53.8(19) . . . . ? O2 Cl1A Cl1B O4B -65.6(19) . . . . ? O4A Cl1A Cl1B O4B -179(2) . . . . ? O3 Cl1A Cl1B O4B 171(2) . . . . ? O1 Cl1A Cl1B O2 119.4(3) . . . . ? O4A Cl1A Cl1B O2 -113.9(18) . . . . ? O3 Cl1A Cl1B O2 -123.3(5) . . . . ? O4B Cl1A Cl1B O2 65.6(19) . . . . ? O2 Cl1A Cl1B O1 -119.4(3) . . . . ? O4A Cl1A Cl1B O1 126.7(18) . . . . ? O3 Cl1A Cl1B O1 117.3(4) . . . . ? O4B Cl1A Cl1B O1 -53.8(19) . . . . ? O2 Cl1A O1 Cl1B 72.3(5) . . . . ? O4A Cl1A O1 Cl1B -163.1(6) . . . . ? O3 Cl1A O1 Cl1B -46.8(5) . . . . ? O4B Cl1A O1 Cl1B 17.2(7) . . . . ? O3 Cl1B O1 Cl1A 81.7(6) . . . . ? O4B Cl1B O1 Cl1A -154.0(11) . . . . ? O2 Cl1B O1 Cl1A -56.7(5) . . . . ? O1 Cl1A O2 Cl1B -76.3(5) . . . . ? O4A Cl1A O2 Cl1B 160.3(6) . . . . ? O3 Cl1A O2 Cl1B 43.1(4) . . . . ? O4B Cl1A O2 Cl1B -19.8(6) . . . . ? O3 Cl1B O2 Cl1A -82.2(7) . . . . ? O4B Cl1B O2 Cl1A 150.4(9) . . . . ? O1 Cl1B O2 Cl1A 52.8(4) . . . . ? O4B Cl1B O3 Cl1A -174.6(12) . . . . ? O2 Cl1B O3 Cl1A 67.9(7) . . . . ? O1 Cl1B O3 Cl1A -61.9(6) . . . . ? O1 Cl1A O3 Cl1B 67.6(6) . . . . ? O2 Cl1A O3 Cl1B -58.1(6) . . . . ? O4A Cl1A O3 Cl1B -176.6(7) . . . . ? O4B Cl1A O3 Cl1B 3.2(7) . . . . ? O3 Cl1B O4B Cl1A 170(2) . . . . ? O2 Cl1B O4B Cl1A -58.5(17) . . . . ? O1 Cl1B O4B Cl1A 46.1(16) . . . . ? O1 Cl1A O4B Cl1B -123(2) . . . . ? O2 Cl1A O4B Cl1B 108.7(19) . . . . ? O4A Cl1A O4B Cl1B 140(100) . . . . ? O3 Cl1A O4B Cl1B -7.3(17) . . . . ? N20 Ni1 N1 C1 -106.2(3) . . . . ? N4 Ni1 N1 C1 165.5(3) . . . . ? N12 Ni1 N1 C1 132.2(3) . . . . ? N9 Ni1 N1 C1 71.2(3) . . . . ? N17 Ni1 N1 C1 -27.9(3) . . . . ? N20 Ni1 N1 C4 78.19(19) . . . . ? N4 Ni1 N1 C4 -10.10(18) . . . . ? N12 Ni1 N1 C4 -43.5(4) . . . . ? N9 Ni1 N1 C4 -104.43(19) . . . . ? N17 Ni1 N1 C4 156.48(19) . . . . ? N20 Ni1 N4 C5 -78.2(2) . . . . ? N12 Ni1 N4 C5 -168.83(19) . . . . ? N9 Ni1 N4 C5 113.56(19) . . . . ? N17 Ni1 N4 C5 -53.6(5) . . . . ? N1 Ni1 N4 C5 19.96(19) . . . . ? N20 Ni1 N4 N5 67.10(19) . . . . ? N12 Ni1 N4 N5 -23.50(18) . . . . ? N9 Ni1 N4 N5 -101.11(18) . . . . ? N17 Ni1 N4 N5 91.7(4) . . . . ? N1 Ni1 N4 N5 165.30(19) . . . . ? C5 N4 N5 C6 -103.4(3) . . . . ? Ni1 N4 N5 C6 111.0(2) . . . . ? C5 N4 N5 Ni2 104.3(2) . . . . ? Ni1 N4 N5 Ni2 -41.2(2) . . . . ? N21 Ni2 N5 C6 -173.6(2) . . . . ? N16 Ni2 N5 C6 -58.0(5) . . . . ? N13 Ni2 N5 C6 -83.0(2) . . . . ? N8 Ni2 N5 C6 14.1(2) . . . . ? N24 Ni2 N5 C6 109.9(2) . . . . ? N21 Ni2 N5 N4 -21.76(19) . . . . ? N16 Ni2 N5 N4 93.9(4) . . . . ? N13 Ni2 N5 N4 68.90(19) . . . . ? N8 Ni2 N5 N4 165.9(2) . . . . ? N24 Ni2 N5 N4 -98.27(19) . . . . ? N5 Ni2 N8 C10 174.3(3) . . . . ? N21 Ni2 N8 C10 143.7(3) . . . . ? N16 Ni2 N8 C10 -19.6(3) . . . . ? N13 Ni2 N8 C10 -98.2(3) . . . . ? N24 Ni2 N8 C10 78.2(3) . . . . ? N5 Ni2 N8 C7 -6.81(19) . . . . ? N21 Ni2 N8 C7 -37.4(4) . . . . ? N16 Ni2 N8 C7 159.24(19) . . . . ? N13 Ni2 N8 C7 80.7(2) . . . . ? N24 Ni2 N8 C7 -102.9(2) . . . . ? N20 Ni1 N9 C11 145.8(4) . . . . ? N4 Ni1 N9 C11 -100.2(2) . . . . ? N12 Ni1 N9 C11 171.8(3) . . . . ? N17 Ni1 N9 C11 76.7(3) . . . . ? N1 Ni1 N9 C11 -22.6(3) . . . . ? N20 Ni1 N9 C14 -34.8(5) . . . . ? N4 Ni1 N9 C14 79.24(19) . . . . ? N12 Ni1 N9 C14 -8.79(19) . . . . ? N17 Ni1 N9 C14 -103.84(19) . . . . ? N1 Ni1 N9 C14 156.81(19) . . . . ? N20 Ni1 N12 C15 -168.2(2) . . . . ? N4 Ni1 N12 C15 -78.1(2) . . . . ? N9 Ni1 N12 C15 17.4(2) . . . . ? N17 Ni1 N12 C15 114.5(2) . . . . ? N1 Ni1 N12 C15 -45.7(4) . . . . ? N20 Ni1 N12 N13 -22.67(19) . . . . ? N4 Ni1 N12 N13 67.43(19) . . . . ? N9 Ni1 N12 N13 163.0(2) . . . . ? N17 Ni1 N12 N13 -99.98(19) . . . . ? N1 Ni1 N12 N13 99.9(3) . . . . ? C15 N12 N13 C16 -111.2(3) . . . . ? Ni1 N12 N13 C16 103.6(2) . . . . ? C15 N12 N13 Ni2 105.4(2) . . . . ? Ni1 N12 N13 Ni2 -39.8(2) . . . . ? N5 Ni2 N13 C16 -167.4(2) . . . . ? N21 Ni2 N13 C16 -78.0(2) . . . . ? N16 Ni2 N13 C16 18.8(2) . . . . ? N8 Ni2 N13 C16 115.5(2) . . . . ? N24 Ni2 N13 C16 -50.1(5) . . . . ? N5 Ni2 N13 N12 -23.63(19) . . . . ? N21 Ni2 N13 N12 65.81(19) . . . . ? N16 Ni2 N13 N12 162.6(2) . . . . ? N8 Ni2 N13 N12 -100.75(19) . . . . ? N24 Ni2 N13 N12 93.7(4) . . . . ? N5 Ni2 N16 C20 143.7(3) . . . . ? N21 Ni2 N16 C20 -101.5(3) . . . . ? N13 Ni2 N16 C20 169.3(3) . . . . ? N8 Ni2 N16 C20 74.2(3) . . . . ? N24 Ni2 N16 C20 -24.1(3) . . . . ? N5 Ni2 N16 C17 -35.1(5) . . . . ? N21 Ni2 N16 C17 79.6(2) . . . . ? N13 Ni2 N16 C17 -9.6(2) . . . . ? N8 Ni2 N16 C17 -104.7(2) . . . . ? N24 Ni2 N16 C17 157.0(2) . . . . ? N20 Ni1 N17 C21 173.5(3) . . . . ? N4 Ni1 N17 C21 148.2(3) . . . . ? N12 Ni1 N17 C21 -97.4(2) . . . . ? N9 Ni1 N17 C21 -18.8(3) . . . . ? N1 Ni1 N17 C21 77.2(3) . . . . ? N20 Ni1 N17 C24 -11.2(2) . . . . ? N4 Ni1 N17 C24 -36.5(5) . . . . ? N12 Ni1 N17 C24 77.9(2) . . . . ? N9 Ni1 N17 C24 156.5(2) . . . . ? N1 Ni1 N17 C24 -107.5(2) . . . . ? N4 Ni1 N20 C25 -168.6(2) . . . . ? N12 Ni1 N20 C25 -79.4(2) . . . . ? N9 Ni1 N20 C25 -54.0(5) . . . . ? N17 Ni1 N20 C25 17.3(2) . . . . ? N1 Ni1 N20 C25 114.3(2) . . . . ? N4 Ni1 N20 N21 -20.5(2) . . . . ? N12 Ni1 N20 N21 68.7(2) . . . . ? N9 Ni1 N20 N21 94.1(4) . . . . ? N17 Ni1 N20 N21 165.3(2) . . . . ? N1 Ni1 N20 N21 -97.6(2) . . . . ? C25 N20 N21 C26 -104.4(3) . . . . ? Ni1 N20 N21 C26 107.2(2) . . . . ? C25 N20 N21 Ni2 105.6(2) . . . . ? Ni1 N20 N21 Ni2 -42.8(3) . . . . ? N5 Ni2 N21 C26 -81.5(2) . . . . ? N16 Ni2 N21 C26 111.7(2) . . . . ? N13 Ni2 N21 C26 -170.5(2) . . . . ? N8 Ni2 N21 C26 -51.7(4) . . . . ? N24 Ni2 N21 C26 16.4(2) . . . . ? N5 Ni2 N21 N20 68.4(2) . . . . ? N16 Ni2 N21 N20 -98.5(2) . . . . ? N13 Ni2 N21 N20 -20.7(2) . . . . ? N8 Ni2 N21 N20 98.1(4) . . . . ? N24 Ni2 N21 N20 166.2(2) . . . . ? N5 Ni2 N24 C30 -99.7(3) . . . . ? N21 Ni2 N24 C30 172.7(3) . . . . ? N16 Ni2 N24 C30 77.3(3) . . . . ? N13 Ni2 N24 C30 144.0(4) . . . . ? N8 Ni2 N24 C30 -21.6(3) . . . . ? N5 Ni2 N24 C27 78.2(2) . . . . ? N21 Ni2 N24 C27 -9.5(2) . . . . ? N16 Ni2 N24 C27 -104.9(2) . . . . ? N13 Ni2 N24 C27 -38.2(5) . . . . ? N8 Ni2 N24 C27 156.2(2) . . . . ? C4 N1 C1 C2 0.3(4) . . . . ? Ni1 N1 C1 C2 -175.2(2) . . . . ? C3 N2 C2 C1 2.3(5) . . . . ? N1 C1 C2 N2 -2.6(5) . . . . ? C2 N2 C3 C4 0.0(5) . . . . ? C1 N1 C4 C3 1.9(4) . . . . ? Ni1 N1 C4 C3 178.2(2) . . . . ? C1 N1 C4 C5 -175.7(2) . . . . ? Ni1 N1 C4 C5 0.5(3) . . . . ? N2 C3 C4 N1 -2.2(5) . . . . ? N2 C3 C4 C5 175.2(3) . . . . ? N5 N4 C5 N3 9.1(4) . . . . ? Ni1 N4 C5 N3 156.5(2) . . . . ? N5 N4 C5 C4 -172.6(2) . . . . ? Ni1 N4 C5 C4 -25.3(3) . . . . ? N1 C4 C5 N4 16.2(3) . . . . ? C3 C4 C5 N4 -161.4(3) . . . . ? N1 C4 C5 N3 -165.5(3) . . . . ? C3 C4 C5 N3 17.0(4) . . . . ? N4 N5 C6 N6 8.1(4) . . . . ? Ni2 N5 C6 N6 161.3(2) . . . . ? N4 N5 C6 C7 -171.3(2) . . . . ? Ni2 N5 C6 C7 -18.1(3) . . . . ? C10 N8 C7 C8 -0.5(4) . . . . ? Ni2 N8 C7 C8 -179.5(2) . . . . ? C10 N8 C7 C6 179.0(2) . . . . ? Ni2 N8 C7 C6 0.0(3) . . . . ? N5 C6 C7 N8 11.6(4) . . . . ? N6 C6 C7 N8 -167.8(3) . . . . ? N5 C6 C7 C8 -168.9(3) . . . . ? N6 C6 C7 C8 11.7(4) . . . . ? C9 N7 C8 C7 -1.9(5) . . . . ? N8 C7 C8 N7 1.8(5) . . . . ? C6 C7 C8 N7 -177.6(3) . . . . ? C8 N7 C9 C10 0.8(5) . . . . ? C7 N8 C10 C9 -0.6(4) . . . . ? Ni2 N8 C10 C9 178.3(2) . . . . ? N7 C9 C10 N8 0.4(5) . . . . ? C14 N9 C11 C12 -0.9(4) . . . . ? Ni1 N9 C11 C12 178.6(2) . . . . ? C13 N10 C12 C11 0.5(5) . . . . ? N9 C11 C12 N10 0.5(5) . . . . ? C12 N10 C13 C14 -1.2(5) . . . . ? C11 N9 C14 C13 0.2(4) . . . . ? Ni1 N9 C14 C13 -179.3(2) . . . . ? C11 N9 C14 C15 179.8(2) . . . . ? Ni1 N9 C14 C15 0.3(3) . . . . ? N10 C13 C14 N9 0.9(5) . . . . ? N10 C13 C14 C15 -178.7(3) . . . . ? N13 N12 C15 N11 9.2(4) . . . . ? Ni1 N12 C15 N11 156.2(3) . . . . ? N13 N12 C15 C14 -169.2(2) . . . . ? Ni1 N12 C15 C14 -22.2(3) . . . . ? N9 C14 C15 N12 14.6(4) . . . . ? C13 C14 C15 N12 -165.8(3) . . . . ? N9 C14 C15 N11 -163.9(3) . . . . ? C13 C14 C15 N11 15.7(4) . . . . ? N12 N13 C16 N14 9.7(4) . . . . ? Ni2 N13 C16 N14 155.4(3) . . . . ? N12 N13 C16 C17 -169.6(2) . . . . ? Ni2 N13 C16 C17 -23.9(3) . . . . ? C20 N16 C17 C18 0.8(4) . . . . ? Ni2 N16 C17 C18 179.8(3) . . . . ? C20 N16 C17 C16 -178.6(3) . . . . ? Ni2 N16 C17 C16 0.4(3) . . . . ? N13 C16 C17 N16 15.8(4) . . . . ? N14 C16 C17 N16 -163.5(3) . . . . ? N13 C16 C17 C18 -163.6(3) . . . . ? N14 C16 C17 C18 17.1(5) . . . . ? C19 N15 C18 C17 -0.5(5) . . . . ? N16 C17 C18 N15 -0.3(5) . . . . ? C16 C17 C18 N15 179.1(3) . . . . ? C18 N15 C19 C20 0.9(6) . . . . ? C17 N16 C20 C19 -0.5(5) . . . . ? Ni2 N16 C20 C19 -179.3(2) . . . . ? N15 C19 C20 N16 -0.4(6) . . . . ? C24 N17 C21 C22 -1.7(4) . . . . ? Ni1 N17 C21 C22 173.5(2) . . . . ? C23 N18 C22 C21 2.2(5) . . . . ? N17 C21 C22 N18 -0.7(5) . . . . ? C22 N18 C23 C24 -1.2(5) . . . . ? C21 N17 C24 C23 2.6(4) . . . . ? Ni1 N17 C24 C23 -173.3(3) . . . . ? C21 N17 C24 C25 -179.2(3) . . . . ? Ni1 N17 C24 C25 4.9(3) . . . . ? N18 C23 C24 N17 -1.2(5) . . . . ? N18 C23 C24 C25 -179.2(3) . . . . ? N21 N20 C25 N19 8.6(5) . . . . ? Ni1 N20 C25 N19 158.1(3) . . . . ? N21 N20 C25 C24 -169.1(2) . . . . ? Ni1 N20 C25 C24 -19.6(3) . . . . ? N17 C24 C25 N20 9.4(4) . . . . ? C23 C24 C25 N20 -172.5(3) . . . . ? N17 C24 C25 N19 -168.5(3) . . . . ? C23 C24 C25 N19 9.7(5) . . . . ? N20 N21 C26 N22 8.0(4) . . . . ? Ni2 N21 C26 N22 159.1(3) . . . . ? N20 N21 C26 C27 -170.7(2) . . . . ? Ni2 N21 C26 C27 -19.6(3) . . . . ? C30 N24 C27 C28 1.4(5) . . . . ? Ni2 N24 C27 C28 -176.6(3) . . . . ? C30 N24 C27 C26 -179.2(3) . . . . ? Ni2 N24 C27 C26 2.8(3) . . . . ? N21 C26 C27 N24 10.9(4) . . . . ? N22 C26 C27 N24 -167.9(3) . . . . ? N21 C26 C27 C28 -169.7(3) . . . . ? N22 C26 C27 C28 11.5(5) . . . . ? C29 N23 C28 C27 -1.0(6) . . . . ? N24 C27 C28 N23 -0.3(6) . . . . ? C26 C27 C28 N23 -179.7(3) . . . . ? C28 N23 C29 C30 1.3(6) . . . . ? C27 N24 C30 C29 -1.2(5) . . . . ? Ni2 N24 C30 C29 176.6(3) . . . . ? N23 C29 C30 N24 -0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.785 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.082 #===END data_l8m (4) _database_code_CSD 158602 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 Cl4 Cu2 N24 O21' _chemical_formula_weight 1341.74 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' '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.7623(8) _cell_length_b 13.3002(6) _cell_length_c 21.6942(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.3990(10) _cell_angle_gamma 90.00 _cell_volume 5125.