Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_General #============================================================================== _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' _audit_creation_date '1999-01-26' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ? #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Prof L Thompson' _publ_contact_author_address ; Prof L Thompson Department of Chemistry Memorial University of Newfoundland St, John's Newfoundland A1B 3X7 CANADA ; #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER ANY FOOTNOTES TO TITLE ; loop_ _publ_author_name 'Liang Zhao' 'Laurence K. Thompson' 'Zhiqiang Xu' 'David. O. Miller' 'David R. Stirling' #============================================================================== # 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. (1997-1998). teXsan for Windows version 1.03. Single Crystal Structure Analysis Software. Version 1.04. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. 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 ; #============================================================================== data_zl-60 _database_code_CSD 158370 #============================================================================== _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 9.722(3) _cell_length_b 23.218(3) _cell_length_c 15.305(2) _cell_angle_alpha 90 _cell_angle_beta 93.62(2) _cell_angle_gamma 90 _cell_volume 3448(1) _cell_formula_units_Z 4 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 13.8 #------------------------------------------------------------------------------ _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 'yellow-green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 882.25 _chemical_formula_analytical ? _chemical_formula_sum 'C27 H33 Cu3 N9 O13 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1796.00 _exptl_absorpt_coefficient_mu 1.911 _exptl_absorpt_correction_type none _exptl_special_details ; The scan width was (1.05+0.35tan\q)\% with an \w scan speed of 4\% per minute (up to 8 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_% -4.02 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 2 -3 -1 1 -3 -2 2 -3 _diffrn_reflns_number 8628 _reflns_number_total 8168 _reflns_number_gt 4771 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.04190 _diffrn_reflns_av_sigmaI/netI 0.139 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04558 _diffrn_orient_matrix_UB_12 0.03802 _diffrn_orient_matrix_UB_13 -0.01216 _diffrn_orient_matrix_UB_21 0.06646 _diffrn_orient_matrix_UB_22 0.01876 _diffrn_orient_matrix_UB_23 0.04371 _diffrn_orient_matrix_UB_31 0.06425 _diffrn_orient_matrix_UB_32 0.00757 _diffrn_orient_matrix_UB_33 -0.04720 #------------------------------------------------------------------------------ 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 0 108 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 52 0.008 0.006 ;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) ; Cu 0 12 0.263 1.266 ;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 Cu(1) 0.70145(6) 0.00818(2) 0.21627(4) 0.0314(2) 1.000 . Uani d ? Cu(2) 0.56223(6) 0.20886(2) 0.25161(4) 0.0283(2) 1.000 . Uani d ? Cu(3) 0.53443(6) 0.42116(2) 0.21783(4) 0.0298(2) 1.000 . Uani d ? O(1) 0.7917(4) 0.0737(1) 0.1606(2) 0.038(1) 1.000 . Uani d ? O(2) 0.6469(4) 0.3702(1) 0.1479(2) 0.036(1) 1.000 . Uani d ? O(3) 0.8026(3) -0.0542(1) 0.1697(2) 0.035(1) 1.000 . Uani d ? O(4) 0.6357(4) -0.0595(2) 0.0666(2) 0.047(1) 1.000 . Uani d ? O(5) 0.3738(3) 0.1920(1) 0.2815(2) 0.036(1) 1.000 . Uani d ? O(6) 0.2982(5) 0.1523(2) 0.1557(3) 0.078(2) 1.000 . Uani d ? O(7) 0.6093(4) 0.2150(2) 0.3890(2) 0.039(1) 1.000 . Uani d ? O(8) 0.8209(4) 0.2381(2) 0.3566(3) 0.073(2) 1.000 . Uani d ? O(9) 0.6098(3) 0.4917(1) 0.1744(2) 0.032(1) 1.000 . Uani d ? O(10) 0.4175(4) 0.5082(2) 0.0954(3) 0.054(1) 1.000 . Uani d ? O(11) 0.5082(4) 0.1343(2) 0.0443(3) 0.064(1) 1.000 . Uani d ? O(12) 0.2643(4) 0.0736(2) 0.5042(2) 0.055(1) 1.000 . Uani d ? O(13) 0.5563(5) 0.2114(2) 0.9152(3) 0.090(2) 1.000 . Uani d ? N(1) 0.5681(4) -0.0376(2) 0.2832(3) 0.033(1) 1.000 . Uani d ? N(2) 0.4832(5) 0.0952(2) 0.3894(3) 0.045(1) 1.000 . Uani d ? N(3) 0.6013(4) 0.0703(2) 0.2653(3) 0.029(1) 1.000 . Uani d ? N(4) 0.6387(4) 0.1256(2) 0.2415(2) 0.028(1) 1.000 . Uani d ? N(5) 0.6985(4) 0.2200(2) 0.1665(2) 0.028(1) 1.000 . Uani d ? N(6) 0.5356(4) 0.2985(2) 0.2222(3) 0.028(1) 1.000 . Uani d ? N(7) 0.4679(4) 0.3473(2) 0.2531(2) 0.027(1) 1.000 . Uani d ? N(8) 0.3044(5) 0.2990(2) 0.3327(3) 0.044(1) 1.000 . Uani d ? N(9) 0.3843(4) 0.4479(2) 0.2915(3) 0.034(1) 1.000 . Uani d ? C(1) 0.5424(6) -0.0929(2) 0.2799(4) 0.039(2) 1.000 . Uani d ? C(2) 0.4488(6) -0.1199(2) 0.3319(4) 0.044(2) 1.000 . Uani d ? C(3) 0.3797(6) -0.0860(3) 0.3881(4) 0.053(2) 1.000 . Uani d ? C(4) 0.4068(6) -0.0271(2) 0.3911(4) 0.047(2) 1.000 . Uani d ? C(5) 0.4976(5) -0.0042(2) 0.3392(3) 0.031(1) 1.000 . Uani d ? C(6) 0.5277(5) 0.0585(2) 0.3318(3) 0.028(1) 1.000 . Uani d ? C(7) 0.7345(5) 0.1208(2) 0.1827(3) 0.032(1) 1.000 . Uani d ? C(8) 0.7722(5) 0.1757(2) 0.1419(3) 0.028(1) 1.000 . Uani d ? C(9) 0.8702(5) 0.1816(2) 0.0818(3) 0.038(2) 1.000 . Uani d ? C(10) 0.8901(6) 0.2351(2) 0.0448(3) 0.042(2) 1.000 . Uani d ? C(11) 0.8099(5) 0.2813(2) 0.0693(3) 0.037(2) 1.000 . Uani d ? C(12) 0.7175(5) 0.2726(2) 0.1322(3) 0.029(1) 1.000 . Uani d ? C(13) 0.6267(5) 0.3175(2) 0.1682(3) 0.028(1) 1.000 . Uani d ? C(14) 0.3656(5) 0.3450(2) 0.3032(3) 0.029(1) 1.000 . Uani d ? C(15) 0.3203(5) 0.4043(2) 0.3295(3) 0.030(1) 1.000 . Uani d ? C(16) 0.2243(6) 0.4139(2) 0.3906(4) 0.047(2) 1.000 . Uani d ? C(17) 0.1919(6) 0.4691(3) 0.4118(4) 0.056(2) 1.000 . Uani d ? C(18) 0.2566(7) 0.5141(2) 0.3707(4) 0.056(2) 1.000 . Uani d ? C(19) 0.3535(6) 0.5019(2) 0.3119(4) 0.045(2) 1.000 . Uani d ? C(20) 0.7479(6) -0.0758(2) 0.0981(3) 0.034(1) 1.000 . Uani d ? C(21) 0.8322(7) -0.1215(3) 0.0566(4) 0.062(2) 1.000 . Uani d ? C(22) 0.2810(6) 0.1683(2) 0.2300(4) 0.039(2) 1.000 . Uani d ? C(23) 0.1447(7) 0.1607(3) 0.2702(5) 0.075(3) 1.000 . Uani d ? C(24) 0.7347(6) 0.2252(2) 0.4089(4) 0.040(2) 1.000 . Uani d ? C(25) 0.7796(7) 0.2222(3) 0.5051(4) 0.055(2) 1.000 . Uani d ? C(26) 0.5350(5) 0.5220(2) 0.1203(3) 0.032(1) 1.000 . Uani d ? C(27) 0.6017(6) 0.5756(2) 0.0859(4) 0.048(2) 1.000 . Uani d ? H(1) 0.5890 -0.1155 0.2393 0.046 1.000 . Uiso c ? H(2) 0.4340 -0.1602 0.3283 0.052 1.000 . Uiso c ? H(3) 0.3149 -0.1025 0.4246 0.063 1.000 . Uiso c ? H(4) 0.3601 -0.0031 0.4295 0.054 1.000 . Uiso c ? H(5) 0.9244 0.1494 0.0664 0.045 1.000 . Uiso c ? H(6) 0.9568 0.2400 0.0027 0.051 1.000 . Uiso c ? H(7) 0.8187 0.3181 0.0431 0.043 1.000 . Uiso c ? H(8) 0.1818 0.3821 0.4178 0.055 1.000 . Uiso c ? H(9) 0.1261 0.4767 0.4537 0.064 1.000 . Uiso c ? H(10) 0.2358 0.5531 0.3836 0.068 1.000 . Uiso c ? H(11) 0.4000 0.5327 0.2851 0.052 1.000 . Uiso c ? H(12) 0.4311 0.0822 0.4210 0.048 1.000 . Uiso c ? H(13) 0.4936 0.1219 0.3880 0.048 1.000 . Uiso c ? H(14) 0.2332 0.2989 0.3555 0.050 1.000 . Uiso c ? H(15) 0.3358 0.2623 0.3211 0.050 1.000 . Uiso c ? H(16) 0.8735 -0.1452 0.1005 0.075 1.000 . Uiso c ? H(17) 0.7729 -0.1437 0.0177 0.075 1.000 . Uiso c ? H(18) 0.9003 -0.1033 0.0244 0.075 1.000 . Uiso c ? H(19) 0.1545 0.1621 0.3332 0.085 1.000 . Uiso c ? H(20) 0.0804 0.1906 0.2515 0.085 1.000 . Uiso c ? H(21) 0.1027 0.1245 0.2540 0.085 1.000 . Uiso c ? H(22) 0.7036 0.2267 0.5414 0.062 1.000 . Uiso c ? H(23) 0.8229 0.1856 0.5203 0.062 1.000 . Uiso c ? H(24) 0.8463 0.2517 0.5218 0.062 1.000 . Uiso c ? H(25) 0.6328 0.5992 0.1332 0.058 1.000 . Uiso c ? H(26) 0.6773 0.5647 0.0529 0.058 1.000 . Uiso c ? H(27) 0.5359 0.5958 0.0489 0.058 1.000 . Uiso c ? H(28) 0.2382 