Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_k014 _database_code_CSD 174283 #------------------------------------------------------------------------------ _journal_coden_Cambridge 186 _audit_creation_date '2001-05-15' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal 'Dalton' _publ_contact_author_name 'Leone Spiccia' _publ_contact_author_address ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; _publ_contact_author_fax '+61 3 9905 4597' _publ_contact_author_email 'leone.spiccia@sci.monash.edu.au' loop_ _publ_author_name _publ_author_address 'Bim Graham' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Leone Spiccia' ;School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Gary D. Fallon' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Milton T. W. Hearn' ; Centre for Bioprocess Technology Department of Biochemistry P.O. Box 130 Monash University Victoria 3800 Australia ; 'Frank E. Mabbs' ; Department of Chemistry University of Manchester Manchester M13 9PL UK ; 'Boujemaa Moubaraki' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Keith S. Murray' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; _publ_section_title ; Structure and Magnetic Properties of Tri- and Hexa-nuclear Hydroxo- Bridged Copper(II) Complexes Formed by a Trimacrocyclic Derivative of 1,4,7-Triazacyclononane ; #------------------------------------------------------------------------------ _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'teXsan (MSC, 1992-1997)' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.1020(5) _cell_length_b 13.6888(7) _cell_length_c 17.053(1) _cell_angle_alpha 67.028(1) _cell_angle_beta 72.983(1) _cell_angle_gamma 67.912(1) _cell_volume 2374.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(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 'acicular' _exptl_crystal_colour 'aqua' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1217.89 _chemical_formula_analytical ? _chemical_formula_sum 'C27 H63.40 Cl4 Cu3 N9 O23.20 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1258.00 _exptl_absorpt_coefficient_mu 1.645 _exptl_absorpt_correction_type numerical #------------------------------------------------------------------------------ _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_reflns_number 21040 _reflns_number_total 12260 _reflns_number_gt 6897 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03385 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.08 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 6 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 54 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 18 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 46 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 126 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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) -0.51826(5) 0.16318(5) 0.71894(4) 0.0281(2) 1.000 . Uani d ? Cu(2) -0.34954(5) 0.18507(5) 0.79758(4) 0.0293(2) 1.000 . Uani d ? Cu(3) 0.11896(5) 0.20637(4) 0.23840(4) 0.0239(2) 1.000 . Uani d ? Cl(1) 0.0404(1) 0.2653(1) 0.92975(9) 0.0355(4) 1.000 . Uani d ? Cl(2) 0.1448(1) 0.0409(1) 0.57156(9) 0.0340(3) 1.000 . Uani d ? Cl(3) 0.3891(1) 0.1200(1) 0.09340(9) 0.0322(3) 1.000 . Uani d ? Cl(4) 0.5124(2) 0.3069(1) 0.2607(1) 0.0544(5) 1.000 . Uani d ? O(1) -0.5066(3) 0.2642(3) 0.7650(3) 0.056(1) 1.000 . Uani d ? O(2) -0.3366(2) 0.1176(2) 0.7081(2) 0.0252(9) 1.000 . Uani d ? O(3) 0.0329(3) 0.1042(3) 0.2430(2) 0.031(1) 1.000 . Uani d ? O(4) 0.2245(3) 0.0762(2) 0.3185(2) 0.0282(9) 1.000 . Uani d ? O(5) -0.0051(7) 0.3379(4) 0.9770(3) 0.127(3) 1.000 . Uani d ? O(6) -0.0148(5) 0.1804(4) 0.9662(3) 0.091(2) 1.000 . Uani d ? O(7) 0.1649(4) 0.2150(6) 0.9336(4) 0.124(2) 1.000 . Uani d ? O(8) 0.0263(3) 0.3259(3) 0.8411(2) 0.047(1) 1.000 . Uani d ? O(9) 0.2057(3) -0.0339(4) 0.6422(3) 0.058(1) 1.000 . Uani d ? O(10) 0.1507(4) 0.1507(3) 0.5505(3) 0.063(2) 1.000 . Uani d ? O(11) 0.0193(3) 0.0445(3) 0.5955(2) 0.041(1) 1.000 . Uani d ? O(12) 0.1959(4) 0.0034(4) 0.4985(3) 0.064(1) 1.000 . Uani d ? O(13) 0.2642(3) 0.1222(3) 0.1283(2) 0.033(1) 1.000 . Uani d ? O(14) 0.4235(3) 0.1750(3) 0.1353(3) 0.049(1) 1.000 . Uani d ? O(15) 0.4645(3) 0.0071(3) 0.1097(3) 0.043(1) 1.000 . Uani d ? O(16) 0.4002(3) 