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 987 _cell_measurement_theta_min 16.03 _cell_measurement_theta_max 27.01 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _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 'Bruker SMART-CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54029 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.49 _reflns_number_total 11750 _reflns_number_gt 10661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+5.6275P] 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 11750 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.003 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 0.135801(11) 0.779644(14) 0.364512(9) 0.01194(5) Uani 1 1 d . . . Cu2 Cu 0.312403(11) 0.629924(14) 0.357910(9) 0.01237(5) Uani 1 1 d . . . Cl3 Cl 0.12869(2) 0.94457(3) 0.568603(18) 0.01738(8) Uani 1 1 d . . . N1 N 0.32406(8) 0.49302(10) 0.40020(6) 0.0137(3) Uani 1 1 d . . . N10 N 0.14555(8) 0.63726(10) 0.33143(6) 0.0127(3) Uani 1 1 d . . . N46 N 0.23110(8) 0.81678(10) 0.32015(6) 0.0139(3) Uani 1 1 d . . . N36 N 0.05333(8) 0.74123(10) 0.42948(6) 0.0134(3) Uani 1 1 d . . . N54 N 0.13759(8) 0.93119(10) 0.37822(6) 0.0133(3) Uani 1 1 d . . . N44 N 0.24542(11) 0.78282(14) 0.19885(8) 0.0274(4) Uani 1 1 d . . . N51 N 0.16697(9) 1.13304(11) 0.40504(7) 0.0202(3) Uani 1 1 d . . . N48 N 0.32821(9) 0.93599(13) 0.32134(9) 0.0242(3) Uani 1 1 d . . . N12 N 0.14772(9) 0.54518(12) 0.23963(7) 0.0189(3) Uani 1 1 d . . . O9 O 0.10373(8) 1.01773(10) 0.61394(6) 0.0230(3) Uani 1 1 d . . . N9 N 0.20711(8) 0.57741(10) 0.35104(6) 0.0128(3) Uani 1 1 d . . . N19 N 0.41078(8) 0.69667(10) 0.39012(7) 0.0145(3) Uani 1 1 d . . . N26 N 0.30912(9) 0.87556(12) 0.48199(8) 0.0214(3) Uani 1 1 d . . . N45 N 0.28328(8) 0.74377(10) 0.29929(6) 0.0132(3) Uani 1 1 d . . . O10 O 0.06500(8) 0.91101(11) 0.53303(6) 0.0258(3) Uani 1 1 d . . . O12 O 0.16318(9) 0.86092(11) 0.59982(7) 0.0327(3) Uani 1 1 d . . . N28 N 0.20100(8) 0.74133(11) 0.45250(6) 0.0141(3) Uani 1 1 d . . . C29 C 0.16138(9) 0.68169(12) 0.48716(8) 0.0145(3) Uani 1 1 d . . . N4 N 0.31761(9) 0.30640(12) 0.45920(8) 0.0228(3) Uani 1 1 d . . . N37 N 0.36245(8) 0.58611(11) 0.26240(7) 0.0177(3) Uani 1 1 d . . . C11 C 0.12247(9) 0.61939(12) 0.27483(8) 0.0136(3) Uani 1 1 d . . . N33 N -0.04702(8) 0.67741(11) 0.52005(7) 0.0178(3) Uani 1 1 d . . . C35 C -0.02080(10) 0.75475(13) 0.42328(8) 0.0160(3) Uani 1 1 d . . . C34 C -0.07088(10) 0.72216(13) 0.46829(8) 0.0173(3) Uani 1 1 d . . . N22 N 0.53494(8) 0.79903(12) 0.43902(8) 0.0217(3) Uani 1 1 d . . . N8 N 0.12121(9) 0.46571(12) 0.39527(7) 0.0175(3) Uani 1 1 d . . . C31 C 0.07856(9) 0.69649(12) 0.48174(7) 0.0137(3) Uani 1 1 d . . . N27 N 0.27715(8) 0.71392(10) 0.44583(6) 0.0140(3) Uani 1 1 d . . . C21 C 0.54266(10) 0.72810(14) 0.39581(9) 0.0213(4) Uani 1 1 d . . . C20 C 0.48080(10) 0.67714(13) 0.37128(8) 0.0179(3) Uani 1 1 d . . . C32 C 0.02780(10) 0.66590(13) 0.52678(8) 0.0170(3) Uani 1 1 d . . . C25 C 0.32462(9) 0.78713(13) 0.45573(8) 0.0152(3) Uani 1 1 d . . . O11 O 0.18276(7) 0.99181(11) 0.52806(6) 0.0248(3) Uani 1 1 d . . . N18 N 0.05040(8) 0.77149(11) 0.28537(7) 0.0157(3) Uani 1 1 d . . . C7 C 0.19050(9) 0.49825(12) 0.38395(7) 0.0136(3) Uani 1 1 d . . . C2 C 0.38615(10) 0.44786(13) 0.42087(8) 0.0171(3) Uani 1 1 d . . . C24 C 0.40258(9) 0.76691(12) 0.43468(8) 0.0149(3) Uani 1 1 d . . . N15 N -0.03809(9) 0.72781(13) 0.18178(8) 0.0253(3) Uani 1 1 d . . . N40 N 0.38972(11) 0.54736(14) 0.13766(8) 0.0333(4) Uani 1 1 d . . . C50 C 0.21821(10) 1.07433(13) 0.37742(9) 0.0201(4) Uani 1 1 d . . . C52 C 0.10093(10) 1.09049(13) 0.41697(8) 0.0179(3) Uani 1 1 d . . . C47 C 0.25862(9) 0.90592(12) 0.33260(8) 0.0154(3) Uani 1 1 d . . . C5 C 0.25510(10) 0.35167(13) 0.43730(8) 0.0190(3) Uani 1 1 d . . . N30 N 0.18865(10) 0.60944(13) 0.52383(8) 0.0213(3) Uani 1 1 d . . . C49 C 0.20409(9) 0.97432(12) 0.36331(8) 0.0151(3) Uani 1 1 d . . . C42 C 0.33273(10) 0.64441(12) 0.21763(8) 0.0164(3) Uani 1 1 d . . . C43 C 0.28455(10) 0.72902(12) 0.23957(8) 0.0160(3) Uani 1 1 d . . . C17 C -0.00585(10) 0.83128(14) 0.26758(8) 0.0191(3) Uani 1 1 d . . . C53 C 0.08577(9) 0.98947(13) 0.40426(8) 0.0151(3) Uani 1 1 d . . . C3 C 0.38219(11) 0.35448(14) 0.45051(9) 0.0214(4) Uani 1 1 d . . . C23 C 0.46490(10) 0.81766(13) 0.45838(9) 0.0192(3) Uani 1 1 d . . . C6 C 0.25769(9) 0.44435(12) 0.40857(7) 0.0139(3) Uani 1 1 d . . . C13 C 0.06220(9) 0.68827(13) 0.25152(8) 0.0149(3) Uani 1 1 d . . . C39 C 0.41995(12) 0.49205(16) 0.18244(10) 0.0295(4) Uani 1 1 d . . . C41 C 0.34585(12) 0.62412(15) 0.15575(9) 0.0249(4) Uani 1 1 d . . . C16 C -0.05061(11) 0.80839(15) 0.21658(9) 0.0226(4) Uani 1 1 d . . . C38 C 0.40614(11) 0.51041(14) 0.24449(9) 0.0221(4) Uani 1 1 d . . . C14 C 0.01863(11) 0.66760(14) 0.19993(9) 0.0216(4) Uani 1 1 d . . . Cl64 Cl 0.09717(2) 0.00740(3) 0.16748(2) 0.02051(9) Uani 1 1 d . . . O68 O 0.11066(9) -0.09953(11) 0.16947(8) 0.0335(3) Uani 1 1 d . . . O65 O 0.12135(11) 0.04441(12) 0.10842(8) 0.0436(4) Uani 1 1 d . . . O66 O 0.01782(8) 0.02582(12) 0.17380(9) 0.0385(4) Uani 1 1 d . . . O67 O 0.13711(11) 0.05746(16) 0.21567(9) 0.0502(5) Uani 1 1 d . . . Cl2 Cl 0.39268(2) 0.92526(4) 0.07285(2) 0.02311(9) Uani 1 1 d . . . O5 O 0.33583(9) 0.99551(14) 0.05358(8) 0.0404(4) Uani 1 1 d . . . O6 O 0.43370(9) 0.96455(12) 0.12541(7) 0.0339(3) Uani 1 1 d . . . O7 O 0.44425(8) 0.90786(12) 0.02316(7) 0.0309(3) Uani 1 1 d . . . O8 O 0.35647(11) 0.83258(14) 0.08960(8) 0.0465(5) Uani 1 1 d . . . Cl59 Cl 0.40380(3) 0.19407(4) 0.29530(2) 0.03022(11) Uani 1 1 d . . . O62 O 0.40025(10) 0.13263(12) 0.34990(8) 0.0372(4) Uani 1 1 d . . . O60 O 0.38659(10) 0.29666(12) 0.30999(8) 0.0392(4) Uani 1 1 d . . . O61 O 0.47609(13) 0.18750(14) 0.26926(11) 0.0636(7) Uani 1 1 d . . . O63 O 0.34843(17) 0.15679(18) 0.25235(12) 0.0816(8) Uani 1 1 d . . . O58 O 0.25244(11) 0.31226(14) 0.06083(8) 0.0399(4) Uani 1 1 d . . . O56 O 0.23768(10) 0.37607(12) 0.26595(8) 0.0320(3) Uani 1 1 d . . . O69 O 0.43700(9) 0.86427(15) 0.24214(8) 0.0312(3) Uani 1 1 d . . . O57 O 0.17821(10) 0.26521(14) 0.17082(8) 0.0350(4) Uani 1 1 d . . . O55 O 0.39268(11) 0.05724(12) 0.47637(9) 0.0380(4) Uani 1 1 d . . . H53 H 0.0407(12) 0.9612(15) 0.4153(9) 0.013(5) Uiso 1 1 d . . . H2 H 0.4314(13) 0.4798(17) 0.4150(10) 0.023(6) Uiso 1 1 d . . . H34 H -0.1208(13) 0.7304(16) 0.4621(10) 0.017(5) Uiso 1 1 d . . . H8B H 0.1128(13) 0.4178(18) 0.4161(11) 0.020(6) Uiso 1 1 d . . . H20 H 0.4861(12) 0.6328(16) 0.3410(10) 0.017(5) Uiso 1 1 d . . . H35 H -0.0401(12) 0.7838(16) 0.3877(10) 0.017(5) Uiso 1 1 d . . . H50 H 0.2646(14) 1.1015(18) 0.3667(11) 0.030(6) Uiso 1 1 d . . . H8A H 0.0842(14) 0.4956(18) 0.3799(11) 0.023(6) Uiso 1 1 d . . . H52 H 0.0639(13) 1.1306(17) 0.4343(10) 0.021(5) Uiso 1 1 d . . . H5 H 0.2081(13) 0.3162(18) 0.4412(11) 0.024(6) Uiso 1 1 d . . . H23 H 0.4590(13) 0.8668(18) 0.4875(11) 0.026(6) Uiso 1 1 d . . . H38 H 0.4271(13) 0.4728(18) 0.2737(11) 0.025(6) Uiso 1 1 d . . . H17 H -0.0168(13) 0.8880(17) 0.2919(11) 0.022(6) Uiso 1 1 d . . . H32 H 0.0448(12) 0.6390(16) 0.5644(10) 0.019(5) Uiso 1 1 d . . . H21 H 0.5906(13) 0.7150(17) 0.3819(11) 0.023(6) Uiso 1 1 d . . . H3 H 0.4263(14) 0.3240(18) 0.4643(11) 0.029(6) Uiso 1 1 d . . . H44A H 0.2161(14) 0.829(2) 0.2096(11) 0.029(6) Uiso 1 1 d . . . H12B H 0.1794(14) 0.5032(19) 0.2523(11) 0.025(6) Uiso 1 1 d . . . H30B H 0.2325(15) 0.6048(18) 0.5297(11) 0.026(6) Uiso 1 1 d . . . H14 H 0.0267(13) 0.6084(18) 0.1751(11) 0.026(6) Uiso 1 1 d . . . H16 H -0.0888(13) 0.8489(18) 0.2063(11) 0.024(6) Uiso 1 1 d . . . H48A H 0.3406(14) 0.995(2) 0.3281(12) 0.031(6) Uiso 1 1 d . . . H30A H 0.1631(15) 0.5755(19) 0.5420(12) 0.027(6) Uiso 1 1 d . . . H12A H 0.1352(14) 0.5410(19) 0.2032(13) 0.031(7) Uiso 1 1 d . . . H39 H 0.4502(16) 0.439(2) 0.1699(13) 0.042(7) Uiso 1 1 d . . . H26B H 0.3381(15) 0.924(2) 0.4808(12) 0.031(6) Uiso 1 1 d . . . H48B H 0.3556(16) 0.900(2) 0.3025(13) 0.040(8) Uiso 1 1 d . . . H41 H 0.3254(14) 0.6638(19) 0.1246(12) 0.032(6) Uiso 1 1 d . . . H26A H 0.2647(15) 0.8858(19) 0.4958(12) 0.031(6) Uiso 1 1 d . . . H56B H 0.2784(18) 0.355(2) 0.2783(14) 0.045(8) Uiso 1 1 d . . . H69A H 0.4569(17) 0.819(2) 0.2379(13) 0.037(8) Uiso 1 1 d . . . H58A H 0.247(2) 0.372(3) 0.0506(17) 0.070(11) Uiso 1 1 d . . . H57A H 0.1778(18) 0.209(3) 0.1800(15) 0.049(9) Uiso 1 1 d . . . H57B H 0.2019(19) 0.271(3) 0.1374(17) 0.061(10) Uiso 1 1 d . . . H44B H 0.2513(18) 0.776(2) 0.1643(15) 0.050(9) Uiso 1 1 d . . . H55B H 0.4010(19) 0.089(3) 0.5081(17) 0.061(10) Uiso 1 1 d . . . H56A H 0.2211(18) 0.341(2) 0.2398(16) 0.054(9) Uiso 1 1 d . . . H69B H 0.4334(17) 0.889(2) 0.2108(15) 0.042(9) Uiso 1 1 d . . . H58B H 0.281(2) 0.291(3) 0.0342(17) 0.065(11) Uiso 1 1 d . . . H55A H 0.4019(19) 0.093(3) 0.4440(17) 0.064(10) 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 0.01147(9) 0.01030(9) 0.01407(10) -0.00029(7) 0.00172(7) -0.00055(7) Cu2 0.01088(9) 0.01106(9) 0.01516(10) 0.00157(7) -0.00035(7) -0.00074(7) Cl3 0.01762(19) 0.01932(19) 0.01522(18) 0.00023(14) 0.00147(14) 0.00273(15) N1 0.0145(7) 0.0131(6) 0.0136(6) -0.0008(5) 0.0000(5) 0.0002(5) N10 0.0118(6) 0.0121(6) 0.0142(6) 0.0011(5) -0.0013(5) -0.0001(5) N46 0.0142(6) 0.0120(6) 0.0155(7) -0.0003(5) 0.0022(5) 0.0012(5) N36 0.0143(6) 0.0118(6) 0.0140(6) -0.0016(5) 0.0007(5) -0.0010(5) N54 0.0137(6) 0.0128(6) 0.0135(6) 0.0008(5) 0.0003(5) -0.0002(5) N44 0.0379(10) 0.0294(9) 0.0150(8) 0.0013(7) 0.0014(7) 0.0173(8) N51 0.0197(7) 0.0149(7) 0.0261(8) -0.0024(6) 0.0014(6) 0.0008(6) N48 0.0192(8) 0.0137(7) 0.0399(10) -0.0055(7) 0.0119(7) -0.0036(6) N12 0.0230(8) 0.0188(7) 0.0148(7) -0.0024(6) -0.0037(6) 0.0052(6) O9 0.0276(7) 0.0236(7) 0.0179(6) -0.0037(5) 0.0023(5) 0.0045(5) N9 0.0119(6) 0.0123(6) 0.0142(6) 0.0006(5) -0.0012(5) 0.0001(5) N19 0.0138(7) 0.0136(6) 0.0161(7) 0.0023(5) 0.0002(5) -0.0004(5) N26 0.0153(7) 0.0179(8) 0.0311(9) -0.0080(6) 0.0047(6) -0.0026(6) N45 0.0127(6) 0.0111(6) 0.0157(7) 0.0001(5) 0.0019(5) 0.0011(5) O10 0.0221(7) 0.0323(7) 0.0231(7) -0.0051(6) 0.0000(5) -0.0049(6) O12 0.0402(9) 0.0281(8) 0.0298(8) 0.0069(6) -0.0008(6) 0.0146(6) N28 0.0113(6) 0.0158(7) 0.0151(7) -0.0011(5) 0.0007(5) -0.0003(5) C29 0.0138(8) 0.0154(8) 0.0144(7) -0.0025(6) 0.0003(6) -0.0006(6) N4 0.0238(8) 0.0169(7) 0.0275(8) 0.0062(6) -0.0016(6) 0.0014(6) N37 0.0192(7) 0.0148(7) 0.0190(7) 0.0003(5) 0.0016(6) 0.0010(5) C11 0.0131(7) 0.0127(7) 0.0150(7) 0.0010(6) 0.0006(6) -0.0028(6) N33 0.0158(7) 0.0186(7) 0.0190(7) 0.0014(6) 0.0036(5) -0.0010(5) C35 0.0165(8) 0.0158(8) 0.0156(8) 0.0002(6) -0.0009(6) 0.0006(6) C34 0.0128(8) 0.0190(8) 0.0199(8) -0.0015(6) 0.0008(6) 