0.0816 0.5494 0.067 1.000 . Uiso c ? H(29) 0.2009 0.0630 0.4766 0.067 1.000 . Uiso c ? H(30) 0.4476 0.1151 0.0136 0.077 1.000 . Uiso c ? H(31) 0.4463 0.1449 0.0733 0.077 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 Cu(1) 0.0373(4) 0.0235(3) 0.0345(3) 0.0041(3) 0.0119(3) -0.0027(3) Cu(2) 0.0330(3) 0.0228(3) 0.0305(3) 0.0004(3) 0.0139(3) -0.0006(3) Cu(3) 0.0371(4) 0.0208(3) 0.0330(3) -0.0002(3) 0.0134(3) 0.0025(3) O(1) 0.043(2) 0.025(2) 0.047(2) 0.010(2) 0.023(2) 0.001(2) O(2) 0.049(2) 0.023(2) 0.036(2) -0.002(2) 0.019(2) 0.003(2) O(3) 0.040(2) 0.033(2) 0.032(2) 0.006(2) 0.003(2) -0.013(2) O(4) 0.046(2) 0.054(3) 0.040(2) 0.009(2) -0.000(2) -0.009(2) O(5) 0.033(2) 0.028(2) 0.048(2) -0.009(2) 0.012(2) -0.003(2) O(6) 0.081(4) 0.104(4) 0.052(3) -0.020(3) 0.021(3) -0.030(3) O(7) 0.039(2) 0.045(2) 0.033(2) -0.006(2) 0.006(2) -0.007(2) O(8) 0.058(3) 0.117(4) 0.047(3) -0.022(3) 0.023(2) -0.005(3) O(9) 0.038(2) 0.024(2) 0.034(2) 0.000(2) 0.005(2) 0.008(2) O(10) 0.045(3) 0.064(3) 0.052(3) -0.011(2) -0.007(2) 0.024(2) O(11) 0.048(3) 0.088(3) 0.055(3) -0.017(2) 0.003(2) -0.013(3) O(12) 0.051(3) 0.071(3) 0.045(2) -0.015(2) 0.022(2) -0.027(2) O(13) 0.066(3) 0.083(4) 0.129(4) 0.035(3) 0.061(3) 0.043(3) N(1) 0.034(2) 0.030(2) 0.034(2) 0.001(2) 0.004(2) -0.006(2) N(2) 0.070(3) 0.025(2) 0.044(3) 0.003(2) 0.035(3) 0.002(2) N(3) 0.036(2) 0.019(2) 0.031(2) 0.001(2) 0.011(2) 0.002(2) N(4) 0.033(2) 0.028(2) 0.024(2) 0.006(2) 0.013(2) 0.001(2) N(5) 0.032(2) 0.025(2) 0.027(2) -0.004(2) 0.012(2) -0.002(2) N(6) 0.034(2) 0.014(2) 0.036(2) -0.001(2) 0.012(2) -0.003(2) N(7) 0.031(2) 0.020(2) 0.032(2) -0.001(2) 0.018(2) -0.003(2) N(8) 0.047(3) 0.026(2) 0.064(3) -0.007(2) 0.036(2) -0.003(2) N(9) 0.040(3) 0.027(2) 0.036(2) 0.003(2) 0.011(2) -0.001(2) C(1) 0.049(4) 0.023(3) 0.045(3) -0.004(2) 0.005(3) -0.003(2) C(2) 0.056(4) 0.027(3) 0.049(4) -0.006(3) 0.002(3) 0.002(3) C(3) 0.047(4) 0.042(4) 0.072(4) -0.007(3) 0.018(3) 0.017(3) C(4) 0.050(4) 0.039(3) 0.053(4) 0.004(3) 0.017(3) 0.002(3) C(5) 0.030(3) 0.025(3) 0.037(3) 0.000(2) 0.004(2) 0.003(2) C(6) 0.025(3) 0.031(3) 0.029(3) 0.003(2) 0.006(2) 0.002(2) C(7) 0.033(3) 0.028(3) 0.034(3) 0.002(2) 0.007(2) 0.003(2) C(8) 0.027(3) 0.029(3) 0.029(3) 0.004(2) 0.008(2) -0.002(2) C(9) 0.041(3) 0.035(3) 0.042(3) 0.003(2) 0.023(3) -0.004(2) C(10) 0.046(3) 0.044(3) 0.041(3) -0.004(3) 0.029(3) -0.005(3) C(11) 0.046(3) 0.026(3) 0.043(3) -0.007(2) 0.021(3) 0.002(2) C(12) 0.030(3) 0.026(3) 0.031(3) -0.006(2) 0.010(2) -0.003(2) C(13) 0.033(3) 0.023(2) 0.030(3) -0.002(2) 0.013(2) -0.001(2) C(14) 0.031(3) 0.028(3) 0.029(3) -0.004(2) 0.008(2) -0.007(2) C(15) 0.029(3) 0.027(3) 0.034(3) -0.001(2) 0.008(2) -0.007(2) C(16) 0.042(3) 0.037(3) 0.067(4) -0.006(3) 0.027(3) -0.014(3) C(17) 0.048(4) 0.043(4) 0.080(5) -0.005(3) 0.036(3) -0.021(3) C(18) 0.063(4) 0.031(3) 0.077(5) 0.002(3) 0.026(4) -0.007(3) C(19) 0.075(4) 0.012(2) 0.051(4) 0.002(3) 0.026(3) -0.006(2) C(20) 0.046(3) 0.028(3) 0.030(3) 0.004(3) 0.007(2) -0.002(2) C(21) 0.075(5) 0.065(4) 0.045(4) 0.034(4) -0.005(3) -0.019(3) C(22) 0.040(3) 0.026(3) 0.053(4) -0.004(2) 0.015(3) 0.008(3) C(23) 0.045(4) 0.096(6) 0.085(5) -0.026(4) 0.012(4) -0.028(5) C(24) 0.050(4) 0.033(3) 0.036(3) -0.006(3) 0.003(3) -0.009(2) C(25) 0.066(4) 0.058(4) 0.040(4) -0.006(3) 0.004(3) 0.005(3) C(26) 0.036(3) 0.030(3) 0.031(3) 0.001(2) 0.012(2) 0.003(2) C(27) 0.062(4) 0.038(3) 0.044(3) -0.011(3) 0.002(3) 0.016(3) #============================================================================== # 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) + 0.00004|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 4771 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_all 0.0620 _refine_ls_wR_factor_ref 0.0540 _refine_ls_goodness_of_fit_all 1.433 _refine_ls_goodness_of_fit_ref 1.650 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.46 _refine_diff_density_max 0.00 #============================================================================== # 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 Cu(1) O(1) 1.975(4) . . ? Cu(1) O(3) 1.913(4) . . ? Cu(1) N(1) 2.006(5) . . ? Cu(1) N(3) 1.920(5) . . ? Cu(2) O(5) 1.955(4) . . ? Cu(2) O(7) 2.128(4) . . ? Cu(2) N(4) 2.080(5) . . ? Cu(2) N(5) 1.933(5) . . ? Cu(2) N(6) 2.141(5) . . ? Cu(3) O(2) 1.971(4) . . ? Cu(3) O(9) 1.929(4) . . ? Cu(3) N(7) 1.921(5) . . ? Cu(3) N(9) 1.999(5) . . ? O(1) C(7) 1.284(7) . . ? O(2) C(13) 1.281(7) . . ? O(3) C(20) 1.288(7) . . ? O(4) C(20) 1.224(7) . . ? O(5) C(22) 1.284(8) . . ? O(6) C(22) 1.219(8) . . ? O(7) C(24) 1.261(8) . . ? O(8) C(24) 1.232(8) . . ? O(9) C(26) 1.278(7) . . ? O(10) C(26) 1.224(8) . . ? O(11) H(30) 0.86 . . no O(11) H(31) 0.81 . . no O(12) H(28) 0.77 . . no O(12) H(29) 0.77 . . no N(1) C(1) 1.309(7) . . ? N(1) C(5) 1.370(7) . . ? N(2) C(6) 1.319(7) . . ? N(2) H(12) 0.78 . . no N(2) H(13) 0.63 . . no N(3) N(4) 1.388(6) . . ? N(3) C(6) 1.309(7) . . ? N(4) C(7) 1.341(7) . . ? N(5) C(8) 1.323(7) . . ? N(5) C(12) 1.346(7) . . ? N(6) N(7) 1.409(6) . . ? N(6) C(13) 1.325(7) . . ? N(7) C(14) 1.293(7) . . ? N(8) C(14) 1.315(7) . . ? N(8) H(14) 0.79 . . no N(8) H(15) 0.93 . . no N(9) C(15) 1.339(7) . . ? N(9) C(19) 1.331(7) . . ? C(1) C(2) 1.395(9) . . ? C(1) H(1) 0.95 . . no C(2) C(3) 1.37(1) . . ? C(2) H(2) 0.95 . . no C(3) C(4) 1.392(9) . . ? C(3) H(3) 0.95 . . no C(4) C(5) 1.335(9) . . ? C(4) H(4) 0.95 . . no C(5) C(6) 1.491(8) . . ? C(7) C(8) 1.474(8) . . ? C(8) C(9) 1.373(8) . . ? C(9) C(10) 1.383(9) . . ? C(9) H(5) 0.95 . . no C(10) C(11) 1.390(9) . . ? C(10) H(6) 0.95 . . no C(11) C(12) 1.373(8) . . ? C(11) H(7) 0.95 . . no C(12) C(13) 1.494(8) . . ? C(14) C(15) 1.509(8) . . ? C(15) C(16) 1.380(8) . . ? C(16) C(17) 1.365(9) . . ? C(16) H(8) 0.95 . . no C(17) C(18) 1.39(1) . . ? C(17) H(9) 0.95 . . no C(18) C(19) 1.372(9) . . ? C(18) H(10) 0.95 . . no C(19) H(11) 0.95 . . no C(20) C(21) 1.507(9) . . ? C(21) H(16) 0.94 . . no C(21) H(17) 0.95 . . no C(21) H(18) 0.95 . . no C(22) C(23) 1.51(1) . . ? C(23) H(19) 0.96 . . no C(23) H(20) 0.97 . . no C(23) H(21) 0.96 . . no C(24) C(25) 1.51(1) . . ? C(25) H(22) 0.96 . . no C(25) H(23) 0.97 . . no C(25) H(24) 0.97 . . no C(26) C(27) 1.513(9) . . ? C(27) H(25) 0.94 . . no C(27) H(26) 0.95 . . no C(27) H(27) 0.95 . . 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) Cu(1) O(3) 99.7(2) . . . ? O(1) Cu(1) N(1) 161.2(2) . . . ? O(1) Cu(1) N(3) 80.8(2) . . . ? O(3) Cu(1) N(1) 98.8(2) . . . ? O(3) Cu(1) N(3) 178.8(2) . . . ? N(1) Cu(1) N(3) 80.7(2) . . . ? O(5) Cu(2) O(7) 85.9(2) . . . ? O(5) Cu(2) N(4) 100.1(2) . . . ? O(5) Cu(2) N(5) 151.2(2) . . . ? O(5) Cu(2) N(6) 98.1(2) . . . ? O(7) Cu(2) N(4) 94.6(2) . . . ? O(7) Cu(2) N(5) 122.9(2) . . . ? O(7) Cu(2) N(6) 99.1(2) . . . ? N(4) Cu(2) N(5) 79.1(2) . . . ? N(4) Cu(2) N(6) 157.9(2) . . . ? N(5) Cu(2) N(6) 78.9(2) . . . ? O(2) Cu(3) O(9) 94.9(2) . . . ? O(2) Cu(3) N(7) 80.0(2) . . . ? O(2) Cu(3) N(9) 160.4(2) . . . ? O(9) Cu(3) N(7) 174.8(2) . . . ? O(9) Cu(3) N(9) 103.8(2) . . . ? N(7) Cu(3) N(9) 81.2(2) . . . ? Cu(1) O(1) C(7) 109.4(4) . . . ? Cu(3) O(2) C(13) 110.0(4) . . . ? Cu(1) O(3) C(20) 114.6(4) . . . ? Cu(2) O(5) C(22) 125.1(4) . . . ? Cu(2) O(7) C(24) 113.2(4) . . . ? Cu(3) O(9) C(26) 118.6(4) . . . ? H(30) O(11) H(31) 87.1 . . . no H(28) O(12) H(29) 105.8 . . . no Cu(1) N(1) C(1) 128.9(5) . . . ? Cu(1) N(1) C(5) 112.6(4) . . . ? C(1) N(1) C(5) 118.5(6) . . . ? C(6) N(2) H(12) 114.5 . . . no C(6) N(2) H(13) 123.6 . . . no H(12) N(2) H(13) 121.0 . . . no Cu(1) N(3) N(4) 116.4(3) . . . ? Cu(1) N(3) C(6) 117.5(4) . . . ? N(4) N(3) C(6) 124.2(5) . . . ? Cu(2) N(4) N(3) 137.6(4) . . . ? Cu(2) N(4) C(7) 113.1(4) . . . ? N(3) N(4) C(7) 107.7(5) . . . ? Cu(2) N(5) C(8) 