0.1773(4) 0.0023(3) 0.056(1) 1.000 . Uani d ? O(17) 0.4643(5) 0.2139(4) 0.3033(4) 0.105(2) 1.000 . Uani d ? O(18) 0.459(1) 0.3810(9) 0.3088(8) 0.095(5) 0.500 . Uani d ? O(19) 0.475(2) 0.367(1) 0.1719(9) 0.107(6) 0.500 . Uani d ? O(20) 0.6312(9) 0.267(1) 0.262(2) 0.125(7) 0.500 . Uani d ? O(21) 0.612(1) 0.278(1) 0.1972(9) 0.103(5) 0.500 . Uani d ? O(22) 0.4202(8) 0.384(1) 0.2276(9) 0.069(4) 0.500 . Uani d ? O(23) 0.553(1) 0.362(2) 0.293(1) 0.162(9) 0.500 . Uani d ? O(24) 0.6649(6) 0.4892(7) 0.0678(5) 0.082(3) 0.700 . Uani d ? O(25) 0.8574(3) 0.1841(4) 0.1508(3) 0.065(2) 1.000 . Uani d ? O(26) 0.3051(5) 0.3718(5) 0.8603(4) 0.083(2) 0.800 . Uani d ? O(27) 0.4907(9) 0.382(1) 0.0430(6) 0.082(4) 0.500 . Uani d ? O(28) 0.376(2) 0.460(2) 0.795(2) 0.09(1) 0.200 . Uani d ? N(1) -0.5592(3) 0.2519(3) 0.5767(3) 0.027(1) 1.000 . Uani d ? N(2) -0.5284(3) 0.0319(3) 0.6982(3) 0.027(1) 1.000 . Uani d ? N(3) -0.7034(3) 0.2042(3) 0.7450(3) 0.032(1) 1.000 . Uani d ? N(4) -0.2235(3) 0.3040(3) 0.7370(3) 0.027(1) 1.000 . Uani d ? N(5) -0.2011(4) 0.0790(3) 0.8475(3) 0.033(1) 1.000 . Uani d ? N(6) -0.3835(4) 0.2445(4) 0.8967(3) 0.041(1) 1.000 . Uani d ? N(7) -0.0300(3) 0.3049(3) 0.3210(3) 0.027(1) 1.000 . Uani d ? N(8) 0.0411(3) 0.3320(3) 0.1405(3) 0.029(1) 1.000 . Uani d ? N(9) 0.2054(3) 0.3102(3) 0.2306(3) 0.027(1) 1.000 . Uani d ? C(1) -0.5006(4) 0.1548(4) 0.5449(3) 0.033(1) 1.000 . Uani d ? C(2) -0.5354(4) 0.0520(4) 0.6075(3) 0.031(1) 1.000 . Uani d ? C(3) -0.6358(4) 0.0037(4) 0.7607(3) 0.033(1) 1.000 . Uani d ? C(4) -0.7432(4) 0.1082(4) 0.7558(4) 0.034(1) 1.000 . Uani d ? C(5) -0.7489(4) 0.3047(4) 0.6746(4) 0.038(2) 1.000 . Uani d ? C(6) -0.6924(4) 0.2864(4) 0.5874(4) 0.035(1) 1.000 . Uani d ? C(7) -0.1059(4) 0.2180(4) 0.7326(4) 0.034(1) 1.000 . Uani d ? C(8) -0.0948(4) 0.1204(4) 0.8150(4) 0.037(2) 1.000 . Uani d ? C(9) -0.2445(5) 0.0577(4) 0.9439(4) 0.041(2) 1.000 . Uani d ? C(10) -0.3058(5) 0.1670(5) 0.9615(4) 0.042(2) 1.000 . Uani d ? C(11) -0.3678(5) 0.3584(4) 0.8585(4) 0.043(2) 1.000 . Uani d ? C(12) -0.2457(5) 0.3547(4) 0.8049(4) 0.037(2) 1.000 . Uani d ? C(13) -0.1245(4) 0.3582(4) 0.2665(4) 0.034(1) 1.000 . Uani d ? C(14) -0.0734(4) 0.4085(4) 0.1719(4) 0.036(2) 1.000 . Uani d ? C(15) 0.1363(4) 0.3875(4) 0.0899(3) 0.031(1) 1.000 . Uani d ? C(16) 0.1884(4) 0.4081(4) 0.1508(4) 0.033(1) 1.000 . Uani d ? C(17) 0.1591(4) 0.3391(4) 0.3116(3) 0.031(1) 1.000 . Uani d ? C(18) 0.0221(4) 0.3832(4) 0.3267(3) 0.030(1) 1.000 . Uani d ? C(19) -0.5172(4) 0.3497(4) 0.5165(4) 0.035(1) 1.000 . Uani d ? C(20) -0.2338(5) 0.3935(4) 0.6525(4) 0.035(1) 1.000 . Uani d ? C(21) -0.0666(4) 0.2289(4) 0.4067(3) 0.032(1) 1.000 . Uani d ? C(22) -0.3885(4) 0.3363(4) 0.5191(3) 0.030(1) 1.000 . Uani d ? C(23) -0.3678(4) 0.3694(4) 0.5797(3) 0.030(1) 1.000 . Uani d ? C(24) -0.2514(4) 0.3588(4) 0.5842(3) 0.030(1) 1.000 . Uani d ? C(25) -0.1542(4) 0.3142(4) 0.5270(3) 0.031(1) 1.000 . Uani d ? C(26) -0.1720(4) 0.2813(4) 0.4661(3) 0.030(1) 1.000 . Uani d ? C(27) -0.2911(4) 0.2929(4) 0.4622(3) 0.030(1) 1.000 . Uani d ? H(1) -0.5242 0.1729 0.4913 0.039 1.000 . Uiso c ? H(2) -0.4153 0.1389 0.5367 0.039 1.000 . Uiso c ? H(3) -0.4822 -0.0107 0.5906 0.037 1.000 . Uiso c ? H(4) -0.6161 0.0610 0.6046 0.037 1.000 . Uiso c ? H(5) -0.4621 -0.0256 0.7123 0.032 1.000 . Uiso c ? H(6) -0.6554 -0.0481 0.7470 0.040 1.000 . Uiso c ? H(7) -0.6175 -0.0281 0.8175 0.040 1.000 . Uiso c ? H(8) -0.8006 0.0958 0.8076 0.041 1.000 . Uiso c ? H(9) -0.7797 0.1247 0.7080 0.041 1.000 . Uiso c ? H(10) -0.7297 0.2207 0.7947 0.039 1.000 . Uiso c ? H(11) -0.8343 0.3221 0.6821 0.045 1.000 . Uiso c ? H(12) -0.7292 0.3646 0.6763 0.045 1.000 . Uiso c ? H(13) -0.7188 0.3536 0.5429 0.042 1.000 . Uiso c ? H(14) -0.7169 0.2301 0.5841 0.042 1.000 . Uiso c ? H(15) -0.0963 0.1917 0.6863 0.041 1.000 . Uiso c ? H(16) -0.0436 0.2502 0.7220 0.041 1.000 . Uiso c ? H(17) -0.0851 0.1429 0.8581 0.045 1.000 . Uiso c ? H(18) -0.0253 0.0617 0.8042 0.045 1.000 . Uiso c ? H(19) -0.1818 0.0151 0.8360 0.039 1.000 . Uiso c ? H(20) -0.3002 0.0159 0.9638 0.049 1.000 . Uiso c ? H(21) -0.1773 0.0173 0.9734 0.049 1.000 . Uiso c ? H(22) -0.2461 0.1981 0.9588 0.051 1.000 . Uiso c ? H(23) -0.3540 0.1551 1.0175 0.051 1.000 . Uiso c ? H(24) -0.4612 0.2509 0.9222 0.049 1.000 . Uiso c ? H(25) -0.4277 