0.0004(6) N22 0.0147(7) 0.0224(8) 0.0280(8) 0.0007(6) -0.0020(6) -0.0025(6) N8 0.0140(7) 0.0168(7) 0.0217(8) 0.0067(6) -0.0008(6) -0.0026(6) C31 0.0149(8) 0.0114(7) 0.0147(7) -0.0010(6) 0.0003(6) -0.0005(6) N27 0.0114(6) 0.0159(7) 0.0147(7) 0.0003(5) 0.0011(5) 0.0002(5) C21 0.0136(8) 0.0241(9) 0.0262(9) 0.0020(7) 0.0027(7) 0.0008(7) C20 0.0162(8) 0.0186(8) 0.0188(8) 0.0009(7) 0.0024(6) 0.0019(6) C32 0.0163(8) 0.0179(8) 0.0168(8) 0.0035(6) 0.0012(6) -0.0004(6) C25 0.0152(8) 0.0169(8) 0.0135(7) 0.0002(6) 0.0001(6) -0.0004(6) O11 0.0202(6) 0.0294(7) 0.0248(7) 0.0005(5) 0.0071(5) -0.0020(5) N18 0.0166(7) 0.0152(7) 0.0154(7) 0.0016(5) 0.0006(5) 0.0003(5) C7 0.0153(8) 0.0129(7) 0.0124(7) -0.0022(6) -0.0006(6) -0.0015(6) C2 0.0145(8) 0.0180(8) 0.0187(8) -0.0009(6) -0.0007(6) 0.0001(6) C24 0.0150(8) 0.0140(7) 0.0158(8) 0.0021(6) 0.0002(6) -0.0003(6) N15 0.0231(8) 0.0311(9) 0.0216(8) -0.0011(7) -0.0079(6) 0.0054(7) N40 0.0433(11) 0.0322(9) 0.0244(9) -0.0059(7) 0.0064(8) 0.0119(8) C50 0.0168(8) 0.0154(8) 0.0282(9) -0.0012(7) 0.0034(7) -0.0016(6) C52 0.0180(8) 0.0170(8) 0.0187(8) -0.0016(6) 0.0001(6) 0.0035(6) C47 0.0160(8) 0.0136(7) 0.0167(8) 0.0015(6) 0.0026(6) 0.0007(6) C5 0.0189(8) 0.0161(8) 0.0220(9) 0.0032(7) -0.0005(7) -0.0017(7) N30 0.0121(7) 0.0273(8) 0.0245(8) 0.0108(7) 0.0018(6) 0.0000(6) C49 0.0149(8) 0.0143(8) 0.0163(8) 0.0010(6) 0.0014(6) 0.0003(6) C42 0.0172(8) 0.0133(7) 0.0187(8) 0.0004(6) 0.0030(6) 0.0007(6) C43 0.0174(8) 0.0135(7) 0.0171(8) 0.0020(6) 0.0027(6) -0.0003(6) C17 0.0218(9) 0.0174(8) 0.0181(8) 0.0024(7) 0.0009(7) 0.0030(7) C53 0.0141(8) 0.0167(8) 0.0145(8) 0.0008(6) 0.0006(6) 0.0009(6) C3 0.0197(9) 0.0196(8) 0.0248(9) 0.0035(7) -0.0032(7) 0.0036(7) C23 0.0172(8) 0.0171(8) 0.0233(9) -0.0023(7) -0.0015(7) -0.0019(6) C6 0.0149(8) 0.0131(7) 0.0138(7) -0.0011(6) 0.0000(6) -0.0004(6) C13 0.0143(7) 0.0159(8) 0.0144(8) 0.0018(6) 0.0008(6) -0.0003(6) C39 0.0337(11) 0.0229(10) 0.0320(11) -0.0065(8) 0.0067(9) 0.0097(8) C41 0.0317(10) 0.0236(9) 0.0196(9) -0.0012(7) 0.0035(8) 0.0061(8) C16 0.0195(9) 0.0259(9) 0.0224(9) 0.0043(7) -0.0020(7) 0.0054(7) C38 0.0232(9) 0.0169(8) 0.0263(10) 0.0005(7) 0.0019(7) 0.0044(7) C14 0.0220(9) 0.0233(9) 0.0195(9) -0.0033(7) -0.0038(7) 0.0030(7) Cl64 0.01751(19) 0.0216(2) 0.0224(2) -0.00135(16) -0.00080(15) 0.00170(15) O68 0.0329(8) 0.0239(7) 0.0438(9) 0.0084(6) 0.0084(7) 0.0088(6) O65 0.0690(12) 0.0278(8) 0.0344(9) 0.0068(7) 0.0195(8) 0.0125(8) O66 0.0199(7) 0.0369(9) 0.0587(11) -0.0125(8) -0.0021(7) 0.0082(6) O67 0.0461(10) 0.0617(12) 0.0424(10) -0.0124(9) -0.0163(8) -0.0129(9) Cl2 0.0201(2) 0.0281(2) 0.0212(2) 0.00223(17) -0.00144(16) -0.00710(17) O5 0.0290(8) 0.0557(11) 0.0365(9) 0.0067(8) 0.0013(7) 0.0109(7) O6 0.0322(8) 0.0434(9) 0.0262(7) -0.0045(6) -0.0060(6) -0.0117(7) O7 0.0254(7) 0.0408(9) 0.0265(7) -0.0008(6) 0.0018(6) 0.0001(6) O8 0.0581(11) 0.0431(10) 0.0383(9) 0.0042(8) 0.0019(8) -0.0314(9) Cl59 0.0375(3) 0.0196(2) 0.0337(3) 0.00091(18) 0.0089(2) -0.00305(19) O62 0.0459(10) 0.0313(8) 0.0347(8) 0.0066(6) 0.0049(7) -0.0111(7) O60 0.0394(9) 0.0250(8) 0.0533(10) -0.0018(7) 0.0042(8) 0.0043(7) O61 0.0717(14) 0.0338(10) 0.0861(16) 0.0015(10) 0.0548(12) 0.0015(9) O63 0.121(2) 0.0516(13) 0.0720(16) -0.0001(11) -0.0472(15) -0.0236(14) O58 0.0527(11) 0.0293(9) 0.0378(9) -0.0021(7) 0.0155(8) 0.0063(8) O56 0.0299(8) 0.0255(8) 0.0405(9) -0.0119(7) -0.0101(7) 0.0097(6) O69 0.0259(8) 0.0384(9) 0.0293(9) -0.0010(7) 0.0095(6) 0.0048(7) O57 0.0413(9) 0.0305(9) 0.0332(9) -0.0034(7) -0.0011(7) -0.0060(7) O55 0.0525(11) 0.0276(8) 0.0338(9) -0.0011(7) -0.0087(8) -0.0151(7) _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 N46 2.0144(14) . ? Cu1 N10 2.0330(14) . ? Cu1 N54 2.0376(14) . ? Cu1 N36 2.1030(14) . ? Cu1 N28 2.2834(14) . ? Cu1 N18 2.2857(15) . ? Cu2 N9 2.0010(14) . ? Cu2 N45 2.0417(14) . ? Cu2 N1 2.0488(14) . ? Cu2 N19 2.0768(14) . ? Cu2 N27 2.3011(14) . ? Cu2 N37 2.3343(15) . ? Cl3 O10 1.4361(14) . ? Cl3 O12 1.4374(14) . ? Cl3 O11 1.4500(14) . ? Cl3 O9 1.4549(13) . ? N1 C2 1.331(2) . ? N1 C6 1.358(2) . ? N10 C11 1.313(2) . ? N10 N9 1.4156(18) . ? N46 C47 1.310(2) . ? N46 N45 1.4186(19) . ? N36 C35 1.335(2) . ? N36 C31 1.354(2) . ? N54 C53 1.332(2) . ? N54 C49 1.354(2) . ? N44 C43 1.329(2) . ? N51 C52 1.330(2) . ? N51 C50 1.343(2) . ? N48 C47 1.324(2) . ? N12 C11 1.328(2) . ? N9 C7 1.307(2) . ? N19 C20 1.337(2) . ? N19 C24 1.353(2) . ? N26 C25 1.336(2) . ? N45 C43 1.311(2) . ? N28 C29 1.303(2) . ? N28 N27 1.4094(19) . ? C29 N30 1.336(2) . ? C29 C31 1.488(2) . ? N4 C3 1.328(2) . ? N4 C5 1.347(2) . ? N37 C38 1.331(2) . ? N37 C42 1.348(2) . ? C11 C13 1.495(2) . ? N33 C34 1.337(2) . ? N33 C32 1.345(2) . ? C35 C34 1.395(2) . ? N22 C21 1.338(3) . ? N22 C23 1.339(2) . ? N8 C7 1.329(2) . ? C31 C32 1.395(2) . ? N27 C25 1.305(2) . ? C21 C20 1.393(3) . ? C25 C24 1.486(2) . ? N18 C17 1.332(2) . ? N18 C13 1.346(2) . ? C7 C6 1.488(2) . ? C2 C3 1.401(2) . ? C24 C23 1.392(2) . ? N15 C16 1.331(3) . ? N15 C14 1.344(2) . ? N40 C39 1.329(3) . ? N40 C41 1.344(3) . ? C50 C49 1.387(2) . ? C52 C53 1.397(2) . ? C47 C49 1.489(2) . ? C5 C6 1.382(2) . ? C42 C41 1.391(3) . ? C42 C43 1.494(2) . ? C17 C16 1.392(3) . ? C13 C14 1.384(2) . ? C39 C38 1.392(3) . ? Cl64 O67 1.4246(17) . ? Cl64 O66 1.4379(15) . ? Cl64 O65 1.4410(16) . ? Cl64 O68 1.4428(15) . ? Cl2 O5 1.4357(17) . ? Cl2 O7 1.4382(15) . ? Cl2 O8 1.4382(16) . ? Cl2 O6 1.4467(15) . ? Cl59 O61 1.4092(19) . ? Cl59 O60 1.4347(16) . ? Cl59 O63 1.438(2) . ? Cl59 O62 1.4407(16) . ? 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 N46 Cu1 N10 89.19(5) . . ? N46 Cu1 N54 79.33(6) . . ? N10 Cu1 N54 166.33(6) . . ? N46 Cu1 N36 166.25(6) . . ? N10 Cu1 N36 94.11(5) . . ? N54 Cu1 N36 98.79(5) . . ? N46 Cu1 N28 91.78(5) . . ? N10 Cu1 N28 92.48(5) . . ? N54 Cu1 N28 95.25(5) . . ? N36 Cu1 N28 74.75(5) . . ? N46 Cu1 N18 102.02(5) . . ? N10 Cu1 N18 75.43(5) . . ? N54 Cu1 N18 99.56(5) . . ? N36 Cu1 N18 91.73(5) . . ? N28 Cu1 N18 161.34(5) . . ? N9 Cu2 N45 88.85(6) . . ? N9 Cu2 N1 79.32(6) . . ? N45 Cu2 N1 164.25(6) . . ? N9 Cu2 N19 163.35(6) . . ? N45 Cu2 N19 95.83(5) . . ? N1 Cu2 N19 98.46(5) . . ? N9 Cu2 N27 88.38(5) . . ? N45 Cu2 N27 94.99(5) . . ? N1 Cu2 N27 95.02(5) . . ? N19 Cu2 N27 75.33(5) . . ? N9 Cu2 N37 102.02(5) . . ? N45 Cu2 N37 74.26(5) . . ? N1 Cu2 N37 97.92(5) . . ? N19 Cu2 N37 94.62(5) . . ? N27 Cu2 N37 164.69(5) . . ? O10 Cl3 O12 110.13(9) . . ? O10 Cl3 O11 109.35(8) . . ? O12 Cl3 O11 109.84(9) . . ? O10 Cl3 O9 109.17(8) . . ? O12 Cl3 O9 109.27(8) . . ? O11 Cl3 O9 109.06(8) . . ? C2 N1 C6 117.25(14) . . ? C2 N1 Cu2 129.26(12) . . ? C6 N1 Cu2 113.47(11) . . ? C11 N10 N9 114.49(13) . . ? C11 N10 Cu1 118.15(11) . . ? N9 N10 Cu1 119.03(10) . . ? C47 N46 N45 116.20(14) . . ? C47 N46 Cu1 115.92(11) . . ? N45 N46 Cu1 122.52(10) . . ? C35 N36 C31 117.66(14) . . ? C35 N36 Cu1 126.22(12) . . ? C31 N36 Cu1 116.10(11) . . ? C53 N54 C49 117.46(14) . . ? C53 N54 Cu1 128.85(12) . . ? C49 N54 Cu1 113.38(11) . . ? C52 N51 C50 116.15(15) . . ? C7 N9 N10 116.12(13) . . ? C7 N9 Cu2 117.06(11) . . ? N10 N9 Cu2 123.07(10) . . ? C20 N19 C24 117.23(15) . . ? C20 N19 Cu2 126.60(12) . . ? C24 N19 Cu2 116.17(11) . . ? C43 N45 N46 115.70(14) . . ? C43 N45 Cu2 119.91(11) . . ? N46 N45 Cu2 118.18(10) . . ? C29 N28 N27 115.12(14) . . ? C29 N28 Cu1 110.22(11) . . ? N27 N28 Cu1 116.97(10) . . ? N28 C29 N30 125.90(16) . . ? N28 C29 C31 114.30(15) . . ? N30 C29 C31 119.76(15) . . ? C3 N4 C5 116.46(15) . . ? C38 N37 C42 116.83(16) . . ? C38 N37 Cu2 132.41(13) . . ? C42 N37 Cu2 110.26(11) . . ? N10 C11 N12 124.59(16) . . ? N10 C11 C13 115.06(14) . . ? N12 C11 C13 120.33(15) . . ? C34 N33 C32 116.68(15) . . ? N36 C35 C34 121.41(16) . . ? N33 C34 C35 121.75(16) . . ? C21 N22 C23 116.76(16) . . ? N36 C31 C32 120.19(15) . . ? N36 C31 C29 116.46(14) . . ? C32 C31 C29 123.34(15) . . ? C25 N27 N28 114.19(14) . . ? C25 N27 Cu2 108.63(11) . . ? N28 N27 Cu2 118.53(10) . . ? N22 C21 C20 121.76(17) . . ? N19 C20 C21 121.41(17) . . ? N33 C32 C31 122.28(16) . . ? N27 C25 N26 126.30(16) . . ? N27 C25 C24 114.65(15) . . ? N26 C25 C24 119.05(15) . . ? C17 N18 C13 116.89(15) . . ? C17 N18 Cu1 132.99(12) . . ? C13 N18 Cu1 110.12(11) . . ? N9 C7 N8 125.17(16) . . ? N9 C7 C6 113.61(14) . . ? N8 C7 C6 121.21(15) . . ? N1 C2 C3 120.71(16) . . ? N19 C24 C23 120.63(16) . . ? N19 C24 C25 116.73(14) . . ? C23 C24 C25 122.63(15) . . ? C16 N15 C14 116.20(16) . . ? C39 N40 C41 116.04(18) . . ? N51 C50 C49 122.26(17) . . ? N51 C52 C53 122.68(16) . . ? N46 C47 N48 125.68(16) . . ? N46 C47 C49 113.71(14) . . ? N48 C47 C49 120.59(16) . . ? N4 C5 C6 121.85(16) . . ? N54 C49 C50 120.66(15) . . ? N54 C49 C47 114.77(14) . . ? C50 C49 C47 124.56(16) . . ? N37 C42 C41 121.10(16) . . ? N37 C42 C43 115.24(15) . . ? C41 C42 C43 123.65(16) . . ? N45 C43 N44 124.32(16) . . ? N45 C43 C42 116.21(15) . . ? N44 C43 C42 119.46(16) . . ? N18 C17 C16 121.54(17) . . ? N54 C53 C52 120.69(16) . . ? N4 C3 C2 122.57(17) . . ? N22 C23 C24 122.18(17) . . ? N1 C6 C5 121.13(15) . . ? N1 C6 C7 114.65(14) . . ? C5 C6 C7 124.21(15) . . ? N18 C13 C14 121.10(16) . . ? N18 C13 C11 115.69(14) . . ? C14 C13 C11 123.17(16) . . ? N40 C39 C38 122.48(18) . . ? N40 C41 C42 122.04(18) . . ? N15 C16 C17 122.04(17) . . ? N37 C38 C39 121.49(18) . . ? N15 C14 C13 122.18(17) . . ? O67 Cl64 O66 109.50(11) . . ? O67 Cl64 O65 110.05(12) . . ? O66 Cl64 O65 108.96(11) . . ? O67 Cl64 O68 110.92(11) . . ? O66 Cl64 O68 109.14(10) . . ? O65 Cl64 O68 108.23(9) . . ? O5 Cl2 O7 109.69(9) . . ? O5 Cl2 O8 108.46(12) . . ? O7 Cl2 O8 109.86(11) . . ? O5 Cl2 O6 110.11(11) . . ? O7 Cl2 O6 109.20(9) . . ? O8 Cl2 O6 109.51(10) . . ? O61 Cl59 O60 110.13(11) . . ? O61 Cl59 O63 109.86(18) . . ? O60 Cl59 O63 109.03(13) . . ? O61 Cl59 O62 109.86(13) . . ? O60 Cl59 O62 110.26(11) . . ? O63 Cl59 O62 107.67(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.986 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.062 #===END data__x583(6) _database_code_CSD 158603 #==================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 16.088(2) _cell_length_b 16.950(4) _cell_length_c 11.104(3) _cell_angle_alpha 108.37(2) _cell_angle_beta 101.84(2) _cell_angle_gamma 90.75(2) _cell_volume 2803(1) _cell_formula_units_Z 2 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 21 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 18.0 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'irregular' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.996 