119.6(4) . . . ? Cu(2) N(5) C(12) 120.1(4) . . . ? C(8) N(5) C(12) 120.3(5) . . . ? Cu(2) N(6) N(7) 139.9(4) . . . ? Cu(2) N(6) C(13) 112.3(4) . . . ? N(7) N(6) C(13) 106.6(4) . . . ? Cu(3) N(7) N(6) 116.8(3) . . . ? Cu(3) N(7) C(14) 119.3(4) . . . ? N(6) N(7) C(14) 123.9(5) . . . ? C(14) N(8) H(14) 125.4 . . . no C(14) N(8) H(15) 121.3 . . . no H(14) N(8) H(15) 112.8 . . . no Cu(3) N(9) C(15) 112.8(4) . . . ? Cu(3) N(9) C(19) 127.4(5) . . . ? C(15) N(9) C(19) 119.5(5) . . . ? N(1) C(1) C(2) 123.3(6) . . . ? N(1) C(1) H(1) 118.0 . . . no C(2) C(1) H(1) 118.7 . . . no C(1) C(2) C(3) 117.6(6) . . . ? C(1) C(2) H(2) 120.9 . . . no C(3) C(2) H(2) 121.5 . . . no C(2) C(3) C(4) 119.0(7) . . . ? C(2) C(3) H(3) 120.5 . . . no C(4) C(3) H(3) 120.5 . . . no C(3) C(4) C(5) 120.1(7) . . . ? C(3) C(4) H(4) 120.1 . . . no C(5) C(4) H(4) 119.7 . . . no N(1) C(5) C(4) 121.5(6) . . . ? N(1) C(5) C(6) 113.3(5) . . . ? C(4) C(5) C(6) 125.1(6) . . . ? N(2) C(6) N(3) 127.1(6) . . . ? N(2) C(6) C(5) 120.4(5) . . . ? N(3) C(6) C(5) 112.5(5) . . . ? O(1) C(7) N(4) 125.3(6) . . . ? O(1) C(7) C(8) 120.1(5) . . . ? N(4) C(7) C(8) 114.6(5) . . . ? N(5) C(8) C(7) 113.4(5) . . . ? N(5) C(8) C(9) 121.6(6) . . . ? C(7) C(8) C(9) 125.0(6) . . . ? C(8) C(9) C(10) 119.1(6) . . . ? C(8) C(9) H(5) 120.2 . . . no C(10) C(9) H(5) 120.8 . . . no C(9) C(10) C(11) 119.1(6) . . . ? C(9) C(10) H(6) 120.1 . . . no C(11) C(10) H(6) 120.7 . . . no C(10) C(11) C(12) 118.6(6) . . . ? C(10) C(11) H(7) 120.9 . . . no C(12) C(11) H(7) 120.5 . . . no N(5) C(12) C(11) 121.2(6) . . . ? N(5) C(12) C(13) 113.0(5) . . . ? C(11) C(12) C(13) 125.7(6) . . . ? O(2) C(13) N(6) 126.1(5) . . . ? O(2) C(13) C(12) 118.3(5) . . . ? N(6) C(13) C(12) 115.5(5) . . . ? N(7) C(14) N(8) 128.3(6) . . . ? N(7) C(14) C(15) 111.6(5) . . . ? N(8) C(14) C(15) 120.1(5) . . . ? N(9) C(15) C(14) 114.9(5) . . . ? N(9) C(15) C(16) 121.7(6) . . . ? C(14) C(15) C(16) 123.3(6) . . . ? C(15) C(16) C(17) 119.2(7) . . . ? C(15) C(16) H(8) 120.1 . . . no C(17) C(16) H(8) 120.6 . . . no C(16) C(17) C(18) 118.7(7) . . . ? C(16) C(17) H(9) 120.8 . . . no C(18) C(17) H(9) 120.5 . . . no C(17) C(18) C(19) 119.4(6) . . . ? C(17) C(18) H(10) 120.8 . . . no C(19) C(18) H(10) 119.8 . . . no N(9) C(19) C(18) 121.5(6) . . . ? N(9) C(19) H(11) 119.2 . . . no C(18) C(19) H(11) 119.4 . . . no O(3) C(20) O(4) 121.7(6) . . . ? O(3) C(20) C(21) 115.3(6) . . . ? O(4) C(20) C(21) 123.0(6) . . . ? C(20) C(21) H(16) 109.3 . . . no C(20) C(21) H(17) 108.7 . . . no C(20) C(21) H(18) 108.7 . . . no H(16) C(21) H(17) 110.2 . . . no H(16) C(21) H(18) 110.5 . . . no H(17) C(21) H(18) 109.3 . . . no O(5) C(22) O(6) 124.9(7) . . . ? O(5) C(22) C(23) 113.7(6) . . . ? O(6) C(22) C(23) 121.4(7) . . . ? C(22) C(23) H(19) 111.8 . . . no C(22) C(23) H(20) 111.4 . . . no C(22) C(23) H(21) 111.6 . . . no H(19) C(23) H(20) 107.1 . . . no H(19) C(23) H(21) 107.5 . . . no H(20) C(23) H(21) 107.3 . . . no O(7) C(24) O(8) 125.2(7) . . . ? O(7) C(24) C(25) 116.2(6) . . . ? O(8) C(24) C(25) 118.6(7) . . . ? C(24) C(25) H(22) 112.0 . . . no C(24) C(25) H(23) 111.6 . . . no C(24) C(25) H(24) 111.9 . . . no H(22) C(25) H(23) 107.2 . . . no H(22) C(25) H(24) 107.5 . . . no H(23) C(25) H(24) 106.5 . . . no O(9) C(26) O(10) 122.6(6) . . . ? O(9) C(26) C(27) 116.1(6) . . . ? O(10) C(26) C(27) 121.3(6) . . . ? C(26) C(27) H(25) 109.6 . . . no C(26) C(27) H(26) 109.2 . . . no C(26) C(27) H(27) 109.1 . . . no H(25) C(27) H(26) 109.9 . . . no H(25) C(27) H(27) 109.9 . . . no H(26) C(27) H(27) 109.1 . . . 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 Cu(1) O(9) 2.435(4) . 2_645 no Cu(1) Cu(3) 3.371(1) . 2_645 no Cu(1) C(26) 3.481(7) . 2_645 no Cu(3) O(3) 2.335(4) . 2_655 no Cu(3) C(20) 3.415(7) . 2_655 no O(1) O(9) 3.258(6) . 2_645 no O(1) O(11) 3.482(7) . . no O(2) O(12) 2.857(6) . 4_554 no O(2) C(1) 3.265(9) . 2_655 no O(2) O(3) 3.307(6) . 2_655 no O(3) O(9) 2.701(6) . 2_645 no O(3) N(9) 3.065(7) . 2_645 no O(3) N(7) 3.356(7) . 2_645 no O(3) C(19) 3.582(9) . 2_645 no O(4) O(11) 2.748(7) . 3_655 no O(4) C(17) 3.238(9) . 4_554 no O(4) C(17) 3.291(9) . 2_545 no O(4) C(18) 3.455(9) . 4_554 no O(6) O(11) 2.773(8) . . no O(6) C(18) 3.27(1) . 2_545 no O(6) C(21) 3.485(9) . 3_655 no O(7) C(10) 3.494(7) . 4_455 no O(8) O(13) 2.676(8) . 4_554 no O(9) N(1) 3.230(7) . 2_655 no O(9) N(3) 3.428(7) . 2_655 no O(9) O(12) 3.439(6) . 4_554 no O(10) O(12) 2.722(7) . 2 no O(10) C(4) 3.277(9) . 2 no O(10) C(27) 3.384(9) . 3_665 no O(10) C(26) 3.434(8) . 3_665 no O(10) O(10) 3.44(1) . 3_665 no O(11) O(13) 2.728(8) . 1_554 no O(11) C(7) 2.973(8) . . no O(11) C(8) 3.042(8) . . no O(11) N(4) 3.206(7) . . no O(11) N(5) 3.232(7) . . no O(11) C(16) 3.438(9) . 4_554 no O(11) C(20) 3.481(9) . 3_655 no O(11) C(21) 3.57(1) . 3_655 no O(12) N(2) 2.889(7) . . no O(12) C(4) 3.269(8) . . no O(12) C(11) 3.535(8) . 4_455 no O(12) C(26) 3.582(8) . 2_545 no O(13) N(8) 2.803(7) . 4 no O(13) C(16) 3.368(9) . 4 no O(13) C(24) 3.451(9) . 4_455 no O(13) C(25) 3.460(9) . 4_455 no N(2) C(3) 3.58(1) . 3_656 no N(3) C(27) 3.565(9) . 2_645 no N(7) C(21) 3.474(9) . 2_655 no N(8) C(10) 3.394(9) . 4_455 no C(1) C(16) 3.56(1) . 2_545 no C(2) C(15) 3.53(1) . 2_545 no C(2) C(11) 3.55(1) . 2_645 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 Cu(1) O(1) C(7) N(4) . . . . 6.5(8) no Cu(1) O(1) C(7) C(8) . . . . -173.0(5) no Cu(1) O(3) C(20) O(4) . . . . -4.5(8) no Cu(1) O(3) C(20) C(21) . . . . 175.1(5) no Cu(1) N(1) C(1) C(2) . . . . 178.3(5) no Cu(1) N(1) C(5) C(4) . . . . -178.2(6) no Cu(1) N(1) C(5) C(6) . . . . 4.8(7) no Cu(1) N(3) N(4) Cu(2) . . . . 168.4(3) no Cu(1) N(3) N(4) C(7) . . . . 4.1(6) no Cu(1) N(3) C(6) N(2) . . . . 159.9(6) no Cu(1) N(3) C(6) C(5) . . . . -19.0(7) no Cu(2) O(5) C(22) O(6) . . . . 1(1) no Cu(2) O(5) C(22) C(23) . . . . -179.8(5) no Cu(2) O(7) C(24) O(8) . . . . 9(1) no Cu(2) O(7) C(24) C(25) . . . . -172.1(5) no Cu(2) N(4) N(3) C(6) . . . . -27.7(9) no Cu(2) N(4) C(7) O(1) . . . . -175.7(5) no Cu(2) N(4) C(7) C(8) . . . . 3.7(7) no Cu(2) N(5) C(8) C(7) . . . . 2.1(7) no Cu(2) N(5) C(8) C(9) . . . . -179.9(5) no Cu(2) N(5) C(12) C(11) . . . . -177.6(5) no Cu(2) N(5) C(12) C(13) . . . . 1.0(7) no Cu(2) N(6) N(7) Cu(3) . . . . 160.7(4) no Cu(2) N(6) N(7) C(14) . . . . -19(1) no Cu(2) N(6) C(13) O(2) . . . . -170.7(5) no Cu(2) N(6) C(13) C(12) . . . . 6.0(7) no Cu(3) O(2) C(13) N(6) . . . . 5.5(8) no Cu(3) O(2) C(13) C(12) . . . . -171.2(4) no Cu(3) O(9) C(26) O(10) . . . . 0.3(8) no Cu(3) O(9) C(26) C(27) . . . . -177.7(4) no Cu(3) N(7) N(6) C(13) . . . . -4.8(6) no Cu(3) N(7) C(14) N(8) . . . . 178.6(6) no Cu(3) N(7) C(14) C(15) . . . . -3.1(7) no Cu(3) N(9) C(15) C(14) . . . . -5.0(7) no Cu(3) N(9) C(15) C(16) . . . . 172.6(6) no Cu(3) N(9) C(19) C(18) . . . . -173.1(6) no O(1) Cu(1) O(3) C(20) . . . . -92.1(5) no O(1) Cu(1) N(1) C(1) . . . . 158.4(6) no O(1) Cu(1) N(1) C(5) . . . . -21.9(9) no O(1) Cu(1) N(3) N(4) . . . . -1.0(4) no O(1) Cu(1) N(3) C(6) . . . . -166.0(5) no O(1) C(7) N(4) N(3) . . . . -7.2(9) no O(1) C(7) C(8) N(5) . . . . 175.6(6) no O(1) C(7) C(8) C(9) . . . . -2(1) no O(2) Cu(3) O(9) C(26) . . . . 106.6(4) no O(2) Cu(3) N(7) N(6) . . . . 6.1(4) no O(2) Cu(3) N(7) C(14) . . . . -174.1(5) no O(2) Cu(3) N(9) C(15) . . . . 18.8(9) no O(2) Cu(3) N(9) C(19) . . . . -168.2(6) no O(2) C(13) N(6) N(7) . . . . -0.7(9) no O(2) C(13) C(12) N(5) . . . . 172.1(6) no O(2) C(13) C(12) C(11) . . . . -9(1) no O(3) Cu(1) O(1) C(7) . . . . 178.5(4) no O(3) Cu(1) N(1) C(1) . . . . -12.1(6) no O(3) Cu(1) N(1) C(5) . . . . 167.6(4) no O(3) Cu(1) N(3) N(4) . . . . 117(10) no O(3) Cu(1) N(3) C(6) . . . . -48(10) no O(5) Cu(2) O(7) C(24) . . . . 