0.4062 0.8234 0.051 1.000 . Uiso c ? H(26) -0.3770 0.3861 0.9039 0.051 1.000 . Uiso c ? H(27) -0.1863 0.3119 0.8411 0.044 1.000 . Uiso c ? H(28) -0.2400 0.4282 0.7782 0.044 1.000 . Uiso c ? H(29) -0.1591 0.3041 0.2708 0.041 1.000 . Uiso c ? H(30) -0.1853 0.4154 0.2867 0.041 1.000 . Uiso c ? H(31) -0.0580 0.4745 0.1656 0.044 1.000 . Uiso c ? H(32) -0.1318 0.4261 0.1376 0.044 1.000 . Uiso c ? H(33) 0.0252 0.3033 0.1072 0.035 1.000 . Uiso c ? H(34) 0.1988 0.3412 0.0599 0.037 1.000 . Uiso c ? H(35) 0.1018 0.4564 0.0495 0.037 1.000 . Uiso c ? H(36) 0.1346 0.4717 0.1662 0.040 1.000 . Uiso c ? H(37) 0.2645 0.4206 0.1226 0.040 1.000 . Uiso c ? H(38) 0.2850 0.2736 0.2283 0.032 1.000 . Uiso c ? H(39) 0.1839 0.2746 0.3587 0.037 1.000 . Uiso c ? H(40) 0.1915 0.3944 0.3079 0.037 1.000 . Uiso c ? H(41) -0.0027 0.4532 0.2842 0.036 1.000 . Uiso c ? H(42) -0.0060 0.3917 0.3826 0.036 1.000 . Uiso c ? H(43) -0.5224 0.3594 0.4593 0.042 1.000 . Uiso c ? H(44) -0.5688 0.4138 0.5320 0.042 1.000 . Uiso c ? H(45) -0.3010 0.4551 0.6608 0.042 1.000 . Uiso c ? H(46) -0.1618 0.4150 0.6325 0.042 1.000 . Uiso c ? H(47) -0.0877 0.1746 0.3973 0.038 1.000 . Uiso c ? H(48) 0.0013 0.1937 0.4355 0.038 1.000 . Uiso c ? H(49) -0.4342 0.3997 0.6183 0.036 1.000 . Uiso c ? H(50) -0.0742 0.3064 0.5304 0.037 1.000 . Uiso c ? H(51) -0.3051 0.2712 0.4203 0.036 1.000 . Uiso c ? H(52) -0.5542 0.3238 0.7696 0.067 1.000 . Uiso c ? H(53) -0.2797 0.0845 0.6787 0.030 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) 0.0188(3) 0.0201(3) 0.0483(4) -0.0042(2) -0.0122(3) -0.0107(3) Cu(2) 0.0250(3) 0.0210(3) 0.0459(4) -0.0086(2) -0.0109(3) -0.0096(3) Cu(3) 0.0237(3) 0.0151(3) 0.0340(4) -0.0061(2) -0.0112(3) -0.0039(3) Cl(1) 0.0422(7) 0.0330(7) 0.0381(8) -0.0084(6) -0.0194(6) -0.0118(6) Cl(2) 0.0319(6) 0.0312(7) 0.0392(8) -0.0151(5) -0.0145(6) 0.0004(6) Cl(3) 0.0254(6) 0.0260(6) 0.0427(8) -0.0075(5) -0.0048(5) -0.0089(6) Cl(4) 0.0529(9) 0.0391(9) 0.063(1) -0.0056(7) -0.0167(8) -0.0103(8) O(1) 0.031(2) 0.033(2) 0.122(4) 0.006(2) -0.034(2) -0.043(2) O(2) 0.017(1) 0.017(2) 0.040(2) -0.002(1) -0.010(1) -0.007(2) O(3) 0.031(2) 0.025(2) 0.041(2) -0.014(1) -0.007(2) -0.009(2) O(4) 0.028(2) 0.016(2) 0.038(2) -0.003(1) -0.012(2) -0.004(2) O(5) 0.260(8) 0.050(3) 0.045(3) 0.006(4) -0.046(4) -0.022(3) O(6) 0.140(5) 0.093(4) 0.076(4) -0.085(4) -0.056(3) 0.013(3) O(7) 0.051(3) 0.170(7) 0.101(5) -0.026(4) -0.045(3) 0.025(5) O(8) 0.047(2) 0.059(3) 0.031(2) -0.011(2) -0.013(2) -0.010(2) O(9) 0.050(2) 0.065(3) 0.053(3) -0.027(2) -0.033(2) 0.016(2) O(10) 0.064(3) 0.044(3) 0.095(4) -0.036(2) -0.034(3) -0.001(2) O(11) 0.031(2) 0.034(2) 0.053(3) -0.015(2) -0.015(2) 0.001(2) O(12) 0.061(3) 0.057(3) 0.045(3) 0.008(2) -0.011(2) -0.010(2) O(13) 0.029(2) 0.030(2) 0.043(2) -0.014(2) 0.002(2) -0.014(2) O(14) 0.034(2) 0.037(2) 0.089(3) -0.010(2) -0.015(2) -0.032(2) O(15) 0.040(2) 0.030(2) 0.060(3) 0.000(2) -0.013(2) -0.020(2) O(16) 0.038(2) 0.061(3) 0.045(3) -0.017(2) -0.005(2) 0.008(2) O(17) 0.093(4) 0.041(3) 0.156(6) -0.030(3) -0.017(4) -0.001(3) O(18) 0.13(1) 0.060(7) 0.095(9) -0.030(7) 0.027(9) -0.057(7) O(19) 0.19(2) 0.078(9) 0.08(1) -0.07(1) -0.08(1) 0.020(8) O(20) 0.024(5) 0.12(1) 0.28(3) 0.014(6) -0.051(9) -0.13(2) O(21) 0.028(6) 0.15(1) 0.11(1) 0.008(7) 0.012(6) -0.07(1) O(22) 0.032(5) 0.071(7) 0.10(1) -0.004(5) -0.015(6) -0.025(8) O(23) 0.058(8) 0.20(2) 0.26(2) -0.09(1) -0.01(1) -0.07(2) O(24) 0.070(5) 0.102(6) 0.076(5) -0.049(5) 0.004(4) -0.019(5) O(25) 0.041(2) 0.106(4) 0.049(3) -0.022(3) -0.016(2) -0.018(3) O(26) 0.061(4) 0.074(5) 0.073(5) 0.014(3) -0.004(3) -0.019(4) O(27) 0.076(7) 0.115(9) 0.049(6) -0.022(6) 0.007(5) -0.039(6) O(28) 0.04(1) 0.06(2) 0.17(3) -0.02(1) 0.00(2) -0.06(2) N(1) 0.019(2) 0.013(2) 0.044(3) -0.004(2) -0.011(2) -0.002(2) N(2) 0.021(2) 0.019(2) 0.039(3) -0.003(2) -0.012(2) -0.005(2) N(3) 0.021(2) 0.032(2) 0.046(3) -0.004(2) -0.008(2) -0.016(2) N(4) 0.027(2) 0.020(2) 0.038(3) -0.008(2) -0.008(2) -0.010(2) N(5) 0.038(2) 0.018(2) 0.050(3) -0.009(2) -0.022(2) -0.008(2) N(6) 0.037(2) 0.040(3) 0.050(3) -0.021(2) 0.006(2) -0.019(2) N(7) 0.027(2) 0.018(2) 0.034(3) -0.007(2) -0.008(2) -0.004(2) N(8) 0.030(2) 0.023(2) 0.034(3) -0.005(2) -0.012(2) -0.007(2) N(9) 0.024(2) 0.020(2) 0.037(3) -0.008(2) -0.013(2) -0.002(2) C(1) 0.025(2) 