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1684.61 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H43 Br8 N18 O3.50 Zn4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1626.00 _exptl_absorpt_coefficient_mu 7.464 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.623 _exptl_special_details ; The scan width was (1.05+0.35tan\q)\% with an \w scan speed of 8\% per minute (up to 11 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #==================================================================== #========= # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.30 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -4 2 1 -1 2 -1 -3 3 _diffrn_reflns_number 13364 _reflns_number_total 12907 _reflns_number_gt 6247 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.05020 _diffrn_reflns_av_sigmaI/netI 0.149 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00068 _diffrn_orient_matrix_UB_12 0.01237 _diffrn_orient_matrix_UB_13 0.09442 _diffrn_orient_matrix_UB_21 -0.03948 _diffrn_orient_matrix_UB_22 -0.05098 _diffrn_orient_matrix_UB_23 -0.02167 _diffrn_orient_matrix_UB_31 0.05002 _diffrn_orient_matrix_UB_32 -0.03376 _diffrn_orient_matrix_UB_33 0.00895 #------------------------------------------------------------------------------ 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 C 0 72 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 86 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 36 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 16 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 7 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Zn 0 8 0.222 1.431 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #==================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy #_atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Br(1) 0.38965(5) 0.52894(5) -0.08416(8) 0.0455(2) 1.000 Uani d ? Br(2) 0.21424(6) 0.53803(6) 0.11710(8) 0.0558(3) 1.000 Uani d ? Br(3) 0.14551(5) 0.50397(6) -0.26188(8) 0.0611(3) 1.000 Uani d ? Br(4) 0.25678(7) 0.72079(6) -0.0041(1) 0.0681(3) 1.000 Uani d ? Br(5) 0.35177(6) 0.10798(6) 0.6494(1) 0.0640(3) 1.000 Uani d ? Br(6) 0.30201(7) -0.02178(7) 0.87133(9) 0.0699(3) 1.000 Uani d ? Br(7) 0.11620(5) 0.02905(6) 0.6155(1) 0.0598(3) 1.000 Uani d ? Br(8) 0.2723(1) -0.13946(7) 0.5109(1) 0.1159(6) 1.000 Uani d ? Zn(1) 0.14898(5) 0.31910(5) 0.24435(8) 0.0316(2) 1.000 Uani d ? Zn(2) 0.36051(5) 0.21322(5) 0.28678(8) 0.0314(2) 1.000 Uani d ? Zn(3) 0.24608(5) 0.57147(6) -0.06253(8) 0.0381(3) 1.000 Uani d ? Zn(4) 0.26439(6) -0.00471(6) 0.66071(9) 0.0471(3) 1.000 Uani d ? O(1) 0.5590(4) 0.4030(4) 0.3267(5) 0.064(2) 1.000 Uani d ? O(2) 0.6661(4) 0.2638(4) 0.2710(6) 0.081(2) 1.000 Uani d ? O(3) 0.9871(7) 0.0789(7) 0.873(1) 0.129(4) 0.750 Uiso d ? O(4) 0.878(1) 0.190(1) 0.796(2) 0.128(6) 0.500 Uiso d ? O(5) 0.916(2) 0.092(2) 0.701(4) 0.14(1) 0.250 Uiso d ? N(1) 0.1500(3) 0.4476(3) 0.3567(5) 0.032(2) 1.000 Uani d ? N(2) 0.3785(4) 0.4722(4) 0.4202(6) 0.046(2) 1.000 Uani d ? N(3) 0.2762(3) 0.3733(3) 0.2643(5) 0.028(2) 1.000 Uani d ? N(4) 0.3427(3) 0.3220(3) 0.2334(5) 0.029(2) 1.000 Uani d ? N(5) 0.3544(5) 0.3850(4) 0.0780(7) 0.063(3) 1.000 Uani d ? N(6) 0.4397(4) 0.2037(4) 0.1448(5) 0.034(2) 1.000 Uani d ? N(7) 0.0392(3) 0.2630(4) 0.2815(6) 0.037(2) 1.000 Uani d ? N(8) 0.1776(4) 0.1616(5) 0.4717(7) 0.065(3) 1.000 Uani d ? N(9) 0.2003(3) 0.2724(4) 0.4009(5) 0.032(2) 1.000 Uani d ? N(10) 0.2887(3) 0.2637(3) 0.4364(5) 0.029(2) 1.000 Uani d ? N(11) 0.2962(4) 0.3720(4) 0.6293(6) 0.055(2) 1.000 Uani d ? N(12) 0.4554(3) 0.2671(4) 0.4697(5) 0.033(2) 1.000 Uani d ? N(13) 0.3563(4) 0.0866(4) 0.2808(6) 0.037(2) 1.000 Uani d ? N(14) 0.1354(4) 0.0548(4) 0.1144(8) 0.068(3) 1.000 Uani d ? N(15) 0.2428(3) 0.1570(3) 0.1519(5) 0.030(2) 1.000 Uani d ? N(16) 0.1793(3) 0.2060(3) 0.1093(6) 0.034(2) 1.000 Uani d ? N(17) 0.2316(5) 0.1754(5) -0.0795(6) 0.064(3) 1.000 Uani d ? N(18) 0.0913(4) 0.3255(4) 0.0560(6) 0.036(2) 1.000 Uani d ? C(1) 0.0820(4) 0.4893(5) 0.3815(7) 0.039(2) 1.000 Uani d ? C(2) 0.0884(5) 0.5743(5) 0.4479(8) 0.050(3) 1.000 Uani d ? C(3) 0.1653(5) 0.6169(5) 0.4900(8) 0.052(3) 1.000 Uani d ? C(4) 0.2364(5) 0.5758(5) 0.4668(7) 0.042(2) 1.000 Uani d ? C(5) 0.2270(4) 0.4913(4) 0.4001(7) 0.030(2) 1.000 Uani d ? C(6) 0.2980(4) 0.4419(4) 0.3599(7) 0.029(2) 1.000 Uani d ? C(7) 0.3723(5) 0.3270(4) 0.1375(7) 0.035(2) 1.000 Uani d ? C(8) 0.4318(4) 0.2640(4) 0.0896(7) 0.033(2) 1.000 Uani d ? C(9) 0.4722(5) 0.2620(5) -0.0096(7) 0.045(3) 1.000 Uani d ? C(10) 0.5189(5) 0.1969(6) -0.0539(7) 0.050(3) 1.000 Uani d ? C(11) 0.5264(5) 0.1366(5) 0.0011(8) 0.049(3) 1.000 Uani d ? C(12) 0.4860(5) 0.1416(5) 0.1016(7) 0.044(2) 1.000 Uani d ? C(13) -0.0419(5) 0.2628(5) 0.2243(8) 0.051(3) 1.000 Uani d ? C(14) -0.1080(5) 0.2151(6) 0.240(1) 0.065(3) 1.000 Uani d ? C(15) -0.0866(5) 0.1677(6) 0.320(1) 0.068(3) 1.000 Uani d ? C(16) -0.0032(5) 0.1693(6) 0.3830(9) 0.063(3) 1.000 Uani d ? C(17) 0.0581(4) 0.2153(5) 0.3596(7) 0.039(2) 1.000 Uani d ? C(18) 0.1516(5) 0.2182(5) 0.4156(7) 0.041(2) 1.000 Uani d ? C(19) 0.3298(4) 0.3157(4) 0.5426(7) 0.031(2) 1.000 Uani d ? C(20) 0.4241(4) 0.3117(4) 0.5723(7) 0.033(2) 1.000 Uani d ? C(21) 0.4757(5) 0.3485(5) 0.6926(7) 0.045(2) 1.000 Uani d ? C(22) 0.5617(5) 0.3435(6) 0.7117(8) 0.058(3) 1.000 Uani d ? C(23) 0.5942(5) 0.2965(6) 0.6089(9) 0.054(3) 1.000 Uani d ? C(24) 0.5392(5) 0.2600(5) 0.4887(7) 0.044(3) 1.000 Uani d ? C(25) 0.0355(5) 0.3781(5) 0.0249(8) 0.047(3) 1.000 Uani d ? C(26) 0.0048(6) 0.3776(6) -0.100(1) 0.065(3) 1.000 Uani d ? C(27) 0.0360(7) 0.3239(7) -0.1983(9) 0.082(4) 1.000 Uani d ? C(28) 0.0934(7) 0.2680(6) -0.1701(8) 0.078(4) 1.000 Uani d ? C(29) 0.1208(5) 0.2718(5) -0.0418(7) 0.043(2) 1.000 Uani d ? C(30) 0.1812(5) 0.2135(5) -0.0032(7) 0.041(2) 1.000 Uani d ? C(31) 0.2154(5) 0.0870(5) 0.1569(7) 0.042(2) 1.000 Uani d ? C(32) 0.2823(5) 0.0413(4) 0.2175(7) 0.035(2) 1.000 Uani d ? C(33) 0.2699(6) -0.0425(5) 0.2014(8) 0.050(3) 1.000 Uani d ? C(34) 0.3354(6) -0.0803(5) 0.2585(8) 0.053(3) 1.000 Uani d ? C(35) 0.4101(6) -0.0352(5) 0.3237(8) 0.050(3) 1.000 Uani d ? C(36) 0.4190(5) 0.0483(5) 0.3343(7) 0.049(3) 1.000 Uani d ? H(1A) 0.0302 0.4530 0.3421 0.046 1.000 Uiso c ? H(1B) 0.5646 0.4097 0.2496 0.080 1.000 Uiso c ? H(1C) 0.5887 0.3703 0.3267 0.080 1.000 Uiso c ? H(2A) 0.3952 0.5101 0.4799 0.050 1.000 Uiso c ? H(2B) 0.0461 0.5906 0.4481 0.055 1.000 Uiso c ? H(2C) 0.4247 0.4459 0.3968 0.050 1.000 Uiso c ? H(2D) 0.6635 0.2955 0.2458 0.098 1.000 Uiso c ? H(2E) 0.6722 0.2192 0.2882 0.098 1.000 Uiso c ? H(3A) 0.1729 0.6742 0.5427 0.062 1.000 Uiso c ? H(3B) 1.0398 0.0463 0.8915 0.153 0.750 Uiso d ? H(3C) 0.9613 0.1142 0.9652 0.153 0.750 Uiso d ? H(4A) 0.9009 0.2088 0.8687 0.154 0.500 Uiso d ? H(4B) 0.2849 0.6030 0.4920 0.048 1.000 Uiso c ? H(5A) 0.9161 0.1477 0.6574 0.167 0.250 Uiso d ? H(5B) 0.9393 0.0535 0.7470 0.167 0.250 Uiso d ? H(5C) 0.4523 0.2942 -0.0435 0.050 1.000 Uiso c ? H(5D) 0.3093 0.4082 0.0957 0.075 1.000 Uiso c ? H(5E) 0.3508 0.3659 0.0060 0.075 1.000 Uiso c ? H(6) 0.5428 0.1955 -0.1153 0.061 1.000 Uiso c ? H(7) 0.5522 0.0963 -0.0172 0.057 1.000 Uiso c ? H(8A) 0.1506 0.1420 0.4924 0.075 1.000 Uiso c ? H(8B) 0.4973 0.1095 0.1463 0.050 1.000 Uiso c ? H(8C) 0.2426 0.1585 0.5059 0.075 1.000 Uiso c ? H(9) -0.0532 0.2788 0.1737 0.059 1.000 Uiso c ? H(10) -0.1631 0.2160 0.1872 0.077 1.000 Uiso c ? H(11A) -0.1304 0.1380 0.3335 0.081 1.000 Uiso c ? H(11B) 0.2369 0.3700 0.5964 0.067 1.000 Uiso c ? H(11C) 0.3266 0.4139 0.7064 0.067 1.000 Uiso c ? H(12) 0.0103 0.1406 0.4381 0.074 1.000 Uiso c ? H(13) 0.4606 0.3821 0.7568 0.053 1.000 Uiso c ? H(14A) 0.1008 0.0654 0.0745 0.076 1.000 Uiso c ? H(14B) 0.6052 0.3623 0.7978 0.068 1.000 Uiso c ? H(14C) 0.1243 0.0082 0.0985 0.076 1.000 Uiso c ? H(15) 0.6381 0.2911 0.6225 0.062 1.000 Uiso c ? H(16) 0.5567 0.2301 0.4215 0.051 1.000 Uiso c ? H(17A) 0.0303 0.4210 0.1133 0.058 1.000 Uiso c ? H(17B) 0.2667 0.1368 -0.0724 0.071 1.000 Uiso c ? H(17C) 0.2296 0.1798 -0.1636 0.071 1.000 Uiso c ? H(18) -0.0289 0.4196 -0.1015 0.076 1.000 Uiso c ? H(19) -0.0005 0.3082 -0.2968 0.098 1.000 Uiso c ? H(20) 0.0959 0.2314 -0.2275 0.090 1.000 Uiso c ? H(21) 0.2103 -0.0767 0.1749 0.061 1.000 Uiso c ? H(22) 0.3335 -0.1415 0.2432 0.065 1.000 Uiso c ? H(23) 0.4646 -0.0562 0.3583 0.059 1.000 Uiso c ? H(24) 0.4643 0.0771 0.3642 0.057 1.000 Uiso c ? 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 Br(1) 0.0329(4) 0.0539(5) 0.0467(5) 0.0084(4) 0.0095(4) 0.0117(4) Br(2) 0.0512(5) 0.0769(7) 0.0594(6) 0.0196(5) 0.0212(4) 0.0438(5) Br(3) 0.0381(5) 0.0849(7) 0.0497(5) 0.0109(5) -0.0039(4) 0.0156(5) Br(4) 0.0784(7) 0.0430(6) 0.0827(7) 0.0092(5) 0.0096(6) 0.0253(5) Br(5) 0.0384(5) 0.0848(7) 0.0802(7) -0.0020(5) 0.0031(5) 0.0494(6) Br(6) 0.0827(7) 0.0774(7) 0.0627(6) 0.0304(6) 0.0115(5) 0.0429(6) Br(7) 0.0381(5) 0.0622(6) 0.0924(7) 0.0039(4) 0.0042(5) 0.0500(6) Br(8) 0.203(2) 0.0643(8) 0.108(1) 0.0517(9) 0.096(1) 0.0256(7) Zn(1) 0.0256(4) 0.0316(5) 0.0423(5) 0.0044(4) 0.0068(4) 0.0187(4) Zn(2) 0.0313(5) 0.0287(5) 0.0362(5) 0.0067(4) 0.0068(4) 0.0138(4) Zn(3) 0.0323(5) 0.0447(6) 0.0406(5) 0.0081(4) 0.0065(4) 0.0194(4) Zn(4) 0.0489(6) 0.0463(6) 0.0565(6) 0.0167(5) 0.0167(5) 0.0273(5) O(1) 0.063(4) 0.070(4) 0.049(4) -0.002(3) 0.006(3) 0.013(3) O(2) 0.081(5) 0.078(5) 0.083(5) 0.007(4) 0.020(4) 0.025(4) N(1) 0.024(3) 0.036(4) 0.041(4) 0.008(3) 0.007(3) 0.020(3) N(2) 0.031(4) 0.041(4) 0.057(4) 0.004(3) 0.008(3) 0.001(3) N(3) 0.023(3) 0.029(3) 0.040(4) 0.008(3) 0.011(3) 0.021(3) N(4) 0.024(3) 0.020(3) 0.046(4) 0.005(2) 0.009(3) 0.014(3) N(5) 0.090(6) 0.063(5) 0.072(5) 0.044(4) 0.055(5) 0.046(4) N(6) 0.034(4) 0.038(4) 0.031(3) 0.008(3) 0.010(3) 0.011(3) N(7) 0.019(3) 0.045(4) 0.057(4) 0.005(3) 0.010(3) 0.029(3) N(8) 0.033(4) 0.088(6) 0.107(6) 0.007(4) 0.009(4) 0.081(5) N(9) 0.025(3) 0.039(4) 0.042(4) 0.002(3) 0.009(3) 0.023(3) N(10) 0.021(3) 0.036(4) 0.036(3) 0.006(3) 0.008(3) 0.018(3) N(11) 0.042(4) 0.062(5) 0.048(4) 0.014(4) 0.007(3) -0.000(4) N(12) 0.029(3) 0.039(4) 0.029(3) 0.008(3) 0.007(3) 0.010(3) N(13) 0.046(4) 0.028(4) 0.044(4) 0.015(3) 0.014(3) 0.017(3) N(14) 0.044(5) 0.046(5) 0.114(7) -0.014(4) 0.003(4) 0.036(5) N(15) 0.030(3) 0.025(3) 0.031(3) 0.004(3) 0.001(3) 0.010(3) N(16) 0.029(3) 0.024(3) 0.050(4) 0.004(3) 0.003(3) 0.017(3) N(17) 0.082(6) 0.067(5) 0.045(4) 0.035(5) 0.018(4) 0.020(4) N(18) 0.034(4) 0.031(4) 0.046(4) 0.005(3) 0.006(3) 0.021(3) C(1) 0.032(4) 0.041(5) 0.045(5) 0.007(4) 0.010(4) 