178.3(5) no O(5) Cu(2) N(4) N(3) . . . . -15.1(6) no O(5) Cu(2) N(4) C(7) . . . . 148.6(4) no O(5) Cu(2) N(5) C(8) . . . . -91.4(6) no O(5) Cu(2) N(5) C(12) . . . . 88.2(6) no O(5) Cu(2) N(6) N(7) . . . . 39.7(6) no O(5) Cu(2) N(6) C(13) . . . . -155.3(4) no O(7) Cu(2) O(5) C(22) . . . . -161.7(5) no O(7) Cu(2) N(4) N(3) . . . . 71.5(6) no O(7) Cu(2) N(4) C(7) . . . . -124.8(5) no O(7) Cu(2) N(5) C(8) . . . . 88.4(5) no O(7) Cu(2) N(5) C(12) . . . . -92.1(5) no O(7) Cu(2) N(6) N(7) . . . . -47.3(6) no O(7) Cu(2) N(6) C(13) . . . . 117.7(4) no O(9) Cu(3) O(2) C(13) . . . . 175.0(4) no O(9) Cu(3) N(7) N(6) . . . . 16(3) no O(9) Cu(3) N(7) C(14) . . . . -164(2) no O(9) Cu(3) N(9) C(15) . . . . -178.7(4) no O(9) Cu(3) N(9) C(19) . . . . -5.7(7) no N(1) Cu(1) O(1) C(7) . . . . 8.0(9) no N(1) Cu(1) O(3) C(20) . . . . 84.9(5) no N(1) Cu(1) N(3) N(4) . . . . -177.6(4) no N(1) Cu(1) N(3) C(6) . . . . 17.4(5) no N(1) C(1) C(2) C(3) . . . . 1(1) no N(1) C(5) C(4) C(3) . . . . -1(1) no N(1) C(5) C(6) N(2) . . . . -170.4(6) no N(1) C(5) C(6) N(3) . . . . 8.6(8) no N(2) C(6) N(3) N(4) . . . . -4(1) no N(2) C(6) C(5) C(4) . . . . 13(1) no N(3) Cu(1) O(1) C(7) . . . . -2.5(4) no N(3) Cu(1) O(3) C(20) . . . . 150(10) no N(3) Cu(1) N(1) C(1) . . . . 168.9(6) no N(3) Cu(1) N(1) C(5) . . . . -11.3(4) no N(3) N(4) Cu(2) N(5) . . . . -165.8(6) no N(3) N(4) Cu(2) N(6) . . . . -160.2(5) no N(3) N(4) C(7) C(8) . . . . 172.3(5) no N(3) C(6) C(5) C(4) . . . . -168.3(7) no N(4) Cu(2) O(5) C(22) . . . . -67.8(5) no N(4) Cu(2) O(7) C(24) . . . . 78.4(5) no N(4) Cu(2) N(5) C(8) . . . . -0.1(5) no N(4) Cu(2) N(5) C(12) . . . . 179.5(5) no N(4) Cu(2) N(6) N(7) . . . . -174.9(5) no N(4) Cu(2) N(6) C(13) . . . . -9.9(8) no N(4) N(3) C(6) C(5) . . . . 177.2(5) no N(4) C(7) C(8) N(5) . . . . -3.9(8) no N(4) C(7) C(8) C(9) . . . . 178.2(6) no N(5) Cu(2) O(5) C(22) . . . . 18.0(7) no N(5) Cu(2) O(7) C(24) . . . . -1.6(5) no N(5) Cu(2) N(4) C(7) . . . . -2.1(5) no N(5) Cu(2) N(6) N(7) . . . . -169.3(6) no N(5) Cu(2) N(6) C(13) . . . . -4.3(4) no N(5) C(8) C(9) C(10) . . . . -1(1) no N(5) C(12) C(11) C(10) . . . . -4(1) no N(5) C(12) C(13) N(6) . . . . -4.9(8) no N(6) Cu(2) O(5) C(22) . . . . 99.7(5) no N(6) Cu(2) O(7) C(24) . . . . -84.2(5) no N(6) Cu(2) N(4) C(7) . . . . 3.5(8) no N(6) Cu(2) N(5) C(8) . . . . -177.9(5) no N(6) Cu(2) N(5) C(12) . . . . 1.6(5) no N(6) N(7) Cu(3) N(9) . . . . -179.4(4) no N(6) N(7) C(14) N(8) . . . . -2(1) no N(6) N(7) C(14) C(15) . . . . 176.7(5) no N(6) C(13) C(12) C(11) . . . . 173.6(7) no N(7) Cu(3) O(2) C(13) . . . . -5.8(4) no N(7) Cu(3) O(9) C(26) . . . . 97(2) no N(7) Cu(3) N(9) C(15) . . . . 2.7(5) no N(7) Cu(3) N(9) C(19) . . . . 175.7(6) no N(7) N(6) C(13) C(12) . . . . 176.0(5) no N(7) C(14) C(15) N(9) . . . . 5.3(8) no N(7) C(14) C(15) C(16) . . . . -172.2(7) no N(8) C(14) C(15) N(9) . . . . -176.3(6) no N(8) C(14) C(15) C(16) . . . . 6(1) no N(9) Cu(3) O(2) C(13) . . . . -22.0(9) no N(9) Cu(3) O(9) C(26) . . . . -67.6(5) no N(9) Cu(3) N(7) C(14) . . . . 0.4(5) no N(9) C(15) C(16) C(17) . . . . 1(1) no N(9) C(19) C(18) C(17) . . . . 2(1) no C(1) N(1) C(5) C(4) . . . . 2(1) no C(1) N(1) C(5) C(6) . . . . -175.4(6) no C(1) C(2) C(3) C(4) . . . . -1(1) no C(2) C(1) N(1) C(5) . . . . -1(1) no C(2) C(3) C(4) C(5) . . . . 1(1) no C(3) C(4) C(5) C(6) . . . . 175.3(7) no C(6) N(3) N(4) C(7) . . . . 168.0(6) no C(7) C(8) N(5) C(12) . . . . -177.5(6) no C(7) C(8) C(9) C(10) . . . . 176.4(7) no C(8) N(5) C(12) C(11) . . . . 2(1) no C(8) N(5) C(12) C(13) . . . . -179.4(6) no C(8) C(9) C(10) C(11) . . . . -0(1) no C(9) C(8) N(5) C(12) . . . . 1(1) no C(9) C(10) C(11) C(12) . . . . 3(1) no C(10) C(11) C(12) C(13) . . . . 178.0(6) no C(13) N(6) N(7) C(14) . . . . 175.4(6) no C(14) C(15) N(9) C(19) . . . . -178.6(6) no C(14) C(15) C(16) C(17) . . . . 178.5(7) no C(15) N(9) C(19) C(18) . . . . -1(1) no C(15) C(16) C(17) C(18) . . . . 0(1) no C(16) C(15) N(9) C(19) . . . . -1(1) no C(16) C(17) C(18) C(19) . . . . -2(1) no #------------------------------------------------------------------------------ #============================================================================== # End of CIF #============================================================================== #===END data_zl-426 _database_code_CSD 158371 #============================================================================== _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 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 14.751(2) _cell_length_b 17.692(2) _cell_length_c 9.773(1) _cell_angle_alpha 93.269(9) _cell_angle_beta 101.909(9) _cell_angle_gamma 110.253(7) _cell_volume 2318.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 299.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 26.7 _cell_measurement_theta_max 30.2 #------------------------------------------------------------------------------ _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 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1265.13 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H32 Cl4 Cu3 N10 O22 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1274.00 _exptl_absorpt_coefficient_mu 4.563 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.552 _exptl_special_details ; The scan width was (1.63+0.14tan\q)\% with an \w scan speed of 4\% per minute (up to 6 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_% 0.49 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -3 2 1 2 2 -2 -2 2 _diffrn_reflns_number 7209 _reflns_number_total 6884 _reflns_number_gt 3300 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.05460 _diffrn_reflns_av_sigmaI/netI 0.148 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 60.79 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03039 _diffrn_orient_matrix_UB_12 0.01092 _diffrn_orient_matrix_UB_13 0.10395 _diffrn_orient_matrix_UB_21 -0.06762 _diffrn_orient_matrix_UB_22 -0.02522 _diffrn_orient_matrix_UB_23 0.01822 _diffrn_orient_matrix_UB_31 0.00695 _diffrn_orient_matrix_UB_32 -0.05429 _diffrn_orient_matrix_UB_33 -0.00412 #------------------------------------------------------------------------------ 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 68 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 20 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 44 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cu 0 6 -2.019 0.589 ;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 Cu(1) -0.2130(1) 0.29032(9) 0.5858(1) 0.0454(5) 1.000 . Uani d ? Cu(2) 0.0821(1) 0.24200(8) 0.5505(1) 0.0381(4) 1.000 . Uani d ? Cu(3) 0.3748(1) 0.22979(8) 0.8257(1) 0.0431(4) 1.000 . Uani d ? Cl(1) -0.1722(2) 0.4289(2) 0.8802(3) 0.063(1) 1.000 . Uani d ? Cl(2) 0.2525(3) 0.1270(2) 1.0686(3) 0.081(1) 1.000 . Uani d ? Cl(3) 0.4590(2) 0.3580(2) 0.5844(3) 0.0568(9) 1.000 . Uani d ? Cl(4) 0.6767(3) 0.1221(2) 0.3029(4) 0.084(1) 1.000 . Uani d ? O(1) -0.0134(5) 0.1860(4) 0.6987(7) 0.052(2) 1.000 . Uani d ? O(2) 0.1708(5) 0.3311(4) 0.7175(6) 0.045(2) 1.000 . Uani d ? O(3) -0.3492(5) 0.2875(5) 0.5584(8) 0.076(3) 1.000 . Uani d ? O(4) 0.4792(5) 0.2052(4) 0.9576(7) 0.062(2) 1.000 . Uani d ? O(5) -0.273(1) 0.3995(9) 0.816(1) 0.197(7) 1.000 . Uani d ? O(6) -0.131(1) 0.5028(7) 0.949(2) 0.212(8) 1.000 . Uani d ? O(7) -0.175(1) 0.381(1) 0.989(1) 0.181(7) 1.000 . Uani d ? O(8) -0.1217(9) 0.4060(6) 0.798(1) 0.152(5) 1.000 . Uani d ? O(9) 0.2851(7) 0.1925(5) 1.1734(8) 0.094(3) 1.000 . Uani d ? O(10) 0.1740(7) 0.0619(6) 1.0867(8) 0.115(4) 1.000 . Uani d ? O(11) 0.341(1) 0.0956(8) 1.089(1) 0.177(8) 1.000 . Uani d ? O(12) 0.2421(7) 0.1458(5) 0.9371(8) 0.117(3) 1.000 . Uani d ? O(13) 0.4082(5) 0.4064(4) 0.6299(9) 0.077(3) 1.000 . Uani d ? O(14) 0.3916(5) 