0.027(3) 0.042(3) -0.007(2) -0.009(2) -0.006(2) C(2) 0.029(3) 0.023(3) 0.045(3) -0.008(2) -0.012(2) -0.011(2) C(3) 0.025(2) 0.031(3) 0.044(3) -0.014(2) -0.010(2) -0.004(3) C(4) 0.024(2) 0.038(3) 0.043(3) -0.014(2) -0.003(2) -0.011(3) C(5) 0.018(2) 0.029(3) 0.064(4) -0.002(2) -0.014(2) -0.013(3) C(6) 0.024(2) 0.026(3) 0.050(4) -0.004(2) -0.016(2) -0.003(3) C(7) 0.025(2) 0.034(3) 0.045(4) -0.011(2) -0.005(2) -0.013(3) C(8) 0.031(3) 0.033(3) 0.057(4) -0.006(2) -0.020(3) -0.018(3) C(9) 0.050(3) 0.025(3) 0.050(4) -0.014(3) -0.024(3) 0.001(3) C(10) 0.041(3) 0.037(3) 0.048(4) -0.020(3) -0.001(3) -0.009(3) C(11) 0.047(3) 0.028(3) 0.056(4) -0.013(3) -0.004(3) -0.018(3) C(12) 0.047(3) 0.023(3) 0.048(4) -0.015(2) -0.014(3) -0.010(3) C(13) 0.025(2) 0.028(3) 0.047(4) -0.001(2) -0.012(2) -0.011(3) C(14) 0.032(3) 0.030(3) 0.042(4) -0.005(2) -0.019(2) -0.002(3) C(15) 0.035(3) 0.020(2) 0.030(3) -0.005(2) -0.007(2) -0.002(2) C(16) 0.038(3) 0.021(3) 0.041(3) -0.012(2) -0.009(2) -0.005(2) C(17) 0.037(3) 0.027(3) 0.036(3) -0.017(2) -0.012(2) -0.006(2) C(18) 0.037(3) 0.020(2) 0.032(3) -0.011(2) -0.002(2) -0.008(2) C(19) 0.029(3) 0.020(3) 0.050(4) -0.006(2) -0.017(2) 0.001(2) C(20) 0.039(3) 0.021(3) 0.046(4) -0.013(2) -0.010(3) -0.004(2) C(21) 0.030(3) 0.025(3) 0.038(3) -0.013(2) -0.012(2) 0.001(2) C(22) 0.029(2) 0.014(2) 0.039(3) -0.008(2) -0.014(2) 0.007(2) C(23) 0.028(2) 0.011(2) 0.039(3) -0.004(2) -0.007(2) 0.003(2) C(24) 0.035(3) 0.014(2) 0.038(3) -0.011(2) -0.012(2) 0.002(2) C(25) 0.029(3) 0.022(2) 0.039(3) -0.012(2) -0.012(2) 0.002(2) C(26) 0.029(3) 0.019(2) 0.036(3) -0.010(2) -0.006(2) 0.000(2) C(27) 0.030(3) 0.021(2) 0.037(3) -0.010(2) -0.010(2) -0.002(2) #------------------------------------------------------------------------------ _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)]' _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 6897 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_all 0.0677 _refine_ls_wR_factor_ref 0.0573 _refine_ls_goodness_of_fit_all 1.517 _refine_ls_goodness_of_fit_ref 1.741 _refine_ls_shift/su_max 3.4056 _refine_ls_shift/su_mean 0.1122 _refine_diff_density_min -0.88 _refine_diff_density_max 1.48 #------------------------------------------------------------------------------ _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) Cu(2) 2.9041(8) . . yes Cu(1) O(1) 1.900(4) . . yes Cu(1) O(2) 2.019(3) . . yes Cu(1) N(1) 2.358(4) . . yes Cu(1) N(2) 2.015(4) . . yes Cu(1) N(3) 2.049(4) . . yes Cu(2) O(1) 1.922(3) . . yes Cu(2) O(2) 2.015(3) . . yes Cu(2) N(4) 2.383(4) . . yes Cu(2) N(5) 2.007(4) . . yes Cu(2) N(6) 2.025(5) . . yes Cu(3) O(3) 2.002(3) . . yes Cu(3) O(4) 2.020(3) . . yes Cu(3) N(7) 2.284(4) . . yes Cu(3) N(8) 2.024(4) . . yes Cu(3) N(9) 2.005(4) . . yes Cl(1) O(5) 1.376(5) . . yes Cl(1) O(6) 1.401(4) . . yes Cl(1) O(7) 1.412(5) . . yes Cl(1) O(8) 1.438(4) . . yes Cl(2) O(9) 1.425(4) . . yes Cl(2) O(10) 1.428(4) . . yes Cl(2) O(11) 1.439(3) . . yes Cl(2) O(12) 1.417(4) . . yes Cl(3) O(13) 1.447(3) . . yes Cl(3) O(14) 1.444(4) . . yes Cl(3) O(15) 1.432(4) . . yes Cl(3) O(16) 1.433(4) . . yes Cl(4) O(17) 1.439(5) . . yes Cl(4) O(18) 1.401(9) . . yes Cl(4) O(19) 1.52(1) . . yes Cl(4) O(20) 1.335(9) . . yes Cl(4) O(21) 1.41(1) . . yes Cl(4) O(22) 1.30(1) . . yes Cl(4) O(23) 1.37(2) . . yes O(1) H(52) 0.82 . . no O(2) H(53) 0.82 . . no O(18) O(22) 1.57(2) . . yes O(18) O(23) 1.04(2) . . yes O(19) O(21) 1.70(2) . . yes O(19) O(22) 1.04(2) . . yes O(20) O(21) 1.13(2) . . yes O(20) O(23) 1.48(3) . . yes O(26) O(28) 1.62(2) . . yes N(1) C(1) 1.480(6) . . yes N(1) C(6) 1.475(6) . . yes N(1) C(19) 1.495(6) . . yes N(2) C(2) 1.484(6) . . yes N(2) C(3) 1.490(6) . . yes N(2) H(5) 0.90 . . no N(3) C(4) 1.493(6) . . yes N(3) C(5) 1.471(7) . . yes N(3) H(10) 0.90 . . no N(4) C(7) 1.471(6) . . yes N(4) C(12) 1.483(6) . . yes N(4) C(20) 1.485(7) . . yes N(5) C(8) 1.473(6) . . yes N(5) C(9) 1.517(7) . . yes N(5) H(19) 0.90 . . no N(6) C(10) 1.475(7) . . yes N(6) C(11) 1.500(6) . . yes N(6) H(24) 0.90 . . no N(7) C(13) 1.473(6) . . yes N(7) C(18) 1.477(6) . . yes N(7) C(21) 1.482(6) . . yes N(8) C(14) 1.488(6) . . yes N(8) C(15) 1.488(6) . . yes N(8) H(33) 0.90 . . no N(9) C(16) 1.491(6) . . yes N(9) C(17) 1.480(6) . . yes N(9) H(38) 0.90 . . no