0.014(4) C(2) 0.045(5) 0.058(6) 0.058(6) 0.033(5) 0.024(4) 0.025(5) C(3) 0.045(5) 0.042(5) 0.060(6) 0.018(4) 0.017(4) 0.002(4) C(4) 0.037(5) 0.037(5) 0.045(5) -0.001(4) 0.002(4) 0.009(4) C(5) 0.030(4) 0.029(4) 0.037(4) 0.006(3) 0.011(3) 0.016(3) C(6) 0.026(4) 0.026(4) 0.041(4) 0.007(3) 0.010(3) 0.015(4) C(7) 0.043(5) 0.029(4) 0.042(5) 0.006(4) 0.020(4) 0.016(4) C(8) 0.029(4) 0.036(4) 0.032(4) 0.001(3) 0.009(3) 0.007(3) C(9) 0.057(5) 0.041(5) 0.038(5) 0.008(4) 0.014(4) 0.015(4) C(10) 0.054(6) 0.063(6) 0.036(5) 0.012(5) 0.020(4) 0.012(4) C(11) 0.041(5) 0.050(5) 0.057(6) 0.023(4) 0.020(4) 0.011(5) C(12) 0.036(5) 0.052(5) 0.047(5) 0.020(4) 0.015(4) 0.017(4) C(13) 0.047(5) 0.052(6) 0.059(6) 0.004(4) 0.004(4) 0.031(5) C(14) 0.018(4) 0.072(7) 0.122(9) 0.002(4) 0.007(5) 0.059(6) C(15) 0.034(5) 0.081(7) 0.106(8) -0.008(5) 0.008(5) 0.060(6) C(16) 0.036(5) 0.081(7) 0.107(8) 0.013(5) 0.024(5) 0.072(6) C(17) 0.028(4) 0.042(5) 0.056(5) 0.005(4) 0.013(4) 0.027(4) C(18) 0.034(4) 0.050(5) 0.052(5) 0.014(4) 0.015(4) 0.031(4) C(19) 0.032(4) 0.036(4) 0.027(4) 0.006(3) 0.009(3) 0.010(3) C(20) 0.026(4) 0.031(4) 0.041(4) 0.003(3) 0.007(3) 0.011(4) C(21) 0.033(5) 0.063(6) 0.038(5) 0.010(4) 0.007(4) 0.013(4) C(22) 0.029(5) 0.079(7) 0.051(5) 0.005(4) 0.001(4) 0.007(5) C(23) 0.029(5) 0.066(6) 0.065(6) 0.006(4) 0.003(4) 0.022(5) C(24) 0.032(5) 0.058(6) 0.047(5) 0.010(4) 0.014(4) 0.019(4) C(25) 0.043(5) 0.044(5) 0.056(5) 0.010(4) 0.004(4) 0.025(4) C(26) 0.067(7) 0.056(6) 0.072(7) 0.016(5) -0.004(5) 0.032(5) C(27) 0.093(8) 0.077(8) 0.063(7) 0.025(6) -0.023(6) 0.030(6) C(28) 0.116(9) 0.079(8) 0.037(5) 0.038(7) 0.007(5) 0.023(5) C(29) 0.052(5) 0.034(5) 0.040(5) 0.003(4) -0.000(4) 0.014(4) C(30) 0.043(5) 0.038(5) 0.038(5) 0.008(4) -0.001(4) 0.013(4) C(31) 0.044(5) 0.031(5) 0.049(5) 0.004(4) 0.010(4) 0.012(4) C(32) 0.046(5) 0.030(4) 0.035(4) 0.010(4) 0.016(4) 0.015(4) C(33) 0.070(6) 0.028(5) 0.057(5) 0.010(4) 0.025(5) 0.016(4) C(34) 0.078(7) 0.031(5) 0.061(6) 0.015(5) 0.035(5) 0.017(4) C(35) 0.073(6) 0.035(5) 0.050(5) 0.031(5) 0.017(5) 0.022(4) C(36) 0.051(5) 0.051(6) 0.046(5) 0.021(4) 0.011(4) 0.015(4) #==================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000004(1) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6247 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1825 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_all 0.0588 _refine_ls_wR_factor_ref 0.0470 _refine_ls_goodness_of_fit_all 1.190 _refine_ls_goodness_of_fit_ref 1.420 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.80 _refine_diff_density_max 0.99 #==================================================================== # MOLECULAR GEOMETRY _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 Br(1) Zn(3) 2.465(1) . . ? Br(2) Zn(3) 2.385(2) . . ? Br(3) Zn(3) 2.390(1) . . ? Br(4) Zn(3) 2.401(2) . . ? Br(5) Zn(4) 2.407(2) . . ? Br(6) Zn(4) 2.402(2) . . ? Br(7) Zn(4) 2.447(1) . . ? Br(8) Zn(4) 2.388(2) . . ? Zn(1) N(1) 2.140(5) . . ? Zn(1) N(3) 2.173(5) . . ? Zn(1) N(7) 2.166(7) . . ? Zn(1) N(9) 2.151(7) . . ? Zn(1) N(16) 2.162(5) . . ? Zn(1) N(18) 2.144(6) . . ? Zn(2) N(4) 2.113(6) . . ? Zn(2) N(6) 2.192(7) . . ? Zn(2) N(10) 2.178(6) . . ? Zn(2) N(12) 2.193(5) . . ? Zn(2) N(13) 2.125(6) . . ? Zn(2) N(15) 2.151(5) . . ? O(1) H(1Oa) 0.92 . . no O(1) H(1Ob) 0.74 . . no O(2) H(2Ob) 0.68 . . no O(2) H(2Oa) 0.84 . . no O(3) H(3Ob) 1.04 . . no O(3) H(3Oa) 1.17 . . no O(4) H(4O) 0.78 . . no O(5) H(5Ob) 1.19 . . no O(5) H(5Oa) 0.98 . . no N(1) C(1) 1.339(9) . . ? N(1) C(5) 1.349(8) . . ? N(2) C(6) 1.342(8) . . ? N(2) H(2Na) 0.76 . . no N(2) H(2Nb) 0.91 . . no N(3) N(4) 1.416(8) . . ? N(3) C(6) 1.289(7) . . ? N(4) C(7) 1.28(1) . . ? N(5) C(7) 1.35(1) . . ? N(5) H(5Nb) 0.86 . . no N(5) H(5Na) 0.75 . . no N(6) C(8) 1.34(1) . . ? N(6) C(12) 1.32(1) . . ? N(7) C(13) 1.329(9) . . ? N(7) C(17) 1.36(1) . . ? N(8) C(18) 1.33(1) . . ? N(8) H(8Nb) 0.66 . . no N(8) H(8Na) 1.05 . . no N(9) N(10) 1.418(7) . . ? N(9) C(18) 1.27(1) . . ? N(10) C(19) 1.271(7) . . ? N(11) C(19) 1.334(9) . . ? N(11) H(11Nb 0.95 . . no N(11) H(11Na 0.95 . . no N(12) C(20) 1.350(9) . . ? N(12) C(24) 1.336(9) . . ? N(13) C(32) 1.339(9) . . ? N(13) C(36) 1.34(1) . . ? N(14) C(31) 1.32(1) . . ? N(14) H(14Na 0.70 . . no N(14) H(14Nb 0.76 . . no N(15) N(16) 1.423(8) . . ? N(15) C(31) 1.28(1) . . ? N(16) C(30) 1.30(1) . . ? N(17) C(30) 1.32(1) . . ? N(17) H(17Na 0.88 . . no N(17) H(17Nb 0.95 . . no N(18) C(25) 1.34(1) . . ? N(18) C(29) 1.35(1) . . ? C(1) C(2) 1.39(1) . . ? C(1) H(1) 0.97 . . no C(2) C(3) 1.34(1) . . ? C(2) H(2) 0.74 . . no C(3) C(4) 1.37(1) . . ? C(3) H(3) 0.95 . . no C(4) C(5) 1.381(9) . . ? C(4) H(4) 0.85 . . no C(5) C(6) 1.48(1) . . ? C(7) C(8) 1.49(1) . . ? C(8) C(9) 1.38(1) . . ? C(9) C(10) 1.36(1) . . ? C(9) H(5) 0.79 . . no C(10) C(11) 1.34(1) . . ? C(10) H(6) 0.84 . . no C(11) C(12) 1.38(1) . . ? C(11) H(7) 0.80 . . no C(12) H(8) 0.84 . . no C(13) C(14) 1.40(1) . . ? C(13) H(9) 0.69 . . no C(14) C(15) 1.38(2) . . ? C(14) H(10) 0.96 . . no C(15) C(16) 1.37(1) . . ? C(15) H(11) 0.92 . . no C(16) C(17) 1.36(1) . . ? C(16) H(12) 0.89 . . no C(17) C(18) 1.50(1) . . ? C(19) C(20) 1.49(1) . . ? C(20) C(21) 1.367(9) . . ? C(21) C(22) 1.36(1) . . ? C(21) H(13) 0.84 . . no C(22) C(23) 1.38(1) . . ? C(22) H(14) 1.02 . . no C(23) C(24) 1.39(1) . . ? C(23) H(15) 0.70 . . no C(24) H(16) 0.86 . . no C(25) C(26) 1.37(1) . . ? C(25) H(17) 1.04 . . no C(26) C(27) 1.37(1) . . ? C(26) H(18) 0.90 . . no C(27) C(28) 1.39(2) . . ? C(27) H(19) 1.08 . . no C(28) C(29) 1.38(1) . . ? C(28) H(20) 0.74 . . no C(29) C(30) 1.49(1) . . ? C(31) C(32) 1.51(1) . . ? C(32) C(33) 1.38(1) . . ? C(33) C(34) 1.39(1) . . ? C(33) H(21) 1.05 . . no C(34) C(35) 1.35(1) . . ? C(34) H(22) 1.00 . . no C(35) C(36) 1.39(1) . . ? C(35) H(23) 1.00 . . no C(36) H(24) 0.82 . . no #------------------------------------------------------------------------------ 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) Zn(1) N(3) 74.8(2) . . . ? N(1) Zn(1) N(7) 102.4(2) . . . ? N(1) Zn(1) N(9) 98.3(2) . . . ? N(1) Zn(1) N(16) 161.6(2) . . . ? N(1) Zn(1) N(18) 99.1(2) . . . ? N(3) Zn(1) N(7) 162.8(2) . . . ? N(3) Zn(1) N(9) 88.2(2) . . . ? N(3) Zn(1) N(16) 88.5(2) . . . ? N(3) Zn(1) N(18) 99.1(2) . . . ? N(7) Zn(1) N(9) 75.3(2) . . . ? N(7) Zn(1) N(16) 95.9(2) . . . ? N(7) Zn(1) N(18) 98.1(2) . . . ? N(9) Zn(1) N(16) 88.8(2) . . . ? N(9) Zn(1) N(18) 162.4(2) . . . ? N(16) Zn(1) N(18) 75.5(2) . . . ? N(4) Zn(2) N(6) 75.1(2) . . . ? N(4) Zn(2) N(10) 88.7(2) . . . ? N(4) Zn(2) N(12) 98.6(2) . . . ? N(4) Zn(2) N(13) 162.3(2) . . . ? N(4) Zn(2) N(15) 88.9(2) . . . ? N(6) Zn(2) N(10) 162.2(2) . . . ? N(6) Zn(2) N(12) 100.8(2) . . . ? N(6) Zn(2) N(13) 98.3(2) . . . ? N(6) Zn(2) N(15) 98.0(2) . . . ? N(10) Zn(2) N(12) 73.9(2) . . . ? N(10) Zn(2) N(13) 99.3(2) . . . ? N(10) Zn(2) N(15) 89.0(2) . . . ? N(12) Zn(2) N(13) 98.8(2) . . . ? N(12) Zn(2) N(15) 161.0(2) . . . ? N(13) Zn(2) N(15) 75.6(2) . . . ? Br(1) Zn(3) Br(2) 107.85(5) . . . ? Br(1) Zn(3) Br(3) 109.66(5) . . . ? Br(1) Zn(3) Br(4) 105.86(5) . . . ? Br(2) Zn(3) Br(3) 112.76(5) . . . ? Br(2) Zn(3) Br(4) 107.15(5) . . . ? Br(3) Zn(3) Br(4) 113.20(6) . . . ? Br(5) Zn(4) Br(6) 111.12(5) . . . ? Br(5) Zn(4) Br(7) 107.17(6) . . . ? Br(5) Zn(4) Br(8) 116.25(7) . . . ? Br(6) Zn(4) Br(7) 110.48(6) . . . ? Br(6) Zn(4) Br(8) 104.73(6) . . . ? Br(7) Zn(4) Br(8) 107.01(6) . . . ? H(1Oa) O(1) H(1Ob) 97.3 . . . no H(2Ob) O(2) H(2Oa) 168.5 . . . no H(3Ob) O(3) H(3Oa) 114.4 . . . no H(5Ob) O(5) H(5Oa) 158.3 . . . no Zn(1) N(1) C(1) 126.6(4) . . . ? Zn(1) N(1) C(5) 115.8(4) . . . ? C(1) N(1) C(5) 117.5(6) . . . ? C(6) N(2) H(2Na) 129.7 . . . no C(6) N(2) H(2Nb) 123.0 . . . no H(2Na) N(2) H(2Nb) 107.2 . . . no Zn(1) N(3) N(4) 120.9(4) . . . ? Zn(1) N(3) C(6) 113.9(5) . . . ? N(4) N(3) C(6) 116.2(5) . . . ? Zn(2) N(4) N(3) 122.1(5) . . . ? Zn(2) N(4) C(7) 118.1(5) . . . ? N(3) N(4) C(7) 115.9(6) . . . ? C(7) N(5) H(5Nb) 110.8 . . . no C(7) N(5) H(5Na) 110.4 . . . no H(5Nb) N(5) H(5Na) 112.0 . . . no Zn(2) N(6) C(8) 114.5(5) . . . ? Zn(2) N(6) C(12) 126.3(6) . . . ? C(8) N(6) C(12) 118.9(7) . . . ? Zn(1) N(7) C(13) 126.8(6) . . . ? Zn(1) N(7) C(17) 114.7(4) . . . ? C(13) N(7) C(17) 118.0(7) . . . ? C(18) N(8) H(8Nb) 120.6 . . . no C(18) N(8) H(8Na) 120.1 . . . no H(8Nb) N(8) H(8Na) 117.4 . . . no Zn(1) N(9) N(10) 121.6(5) . . . ? Zn(1) N(9) C(18) 115.1(5) . . . ? N(10) N(9) C(18) 115.0(6) . . . ? Zn(2) N(10) N(9) 120.2(4) . . . ? Zn(2) N(10) C(19) 116.3(5) . . . ? N(9) N(10) C(19) 116.6(5) . . . ? C(19) N(11) H(11Nb 109.1 . . . no C(19) N(11) H(11Na 126.7 . . . no H(11Nb N(11) H(11Na 123.6 . . . no Zn(2) N(12) C(20) 115.4(4) . . . ? Zn(2) N(12) C(24) 126.7(5) . . . ? C(20) N(12) C(24) 117.9(5) . . . ? Zn(2) N(13) C(32) 115.5(5) . . . ? Zn(2) N(13) C(36) 127.1(5) . . . ? C(32) N(13) C(36) 117.4(7) . . . ? C(31) N(14) H(14Na 130.8 . . . no C(31) N(14) H(14Nb 120.9 . . . no H(14Na N(14) H(14Nb 101.6 . . . no Zn(2) N(15) N(16) 121.8(4) . . . ? Zn(2) N(15) C(31) 115.6(5) . . . ? N(16) N(15) C(31) 115.8(6) . . . ? Zn(1) N(16) N(15) 120.7(4) . . . ? Zn(1) N(16) C(30) 112.7(5) . . . ? N(15) N(16) C(30) 114.0(6) . . . ? C(30) N(17) H(17Na 130.2 . . . no C(30) N(17) H(17Nb 123.5 . . . no H(17Na N(17) H(17Nb 105.7 . . . no Zn(1) N(18) C(25) 129.0(5) . . . ? Zn(1) N(18) C(29) 113.4(5) . . . ? C(25) N(18) C(29) 117.5(7) . . . ? N(1) C(1) C(2) 122.5(7) . . . ? N(1) C(1) H(1) 110.6 . . . no C(2) C(1) H(1) 126.8 . . . no C(1) C(2) C(3) 119.4(8) . . . ? C(1) C(2) H(2) 111.8 . . . no C(3) C(2) H(2) 128.4 . . . no C(2) C(3) C(4) 119.6(7) . . . ? C(2) C(3) H(3) 121.8 . . . no C(4) C(3) H(3) 118.4 . . . no C(3) C(4) C(5) 119.1(7) . . . ? C(3) C(4) H(4) 119.6 . . . no C(5) C(4) H(4) 121.2 . . . no N(1) C(5) C(4) 122.0(6) . . . ? N(1) C(5) C(6) 114.0(5) . . . ? C(4) C(5) C(6) 123.8(6) . . . ? N(2) C(6) N(3) 124.9(6) . . . ? N(2) C(6) C(5) 119.1(5) . . . ? N(3) C(6) C(5) 115.9(5) . . . ? N(4) C(7) N(5) 125.2(7) . . . ? N(4) C(7) C(8) 116.6(7) . . . ? N(5) C(7) C(8) 118.1(8) . . . ? N(6) C(8) C(7) 114.5(7) . . . ? N(6) C(8) C(9) 120.8(7) . . . ? C(7) C(8) C(9) 124.5(8) . . . ? C(8) C(9) C(10) 119.5(8) . . . ? C(8) C(9) H(5) 108.5 . . . no C(10) C(9) H(5) 129.6 . . . no C(9) C(10) C(11) 119.6(9) . . . ? C(9) C(10) H(6) 119.2 . . . no C(11) C(10) H(6) 121.3 . . . no C(10) C(11) C(12) 119.2(8) . . . ? C(10) C(11) H(7) 127.4 . . . no C(12) C(11) H(7) 113.4 . . . no N(6) C(12) C(11) 