0.2929(5) 0.4755(8) 0.079(3) 1.000 . Uani d ? O(15) 0.5415(6) 0.4054(5) 0.5373(9) 0.091(3) 1.000 . Uani d ? O(16) 0.4946(5) 0.3226(5) 0.7055(8) 0.075(3) 1.000 . Uani d ? O(17) 0.5736(8) 0.1036(9) 0.247(2) 0.32(1) 1.000 . Uani d ? O(18) 0.696(1) 0.1173(9) 0.437(1) 0.295(9) 1.000 . Uani d ? O(19) 0.6986(7) 0.0662(6) 0.239(1) 0.121(4) 1.000 . Uani d ? O(20) 0.7378(8) 0.1998(6) 0.283(1) 0.149(5) 1.000 . Uani d ? O(21) 0.5178(6) 0.2421(6) 0.3186(9) 0.101(4) 1.000 . Uani d ? O(22) 0.6560(6) 0.3055(5) 0.0965(9) 0.096(3) 1.000 . Uani d ? N(1) -0.2312(6) 0.2164(5) 0.7329(8) 0.046(3) 1.000 . Uani d ? N(2) -0.0929(5) 0.2667(4) 0.5992(7) 0.038(2) 1.000 . Uani d ? N(3) -0.0348(5) 0.2815(4) 0.5075(7) 0.035(2) 1.000 . Uani d ? N(4) 0.1090(6) 0.3132(5) 0.3710(9) 0.051(3) 1.000 . Uani d ? N(5) -0.1711(6) 0.3734(5) 0.4619(7) 0.044(3) 1.000 . Uani d ? N(6) 0.3868(5) 0.3292(4) 0.9523(8) 0.042(2) 1.000 . Uani d ? N(7) 0.2658(5) 0.2524(4) 0.7175(7) 0.035(2) 1.000 . Uani d ? N(8) 0.1925(5) 0.2044(4) 0.6069(7) 0.035(2) 1.000 . Uani d ? N(9) 0.3539(5) 0.1402(4) 0.6698(8) 0.042(2) 1.000 . Uani d ? N(10) 0.0329(5) 0.1375(4) 0.4173(8) 0.040(2) 1.000 . Uani d ? C(1) -0.3031(8) 0.1958(7) 0.801(1) 0.056(4) 1.000 . Uani d ? C(2) -0.3061(8) 0.1440(7) 0.901(1) 0.070(4) 1.000 . Uani d ? C(3) -0.2335(9) 0.1128(7) 0.931(1) 0.070(4) 1.000 . Uani d ? C(4) -0.1550(8) 0.1356(6) 0.867(1) 0.057(4) 1.000 . Uani d ? C(5) -0.1585(7) 0.1856(6) 0.767(1) 0.042(3) 1.000 . Uani d ? C(6) -0.0804(7) 0.2123(5) 0.6876(9) 0.042(3) 1.000 . Uani d ? C(7) -0.0388(6) 0.3288(5) 0.4137(9) 0.033(3) 1.000 . Uani d ? C(8) 0.0254(7) 0.3260(6) 0.312(1) 0.044(3) 1.000 . Uani d ? C(9) -0.0035(8) 0.3254(6) 0.169(1) 0.057(4) 1.000 . Uani d ? C(10) 0.057(1) 0.3161(8) 0.086(1) 0.081(5) 1.000 . Uani d ? C(11) 0.144(1) 0.3050(8) 0.148(1) 0.081(5) 1.000 . Uani d ? C(12) 0.1664(8) 0.3055(7) 0.288(1) 0.061(4) 1.000 . Uani d ? C(13) -0.0959(8) 0.3838(5) 0.3999(9) 0.042(3) 1.000 . Uani d ? C(14) -0.0631(7) 0.4499(6) 0.328(1) 0.049(3) 1.000 . Uani d ? C(15) -0.1093(9) 0.5066(6) 0.318(1) 0.058(4) 1.000 . Uani d ? C(16) -0.1865(9) 0.4957(6) 0.380(1) 0.056(4) 1.000 . Uani d ? C(17) -0.2133(8) 0.4302(7) 0.450(1) 0.058(4) 1.000 . Uani d ? C(18) 0.4505(8) 0.3647(7) 1.078(1) 0.060(4) 1.000 . Uani d ? C(19) 0.4482(9) 0.4303(7) 1.152(1) 0.069(4) 1.000 . Uani d ? C(20) 0.3825(8) 0.4655(6) 1.098(1) 0.061(4) 1.000 . Uani d ? C(21) 0.3132(8) 0.4278(6) 0.970(1) 0.054(3) 1.000 . Uani d ? C(22) 0.3178(7) 0.3612(5) 0.9020(9) 0.040(3) 1.000 . Uani d ? C(23) 0.2437(7) 0.3141(5) 0.7693(9) 0.037(3) 1.000 . Uani d ? C(24) 0.1929(6) 0.1419(5) 0.5362(8) 0.033(3) 1.000 . Uani d ? C(25) 0.2823(6) 0.1194(5) 0.5462(9) 0.038(3) 1.000 . Uani d ? C(26) 0.2931(7) 0.0803(6) 0.426(1) 0.046(3) 1.000 . Uani d ? C(27) 0.3771(8) 0.0607(7) 0.431(1) 0.062(4) 1.000 . Uani d ? C(28) 0.4456(9) 0.0781(7) 0.555(1) 0.071(4) 1.000 . Uani d ? C(29) 0.4330(7) 0.1187(6) 0.671(1) 0.055(4) 1.000 . Uani d ? C(30) 0.0969(6) 0.0968(6) 0.4327(9) 0.037(3) 1.000 . Uani d ? C(31) 0.0670(7) 0.0182(5) 0.366(1) 0.041(3) 1.000 . Uani d ? C(32) -0.0279(8) -0.0174(6) 0.277(1) 0.051(3) 1.000 . Uani d ? C(33) -0.0898(7) 0.0247(6) 0.257(1) 0.052(3) 1.000 . Uani d ? C(34) -0.0561(7) 0.1025(6) 0.331(1) 0.051(3) 1.000 . Uani d ? H(1) -0.3516 0.2191 0.7807 0.066 1.000 . Uiso c ? H(2) -0.3603 0.1278 0.9465 0.079 1.000 . Uiso c ? H(3) -0.2341 0.0765 0.9972 0.083 1.000 . Uiso c ? H(4) -0.1001 0.1183 0.8882 0.062 1.000 . Uiso c ? H(5) -0.0645 0.3313 0.1272 0.068 1.000 . Uiso c ? H(6) 0.0425 0.3198 -0.0126 0.098 1.000 . Uiso c ? H(7) 0.1851 0.2956 0.0877 0.096 1.000 . Uiso c ? H(8) 0.2254 0.2964 0.3264 0.070 1.000 . Uiso c ? H(9) -0.0067 0.4559 0.2876 0.057 1.000 . Uiso c ? H(10) -0.0872 0.5515 0.2689 0.071 1.000 . Uiso c ? H(11) -0.2194 0.5334 0.3771 0.066 1.000 . Uiso c ? H(12) -0.2670 0.4242 0.4920 0.064 1.000 . Uiso c ? H(13) 0.5018 0.3432 1.1106 0.068 1.000 . Uiso c ? H(14) 0.4943 0.4553 1.2410 0.081 1.000 . Uiso c ? H(15) 0.3782 0.5116 1.1481 0.075 1.000 . Uiso c ? H(16) 0.2650 0.4488 0.9283 0.059 1.000 . Uiso c ? H(17) 0.2433 0.0680 0.3400 0.050 1.000 . Uiso c ? H(18) 0.3849 0.0355 0.3484 0.071 1.000 . Uiso c ? H(19) 0.5011 0.0612 0.5616 0.084 1.000 . Uiso c ? H(20) 0.4848 0.1324 0.7564 0.068 1.000 . Uiso c ? H(21) 0.1111 -0.0104 0.3805 0.044 1.000 . Uiso c ? H(22) -0.0500 -0.0720 0.2309 0.059 1.000 . Uiso c ? H(23) -0.1531 0.0023 0.1957 0.063 1.000 . Uiso c ? H(24) -0.0991 0.1328 0.3229 0.057 1.000 . Uiso c ? H(25) -0.3911 0.2567 0.6150 0.085 1.000 . Uiso c ? H(26) -0.3732 0.3177 0.4941 0.085 1.000 . Uiso c ? H(27) 0.5139 0.2380 1.0445 0.070 1.000 . Uiso c ? H(28) 0.4956 0.1588 0.9309 0.070 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 Cu(1) 0.0423(9) 0.053(1) 0.0523(9) 0.0303(8) 0.0127(8) 0.0116(8) Cu(2) 0.0352(8) 0.0379(8) 0.0450(8) 0.0214(7) 0.0052(7) 0.0006(7) Cu(3) 0.0384(8) 0.0438(9) 0.0483(9) 0.0233(7) 0.0012(7) -0.0020(7) Cl(1) 0.068(2) 0.060(2) 0.059(2) 0.026(2) 0.008(2) -0.001(2) Cl(2) 0.113(3) 0.062(2) 0.046(2) 0.009(2) 0.019(2) 0.001(2) Cl(3) 0.048(2) 0.056(2) 0.063(2) 0.015(1) 0.014(1) 0.004(1) Cl(4) 0.063(2) 0.091(3) 0.088(3) 0.019(2) 0.020(2) -0.026(2) O(1) 0.057(4) 0.063(5) 0.061(4) 0.043(4) 0.025(4) 0.024(3) O(2) 0.040(4) 0.045(4) 0.055(4) 0.028(4) 0.003(3) -0.006(3) O(3) 0.062(5) 0.084(6) 0.098(6) 0.042(5) 0.020(5) 0.033(5) O(4) 0.062(5) 0.067(5) 0.056(4) 0.033(4) -0.001(4) -0.005(4) O(5) 0.14(1) 0.21(2) 0.19(1) 0.06(1) -0.05(1) -0.02(1) O(6) 0.17(1) 0.106(8) 0.34(2) 0.023(9) 0.10(1) -0.09(1) O(7) 0.17(1) 0.28(2) 0.13(1) 0.09(1) 0.047(9) 0.10(1) O(8) 0.19(1) 0.088(8) 0.17(1) 0.009(8) 0.12(1) -0.033(7) O(9) 0.143(8) 0.064(6) 0.067(6) 0.043(6) 0.010(6) -0.023(4) O(10) 0.105(8) 0.118(9) 0.070(6) -0.027(7) 0.025(5) 0.018(6) O(11) 0.29(2) 0.16(1) 0.16(1) 0.16(1) 0.07(1) 0.04(1) O(12) 0.107(8) 0.104(7) 0.056(5) -0.040(6) -0.031(5) 0.027(5) O(13) 0.076(5) 0.051(5) 0.120(7) 0.032(4) 0.045(5) 0.001(5) O(14) 0.065(5) 0.076(6) 0.083(6) 0.018(5) 0.011(5) -0.018(4) O(15) 0.067(6) 0.097(7) 0.117(7) 0.025(5) 0.043(5) 0.033(5) O(16) 0.049(5) 0.081(6) 0.093(6) 0.023(4) 0.014(4) 0.017(5) O(17) 0.048(8) 0.21(1) 0.65(4) 0.044(9) 0.02(1) -0.15(2) O(18) 0.38(3) 0.22(2) 0.09(1) -0.11(2) 0.04(1) -0.02(1) O(19) 0.112(8) 0.107(7) 0.17(1) 0.056(7) 0.069(8) 0.014(7) O(20) 0.103(8) 0.067(7) 0.22(1) -0.011(6) -0.022(8) 0.029(7) O(21) 0.085(6) 0.144(9) 0.098(7) 0.068(6) 0.022(5) 0.045(6) O(22) 0.067(6) 0.111(7) 0.093(6) 0.020(5) 0.008(5) 0.001(5) N(1) 0.055(5) 0.040(5) 0.051(5) 0.027(4) 0.010(5) 0.004(4) N(2) 0.034(4) 0.047(5) 0.044(5) 0.026(4) 0.015(4) 0.005(4) N(3) 0.037(4) 0.031(5) 0.044(5) 0.020(4) 0.014(4) 0.010(4) N(4) 0.057(5) 0.050(5) 0.054(6) 0.025(5) 0.022(5) 0.007(4) N(5) 0.055(5) 0.047(5) 0.037(5) 0.031(5) 0.006(4) 0.003(4) N(6) 0.037(5) 0.036(5) 0.050(5) 0.018(4) -0.003(4) -0.001(4) N(7) 0.035(4) 0.040(5) 0.033(4) 0.016(4) 0.009(3) 0.004(3) N(8) 0.034(4) 0.037(5) 0.036(4) 0.017(4) 0.008(4) 0.006(4) N(9) 0.036(5) 0.038(5) 0.053(5) 0.016(4) 0.006(4) 0.003(4) N(10) 0.043(5) 0.043(5) 0.044(5) 0.030(4) 0.011(4) 0.010(4) C(1) 0.047(6) 0.063(8) 0.076(8) 0.029(6) 0.031(6) 0.021(6) C(2) 0.064(8) 0.073(8) 0.095(9) 0.033(7) 0.051(7) 0.030(7) C(3) 0.082(9) 0.09(1) 0.069(8) 0.047(8) 0.043(7) 0.036(7) C(4) 0.071(7) 0.058(8) 0.056(7) 0.038(6) 0.018(6) 0.017(6) C(5) 0.044(6) 0.048(6) 0.037(6) 0.021(5) 0.013(5) 0.004(5) C(6) 0.045(6) 0.039(6) 0.046(6) 0.023(5) 0.005(5) 0.006(5) C(7) 0.034(5) 0.025(5) 0.042(5) 0.018(4) 0.004(4) 0.006(4) C(8) 0.043(6) 0.038(6) 0.052(7) 0.019(5) 0.007(5) -0.002(5) C(9) 0.063(8) 0.054(7) 0.054(7) 0.021(6) 0.014(6) 0.001(6) C(10) 0.12(1) 0.09(1) 0.055(8) 0.042(9) 0.049(8) 0.031(7) C(11) 0.10(1) 0.08(1) 0.09(1) 0.048(9) 0.068(9) 