C(1) C(2) 1.520(7) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(3) C(4) 1.521(7) . . yes C(3) H(6) 0.95 . . no C(3) H(7) 0.95 . . no C(4) H(8) 0.95 . . no C(4) H(9) 0.95 . . no C(5) C(6) 1.518(8) . . yes C(5) H(11) 0.95 . . no C(5) H(12) 0.95 . . no C(6) H(13) 0.95 . . no C(6) H(14) 0.95 . . no C(7) C(8) 1.513(8) . . yes C(7) H(15) 0.95 . . no C(7) H(16) 0.95 . . no C(8) H(17) 0.95 . . no C(8) H(18) 0.95 . . no C(9) C(10) 1.505(7) . . yes C(9) H(20) 0.95 . . no C(9) H(21) 0.95 . . no C(10) H(22) 0.95 . . no C(10) H(23) 0.95 . . no C(11) C(12) 1.487(7) . . yes C(11) H(25) 0.95 . . no C(11) H(26) 0.95 . . no C(12) H(27) 0.95 . . no C(12) H(28) 0.95 . . no C(13) C(14) 1.526(8) . . yes C(13) H(29) 0.95 . . no C(13) H(30) 0.95 . . no C(14) H(31) 0.95 . . no C(14) H(32) 0.95 . . no C(15) C(16) 1.517(7) . . yes C(15) H(34) 0.95 . . no C(15) H(35) 0.95 . . no C(16) H(36) 0.95 . . no C(16) H(37) 0.95 . . no C(17) C(18) 1.516(7) . . yes C(17) H(39) 0.95 . . no C(17) H(40) 0.95 . . no C(18) H(41) 0.95 . . no C(18) H(42) 0.95 . . no C(19) C(22) 1.510(6) . . yes C(19) H(43) 0.95 . . no C(19) H(44) 0.95 . . no C(20) C(24) 1.509(7) . . yes C(20) H(45) 0.95 . . no C(20) H(46) 0.95 . . no C(21) C(26) 1.513(7) . . yes C(21) H(47) 0.95 . . no C(21) H(48) 0.95 . . no C(22) C(23) 1.392(7) . . yes C(22) C(27) 1.392(7) . . yes C(23) C(24) 1.383(7) . . yes C(23) H(49) 0.95 . . no C(24) C(25) 1.400(7) . . yes C(25) C(26) 1.377(7) . . yes C(25) H(50) 0.95 . . no C(26) C(27) 1.408(6) . . yes C(27) H(51) 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 Cu(2) Cu(1) O(1) 40.8(1) . . . yes Cu(2) Cu(1) O(2) 43.90(9) . . . yes Cu(2) Cu(1) N(1) 129.09(9) . . . yes Cu(2) Cu(1) N(2) 131.8(1) . . . yes Cu(2) Cu(1) N(3) 131.0(1) . . . yes O(1) Cu(1) O(2) 80.7(1) . . . yes O(1) Cu(1) N(1) 111.5(2) . . . yes O(1) Cu(1) N(2) 166.7(2) . . . yes O(1) Cu(1) N(3) 96.1(2) . . . yes O(2) Cu(1) N(1) 106.0(1) . . . yes O(2) Cu(1) N(2) 97.7(1) . . . yes O(2) Cu(1) N(3) 173.4(2) . . . yes N(1) Cu(1) N(2) 81.7(1) . . . yes N(1) Cu(1) N(3) 80.5(2) . . . yes N(2) Cu(1) N(3) 84.1(2) . . . yes Cu(1) Cu(2) O(1) 40.3(1) . . . yes Cu(1) Cu(2) O(2) 44.01(8) . . . yes Cu(1) Cu(2) N(4) 129.0(1) . . . yes Cu(1) Cu(2) N(5) 133.5(1) . . . yes Cu(1) Cu(2) N(6) 129.2(1) . . . yes O(1) Cu(2) O(2) 80.3(1) . . . yes O(1) Cu(2) N(4) 110.0(2) . . . yes O(1) Cu(2) N(5) 168.6(2) . . . yes O(1) Cu(2) N(6) 95.3(2) . . . yes O(2) Cu(2) N(4) 107.6(1) . . . yes O(2) Cu(2) N(5) 98.4(1) . . . yes O(2) Cu(2) N(6) 171.7(1) . . . yes N(4) Cu(2) N(5) 81.2(1) . . . yes N(4) Cu(2) N(6) 80.6(2) . . . yes N(5) Cu(2) N(6) 84.5(2) . . . yes O(3) Cu(3) O(4) 88.5(1) . . . yes O(3) Cu(3) N(7) 98.5(1) . . . yes O(3) Cu(3) N(8) 94.0(1) . . . yes O(3) Cu(3) N(9) 178.6(2) . . . yes O(4) Cu(3) N(7) 107.4(1) . . . yes O(4) Cu(3) N(8) 169.1(1) . . . yes O(4) Cu(3) N(9) 92.5(1) . . . yes N(7) Cu(3) N(8) 82.8(2) . . . yes N(7) Cu(3) N(9) 82.2(1) . . . yes N(8) Cu(3) N(9) 84.9(2) . . . yes O(5) Cl(1) O(6) 110.6(4) . . . yes O(5) Cl(1) O(7) 108.1(5) . . . yes O(5) Cl(1) O(8) 109.4(3) . . . yes O(6) Cl(1) O(7) 107.3(4) . . . yes O(6) Cl(1) O(8) 112.5(3) . . . yes O(7) Cl(1) O(8) 108.8(3) . . . yes O(9) Cl(2) O(10) 111.1(3) . . . yes O(9) Cl(2) O(11) 109.0(2) . . . yes O(9) Cl(2) O(12) 110.1(3) . . . yes O(10) Cl(2) O(11) 108.1(2) . . . yes O(10) Cl(2) O(12) 110.1(3) . . . yes O(11) Cl(2) O(12) 108.5(3) . . . yes O(13) Cl(3) O(14) 108.6(2) . . . yes O(13) Cl(3) O(15) 109.5(2) . . . yes O(13) Cl(3) O(16) 109.0(2) . . . yes O(14) Cl(3) O(15) 109.6(2) . . . yes O(14) Cl(3) O(16) 109.8(3) . . . yes O(15) Cl(3) O(16) 110.3(3) . . . yes O(17) Cl(4) O(18) 108.3(6) . . . yes O(17) Cl(4) O(19) 108.4(5) . . . yes O(17) Cl(4) O(20) 107.1(8) . . . yes O(17) Cl(4) O(21) 107.7(7) . . . yes O(17) Cl(4) O(22) 101.2(6) . . . yes O(17) Cl(4) O(23) 131.2(9) . . . yes O(18) Cl(4) O(19) 107.8(8) . . . yes O(18) Cl(4) O(20) 109(1) . . . yes O(18) Cl(4) O(21) 142.2(9) . . . yes O(18) Cl(4) O(22) 71.0(8) . . . yes O(18) Cl(4) O(23) 44.1(8) . . . yes O(19) Cl(4) O(20) 116(1) . . . yes O(19) Cl(4) O(21) 70.8(9) . . . yes O(19) Cl(4) O(22) 42.4(6) . . . yes O(19) Cl(4) O(23) 118(1) . . . yes O(20) Cl(4) O(21) 48.4(8) . . . yes O(20) Cl(4) O(22) 150(1) . . . yes O(20) Cl(4) O(23) 66.2(9) . . . yes