122.1(8) . . . ? N(6) C(12) H(8) 116.8 . . . no C(11) C(12) H(8) 120.2 . . . no N(7) C(13) C(14) 123.1(9) . . . ? N(7) C(13) H(9) 121.3 . . . no C(14) C(13) H(9) 114.1 . . . no C(13) C(14) C(15) 117.3(7) . . . ? C(13) C(14) H(10) 115.4 . . . no C(15) C(14) H(10) 127.1 . . . no C(14) C(15) C(16) 120.1(9) . . . ? C(14) C(15) H(11) 117.3 . . . no C(16) C(15) H(11) 122.5 . . . no C(15) C(16) C(17) 119(1) . . . ? C(15) C(16) H(12) 120.1 . . . no C(17) C(16) H(12) 120.9 . . . no N(7) C(17) C(16) 122.3(7) . . . ? N(7) C(17) C(18) 113.4(7) . . . ? C(16) C(17) C(18) 124.2(8) . . . ? N(8) C(18) N(9) 124.9(7) . . . ? N(8) C(18) C(17) 117.5(7) . . . ? N(9) C(18) C(17) 117.5(8) . . . ? N(10) C(19) N(11) 125.9(6) . . . ? N(10) C(19) C(20) 116.2(6) . . . ? N(11) C(19) C(20) 117.8(5) . . . ? N(12) C(20) C(19) 114.3(5) . . . ? N(12) C(20) C(21) 121.8(6) . . . ? C(19) C(20) C(21) 123.9(7) . . . ? C(20) C(21) C(22) 120.5(7) . . . ? C(20) C(21) H(13) 125.4 . . . no C(22) C(21) H(13) 113.3 . . . no C(21) C(22) C(23) 118.2(7) . . . ? C(21) C(22) H(14) 127.4 . . . no C(23) C(22) H(14) 113.5 . . . no C(22) C(23) C(24) 119.0(7) . . . ? C(22) C(23) H(15) 116.5 . . . no C(24) C(23) H(15) 124.4 . . . no N(12) C(24) C(23) 122.4(7) . . . ? N(12) C(24) H(16) 115.3 . . . no C(23) C(24) H(16) 122.3 . . . no N(18) C(25) C(26) 123.6(7) . . . ? N(18) C(25) H(17) 105.4 . . . no C(26) C(25) H(17) 130.4 . . . no C(25) C(26) C(27) 118.7(9) . . . ? C(25) C(26) H(18) 111.3 . . . no C(27) C(26) H(18) 129.4 . . . no C(26) C(27) C(28) 119(1) . . . ? C(26) C(27) H(19) 118.9 . . . no C(28) C(27) H(19) 117.5 . . . no C(27) C(28) C(29) 118.5(8) . . . ? C(27) C(28) H(20) 113.9 . . . no C(29) C(28) H(20) 125.0 . . . no N(18) C(29) C(28) 122.3(8) . . . ? N(18) C(29) C(30) 115.6(7) . . . ? C(28) C(29) C(30) 122.0(7) . . . ? N(16) C(30) N(17) 125.3(8) . . . ? N(16) C(30) C(29) 114.1(7) . . . ? N(17) C(30) C(29) 120.6(8) . . . ? N(14) C(31) N(15) 125.0(8) . . . ? N(14) C(31) C(32) 120.2(8) . . . ? N(15) C(31) C(32) 114.8(6) . . . ? N(13) C(32) C(31) 114.9(7) . . . ? N(13) C(32) C(33) 122.8(7) . . . ? C(31) C(32) C(33) 122.2(6) . . . ? C(32) C(33) C(34) 118.6(7) . . . ? C(32) C(33) H(21) 125.2 . . . no C(34) C(33) H(21) 113.5 . . . no C(33) C(34) C(35) 119.2(8) . . . ? C(33) C(34) H(22) 123.0 . . . no C(35) C(34) H(22) 117.1 . . . no C(34) C(35) C(36) 119.3(8) . . . ? C(34) C(35) H(23) 127.4 . . . no C(36) C(35) H(23) 112.9 . . . no N(13) C(36) C(35) 122.7(7) . . . ? N(13) C(36) H(24) 113.2 . . . no C(35) C(36) H(24) 123.6 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) N(11) 3.472(6) . 1_554 no Br(1) O(1) 3.480(7) . 2_665 no Br(1) N(5) 3.560(9) . . no Br(2) N(5) 3.443(8) . . no Br(2) C(5) 3.443(8) . . no Br(3) N(11) 3.462(7) . 1_554 no Br(4) O(4) 3.50(2) . 2_666 no Br(4) O(2) 3.518(8) . 2_665 no Br(5) N(8) 3.391(7) . . no Br(6) N(17) 3.457(8) . 1_556 no Br(7) N(8) 3.380(9) . . no Br(7) O(5) 3.39(3) . 2_656 no Br(8) C(23) 3.543(9) . 2_656 no Br(8) C(34) 3.58(1) . . no Br(8) O(4) 3.59(2) . 2_656 no O(1) N(2) 2.903(7) . 2_666 no O(1) O(2) 2.923(9) . . no O(1) C(8) 3.228(7) . . no O(1) C(7) 3.270(8) . . no O(1) N(2) 3.382(9) . . no O(1) C(24) 3.49(1) . . no O(1) N(4) 3.545(8) . . no O(1) C(4) 3.547(9) . 2_666 no O(2) C(4) 3.370(8) . 2_666 no O(2) C(12) 3.372(9) . . no O(2) C(11) 3.424(9) . . no O(2) C(3) 3.466(9) . 2_666 no O(2) C(24) 3.48(1) . . no O(3) O(5) 2.09(4) . . no O(3) O(4) 2.81(2) . . no O(3) N(14) 3.04(2) . 2_656 no O(3) N(14) 3.34(1) . 1_656 no O(3) C(30) 3.59(1) . 1_656 no O(4) O(5) 1.86(4) . . no O(4) C(27) 3.35(2) . 1_656 no O(4) C(33) 3.45(2) . 2_656 no O(4) C(26) 3.48(2) . 1_656 no O(4) C(28) 3.59(2) . 1_656 no O(5) C(33) 3.56(4) . 2_656 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Zn(1) N(1) C(1) C(2) . . . . -175.4(7) no Zn(1) N(1) C(5) C(4) . . . . 175.9(6) no Zn(1) N(1) C(5) C(6) . . . . 0.9(9) no Zn(1) N(3) N(4) Zn(2) . . . . -41.9(6) no Zn(1) N(3) N(4) C(7) . . . . 115.3(5) no Zn(1) N(3) C(6) N(2) . . . . 156.0(7) no Zn(1) N(3) C(6) C(5) . . . . -26.5(9) no Zn(1) N(7) C(13) C(14) . . . . 170.4(6) no Zn(1) N(7) C(17) C(16) . . . . -173.7(6) no Zn(1) N(7) C(17) C(18) . . . . 5.9(7) no Zn(1) N(9) N(10) Zn(2) . . . . -42.4(6) no Zn(1) N(9) N(10) C(19) . . . . 107.5(7) no Zn(1) N(9) C(18) N(8) . . . . 155.8(6) no Zn(1) N(9) C(18) C(17) . . . . -21.0(8) no Zn(1) N(16) N(15) Zn(2) . . . . -40.9(7) no Zn(1) N(16) N(15) C(31) . . . . 108.8(6) no Zn(1) N(16) C(30) N(17) . . . . 147.4(6) no Zn(1) N(16) C(30) C(29) . . . . -31.7(7) no Zn(1) N(18) C(25) C(26) . . . . 178.1(7) no Zn(1) N(18) C(29) C(28) . . . . -178.1(7) no Zn(1) N(18) C(29) C(30) . . . . 5.2(8) no Zn(2) N(4) N(3) C(6) . . . . 103.4(7) no Zn(2) N(4) C(7) N(5) . . . . 168.4(5) no Zn(2) N(4) C(7) C(8) . . . . -12.2(7) no Zn(2) N(6) C(8) C(7) . . . . 1.3(6) no Zn(2) N(6) C(8) C(9) . . . . -174.4(5) no Zn(2) N(6) C(12) C(11) . . . . 172.5(5) no Zn(2) N(10) N(9) C(18) . . . . 104.5(6) no Zn(2) N(10) C(19) N(11) . . . . 158.3(7) no Zn(2) N(10) C(19) C(20) . . . . -22.7(9) no Zn(2) N(12) C(20) C(19) . . . . 0.4(9) no Zn(2) N(12) C(20) C(21) . . . . 179.6(7) no Zn(2) N(12) C(24) C(23) . . . . -179.8(7) no Zn(2) N(13) C(32) C(31) . . . . 2.1(9) no Zn(2) N(13) C(32) C(33) . . . . 178.0(7) no Zn(2) N(13) C(36) C(35) . . . . -179.3(6) no Zn(2) N(15) N(16) C(30) . . . . 98.1(6) no Zn(2) N(15) C(31) N(14) . . . . 158.3(7) no Zn(2) N(15) C(31) C(32) . . . . -21.3(8) no N(1) Zn(1) N(3) N(4) . . . . 166.2(5) no N(1) Zn(1) N(3) C(6) . . . . 20.3(5) no N(1) Zn(1) N(7) C(13) . . . . 80.9(6) no N(1) Zn(1) N(7) C(17) . . . . -107.6(5) no N(1) Zn(1) N(9) N(10) . . . . -94.4(4) no N(1) Zn(1) N(9) C(18) . . . . 118.8(5) no N(1) Zn(1) N(16) N(15) . . . . 91.0(9) no N(1) Zn(1) N(16) C(30) . . . . -48.4(9) no N(1) Zn(1) N(18) C(25) . . . . -29.5(7) no N(1) Zn(1) N(18) C(29) . . . . 146.0(5) no N(1) C(1) C(2) C(3) . . . . -0(1) no N(1) C(5) C(4) C(3) . . . . 0(1) no N(1) C(5) C(6) N(2) . . . . -165.0(7) no N(1) C(5) C(6) N(3) . . . . 17(1) no N(2) C(6) N(3) N(4) . . . . 8(1) no N(2) C(6) C(5) C(4) . . . . 20(1) no N(3) Zn(1) N(1) C(1) . . . . 165.5(7) no N(3) Zn(1) N(1) C(5) . . . . -10.5(5) no N(3) Zn(1) N(7) C(13) . . . . 159.5(7) no N(3) Zn(1) N(7) C(17) . . . . -29(1) no N(3) Zn(1) N(9) N(10) . . . . -20.0(4) no N(3) Zn(1) N(9) C(18) . . . . -166.8(5) no N(3) Zn(1) N(16) N(15) . . . . 66.1(5) no N(3) Zn(1) N(16) C(30) . . . . -73.4(5) no N(3) Zn(1) N(18) C(25) . . . . -105.4(7) no N(3) Zn(1) N(18) C(29) . . . . 70.1(5) no N(3) N(4) Zn(2) N(6) . . . . 166.4(4) no N(3) N(4) Zn(2) N(10) . . . . -21.2(4) no N(3) N(4) Zn(2) N(12) . . . . -94.7(4) no N(3) N(4) Zn(2) N(13) . . . . 96.2(9) no N(3) N(4) Zn(2) N(15) . . . . 67.8(4) no N(3) N(4) C(7) N(5) . . . . 10.3(9) no N(3) N(4) C(7) C(8) . . . . -170.3(5) no N(3) C(6) C(5) C(4) . . . . -157.5(8) no N(4) Zn(2) N(6) C(8) . . . . -5.4(4) no N(4) Zn(2) N(6) C(12) . . . . -178.4(5) no N(4) Zn(2) N(10) N(9) . . . . 67.9(5) no N(4) Zn(2) N(10) C(19) . . . . -82.1(6) no N(4) Zn(2) N(12) C(20) . . . . 77.7(6) no N(4) Zn(2) N(12) C(24) . . . . -102.5(7) no N(4) Zn(2) N(13) C(32) . . . . -39(1) no N(4) Zn(2) N(13) C(36) . . . . 141.7(8) no N(4) Zn(2) N(15) N(16) . . . . -21.7(5) no N(4) Zn(2) N(15) C(31) . . . . -171.4(6) no N(4) N(3) Zn(1) N(7) . . . . 83.4(8) no N(4) N(3) Zn(1) N(9) . . . . 67.2(5) no N(4) N(3) Zn(1) N(16) . . . . -21.7(5) no N(4) N(3) Zn(1) N(18) . . . . -96.7(5) no N(4) N(3) C(6) C(5) . . . . -174.1(7) no N(4) C(7) C(8) N(6) . . . . 6.9(8) no N(4) C(7) C(8) C(9) . . . . -177.5(6) no N(5) C(7) C(8) N(6) . . . . -173.6(6) no N(5) C(7) C(8) C(9) . . . . 2.0(9) no N(6) Zn(2) N(4) C(7) . . . . 9.7(4) no N(6) Zn(2) N(10) N(9) . . . . 92.5(7) no N(6) Zn(2) N(10) C(19) . . . . -58(1) no N(6) Zn(2) N(12) C(20) . . . . 154.0(6) no N(6) Zn(2) N(12) C(24) . . . . -26.1(7) no N(6) Zn(2) N(13) C(32) . . . . -105.7(6) no N(6) Zn(2) N(13) C(36) . . . . 74.9(7) no N(6) Zn(2) N(15) N(16) . . . . -96.4(5) no N(6) Zn(2) N(15) C(31) . . . . 113.8(6) no N(6) C(8) C(9) C(10) . . . . 2(1) no N(6) C(12) C(11) C(10) . . . . 0(1) no N(7) Zn(1) N(1) C(1) . . . . -32.0(7) no N(7) Zn(1) N(1) C(5) . . . . 152.0(6) no N(7) Zn(1) N(3) C(6) . . . . -63(1) no N(7) Zn(1) N(9) N(10) . . . . 164.9(5) no N(7) Zn(1) N(9) C(18) . . . . 18.1(5) no N(7) Zn(1) N(16) N(15) . . . . -97.2(5) no N(7) Zn(1) N(16) C(30) . . . . 123.3(5) no N(7) Zn(1) N(18) C(25) . . . . 74.5(7) no N(7) Zn(1) N(18) C(29) . . . . -110.0(5) no N(7) C(13) C(14) C(15) . . . . 1(1) no N(7) C(17) C(16) C(15) . . . . 3(1) no N(7) C(17) C(18) N(8) . . . . -167.1(7) no N(7) C(17) C(18) N(9) . . . . 10.1(9) no N(8) C(18) N(9) N(10) . . . . 7(1) no N(8) C(18) C(17) C(16) . . . . 13(1) no N(9) Zn(1) N(1) C(1) . . . . -108.6(7) no N(9) Zn(1) N(1) C(5) . . . . 75.3(6) no N(9) Zn(1) N(3) C(6) . . . . -78.8(6) no N(9) Zn(1) N(7) C(13) . . . . 176.3(6) no N(9) Zn(1) N(7) C(17) . . . . -12.2(4) no N(9) Zn(1) N(16) N(15) . . . . -22.2(5) no N(9) Zn(1) N(16) C(30) . . . . -161.6(5) no N(9) Zn(1) N(18) C(25) . . . . 141.0(8) no N(9) Zn(1) N(18) C(29) . . . . -43(1) no N(9) N(10) Zn(2) N(12) . . . . 167.2(6) no N(9) N(10) Zn(2) N(13) . . . . -96.2(5) no N(9) N(10) Zn(2) N(15) . . . . -21.0(5) no N(9) N(10) C(19) N(11) . . . . 7(1) no N(9) N(10) C(19) C(20) . . . . -173.8(7) no N(9) C(18) C(17) C(16) . . . . -170.3(7) no N(10) Zn(2) N(4) C(7) . . . . -177.9(5) no N(10) Zn(2) N(6) C(8) . . . . -30.9(9) no N(10) Zn(2) N(6) C(12) . . . . 156.1(6) no N(10) Zn(2) N(12) C(20) . . . . -8.5(5) no N(10) Zn(2) N(12) C(24) . . . . 171.4(8) no N(10) Zn(2) N(13) C(32) . . . . 77.0(6) no N(10) Zn(2) N(13) C(36) . . . . -102.4(7) no N(10) Zn(2) N(15) N(16) . . . . 67.1(5) no N(10) Zn(2) N(15) C(31) . . . . -82.7(6) no N(10) N(9) Zn(1) N(16) . . . . 68.5(4) no N(10) N(9) Zn(1) N(18) . . . . 95.1(8) no N(10) N(9) C(18) C(17) . . . . -170.1(6) no N(10) C(19) C(20) N(12) . . . . 15(1) no N(10) C(19) C(20) C(21) . . . . -164.4(8) no N(11) C(19) C(20) N(12) . . . . -166.2(8) no N(11) C(19) C(20) C(21) . . . . 15(1) no N(12) Zn(2) N(4) C(7) . . . . 108.6(5) no N(12) Zn(2) N(6) C(8) . . . . -101.6(4) no N(12) Zn(2) N(6) C(12) . . . . 85.4(5) no N(12) Zn(2) N(10) C(19) . . . . 17.2(6) no N(12) Zn(2) N(13) C(32) . . . . 152.0(5) no N(12) Zn(2) N(13) C(36) . . . . -27.4(7) no N(12) Zn(2) N(15) N(16) . . . . 92.1(9) no N(12) Zn(2) N(15) C(31) . . . . -57.6(9) no N(12) C(20) C(21) C(22) . . . . 