0.035(8) C(12) 0.056(7) 0.073(8) 0.076(9) 0.037(7) 0.033(7) 0.026(7) C(13) 0.051(7) 0.036(6) 0.032(5) 0.019(5) -0.008(5) 0.003(4) C(14) 0.057(7) 0.051(7) 0.038(6) 0.026(6) -0.003(5) 0.001(5) C(15) 0.081(9) 0.047(7) 0.048(7) 0.032(7) 0.006(6) 0.007(5) C(16) 0.073(9) 0.041(7) 0.062(7) 0.035(7) 0.003(7) 0.016(6) C(17) 0.055(7) 0.076(8) 0.054(7) 0.047(7) -0.001(6) -0.009(6) C(18) 0.062(7) 0.047(7) 0.055(7) 0.020(6) -0.016(6) -0.012(6) C(19) 0.070(8) 0.065(8) 0.055(8) 0.020(7) -0.003(6) -0.011(6) C(20) 0.074(8) 0.045(6) 0.061(8) 0.022(6) 0.012(7) -0.015(6) C(21) 0.059(7) 0.044(7) 0.060(6) 0.029(6) 0.003(6) -0.014(5) C(22) 0.041(6) 0.036(6) 0.039(5) 0.013(5) 0.007(5) 0.001(4) C(23) 0.048(6) 0.034(6) 0.039(6) 0.025(5) 0.013(5) 0.006(4) C(24) 0.041(5) 0.038(6) 0.034(5) 0.025(5) 0.017(4) 0.015(4) C(25) 0.031(5) 0.040(6) 0.046(6) 0.010(4) 0.019(4) 0.010(4) C(26) 0.051(6) 0.052(7) 0.047(6) 0.031(6) 0.018(5) 0.007(5) C(27) 0.064(7) 0.076(8) 0.058(7) 0.040(6) 0.017(6) -0.001(6) C(28) 0.056(8) 0.074(8) 0.09(1) 0.041(7) 0.010(7) -0.017(7) C(29) 0.042(6) 0.051(7) 0.076(8) 0.030(6) 0.002(6) -0.004(6) C(30) 0.029(5) 0.039(6) 0.039(5) 0.011(5) 0.006(4) 0.001(5) C(31) 0.040(5) 0.034(5) 0.048(6) 0.014(4) 0.014(5) -0.002(4) C(32) 0.062(7) 0.046(7) 0.036(6) 0.014(6) 0.004(6) -0.003(5) C(33) 0.046(6) 0.039(6) 0.065(7) 0.016(5) -0.004(5) -0.001(5) C(34) 0.048(6) 0.054(7) 0.047(6) 0.019(5) 0.003(5) 0.007(5) #============================================================================== # 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) + 0.00011|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 3300 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1906 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_all 0.1850 _refine_ls_wR_factor_ref 0.2160 _refine_ls_goodness_of_fit_all 1.575 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.68 _refine_diff_density_max 0.85 #============================================================================== # 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 Cu(1) O(3) 1.95(1) . . ? Cu(1) N(1) 2.00(1) . . ? Cu(1) N(2) 1.933(9) . . ? Cu(1) N(5) 1.97(1) . . ? Cu(2) O(1) 2.259(9) . . ? Cu(2) O(2) 2.057(8) . . ? Cu(2) N(3) 2.051(9) . . ? Cu(2) N(4) 2.24(1) . . ? Cu(2) N(8) 1.95(1) . . ? Cu(2) N(10) 2.01(1) . . ? Cu(3) O(4) 1.984(9) . . ? Cu(3) N(6) 2.03(1) . . ? Cu(3) N(7) 1.912(9) . . ? Cu(3) N(9) 2.03(1) . . ? Cl(1) O(5) 1.35(2) . . ? Cl(1) O(6) 1.29(2) . . ? Cl(1) O(7) 1.37(2) . . ? Cl(1) O(8) 1.34(1) . . ? Cl(2) O(9) 1.38(1) . . ? Cl(2) O(10) 1.36(1) . . ? Cl(2) O(11) 1.58(2) . . ? Cl(2) O(12) 1.33(1) . . ? Cl(3) O(13) 1.43(1) . . ? Cl(3) O(14) 1.43(1) . . ? Cl(3) O(15) 1.40(1) . . ? Cl(3) O(16) 1.44(1) . . ? Cl(4) O(17) 1.39(2) . . ? Cl(4) O(18) 1.32(2) . . ? Cl(4) O(19) 1.31(1) . . ? Cl(4) O(20) 1.41(1) . . ? O(1) C(6) 1.23(1) . . ? O(2) C(23) 1.24(1) . . ? O(3) H(25) 0.97 . . no O(3) H(26) 0.94 . . no O(4) H(27) 0.94 . . no O(4) H(28) 0.96 . . no N(1) C(1) 1.29(2) . . ? N(1) C(5) 1.34(2) . . ? N(2) N(3) 1.35(1) . . ? N(2) C(6) 1.36(1) . . ? N(3) C(7) 1.29(1) . . ? N(4) C(8) 1.36(2) . . ? N(4) C(12) 1.34(2) . . ? N(5) C(13) 1.33(2) . . ? N(5) C(17) 1.35(2) . . ? N(6) C(18) 1.34(2) . . ? N(6) C(22) 1.35(1) . . ? N(7) N(8) 1.35(1) . . ? N(7) C(23) 1.34(1) . . ? N(8) C(24) 1.27(1) . . ? N(9) C(25) 1.36(1) . . ? N(9) C(29) 1.34(2) . . ? N(10) C(30) 1.36(1) . . ? N(10) C(34) 1.31(2) . . ? C(1) C(2) 1.41(2) . . ? C(1) H(1) 0.95 . . no C(2) C(3) 1.36(2) . . ? C(2) H(2) 0.96 . . no C(3) C(4) 1.38(2) . . ? C(3) H(3) 0.95 . . no C(4) C(5) 1.35(2) . . ? C(4) H(4) 0.95 . . no C(5) C(6) 1.45(2) . . ? C(7) C(8) 1.50(2) . . ? C(7) C(13) 1.48(2) . . ? C(8) C(9) 1.38(2) . . ? C(9) C(10) 1.38(2) . . ? C(9) H(5) 0.96 . . no C(10) C(11) 1.36(2) . . ? C(10) H(6) 0.95 . . no C(11) C(12) 1.35(2) . . ? C(11) H(7) 0.95 . . no C(12) H(8) 0.94 . . no C(13) C(14) 1.39(2) . . ? C(14) C(15) 1.38(2) . . ? C(14) H(9) 0.97 . . no C(15) C(16) 1.36(2) . . ? C(15) H(10) 0.94 . . no C(16) C(17) 1.36(2) . . ? C(16) H(11) 0.96 . . no C(17) H(12) 0.96 . . no C(18) C(19) 1.39(2) . . ? C(18) H(13) 0.96 . . no C(19) C(20) 1.37(2) . . ? C(19) H(14) 0.94 . . no C(20) C(21) 1.39(2) . . ? C(20) H(15) 0.94 . . no C(21) C(22) 1.35(2) . . ? C(21) H(16) 0.96 . . no C(22) C(23) 1.48(2) . . ? C(24) C(25) 1.49(2) . . ? C(24) C(30) 1.49(2) . . ? C(25) C(26) 1.40(2) . . ? C(26) C(27) 1.38(2) . . ? C(26) H(17) 0.96 . . no C(27) C(28) 1.35(2) . . ? C(27) H(18) 0.94 . . no C(28) C(29) 1.40(2) . . ? C(28) H(19) 0.96 . . no C(29) H(20) 0.96 . . no C(30) C(31) 1.38(2) . . ? C(31) C(32) 1.39(2) . . ? C(31) H(21) 0.95 . . no C(32) C(33) 1.35(2) . . ? C(32) H(22) 0.95 . . no C(33) C(34) 1.40(2) . . ? C(33) H(23) 0.95 . . no C(34) H(24) 0.96 . . 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(3) Cu(1) N(1) 92.2(4) . . . ? O(3) Cu(1) N(2) 167.0(5) . . . ? O(3) Cu(1) N(5) 95.9(4) . . . ? N(1) Cu(1) N(2) 81.5(5) . . . ? N(1) Cu(1) N(5) 169.8(5) . . . ? N(2) Cu(1) N(5) 91.8(4) . . . ? O(1) Cu(2) O(2) 87.0(4) . . . ? O(1) Cu(2) N(3) 75.3(4) . . . ? O(1) Cu(2) N(4) 151.3(4) . . . ? O(1) Cu(2) N(8) 100.5(4) . . . ? O(1) Cu(2) N(10) 93.4(4) . . . ? O(2) Cu(2) N(3) 97.4(4) . . . ? O(2) Cu(2) N(4) 99.7(4) . . . ? O(2) Cu(2) N(8) 79.7(4) . . . ? O(2) Cu(2) N(10) 158.8(4) . . . ? N(3) Cu(2) N(4) 76.1(4) . . . ? N(3) Cu(2) N(8) 175.1(4) . . . ? N(3) Cu(2) N(10) 103.2(4) . . . ? N(4) Cu(2) N(8) 108.2(4) . . . ? N(4) Cu(2) N(10) 90.1(4) . . . ? N(8) Cu(2) N(10) 79.4(4) . . . ? O(4) Cu(3) N(6) 95.3(4) . . . ? O(4) Cu(3) N(7) 172.9(4) . . . ? O(4) Cu(3) N(9) 94.1(4) . . . ? N(6) Cu(3) N(7) 81.1(4) . . . ? N(6) Cu(3) N(9) 169.5(4) . . . ? N(7) Cu(3) N(9) 90.1(4) . . . ? O(5) Cl(1) O(6) 116(1) . . . ? O(5) Cl(1) O(7) 100(1) . . . ? O(5) Cl(1) O(8) 111(1) . . . ? O(6) Cl(1) O(7) 107(1) . . . ? O(6) Cl(1) O(8) 116(1) . . . ? O(7) Cl(1) O(8) 105(1) . . . ? O(9) Cl(2) O(10) 113.8(9) . . . ? O(9) Cl(2) O(11) 103(1) . . . ? O(9) Cl(2) O(12) 116.2(8) . . . ? O(10) Cl(2) O(11) 105(1) . . . ? O(10) Cl(2) O(12) 114.3(8) . . . ? O(11) Cl(2) O(12) 103(1) . . . ? O(13) Cl(3) O(14) 110.1(7) . . . ? O(13) Cl(3) O(15) 111.9(7) . . . ? O(13) Cl(3) O(16) 107.9(7) . . . ? O(14) Cl(3) O(15) 109.7(8) . . . ? O(14) Cl(3) O(16) 108.6(7) . . . ? O(15) Cl(3) O(16) 108.6(7) . . . ? O(17) Cl(4) O(18) 113(2) . . . ? O(17) Cl(4) O(19) 106(1) . . . ? O(17) Cl(4) O(20) 113(1) . . . ? O(18) Cl(4) O(19) 106(2) . . . ? O(18) Cl(4) O(20) 108(1) . . . ? O(19) Cl(4) O(20) 111(1) . . . ? Cu(2) O(1) C(6) 108.7(8) . . . ? Cu(2) O(2) C(23) 108.6(8) . . . ? Cu(1) O(3) H(25) 119.3 . . . no Cu(1) O(3) H(26) 121.5 . . . no H(25) O(3) H(26) 119.1 . . . no Cu(3) O(4) H(27) 120.9 . . . no Cu(3) O(4) H(28) 119.6 . . . no H(27) O(4) H(28) 119.5 . . . no Cu(1) N(1) C(1) 128(1) . . . ? Cu(1) N(1) C(5) 113.6(9) . . . ? C(1) N(1) C(5) 119(1) . . . ? Cu(1) N(2) N(3) 126.0(8) . . . ? Cu(1) N(2) C(6) 116.1(9) . . . ? N(3) N(2) C(6) 115(1) . . . ? Cu(2) N(3) N(2) 115.1(7) . . . ? Cu(2) N(3) C(7) 120.0(8) . . . ? N(2) N(3) C(7) 124(1) . . . ? Cu(2) N(4) C(8) 108.5(9) . . . ? Cu(2) N(4) C(12) 124(1) . . . ? C(8) N(4) C(12) 118(1) . . . ? Cu(1) N(5) C(13) 124.6(9) . . . ? Cu(1) N(5) C(17) 119(1) . . . ? C(13) N(5) C(17) 116(1) . . . ? Cu(3) N(6) C(18) 128.5(9) . . . ? Cu(3) N(6) C(22) 112.9(8) . . . ? C(18) N(6) C(22) 119(1) . . . ? Cu(3) N(7) N(8) 128.1(8) . . . ? Cu(3) N(7) C(23) 118.5(8) . . . ? N(8) N(7) C(23) 112(1) . . . ? Cu(2) N(8) N(7) 114.6(7) . . . ? Cu(2) N(8) C(24) 119.6(8) . . . ? N(7) N(8) C(24) 126(1) . . . ? Cu(3) N(9) C(25) 124.7(9) . . . ? Cu(3) N(9) C(29) 115.4(9) . . . ? C(25) N(9) C(29) 117(1) . . . ? Cu(2) N(10) C(30) 113.8(8) . . . ? Cu(2) N(10) C(34) 126.5(9) . . . ? C(30) N(10) C(34) 