O(21) Cl(4) O(22) 112.7(8) . . . yes O(21) Cl(4) O(23) 102(1) . . . yes O(22) Cl(4) O(23) 102(1) . . . yes Cu(1) O(1) Cu(2) 98.9(2) . . . yes Cu(1) O(1) H(52) 130.5 . . . no Cu(2) O(1) H(52) 130.6 . . . no Cu(1) O(2) Cu(2) 92.1(1) . . . yes Cu(1) O(2) H(53) 134.0 . . . no Cu(2) O(2) H(53) 133.9 . . . no Cl(4) O(18) O(22) 51.6(5) . . . yes Cl(4) O(18) O(23) 66(2) . . . yes O(22) O(18) O(23) 104(2) . . . yes Cl(4) O(19) O(21) 51.5(6) . . . yes Cl(4) O(19) O(22) 57.4(9) . . . yes O(21) O(19) O(22) 108(1) . . . yes Cl(4) O(20) O(21) 69.4(8) . . . yes Cl(4) O(20) O(23) 58.0(7) . . . yes O(21) O(20) O(23) 111(2) . . . yes Cl(4) O(21) O(19) 57.7(6) . . . yes Cl(4) O(21) O(20) 62.2(9) . . . yes O(19) O(21) O(20) 117(1) . . . yes Cl(4) O(22) O(18) 57.5(6) . . . yes Cl(4) O(22) O(19) 80(1) . . . yes O(18) O(22) O(19) 129(1) . . . yes Cl(4) O(23) O(18) 70(1) . . . yes Cl(4) O(23) O(20) 56(1) . . . yes O(18) O(23) O(20) 124(2) . . . yes Cu(1) N(1) C(1) 98.2(3) . . . yes Cu(1) N(1) C(6) 104.3(3) . . . yes Cu(1) N(1) C(19) 122.2(3) . . . yes C(1) N(1) C(6) 112.7(4) . . . yes C(1) N(1) C(19) 111.3(4) . . . yes C(6) N(1) C(19) 107.9(3) . . . yes Cu(1) N(2) C(2) 114.1(3) . . . yes Cu(1) N(2) C(3) 104.9(3) . . . yes Cu(1) N(2) H(5) 108.4 . . . no C(2) N(2) C(3) 112.8(4) . . . yes C(2) N(2) H(5) 108.2 . . . no C(3) N(2) H(5) 108.3 . . . no Cu(1) N(3) C(4) 110.2(3) . . . yes Cu(1) N(3) C(5) 107.1(3) . . . yes Cu(1) N(3) H(10) 108.5 . . . no C(4) N(3) C(5) 113.8(4) . . . yes C(4) N(3) H(10) 108.6 . . . no C(5) N(3) H(10) 108.5 . . . no Cu(2) N(4) C(7) 98.0(3) . . . yes Cu(2) N(4) C(12) 103.2(3) . . . yes Cu(2) N(4) C(20) 122.5(3) . . . yes C(7) N(4) C(12) 113.2(4) . . . yes C(7) N(4) C(20) 110.7(4) . . . yes C(12) N(4) C(20) 108.8(4) . . . yes Cu(2) N(5) C(8) 114.6(3) . . . yes Cu(2) N(5) C(9) 102.8(3) . . . yes Cu(2) N(5) H(19) 108.8 . . . no C(8) N(5) C(9) 113.0(4) . . . yes C(8) N(5) H(19) 108.7 . . . no C(9) N(5) H(19) 108.7 . . . no Cu(2) N(6) C(10) 110.7(3) . . . yes Cu(2) N(6) C(11) 107.3(3) . . . yes Cu(2) N(6) H(24) 108.3 . . . no C(10) N(6) C(11) 113.8(4) . . . yes C(10) N(6) H(24) 108.3 . . . no C(11) N(6) H(24) 108.3 . . . no Cu(3) N(7) C(13) 100.2(3) . . . yes Cu(3) N(7) C(18) 105.3(3) . . . yes Cu(3) N(7) C(21) 110.4(3) . . . yes C(13) N(7) C(18) 114.0(4) . . . yes C(13) N(7) C(21) 113.2(4) . . . yes C(18) N(7) C(21) 112.7(4) . . . yes Cu(3) N(8) C(14) 112.5(3) . . . yes Cu(3) N(8) C(15) 104.2(3) . . . yes Cu(3) N(8) H(33) 109.0 . . . no C(14) N(8) C(15) 113.1(4) . . . yes C(14) N(8) H(33) 109.0 . . . no C(15) N(8) H(33) 109.0 . . . no Cu(3) N(9) C(16) 110.7(3) . . . yes Cu(3) N(9) C(17) 106.5(3) . . . yes Cu(3) N(9) H(38) 108.5 . . . no C(16) N(9) C(17) 113.9(4) . . . yes C(16) N(9) H(38) 108.6 . . . no C(17) N(9) H(38) 108.5 . . . no N(1) C(1) C(2) 112.5(4) . . . yes N(1) C(1) H(1) 108.7 . . . no N(1) C(1) H(2) 108.7 . . . no C(2) C(1) H(1) 108.7 . . . no C(2) C(1) H(2) 108.7 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 112.8(4) . . . yes N(2) C(2) H(3) 108.7 . . . no N(2) C(2) H(4) 108.7 . . . no C(1) C(2) H(3) 108.6 . . . no C(1) C(2) H(4) 108.6 . . . no H(3) C(2) H(4) 109.4 . . . no N(2) C(3) C(4) 110.0(4) . . . yes N(2) C(3) H(6) 109.3 . . . no N(2) C(3) H(7) 109.2 . . . no C(4) C(3) H(6) 109.4 . . . no C(4) C(3) H(7) 109.4 . . . no H(6) C(3) H(7) 109.5 . . . no N(3) C(4) C(3) 110.6(4) . . . yes N(3) C(4) H(8) 109.2 . . . no N(3) C(4) H(9) 109.3 . . . no C(3) C(4) H(8) 109.2 . . . no C(3) C(4) H(9) 109.3 . . . no H(8) C(4) H(9) 109.4 . . . no N(3) C(5) C(6) 110.7(4) . . . yes N(3) C(5) H(11) 109.2 . . . no N(3) C(5) H(12) 109.2 . . . no C(6) C(5) H(11) 109.2 . . . no C(6) C(5) H(12) 109.2 . . . no H(11) C(5) H(12) 109.5 . . . no N(1) C(6) C(5) 110.2(4) . . . yes N(1) C(6) H(13) 109.3 . . . no N(1) C(6) H(14) 109.3 . . . no C(5) C(6) H(13) 109.2 . . . no C(5) C(6) H(14) 109.2 . . . no H(13) C(6) H(14) 109.5 . . . no N(4) C(7) C(8) 112.7(4) . . . yes N(4) C(7) H(15) 108.7 . . . no N(4) C(7) H(16) 108.7 . . . no C(8) C(7) H(15) 108.6 . . . no C(8) C(7) H(16) 108.6 . . . no H(15) C(7) H(16) 109.5 . . . no N(5) C(8) C(7) 113.1(4) . . . yes N(5) C(8) H(17) 108.6 . . . no N(5) C(8) H(18) 108.6 . . . no C(7) C(8) H(17) 108.6 . . . no C(7) C(8) H(18) 108.6 . . . no