2(1) no N(12) C(24) C(23) C(22) . . . . -2(2) no N(13) Zn(2) N(4) C(7) . . . . -60(1) no N(13) Zn(2) N(6) C(8) . . . . 157.7(4) no N(13) Zn(2) N(6) C(12) . . . . -15.3(5) no N(13) Zn(2) N(10) C(19) . . . . 113.8(6) no N(13) Zn(2) N(12) C(20) . . . . -105.7(6) no N(13) Zn(2) N(12) C(24) . . . . 74.2(7) no N(13) Zn(2) N(15) N(16) . . . . 167.0(6) no N(13) Zn(2) N(15) C(31) . . . . 17.2(5) no N(13) C(32) C(31) N(14) . . . . -166.8(7) no N(13) C(32) C(31) N(15) . . . . 13(1) no N(13) C(32) C(33) C(34) . . . . 3(1) no N(13) C(36) C(35) C(34) . . . . -1(1) no N(14) C(31) N(15) N(16) . . . . 7(1) no N(14) C(31) C(32) C(33) . . . . 17(1) no N(15) Zn(2) N(4) C(7) . . . . -88.9(5) no N(15) Zn(2) N(6) C(8) . . . . 81.2(4) no N(15) Zn(2) N(6) C(12) . . . . -91.8(5) no N(15) Zn(2) N(10) C(19) . . . . -171.0(6) no N(15) Zn(2) N(12) C(20) . . . . -35(1) no N(15) Zn(2) N(12) C(24) . . . . 145.3(8) no N(15) Zn(2) N(13) C(32) . . . . -9.5(5) no N(15) Zn(2) N(13) C(36) . . . . 171.1(7) no N(15) N(16) Zn(1) N(18) . . . . 165.9(6) no N(15) N(16) C(30) N(17) . . . . 5(1) no N(15) N(16) C(30) C(29) . . . . -174.0(5) no N(15) C(31) C(32) C(33) . . . . -163.1(8) no N(16) Zn(1) N(1) C(1) . . . . 139.6(8) no N(16) Zn(1) N(1) C(5) . . . . -36(1) no N(16) Zn(1) N(3) C(6) . . . . -167.7(6) no N(16) Zn(1) N(7) C(13) . . . . -96.5(6) no N(16) Zn(1) N(7) C(17) . . . . 75.0(5) no N(16) Zn(1) N(9) C(18) . . . . -78.3(5) no N(16) Zn(1) N(18) C(25) . . . . 168.5(7) no N(16) Zn(1) N(18) C(29) . . . . -16.0(5) no N(16) N(15) C(31) C(32) . . . . -172.8(6) no N(16) C(30) C(29) N(18) . . . . 18(1) no N(16) C(30) C(29) C(28) . . . . -158.6(8) no N(17) C(30) C(29) N(18) . . . . -161.0(7) no N(17) C(30) C(29) C(28) . . . . 22(1) no N(18) Zn(1) N(1) C(1) . . . . 68.5(7) no N(18) Zn(1) N(1) C(5) . . . . -107.6(6) no N(18) Zn(1) N(3) C(6) . . . . 117.3(6) no N(18) Zn(1) N(7) C(13) . . . . -20.3(6) no N(18) Zn(1) N(7) C(17) . . . . 151.1(5) no N(18) Zn(1) N(9) C(18) . . . . -52(1) no N(18) Zn(1) N(16) C(30) . . . . 26.4(5) no N(18) C(25) C(26) C(27) . . . . -4(1) no N(18) C(29) C(28) C(27) . . . . 3(2) no C(1) N(1) C(5) C(4) . . . . -1(1) no C(1) N(1) C(5) C(6) . . . . -175.5(7) no C(1) C(2) C(3) C(4) . . . . -0(1) no C(2) C(1) N(1) C(5) . . . . 1(1) no C(2) C(3) C(4) C(5) . . . . 0(1) no C(3) C(4) C(5) C(6) . . . . 174.7(8) no C(6) N(3) N(4) C(7) . . . . -99.5(8) no C(7) C(8) N(6) C(12) . . . . 174.9(5) no C(7) C(8) C(9) C(10) . . . . -173.7(6) no C(8) N(6) C(12) C(11) . . . . -0.2(9) no C(8) C(9) C(10) C(11) . . . . -1(1) no C(9) C(8) N(6) C(12) . . . . -0.8(9) no C(9) C(10) C(11) C(12) . . . . 0(1) no C(13) N(7) C(17) C(16) . . . . -1(1) no C(13) N(7) C(17) C(18) . . . . 178.2(6) no C(13) C(14) C(15) C(16) . . . . 1(1) no C(14) C(13) N(7) C(17) . . . . -1(1) no C(14) C(15) C(16) C(17) . . . . -3(1) no C(15) C(16) C(17) C(18) . . . . -176.3(7) no C(18) N(9) N(10) C(19) . . . . -105.6(8) no C(19) C(20) N(12) C(24) . . . . -179.5(7) no C(19) C(20) C(21) C(22) . . . . -178.7(9) no C(20) N(12) C(24) C(23) . . . . 0(1) no C(20) C(21) C(22) C(23) . . . . -4(2) no C(21) C(20) N(12) C(24) . . . . -0(1) no C(21) C(22) C(23) C(24) . . . . 3(2) no C(25) N(18) C(29) C(28) . . . . -2(1) no C(25) N(18) C(29) C(30) . . . . -178.8(7) no C(25) C(26) C(27) C(28) . . . . 4(2) no C(26) C(25) N(18) C(29) . . . . 3(1) no C(26) C(27) C(28) C(29) . . . . -4(2) no C(27) C(28) C(29) C(30) . . . . 179.0(9) no C(30) N(16) N(15) C(31) . . . . -112.3(7) no C(31) C(32) N(13) C(36) . . . . -178.5(7) no C(31) C(32) C(33) C(34) . . . . 178.8(8) no C(32) N(13) C(36) C(35) . . . . 1(1) no C(32) C(33) C(34) C(35) . . . . -2(1) no C(33) C(32) N(13) C(36) . . . . -3(1) no C(33) C(34) C(35) C(36) . . . . 1(1) no #------------------------------------------------------------------------------ #===END #==================================================================== data__x551(7) _database_code_CSD 158604 #==================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 23.870(3) _cell_length_b 13.418(8) _cell_length_c 14.721(5) _cell_angle_alpha 90 _cell_angle_beta 119.90(1) _cell_angle_gamma 90 _cell_volume 4087(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 22.7 _cell_measurement_theta_max 24.6 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, -y, -z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2-y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'hexagonal rod' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1081.50 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H40 Cd2 N16 O19 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2176.00 _exptl_absorpt_coefficient_mu 1.136 _exptl_absorpt_correction_type none _exptl_special_details ; The scan width was (1.57+0.35tan\q)\% with an \w scan speed of 8\% per minute (up to 11 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #==================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 299.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.84 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 -2 -3 1 -2 2 0 -4 _diffrn_reflns_number 5040 _reflns_number_total 4924 _reflns_number_gt 3968 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.09712 _diffrn_reflns_av_sigmaI/netI 0.042 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00367 _diffrn_orient_matrix_UB_12 -0.00709 _diffrn_orient_matrix_UB_13 -0.07039 _diffrn_orient_matrix_UB_21 -0.04783 _diffrn_orient_matrix_UB_22 0.00957 _diffrn_orient_matrix_UB_23 -0.03434 _diffrn_orient_matrix_UB_31 0.00587 _diffrn_orient_matrix_UB_32 0.07357 _diffrn_orient_matrix_UB_33 -0.00231 #------------------------------------------------------------------------------ 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 C 0 96 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 160 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 64 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 76 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cd 0 8 -1.005 1.202 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #==================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cd(1) 0.388728(8) 0.05519(1) 0.70398(1) 0.03574(5) 1.000 . Uani d ? O(1) 0.31061(8) 0.0994(1) 0.5313(1) 0.0491(5) 1.000 . Uani d ? O(2) 0.29580(9) 0.0410(2) 0.7259(1) 0.0657(7) 1.000 . Uani d ? O(3) 0.37193(9) -0.0058(2) 0.8754(2) 0.0794(8) 1.000 . Uani d ? O(4) 0.28102(9) 0.0390(2) 0.8589(1) 0.0647(7) 1.000 . Uani d ? O(5) 0.31446(9) 0.3539(2) 0.5038(2) 0.0626(7) 1.000 . Uani d ? O(6) 0.4067(1) 0.4290(2) 0.5809(2) 0.0803(8) 1.000 . Uani d ? O(7) 0.3256(1) 0.4912(2) 0.5860(2) 0.090(1) 1.000 . Uani d ? O(8) 0.5000 0.5594(2) 0.7500 0.069(1) 1.000 S Uani d ? O(9) 0.1725(1) 0.1613(2) 0.6805(2) 0.108(1) 1.000 . Uani d ? O(10) 0.45344(9) -0.3129(2) 0.8581(2) 0.0681(7) 1.000 . Uani d ? N(1) 0.39189(9) 0.2151(2) 0.7649(2) 0.0391(6) 1.000 . Uani d ? N(2) 0.56465(9) 0.2161(2) 0.9280(2) 0.0475(6) 1.000 . Uani d ? N(3) 0.49156(8) 0.0886(1) 0.8499(1) 0.0312(5) 1.000 . Uani d ? N(4) 0.54546(8) 0.0251(1) 0.8717(1) 0.0299(5) 1.000 . Uani d ? N(5) 0.49115(9) -0.1052(2) 0.8997(2) 0.0434(6) 1.000 . Uani d ? N(6) 0.62333(9) -0.1092(1) 0.8503(1) 0.0361(5) 1.000 . Uani d ? N(7) 0.3165(1) 0.0239(2) 0.8214(2) 0.0454(7) 1.000 . Uani d ? N(8) 0.3484(1) 0.4265(2) 0.5560(2) 0.0567(8) 1.000 . Uani d ? C(1) 0.3400(1) 0.2732(2) 0.7343(2) 0.0517(8) 1.000 . Uani d ? C(2) 0.3432(1) 0.3662(2) 0.7763(2) 0.0581(9) 1.000 . Uani d ? C(3) 0.4021(2) 0.4002(2) 0.8519(3) 0.059(1) 1.000 . Uani d ? C(4) 0.4564(1) 0.3419(2) 0.8855(2) 0.0468(8) 1.000 . Uani d ? C(5) 0.4497(1) 0.2488(2) 0.8409(2) 0.0342(6) 1.000 . Uani d ? C(6) 0.5050(1) 0.1794(2) 0.8741(2) 0.0323(6) 1.000 . Uani d ? C(7) 0.5387(1) -0.0674(2) 0.8878(2) 0.0331(6) 1.000 . Uani d ? C(8) 0.5888(1) -0.1376(2) 0.8949(2) 0.0329(6) 1.000 . Uani d ? C(9) 0.5993(1) -0.2269(2) 0.9453(2) 0.0492(8) 1.000 . Uani d ? C(10) 0.6441(1) -0.2922(2) 0.9452(2) 0.0560(9) 1.000 . Uani d ? C(11) 0.6781(1) -0.2648(2) 0.8974(2) 0.0526(9) 1.000 . Uani d ? C(12) 0.6674(1) -0.1714(2) 0.8523(2) 0.0475(8) 1.000 . Uani d ? H(1) 0.2984 0.2363 0.6804 0.057 1.000 . Uiso c ? H(2) 0.3042 0.4008 0.7538 0.064 1.000 . Uiso c ? H(3) 0.4045 0.4406 0.8733 0.063 1.000 . Uiso c ? H(4) 0.4953 0.3613 0.9339 0.053 1.000 . Uiso c ? H(5) 0.5691 0.2791 0.9297 0.057 1.000 . Uiso c ? H(6) 0.5936 0.1801 0.9439 0.057 1.000 . Uiso c ? H(7) 0.4639 -0.0737 0.8913 0.052 1.000 . Uiso c ? H(8) 0.4850 -0.1598 0.8945 0.052 1.000 . Uiso c ? H(9) 0.5727 -0.2453 0.9632 0.056 1.000 . Uiso c ? H(10) 0.6537 -0.3418 0.9793 0.064 1.000 . Uiso c ? H(11) 0.7123 -0.3041 0.9002 0.060 1.000 . Uiso c ? H(12) 0.6922 -0.1477 0.8233 0.054 1.000 . Uiso c ? H(13) 0.2990 0.0659 0.4873 0.059 1.000 . Uiso c ? H(14) 0.2725 0.1387 0.5192 0.059 1.000 . Uiso c ? H(15) 0.5215 0.6159 0.7063 0.083 1.000 . Uiso c ? H(16) 0.4693 0.4965 0.6971 0.083 1.000 . Uiso c ? H(17) 0.1822 0.1871 0.6435 0.132 1.000 . Uiso c ? H(18) 0.2065 0.1479 0.7282 0.132 1.000 . Uiso c ? H(19) 0.4141 -0.3121 0.8448 0.084 1.000 . Uiso c ? H(20) 0.4606 -0.2933 0.8379 0.084 1.000 . Uiso c ? 