119(1) . . . ? N(1) C(1) C(2) 122(1) . . . ? N(1) C(1) H(1) 120.1 . . . no C(2) C(1) H(1) 117.5 . . . no C(1) C(2) C(3) 117(1) . . . ? C(1) C(2) H(2) 121.3 . . . no C(3) C(2) H(2) 121.7 . . . no C(2) C(3) C(4) 121(2) . . . ? C(2) C(3) H(3) 118.7 . . . no C(4) C(3) H(3) 120.1 . . . no C(3) C(4) C(5) 117(1) . . . ? C(3) C(4) H(4) 121.6 . . . no C(5) C(4) H(4) 121.4 . . . no N(1) C(5) C(4) 123(1) . . . ? N(1) C(5) C(6) 115(1) . . . ? C(4) C(5) C(6) 121(1) . . . ? O(1) C(6) N(2) 124(1) . . . ? O(1) C(6) C(5) 123(1) . . . ? N(2) C(6) C(5) 113(1) . . . ? N(3) C(7) C(8) 112(1) . . . ? N(3) C(7) C(13) 127(1) . . . ? C(8) C(7) C(13) 121(1) . . . ? N(4) C(8) C(7) 115(1) . . . ? N(4) C(8) C(9) 120(1) . . . ? C(7) C(8) C(9) 125(1) . . . ? C(8) C(9) C(10) 120(2) . . . ? C(8) C(9) H(5) 119.6 . . . no C(10) C(9) H(5) 120.4 . . . no C(9) C(10) C(11) 120(2) . . . ? C(9) C(10) H(6) 120.2 . . . no C(11) C(10) H(6) 120.2 . . . no C(10) C(11) C(12) 118(2) . . . ? C(10) C(11) H(7) 120.2 . . . no C(12) C(11) H(7) 121.7 . . . no N(4) C(12) C(11) 124(2) . . . ? N(4) C(12) H(8) 118.7 . . . no C(11) C(12) H(8) 117.2 . . . no N(5) C(13) C(7) 122(1) . . . ? N(5) C(13) C(14) 121(1) . . . ? C(7) C(13) C(14) 117(1) . . . ? C(13) C(14) C(15) 121(1) . . . ? C(13) C(14) H(9) 118.7 . . . no C(15) C(14) H(9) 120.1 . . . no C(14) C(15) C(16) 118(1) . . . ? C(14) C(15) H(10) 122.7 . . . no C(16) C(15) H(10) 119.5 . . . no C(15) C(16) C(17) 118(1) . . . ? C(15) C(16) H(11) 122.6 . . . no C(17) C(16) H(11) 119.7 . . . no N(5) C(17) C(16) 126(1) . . . ? N(5) C(17) H(12) 117.0 . . . no C(16) C(17) H(12) 116.6 . . . no N(6) C(18) C(19) 122(1) . . . ? N(6) C(18) H(13) 118.4 . . . no C(19) C(18) H(13) 119.4 . . . no C(18) C(19) C(20) 119(1) . . . ? C(18) C(19) H(14) 121.0 . . . no C(20) C(19) H(14) 119.7 . . . no C(19) C(20) C(21) 118(1) . . . ? C(19) C(20) H(15) 121.3 . . . no C(21) C(20) H(15) 121.0 . . . no C(20) C(21) C(22) 121(1) . . . ? C(20) C(21) H(16) 120.9 . . . no C(22) C(21) H(16) 118.0 . . . no N(6) C(22) C(21) 121(1) . . . ? N(6) C(22) C(23) 115(1) . . . ? C(21) C(22) C(23) 124(1) . . . ? O(2) C(23) N(7) 125(1) . . . ? O(2) C(23) C(22) 122(1) . . . ? N(7) C(23) C(22) 113(1) . . . ? N(8) C(24) C(25) 124(1) . . . ? N(8) C(24) C(30) 113(1) . . . ? C(25) C(24) C(30) 123(1) . . . ? N(9) C(25) C(24) 120(1) . . . ? N(9) C(25) C(26) 121(1) . . . ? C(24) C(25) C(26) 119(1) . . . ? C(25) C(26) C(27) 121(1) . . . ? C(25) C(26) H(17) 119.7 . . . no C(27) C(26) H(17) 119.7 . . . no C(26) C(27) C(28) 119(1) . . . ? C(26) C(27) H(18) 121.1 . . . no C(28) C(27) H(18) 120.4 . . . no C(27) C(28) C(29) 119(1) . . . ? C(27) C(28) H(19) 120.7 . . . no C(29) C(28) H(19) 120.1 . . . no N(9) C(29) C(28) 124(1) . . . ? N(9) C(29) H(20) 118.7 . . . no C(28) C(29) H(20) 117.5 . . . no N(10) C(30) C(24) 114(1) . . . ? N(10) C(30) C(31) 120(1) . . . ? C(24) C(30) C(31) 126(1) . . . ? C(30) C(31) C(32) 120(1) . . . ? C(30) C(31) H(21) 119.8 . . . no C(32) C(31) H(21) 120.6 . . . no C(31) C(32) C(33) 119(1) . . . ? C(31) C(32) H(22) 120.8 . . . no C(33) C(32) H(22) 120.0 . . . no C(32) C(33) C(34) 119(1) . . . ? C(32) C(33) H(23) 121.3 . . . no C(34) C(33) H(23) 120.1 . . . no N(10) C(34) C(33) 123(1) . . . ? N(10) C(34) H(24) 117.6 . . . no C(33) C(34) H(24) 119.3 . . . 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 Cu(1) O(8) 2.61(1) . . no Cu(1) O(18) 3.04(2) . 1_455 no Cu(1) O(20) 3.10(2) . 1_455 no Cu(1) O(5) 3.33(2) . . no Cu(1) Cl(1) 3.479(5) . . no Cu(3) O(12) 2.51(1) . . no Cu(3) O(16) 2.51(1) . . no Cu(3) Cl(3) 3.482(5) . . no Cu(3) Cl(2) 3.488(5) . . no Cu(3) O(11) 3.58(2) . . no Cl(2) O(4) 3.58(1) . . no Cl(3) N(7) 3.38(1) . . no Cl(3) O(3) 3.51(1) . 1_655 no O(1) C(32) 3.25(2) . 2_556 no O(1) C(31) 3.42(2) . 2_556 no O(2) C(16) 3.20(2) . 2_566 no O(2) C(15) 3.33(2) . 2_566 no O(2) O(13) 3.59(1) . . no O(3) O(21) 2.61(2) . 1_455 no O(3) O(5) 2.89(2) . . no O(3) O(15) 3.03(1) . 1_455 no O(3) O(16) 3.17(1) . 1_455 no O(3) O(18) 3.54(3) . 1_455 no O(3) O(8) 3.54(2) . . no O(4) O(22) 2.61(1) . 1_556 no O(4) O(11) 2.85(2) . . no O(4) O(12) 3.25(2) . . no O(4) O(16) 3.32(1) . . no O(4) O(21) 3.44(2) . 1_556 no O(5) O(16) 3.18(2) . 1_455 no O(5) C(20) 3.44(2) . 2_567 no O(5) O(22) 3.48(3) . 1_456 no O(5) O(15) 3.49(2) . 1_455 no O(5) C(1) 3.50(3) . . no O(6) C(10) 3.04(3) . 2_566 no O(6) C(9) 3.37(3) . 2_566 no O(6) C(21) 3.54(2) . 2_567 no O(6) C(11) 3.59(3) . 2_566 no O(7) O(22) 2.86(2) . 1_456 no O(7) C(9) 3.27(2) . 1_556 no O(7) C(1) 3.34(3) . . no O(7) C(14) 3.36(2) . 1_556 no O(7) N(1) 3.45(2) . . no O(7) C(15) 3.58(2) . 1_556 no O(8) N(1) 3.14(2) . . no O(8) N(5) 3.19(2) . . no O(8) N(2) 3.24(2) . . no O(8) C(17) 3.51(2) . . no O(8) C(14) 3.51(2) . 2_566 no O(9) O(14) 3.14(1) . 1_556 no O(9) O(21) 3.19(2) . 1_556 no O(9) C(26) 3.26(2) . 1_556 no O(9) C(11) 3.34(2) . 1_556 no O(9) C(12) 3.35(2) . 1_556 no O(9) N(6) 3.49(2) . . no O(9) C(18) 3.50(2) . . no O(10) C(26) 3.36(2) . 1_556 no O(10) C(33) 3.42(2) . 2_556 no O(10) C(31) 3.42(2) . 1_556 no O(10) C(4) 3.52(2) . 2_557 no O(10) C(3) 3.53(2) . 2_557 no O(11) O(21) 3.28(3) . 1_556 no O(11) C(27) 3.40(2) . 1_556 no O(11) O(17) 3.44(3) . 1_556 no O(11) C(3) 3.48(3) . 2_557 no O(11) C(26) 3.53(2) . 1_556 no O(12) N(7) 2.94(1) . . no O(12) N(6) 3.20(2) . . no O(12) C(33) 3.25(2) . 2_556 no O(12) C(32) 3.35(2) . 2_556 no O(12) N(9) 3.37(2) . . no O(12) N(8) 3.45(1) . . no O(12) C(23) 3.49(2) . . no O(13) C(23) 3.03(2) . . no O(13) N(7) 3.10(1) . . no O(13) C(22) 3.24(2) . . no O(13) C(19) 3.24(2) . 2_667 no O(13) N(6) 3.54(2) . . no O(13) C(20) 3.60(2) . 2_667 no O(14) O(21) 2.96(2) . . no O(14) C(25) 3.13(2) . . no O(14) N(7) 3.27(1) . . no O(14) N(9) 3.35(2) . . no O(14) N(8) 3.39(1) . . no O(14) C(24) 3.41(2) . . no O(14) C(26) 3.50(2) . . no O(14) C(12) 3.55(2) . . no O(15) O(21) 3.36(2) . . no O(16) N(9) 3.13(1) . . no O(16) N(6) 3.18(2) . . no O(16) N(7) 3.20(1) . . no O(16) C(29) 3.39(2) . . no O(17) O(21) 2.94(2) . . no O(18) N(1) 3.07(2) . 1_655 no O(18) N(2) 3.30(2) . 1_655 no O(18) C(5) 3.35(2) . 1_655 no O(18) C(27) 3.35(3) . 2_656 no O(18) C(28) 3.37(3) . 2_656 no O(18) C(6) 3.43(3) . 1_655 no O(19) C(34) 3.38(2) . 1_655 no O(19) C(29) 3.43(2) . 2_656 no O(19) C(33) 3.44(2) . 1_655 no O(19) C(3) 3.45(2) . 1_654 no O(20) O(22) 3.06(2) . . no O(20) N(5) 3.14(2) . 1_655 no O(20) C(7) 3.24(2) . 1_655 no O(20) C(13) 3.29(2) . 1_655 no O(20) N(3) 3.38(2) . 1_655 no O(20) N(2) 3.41(2) . 1_655 no O(21) O(22) 3.26(2) . . no O(21) C(18) 3.52(2) . 1_554 no O(21) C(27) 3.54(2) . . no O(22) C(18) 3.49(2) . 1_554 no C(1) C(29) 3.59(2) . 1_455 no C(7) C(15) 3.53(2) . 2_566 no C(11) C(21) 3.52(2) . 1_554 no C(13) C(15) 3.51(2) . 2_566 no C(14) C(14) 3.52(3) . 2_566 no C(24) C(32) 3.56(2) . 2_556 no C(30) C(32) 3.41(2) . 2_556 no C(30) C(31) 3.58(2) . 2_556 no C(31) C(31) 3.55(3) . 2_556 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 Cu(1) N(1) C(1) C(2) . . . . 180(1) no Cu(1) N(1) C(5) C(4) . . . . 179(1) no Cu(1) N(1) C(5) C(6) . . . . -1(2) no Cu(1) N(2) N(3) Cu(2) . . . . -176.3(5) no Cu(1) N(2) N(3) C(7) . . . . 16(2) no Cu(1) N(2) C(6) O(1) . . . . 174(1) no Cu(1) N(2) C(6) C(5) . . . . -5(1) no Cu(1) N(5) C(13) C(7) . . . . 3(2) no Cu(1) N(5) C(13) C(14) . . . . -172.2(9) no Cu(1) N(5) C(17) C(16) . . . . 173(1) no Cu(2) O(1) C(6) N(2) . . . . -1(2) no Cu(2) O(1) C(6) C(5) . . . . 178(1) no Cu(2) O(2) C(23) N(7) . . . . 4(2) no Cu(2) O(2) C(23) C(22) . . . . -173(1) no Cu(2) N(3) N(2) C(6) . . . . -15(1) no Cu(2) N(3) C(7) C(8) . . . . 20(1) no Cu(2) N(3) C(7) C(13) . . . . -159(1) no Cu(2) N(4) C(8) C(7) . . . . 28(1) no Cu(2) N(4) C(8) C(9) . . . . -144(1) no Cu(2) N(4) C(12) C(11) . . . . 