H(17) C(8) H(18) 109.4 . . . no N(5) C(9) C(10) 109.3(4) . . . yes N(5) C(9) H(20) 109.6 . . . no N(5) C(9) H(21) 109.5 . . . no C(10) C(9) H(20) 109.5 . . . no C(10) C(9) H(21) 109.4 . . . no H(20) C(9) H(21) 109.5 . . . no N(6) C(10) C(9) 110.1(5) . . . yes N(6) C(10) H(22) 109.3 . . . no N(6) C(10) H(23) 109.3 . . . no C(9) C(10) H(22) 109.3 . . . no C(9) C(10) H(23) 109.3 . . . no H(22) C(10) H(23) 109.5 . . . no N(6) C(11) C(12) 110.6(4) . . . yes N(6) C(11) H(25) 109.2 . . . no N(6) C(11) H(26) 109.2 . . . no C(12) C(11) H(25) 109.2 . . . no C(12) C(11) H(26) 109.2 . . . no H(25) C(11) H(26) 109.4 . . . no N(4) C(12) C(11) 111.2(4) . . . yes N(4) C(12) H(27) 109.0 . . . no N(4) C(12) H(28) 109.0 . . . no C(11) C(12) H(27) 109.0 . . . no C(11) C(12) H(28) 109.0 . . . no H(27) C(12) H(28) 109.5 . . . no N(7) C(13) C(14) 111.6(4) . . . yes N(7) C(13) H(29) 108.9 . . . no N(7) C(13) H(30) 108.9 . . . no C(14) C(13) H(29) 109.0 . . . no C(14) C(13) H(30) 109.0 . . . no H(29) C(13) H(30) 109.5 . . . no N(8) C(14) C(13) 112.8(4) . . . yes N(8) C(14) H(31) 108.7 . . . no N(8) C(14) H(32) 108.6 . . . no C(13) C(14) H(31) 108.6 . . . no C(13) C(14) H(32) 108.6 . . . no H(31) C(14) H(32) 109.5 . . . no N(8) C(15) C(16) 109.4(4) . . . yes N(8) C(15) H(34) 109.5 . . . no N(8) C(15) H(35) 109.4 . . . no C(16) C(15) H(34) 109.5 . . . no C(16) C(15) H(35) 109.4 . . . no H(34) C(15) H(35) 109.5 . . . no N(9) C(16) C(15) 110.4(4) . . . yes N(9) C(16) H(36) 109.2 . . . no N(9) C(16) H(37) 109.2 . . . no C(15) C(16) H(36) 109.3 . . . no C(15) C(16) H(37) 109.2 . . . no H(36) C(16) H(37) 109.5 . . . no N(9) C(17) C(18) 110.9(4) . . . yes N(9) C(17) H(39) 109.0 . . . no N(9) C(17) H(40) 109.1 . . . no C(18) C(17) H(39) 109.1 . . . no C(18) C(17) H(40) 109.2 . . . no H(39) C(17) H(40) 109.5 . . . no N(7) C(18) C(17) 110.1(4) . . . yes N(7) C(18) H(41) 109.3 . . . no N(7) C(18) H(42) 109.3 . . . no C(17) C(18) H(41) 109.4 . . . no C(17) C(18) H(42) 109.4 . . . no H(41) C(18) H(42) 109.4 . . . no N(1) C(19) C(22) 113.1(4) . . . yes N(1) C(19) H(43) 108.6 . . . no N(1) C(19) H(44) 108.6 . . . no C(22) C(19) H(43) 108.6 . . . no C(22) C(19) H(44) 108.6 . . . no H(43) C(19) H(44) 109.4 . . . no N(4) C(20) C(24) 113.4(4) . . . yes N(4) C(20) H(45) 108.5 . . . no N(4) C(20) H(46) 108.5 . . . no C(24) C(20) H(45) 108.5 . . . no C(24) C(20) H(46) 108.5 . . . no H(45) C(20) H(46) 109.4 . . . no N(7) C(21) C(26) 116.5(4) . . . yes N(7) C(21) H(47) 107.7 . . . no N(7) C(21) H(48) 107.7 . . . no C(26) C(21) H(47) 107.7 . . . no C(26) C(21) H(48) 107.7 . . . no H(47) C(21) H(48) 109.5 . . . no C(19) C(22) C(23) 118.7(5) . . . yes C(19) C(22) C(27) 121.7(5) . . . yes C(23) C(22) C(27) 119.6(4) . . . yes C(22) C(23) C(24) 120.6(5) . . . yes C(22) C(23) H(49) 119.8 . . . no C(24) C(23) H(49) 119.6 . . . no C(20) C(24) C(23) 118.4(5) . . . yes C(20) C(24) C(25) 122.4(4) . . . yes C(23) C(24) C(25) 119.1(5) . . . yes C(24) C(25) C(26) 121.6(4) . . . yes C(24) C(25) H(50) 119.2 . . . no C(26) C(25) H(50) 119.3 . . . no C(21) C(26) C(25) 121.5(4) . . . yes C(21) C(26) C(27) 119.9(5) . . . yes C(25) C(26) C(27) 118.6(5) . . . yes C(22) C(27) C(26) 120.5(5) . . . yes C(22) C(27) H(51) 119.7 . . . no C(26) C(27) H(51) 119.7 . . . 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(15) 3.008(4) . 2_556 no Cu(2) O(15) 3.094(4) . 2_556 no Cu(3) O(13) 2.485(3) . . no Cu(3) O(14) 3.531(4) . . no Cu(3) Cl(3) 3.583(1) . . no Cl(2) O(3) 3.591(4) . 2_556 no Cl(4) O(27) 3.51(1) . . no O(1) O(26) 2.679(7) . 1_455 no O(1) O(28) 2.69(2) . 1_455 no O(1) O(15) 3.411(5) . 2_556 no O(2) O(4) 2.637(4) . 2_556 no O(2) O(15) 3.161(5) . 2_556 no O(2) O(13) 3.383(5) . 2_556 no O(3) O(25) 2.656(5) . 1_455 no O(3) O(11) 2.775(5) . 2_556 no O(3) O(13) 2.942(4) . . no O(3) N(5) 3.187(5) . 2_556 no O(3) O(9) 3.226(5) . 2_556 no O(3) C(8) 3.347(6) . 2_556 no O(4) O(12) 2.790(5) . . no O(4) O(13) 2.978(5) . . no O(4) N(2) 3.379(5) . 2_556 no O(4) O(14) 3.483(5) . . no O(4) O(11) 3.583(4) . 2_556 no O(5) N(8) 2.966(7) . 1_556 no O(5) O(25) 3.296(8) . 1_456 no O(5) C(15) 3.305(8) . 1_556 no O(5) C(15) 3.342(7) . 2_566 no O(5) C(16) 3.587(8) . 2_566 no O(6) O(25) 3.085(7) . 1_456 no O(6) C(8) 3.460(7) . . no O(7) O(26) 2.906(9) . . no O(7) N(3) 3.178(8) . 