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 Cd(1) 0.02494(9) 0.0465(1) 0.0358(1) -0.00213(8) 0.01513(8) -0.00561(8) O(1) 0.0303(9) 0.071(1) 0.038(1) 0.0069(9) 0.0105(8) -0.0018(9) O(2) 0.047(1) 0.115(2) 0.041(1) -0.003(1) 0.027(1) 0.005(1) O(3) 0.041(1) 0.128(2) 0.066(1) 0.023(1) 0.024(1) 0.014(1) O(4) 0.046(1) 0.109(2) 0.057(1) 0.007(1) 0.039(1) 0.009(1) O(5) 0.047(1) 0.069(1) 0.068(1) -0.002(1) 0.026(1) -0.005(1) O(6) 0.051(1) 0.068(2) 0.125(2) -0.007(1) 0.047(1) -0.020(1) O(7) 0.101(2) 0.054(1) 0.150(2) 0.009(1) 0.090(2) -0.004(2) O(8) 0.069(2) 0.060(2) 0.078(2) 0.0000 0.036(2) 0.0000 O(9) 0.073(2) 0.175(3) 0.081(2) 0.053(2) 0.043(1) 0.019(2) O(10) 0.052(1) 0.069(1) 0.077(1) -0.009(1) 0.027(1) -0.006(1) N(1) 0.031(1) 0.045(1) 0.041(1) 0.0066(9) 0.0182(9) 0.002(1) N(2) 0.033(1) 0.039(1) 0.062(1) -0.003(1) 0.017(1) -0.009(1) N(3) 0.0237(9) 0.041(1) 0.029(1) 0.0032(8) 0.0130(8) -0.0007(8) N(4) 0.0230(9) 0.035(1) 0.030(1) 0.0043(8) 0.0125(8) 0.0031(8) N(5) 0.040(1) 0.041(1) 0.055(1) 0.001(1) 0.028(1) 0.006(1) N(6) 0.031(1) 0.039(1) 0.037(1) 0.0053(9) 0.0164(9) 0.0025(9) N(7) 0.033(1) 0.059(1) 0.048(1) -0.005(1) 0.023(1) -0.003(1) N(8) 0.054(2) 0.046(2) 0.081(2) 0.010(1) 0.042(1) 0.013(1) C(1) 0.037(1) 0.058(2) 0.055(2) 0.011(1) 0.020(1) 0.004(1) C(2) 0.048(2) 0.057(2) 0.069(2) 0.020(1) 0.029(2) 0.009(2) C(3) 0.075(2) 0.038(2) 0.076(2) 0.009(2) 0.046(2) -0.002(1) C(4) 0.045(2) 0.044(2) 0.053(2) 0.000(1) 0.025(1) -0.002(1) C(5) 0.034(1) 0.039(1) 0.035(1) 0.002(1) 0.021(1) 0.002(1) C(6) 0.029(1) 0.038(1) 0.030(1) -0.001(1) 0.015(1) -0.001(1) C(7) 0.027(1) 0.044(1) 0.026(1) 0.001(1) 0.0120(9) 0.001(1) C(8) 0.028(1) 0.033(1) 0.033(1) 0.003(1) 0.012(1) 0.001(1) C(9) 0.046(2) 0.052(2) 0.052(2) 0.006(1) 0.026(1) 0.011(1) C(10) 0.058(2) 0.039(2) 0.063(2) 0.016(1) 0.024(2) 0.011(1) C(11) 0.044(2) 0.054(2) 0.055(2) 0.016(1) 0.021(1) 0.001(1) C(12) 0.038(1) 0.055(2) 0.051(2) 0.010(1) 0.024(1) 0.001(1) #==================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000188(5) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3968 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_all 0.0400 _refine_ls_wR_factor_ref 0.0400 _refine_ls_goodness_of_fit_all 2.873 _refine_ls_goodness_of_fit_ref 3.110 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.63 _refine_diff_density_max 0.46 #==================================================================== #========= # MOLECULAR GEOMETRY _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 Cd(1) O(1) 2.359(3) . . ? Cd(1) O(2) 2.403(3) . . ? Cd(1) N(1) 2.313(4) . . ? Cd(1) N(3) 2.363(3) . . ? Cd(1) N(4) 2.369(3) . . ? Cd(1) N(6) 2.314(4) . . ? O(1) H(13) 0.72 . . no O(1) H(14) 0.99 . . no O(2) N(7) 1.258(5) . . ? O(3) N(7) 1.222(4) . . ? O(4) N(7) 1.236(4) . . ? O(5) N(8) 1.255(5) . . ? O(6) N(8) 1.251(5) . . ? O(7) N(8) 1.220(5) . . ? O(8) H(15) 1.26 . . no O(8) H(15) 1.26 . . no O(8) H(16) 1.13 . . no O(8) H(16) 1.13 . . no O(9) H(17) 0.77 . . no O(9) H(18) 0.78 . . no O(10) H(19) 0.86 . . no O(10) H(20) 0.49 . . no N(1) C(1) 1.337(5) . . ? N(1) C(5) 1.349(5) . . ? N(2) C(6) 1.331(5) . . ? N(2) H(5) 0.85 . . no N(2) H(6) 0.78 . . no N(3) N(4) 1.440(4) . . ? N(3) C(6) 1.265(5) . . ? N(4) C(7) 1.289(5) . . ? N(5) C(7) 1.331(5) . . ? N(5) H(7) 0.73 . . no N(5) H(8) 0.74 . . no N(6) C(8) 1.341(5) . . ? N(6) C(12) 1.330(5) . . ? C(1) C(2) 1.378(7) . . ? C(1) H(1) 1.04 . . no C(2) C(3) 1.364(7) . . ? C(2) H(2) 0.94 . . no C(3) C(4) 1.378(6) . . ? C(3) H(3) 0.62 . . no C(4) C(5) 1.383(6) . . ? C(4) H(4) 0.88 . . no C(5) C(6) 1.486(5) . . ? C(7) C(8) 1.485(5) . . ? C(8) C(9) 1.365(6) . . ? C(9) C(10) 1.383(6) . . ? C(9) H(9) 0.84 . . no C(10) C(11) 1.365(7) . . ? C(10) H(10) 0.80 . . no C(11) C(12) 1.381(7) . . ? C(11) H(11) 0.95 . . no C(12) H(12) 0.94 . . no #------------------------------------------------------------------------------ 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) Cd(1) O(2) 83.0(1) . . . ? O(1) Cd(1) N(1) 92.3(1) . . . ? O(1) Cd(1) N(3) 146.8(1) . . . ? O(1) Cd(1) N(4) 83.7(1) . . . ? O(1) Cd(1) N(6) 88.4(1) . . . ? O(2) Cd(1) N(1) 82.8(1) . . . ? O(2) Cd(1) N(3) 120.2(1) . . . ? O(2) Cd(1) N(4) 157.2(1) . . . ? O(2) Cd(1) N(6) 90.4(1) . . . ? N(1) Cd(1) N(3) 69.7(1) . . . ? N(1) Cd(1) N(4) 116.1(1) . . . ? N(1) Cd(1) N(6) 173.0(1) . . . ? N(3) Cd(1) N(4) 80.1(1) . . . ? N(3) Cd(1) N(6) 112.9(1) . . . ? N(4) Cd(1) N(6) 70.9(1) 2_656 2_656 2_656 ? Cd(1) O(1) H(13) 123.7 . . . no Cd(1) O(1) H(14) 119.4 . . . no H(13) O(1) H(14) 105.2 . . . no Cd(1) O(2) N(7) 106.9(3) . . . ? H(15) O(8) H(15) 105.8 . . . no H(15) O(8) H(16) 112.7 . . . no H(15) O(8) H(16) 120.8 . . . no H(15) O(8) H(16) 120.8 2_656 2_656 2_656 no H(15) O(8) H(16) 112.7 2_656 2_656 2_656 no H(16) O(8) H(16) 83.9 . . . no H(17) O(9) H(18) 101.4 . . . no H(19) O(10) H(20) 121.9 . . . no Cd(1) N(1) C(1) 124.3(3) . . . ? Cd(1) N(1) C(5) 117.0(3) . . . ? C(1) N(1) C(5) 118.5(4) . . . ? C(6) N(2) H(5) 117.8 . . . no C(6) N(2) H(6) 118.4 . . . no H(5) N(2) H(6) 121.9 . . . no Cd(1) N(3) N(4) 119.9(2) . . . ? Cd(1) N(3) C(6) 116.2(3) . . . ? N(4) N(3) C(6) 115.7(3) . . . ? Cd(1) N(4) N(3) 121.5(2) 2_656 2_656 2_656 ? Cd(1) N(4) C(7) 115.1(3) 2_656 2_656 2_656 ? N(3) N(4) C(7) 115.5(3) . . . ? C(7) N(5) H(7) 120.1 . . . no C(7) N(5) H(8) 120.0 . . . no H(7) N(5) H(8) 115.9 . . . no Cd(1) N(6) C(8) 116.0(3) 2_656 2_656 2_656 ? Cd(1) N(6) C(12) 124.5(3) 2_656 2_656 2_656 ? C(8) N(6) C(12) 118.9(4) . . . ? O(2) N(7) O(3) 118.7(4) . . . ? O(2) N(7) O(4) 119.7(4) . . . ? O(3) N(7) O(4) 121.6(4) . . . ? O(5) N(8) O(6) 119.1(4) . . . ? O(5) N(8) O(7) 120.3(5) . . . ? O(6) N(8) O(7) 120.5(5) . . . ? N(1) C(1) C(2) 122.8(4) . . . ? N(1) C(1) H(1) 110.6 . . . no C(2) C(1) H(1) 126.5 . . . no C(1) C(2) C(3) 118.2(4) . . . ? C(1) C(2) H(2) 117.7 . . . no C(3) C(2) H(2) 123.9 . . . no C(2) C(3) C(4) 120.4(5) . . . ? C(2) C(3) H(3) 120.6 . . . no C(4) C(3) H(3) 118.9 . . . no C(3) C(4) C(5) 118.4(4) . . . ? C(3) C(4) H(4) 123.2 . . . no C(5) C(4) H(4) 118.4 . . . no N(1) C(5) C(4) 121.6(4) . . . ? N(1) C(5) C(6) 115.9(4) . . . ? C(4) C(5) C(6) 122.5(4) . . . ? N(2) C(6) N(3) 124.8(4) . . . ? N(2) C(6) C(5) 118.4(4) . . . ? N(3) C(6) C(5) 116.8(4) . . . ? N(4) C(7) N(5) 125.8(4) . . . ? N(4) C(7) C(8) 116.9(3) . . . ? N(5) C(7) C(8) 117.3(4) . . . ? N(6) C(8) C(7) 117.1(4) . . . ? N(6) C(8) C(9) 121.6(4) . . . ? C(7) C(8) C(9) 121.3(4) . . . ? C(8) C(9) C(10) 119.3(4) . . . ? C(8) C(9) H(9) 117.8 . . . no C(10) C(9) H(9) 121.4 . . . no C(9) C(10) C(11) 119.3(5) . . . ? C(9) C(10) H(10) 120.7 . . . no C(11) C(10) H(10) 119.4 . . . no C(10) C(11) C(12) 118.4(4) . . . ? C(10) C(11) H(11) 123.0 . . . no C(12) C(11) H(11) 118.2 . . . no N(6) C(12) C(11) 122.4(4) . . . ? N(6) C(12) H(12) 116.6 . . . no C(11) C(12) H(12) 120.9 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(5) 2.835(4) . 7_556 no O(1) O(4) 2.933(5) . 4_554 no O(1) O(7) 3.071(5) . 7_556 no O(1) N(8) 3.365(5) . 7_556 no O(1) O(5) 3.444(5) . . no O(1) O(3) 3.512(5) . 4_554 no O(1) N(7) 3.569(5) . 4_554 no O(2) O(9) 3.122(5) . . no O(2) O(5) 3.388(5) . 7_556 no O(3) C(7) 3.202(5) . 3_657 no O(3) N(4) 3.241(5) . 3_657 no O(3) C(8) 3.585(6) . 3_657 no O(4) O(9) 3.084(5) . . no O(4) O(7) 3.099(5) . 6_546 no O(4) C(2) 3.500(6) . 6_546 no O(5) O(9) 2.887(5) . 7_556 no O(5) N(2) 3.141(5) . 2_656 no O(5) C(1) 3.316(6) . . no O(6) O(8) 2.948(5) . . no O(6) N(2) 2.956(5) . 2_656 no O(6) C(4) 3.266(6) . 2_656 no O(6) O(9) 3.549(6) . 7_556 no O(7) C(10) 3.085(6) . 2_666 no O(7) C(2) 3.107(7) . . no O(7) C(11) 3.289(7) . 2_666 no O(7) C(1) 3.562(7) . . no O(8) O(10) 2.910(5) . 1_565 no O(8) O(10) 2.910(5) . 2_666 no O(9) O(10) 2.790(5) . 6_556 no O(9) C(11) 3.282(7) . 5_455 no O(9) C(12) 3.431(7) . 5_455 no O(9) N(8) 3.466(7) . 7_556 no O(9) N(7) 3.521(5) . . no O(10) N(5) 2.899(5) . . no O(10) C(9) 3.263(6) . . no O(10) C(4) 3.306(6) . 3_657 no O(10) C(12) 3.552(6) . 2_656 no O(10) C(11) 3.557(6) . 2_656 no N(2) N(8) 3.441(6) . 2_656 no N(3) N(5) 3.506(5) . 3_657 no N(5) C(6) 3.432(5) . 3_657 no N(8) C(2) 3.404(7) . . no N(8) C(1) 3.419(7) . . no C(11) C(11) 3.274(9) . 7_647 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cd(1) O(2) N(7) O(3) . . . . -17.7(5) no Cd(1) O(2) N(7) O(4) . . . . 161.1(3) no Cd(1) N(1) C(1) C(2) . . . . 176.5(4) no Cd(1) N(1) C(5) C(4) . . . . -177.6(3) no Cd(1) N(1) C(5) C(6) . . . . 1.8(5) no Cd(1) N(3) N(4) C(7) . . . . -59.4(4) no Cd(1) N(3) C(6) N(2) . . . . -156.8(3) no Cd(1) N(3) C(6) C(5) . . . . 24.2(4) no Cd(1) N(4) N(3) C(6) . . . . -59.2(4) no Cd(1) N(4) C(7) N(5) . . . . -159.1(3) no Cd(1) N(4) C(7) C(8) . . . . 21.5(4) no Cd(1) N(6) C(8) C(7) . . . . 10.4(4) no Cd(1) N(6) C(8) C(9) . . . . -169.2(3) no Cd(1) N(6) C(12) C(11) . . . . 171.7(4) no O(1) Cd(1) O(2) N(7) . . . . -174.3(3) no O(1) Cd(1) N(1) C(1) . . . . 39.7(4) no O(1) Cd(1) N(1) C(5) . . . . -144.4(3) no O(1) Cd(1) N(3) N(4) . . . . -103.5(3) no O(1) Cd(1) N(3) C(6) . . . . 43.7(4) no O(1) Cd(1) N(4) N(3) . . . . 109.8(3) no O(1) Cd(1) N(4) C(7) . . . . -102.5(3) no O(1) Cd(1) N(6) C(8) . . . . 83.9(3) no O(1) Cd(1) N(6) C(12) . . . . -87.1(4) no O(2) Cd(1) N(1) C(1) . . . . -42.9(4) no O(2) Cd(1) N(1) C(5) . . . . 133.0(3) no O(2) Cd(1) N(3) N(4) . . . . 127.4(2) no O(2) Cd(1) N(3) C(6) . . . . -85.4(3) no O(2) Cd(1) N(4) N(3) . . . . 164.2(3) no O(2) Cd(1) N(4) C(7) . . . . -48.1(5) no O(2) Cd(1) N(6) C(8) . . . . 166.9(3) no O(2) Cd(1) N(6) C(12) . . . . -4.1(4) no N(1) Cd(1) O(2) N(7) . . . . -81.0(3) no N(1) Cd(1) N(3) N(4) . . . . -164.3(3) no N(1) Cd(1) N(3) C(6) . . . . -17.1(3) no N(1) Cd(1) N(4) N(3) . . . . 20.4(3) no N(1) Cd(1) N(4) C(7) . . . . 168.1(3) no N(1) Cd(1) N(6) C(8) . . . . 179.8(8) no N(1) Cd(1) N(6) C(12) . . . . 9(1) no N(1) C(1) C(2) C(3) . . . . 0.3(8) no N(1) C(5) C(4) C(3) . . . . 1.2(7) no N(1) C(5) C(6) N(2) . . . . 163.3(4) no N(1) C(5) C(6) N(3) . . . . -17.7(5) no N(2) C(6) N(3) N(4) . . . . -8.2(6) no N(2) C(6) C(5) C(4) . . . . -17.3(6) no N(3) Cd(1) O(2) N(7) . . . . -19.6(4) no N(3) Cd(1) N(1) C(1) . . . . -168.9(4) no N(3) Cd(1) N(1) C(5) . . . . 7.0(3) no N(3) Cd(1) N(4) C(7) . . . . 106.6(3) no N(3) Cd(1) N(6) C(8) . . . . -69.8(3) no N(3) Cd(1) N(6) C(12) . . . . 119.2(3) no N(3) N(4) Cd(1) N(6) . . . . -159.7(3) no N(3) N(4) C(7) N(5) . . . . -9.4(6) no N(3) N(4) C(7) C(8) . . . . 171.2(3) no N(3) C(6) C(5) C(4) . . . . 161.7(4) no N(4) Cd(1) O(2) N(7) . . . . 131.3(3) no N(4) Cd(1) N(1) C(1) . . . . 123.8(4) no N(4) Cd(1) N(1) C(5) . . . . -60.3(3) no N(4) Cd(1) N(3) C(6) . . . . 105.6(3) no N(4) Cd(1) N(6) C(8) . . . . 0.1(3) no N(4) Cd(1) N(6) C(12) . . . . -170.9(4) no N(4) N(3) Cd(1) N(6) . . . . 22.7(3) no N(4) N(3) C(6) C(5) . . . . 172.8(3) no N(4) C(7) C(8) N(6) . . . . -22.0(5) no N(4) C(7) C(8) C(9) . . . . 157.6(4) no N(5) C(7) C(8) N(6) . . . . 158.6(4) no N(5) C(7) C(8) C(9) . . . . -21.8(6) no N(6) Cd(1) O(2) N(7) . . . . 97.4(3) no N(6) Cd(1) N(1) C(1) . . . . -56(1) no N(6) Cd(1) N(1) C(5) . . . . 120.0(9) no N(6) Cd(1) N(3) C(6) . . . . 169.9(3) no N(6) Cd(1) N(4) C(7) . . . . -12.0(3) no N(6) C(8) C(9) C(10) . . . . -3.8(7) no N(6) C(12) C(11) C(10) . . . . -2.8(8) no C(1) N(1) C(5) C(4) . . . . -1.5(6) no C(1) N(1) C(5) C(6) . . . . 177.9(4) no C(1) C(2) C(3) C(4) . . . . -0.6(8) no C(2) C(1) N(1) C(5) . . . . 0.7(7) no C(2) C(3) C(4) C(5) . . . . -0.2(8) no C(3) C(4) C(5) C(6) . . . . -178.1(4) no C(6) N(3) N(4) C(7) . . . . 153.2(4) no C(7) C(8) N(6) C(12) . . . . -178.0(4) no C(7) C(8) C(9) C(10) . . . . 176.6(4) no C(8) N(6) C(12) C(11) . . . . 1.0(7) no C(8) C(9) C(10) C(11) . . . . 1.9(8) no C(9) C(8) N(6) C(12) . . . . 2.4(6) no C(9) C(10) C(11) C(12) . . . . 1.3(8) no #------------------------------------------------------------------------------ # End of CIF #====================================================================