140(2) no Cu(2) N(8) N(7) Cu(3) . . . . 169.0(5) no Cu(2) N(8) N(7) C(23) . . . . 3(1) no Cu(2) N(8) C(24) C(25) . . . . 163.8(9) no Cu(2) N(8) C(24) C(30) . . . . -12(1) no Cu(2) N(10) C(30) C(24) . . . . -5(1) no Cu(2) N(10) C(30) C(31) . . . . 170(1) no Cu(2) N(10) C(34) C(33) . . . . -170(1) no Cu(3) N(6) C(18) C(19) . . . . -179(1) no Cu(3) N(6) C(22) C(21) . . . . -179(1) no Cu(3) N(6) C(22) C(23) . . . . 3(2) no Cu(3) N(7) N(8) C(24) . . . . -16(2) no Cu(3) N(7) C(23) O(2) . . . . -173(1) no Cu(3) N(7) C(23) C(22) . . . . 5(2) no Cu(3) N(9) C(25) C(24) . . . . -21(2) no Cu(3) N(9) C(25) C(26) . . . . 157(1) no Cu(3) N(9) C(29) C(28) . . . . -160(1) no O(1) Cu(2) O(2) C(23) . . . . 99.6(9) no O(1) Cu(2) N(3) N(2) . . . . 10.6(7) no O(1) Cu(2) N(3) C(7) . . . . 179(1) no O(1) Cu(2) N(4) C(8) . . . . -8(2) no O(1) Cu(2) N(4) C(12) . . . . -153(1) no O(1) Cu(2) N(8) N(7) . . . . -86.0(8) no O(1) Cu(2) N(8) C(24) . . . . 99(1) no O(1) Cu(2) N(10) C(30) . . . . -100.2(9) no O(1) Cu(2) N(10) C(34) . . . . 72(1) no O(1) C(6) N(2) N(3) . . . . 11(2) no O(1) C(6) C(5) N(1) . . . . -175(1) no O(1) C(6) C(5) C(4) . . . . 5(2) no O(2) Cu(2) O(1) C(6) . . . . 93.3(9) no O(2) Cu(2) N(3) N(2) . . . . -74.3(8) no O(2) Cu(2) N(3) C(7) . . . . 94(1) no O(2) Cu(2) N(4) C(8) . . . . -109.2(9) no O(2) Cu(2) N(4) C(12) . . . . 105(1) no O(2) Cu(2) N(8) N(7) . . . . -1.1(8) no O(2) Cu(2) N(8) C(24) . . . . -176(1) no O(2) Cu(2) N(10) C(30) . . . . -10(2) no O(2) Cu(2) N(10) C(34) . . . . 163(1) no O(2) C(23) N(7) N(8) . . . . -5(2) no O(2) C(23) C(22) N(6) . . . . 173(1) no O(2) C(23) C(22) C(21) . . . . -6(2) no O(3) Cu(1) N(1) C(1) . . . . -15(1) no O(3) Cu(1) N(1) C(5) . . . . 167(1) no O(3) Cu(1) N(2) N(3) . . . . 104(2) no O(3) Cu(1) N(2) C(6) . . . . -58(2) no O(3) Cu(1) N(5) C(13) . . . . -157(1) no O(3) Cu(1) N(5) C(17) . . . . 31(1) no O(4) Cu(3) N(6) C(18) . . . . 4(1) no O(4) Cu(3) N(6) C(22) . . . . -174.3(9) no O(4) Cu(3) N(7) N(8) . . . . -108(3) no O(4) Cu(3) N(7) C(23) . . . . 56(4) no O(4) Cu(3) N(9) C(25) . . . . 175(1) no O(4) Cu(3) N(9) C(29) . . . . -26(1) no N(1) Cu(1) N(2) N(3) . . . . 165(1) no N(1) Cu(1) N(2) C(6) . . . . 3.8(9) no N(1) Cu(1) N(5) C(13) . . . . 61(3) no N(1) Cu(1) N(5) C(17) . . . . -111(3) no N(1) C(1) C(2) C(3) . . . . 1(3) no N(1) C(5) C(4) C(3) . . . . 2(2) no N(1) C(5) C(6) N(2) . . . . 4(2) no N(2) Cu(1) N(1) C(1) . . . . 177(1) no N(2) Cu(1) N(1) C(5) . . . . -1(1) no N(2) Cu(1) N(5) C(13) . . . . 13(1) no N(2) Cu(1) N(5) C(17) . . . . -159(1) no N(2) N(3) Cu(2) N(4) . . . . -172.5(9) no N(2) N(3) Cu(2) N(8) . . . . -20(6) no N(2) N(3) Cu(2) N(10) . . . . 100.7(8) no N(2) N(3) C(7) C(8) . . . . -173(1) no N(2) N(3) C(7) C(13) . . . . 8(2) no N(2) C(6) C(5) C(4) . . . . -176(1) no N(3) Cu(2) O(1) C(6) . . . . -5.2(9) no N(3) Cu(2) O(2) C(23) . . . . 174.4(9) no N(3) Cu(2) N(4) C(8) . . . . -13.9(9) no N(3) Cu(2) N(4) C(12) . . . . -159(1) no N(3) Cu(2) N(8) N(7) . . . . -56(5) no N(3) Cu(2) N(8) C(24) . . . . 129(5) no N(3) Cu(2) N(10) C(30) . . . . -175.9(9) no N(3) Cu(2) N(10) C(34) . . . . -4(1) no N(3) N(2) Cu(1) N(5) . . . . -23(1) no N(3) N(2) C(6) C(5) . . . . -169(1) no N(3) C(7) C(8) N(4) . . . . -33(2) no N(3) C(7) C(8) C(9) . . . . 139(1) no N(3) C(7) C(13) N(5) . . . . -18(2) no N(3) C(7) C(13) C(14) . . . . 157(1) no N(4) Cu(2) O(1) C(6) . . . . -11(1) no N(4) Cu(2) O(2) C(23) . . . . -108.5(9) no N(4) Cu(2) N(3) C(7) . . . . -4.2(9) no N(4) Cu(2) N(8) N(7) . . . . 95.8(8) no N(4) Cu(2) N(8) C(24) . . . . -80(1) no N(4) Cu(2) N(10) C(30) . . . . 108.3(9) no N(4) Cu(2) N(10) C(34) . . . . -79(1) no N(4) C(8) C(7) C(13) . . . . 146(1) no N(4) C(8) C(9) C(10) . . . . -4(2) no N(4) C(12) C(11) C(10) . . . . 1(3) no N(5) Cu(1) N(1) C(1) . . . . 127(3) no N(5) Cu(1) N(1) C(5) . . . . -51(3) no N(5) Cu(1) N(2) C(6) . . . . 176.1(9) no N(5) C(13) C(7) C(8) . . . . 163(1) no N(5) C(13) C(14) C(15) . . . . -0(2) no N(5) C(17) C(16) C(15) . . . . -2(2) no N(6) Cu(3) N(7) N(8) . . . . -167(1) no N(6) Cu(3) N(7) C(23) . . . . -2.6(9) no N(6) Cu(3) N(9) C(25) . . . . -32(3) no N(6) Cu(3) N(9) C(29) . . . . 127(2) no N(6) C(18) C(19) C(20) . . . . -2(3) no N(6) C(22) C(21) C(20) . . . . -2(2) no N(6) C(22) C(23) N(7) . . . . -5(2) no N(7) Cu(3) N(6) C(18) . . . . 178(1) no N(7) Cu(3) N(6) C(22) . . . . -0.4(9) no N(7) Cu(3) N(9) C(25) . . . . 1(1) no N(7) Cu(3) N(9) C(29) . . . . 160(1) no N(7) N(8) Cu(2) N(10) . . . . -177.6(9) no N(7) N(8) C(24) C(25) . . . . -11(2) no N(7) N(8) C(24) C(30) . . . . 174(1) no N(7) C(23) C(22) C(21) . . . . 177(1) no N(8) Cu(2) O(1) C(6) . . . . 172.2(9) no N(8) Cu(2) O(2) C(23) . . . . -1.6(9) no N(8) Cu(2) N(3) C(7) . . . . 148(5) no N(8) Cu(2) N(4) C(8) . . . . 168.5(9) no N(8) Cu(2) N(4) C(12) . . . . 23(1) no N(8) Cu(2) N(10) C(30) . . . . -0.2(9) no N(8) Cu(2) N(10) C(34) . . . . 172(1) no N(8) N(7) Cu(3) N(9) . . . . 18(1) no N(8) N(7) C(23) C(22) . . . . 172(1) no N(8) C(24) C(25) N(9) . . . . 30(2) no N(8) C(24) C(25) C(26) . . . . -148(1) no N(8) C(24) C(30) N(10) . . . . 11(2) no N(8) C(24) C(30) C(31) . . . . -164(1) no N(9) Cu(3) N(6) C(18) . . . . -149(2) no N(9) Cu(3) N(6) C(22) . . . . 32(3) no N(9) Cu(3) N(7) C(23) . . . . -177(1) no N(9) C(25) C(24) C(30) . . . . -155(1) no N(9) C(25) C(26) C(27) . . . . 1(2) no N(9) C(29) C(28) C(27) . . . . 1(3) no N(10) Cu(2) O(1) C(6) . . . . -108.0(9) no N(10) Cu(2) O(2) C(23) . . . . 8(2) no N(10) Cu(2) N(3) C(7) . . . . -91(1) no N(10) Cu(2) N(4) C(8) . . . . 89.7(9) no N(10) Cu(2) N(4) C(12) . . . . -56(1) no N(10) Cu(2) N(8) C(24) . . . . 7(1) no N(10) C(30) C(24) C(25) . . . . -165(1) no N(10) C(30) C(31) C(32) . . . . 3(2) no N(10) C(34) C(33) C(32) . . . . 1(2) no C(1) N(1) C(5) C(4) . . . . 1(2) no C(1) N(1) C(5) C(6) . . . . -180(1) no C(1) C(2) C(3) C(4) . . . . 1(3) no C(2) C(1) N(1) C(5) . . . . -2(2) no C(2) C(3) C(4) C(5) . . . . -3(3) no C(3) C(4) C(5) C(6) . . . . -178(1) no C(6) N(2) N(3) C(7) . . . . 177(1) no C(7) C(8) N(4) C(12) . . . . 176(1) no C(7) C(8) C(9) C(10) . . . . -175(1) no C(7) C(13) N(5) C(17) . . . . 176(1) no C(7) C(13) C(14) C(15) . . . . -176(1) no C(8) N(4) C(12) C(11) . . . . -2(2) no C(8) C(7) C(13) C(14) . . . . -22(2) no C(8) C(9) C(10) C(11) . . . . 2(3) no C(9) C(8) N(4) C(12) . . . . 4(2) no C(9) C(8) C(7) C(13) . . . . -42(2) no C(9) C(10) C(11) C(12) . . . . -1(3) no C(13) N(5) C(17) C(16) . . . . 1(2) no C(13) C(14) C(15) C(16) . . . . -1(2) no C(14) C(13) N(5) C(17) . . . . 0(2) no C(14) C(15) C(16) C(17) . . . . 1(2) no C(18) N(6) C(22) C(21) . . . . 3(2) no C(18) N(6) C(22) C(23) . . . . -176(1) no C(18) C(19) C(20) C(21) . . . . 2(3) no C(19) C(18) N(6) C(22) . . . . -0(2) no C(19) C(20) C(21) C(22) . . . . -0(2) no C(20) C(21) C(22) C(23) . . . . 176(1) no C(23) N(7) N(8) C(24) . . . . 178(1) no C(24) C(25) N(9) C(29) . . . . -180(1) no C(24) C(25) C(26) C(27) . . . . 179(1) no C(24) C(30) N(10) C(34) . . . . -178(1) no C(24) C(30) C(31) C(32) . . . . 177(1) no C(25) N(9) C(29) C(28) . . . . 1(2) no C(25) C(24) C(30) C(31) . . . . 21(2) no C(25) C(26) C(27) C(28) . . . . 1(2) no C(26) C(25) N(9) C(29) . . . . -2(2) no C(26) C(25) C(24) C(30) . . . . 27(2) no C(26) C(27) C(28) C(29) . . . . -2(3) no C(30) N(10) C(34) C(33) . . . . 2(2) no C(30) C(31) C(32) C(33) . . . . -0(2) no C(31) C(30) N(10) C(34) . . . . -3(2) no C(31) C(32) C(33) C(34) . . . . -2(2) no #------------------------------------------------------------------------------ #============================================================================== # End of CIF #==============================================================================