1_655 no O(7) O(16) 3.181(6) . 1_556 no O(7) C(9) 3.408(8) . 2_557 no O(7) O(13) 3.461(7) . 1_556 no O(7) C(4) 3.583(9) . 1_655 no O(8) N(3) 3.325(5) . 1_655 no O(8) C(5) 3.328(7) . 1_655 no O(8) C(12) 3.375(6) . . no O(9) O(20) 3.14(2) . 2_656 no O(9) O(25) 3.348(6) . 2_656 no O(9) C(3) 3.443(6) . 1_655 no O(9) C(4) 3.530(7) . 1_655 no O(9) C(2) 3.563(6) . 1_655 no O(10) C(6) 3.424(6) . 1_655 no O(10) C(25) 3.569(6) . . no O(11) C(21) 3.385(6) . . no O(11) C(25) 3.411(6) . . no O(11) C(26) 3.535(6) . . no O(11) C(21) 3.581(6) . 2_556 no O(11) C(7) 3.599(7) . . no O(12) C(1) 3.534(6) . 2_556 no O(13) N(5) 2.974(5) . 2_556 no O(13) N(8) 3.144(5) . . no O(13) C(15) 3.244(6) . . no O(13) C(9) 3.258(6) . 2_556 no O(13) N(9) 3.401(5) . . no O(14) O(27) 2.94(1) . . no O(14) N(9) 3.032(5) . . no O(14) C(3) 3.207(6) . 2_556 no O(14) O(19) 3.22(1) . . no O(14) N(2) 3.289(6) . 2_556 no O(14) O(17) 3.308(8) . . no O(14) C(16) 3.426(6) . . no O(15) C(3) 3.376(6) . 2_556 no O(15) N(2) 3.379(6) . 2_556 no O(15) O(16) 3.395(6) . 2_655 no O(15) C(9) 3.542(6) . 2_556 no O(15) N(5) 3.588(5) . 2_556 no O(16) O(26) 2.927(8) . 1_554 no O(16) N(6) 2.950(5) . 1_654 no O(16) C(10) 3.379(7) . 1_654 no O(17) N(2) 3.165(7) . 2_556 no O(17) C(2) 3.224(7) . 2_556 no O(17) C(3) 3.307(8) . 2_556 no O(17) N(9) 3.315(7) . . no O(17) C(17) 3.424(7) . . no O(18) O(28) 3.17(3) . 2_666 no O(18) C(20) 3.41(1) . 2_566 no O(18) C(19) 3.48(1) . 1_655 no O(19) O(27) 2.08(2) . . no O(19) O(24) 3.07(2) . . no O(19) C(11) 3.37(2) . 2_566 no O(19) C(16) 3.40(2) . . no O(19) N(9) 3.41(2) . . no O(20) O(25) 2.94(2) . . no O(20) O(28) 3.44(3) . 2_666 no O(20) O(24) 3.55(2) . . no O(21) O(25) 2.76(1) . . no O(21) O(27) 2.98(2) . . no O(21) O(24) 3.03(2) . . no O(21) C(3) 3.56(2) . 2_556 no O(22) O(27) 3.02(2) . . no O(22) N(9) 3.10(1) . . no O(22) C(11) 3.13(1) . 2_566 no O(22) C(17) 3.25(1) . . no O(22) C(16) 3.29(1) . . no O(22) C(12) 3.32(1) . 2_566 no O(23) O(28) 2.62(3) . 2_666 no O(23) C(27) 3.54(2) . 1_655 no O(24) O(28) 2.56(3) . 2_666 no O(24) O(27) 2.69(1) . 2_665 no O(24) O(26) 2.80(1) . 2_666 no O(24) O(27) 3.18(1) . . no O(24) C(15) 3.404(8) . 2_665 no O(24) C(11) 3.553(9) . 2_566 no O(24) C(16) 3.596(9) . 2_665 no O(25) N(8) 3.458(6) . 1_655 no O(26) C(14) 3.238(8) . 2_566 no O(27) O(27) 3.05(2) . 2_665 no O(27) C(11) 3.19(1) . 1_654 no O(27) N(6) 3.37(1) . 1_654 no O(27) C(10) 3.52(1) . 1_654 no O(27) C(16) 3.53(1) . . no O(28) C(11) 3.21(3) . 1_655 no O(28) C(13) 3.27(3) . 2_566 no O(28) C(14) 3.40(2) . 2_566 no O(28) N(6) 3.56(3) . 1_655 no C(19) C(23) 3.435(7) . 2_466 no #------------------------------------------------------------------------------ #====END data_k044 _database_code_CSD 174284 _journal_coden_Cambridge 186 #------------------------------------------------------------------------------ _audit_creation_date '2001-05-12' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal 'Dalton' _publ_contact_author_name 'Dr. Leone Spiccia' _publ_contact_author_address ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; _publ_contact_author_fax '+61 3 9905 4597' _publ_contact_author_email 'leone.spiccia@sci.monash.edu.au' loop_ _publ_author_name _publ_author_address 'Bim Graham' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Leone Spiccia' ;School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Gary D. Fallon' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Milton T. W. Hearn' ; Centre for Bioprocess Technology Department of Biochemistry P.O. Box 130 Monash University Victoria 3800 Australia ; 'Frank E. Mabbs' ; Department of Chemistry University of Manchester Manchester M13 9PL UK ; 'Boujemaa Moubaraki' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; 'Keith S. Murray' ; School of Chemistry P.O. Box 23 Monash University Victoria 3800 Australia ; _publ_section_title ; Structure and Magnetic Properties of Tri- and Hexa-nuclear Hydroxo- Bridged Copper(II) Complexes Formed by a Trimacrocyclic Derivative of 1,4,7-Triazacyclononane ; #------------------------------------------------------------------------------ _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'teXsan (MSC, 1992-1997)' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 14.4299(4) _cell_length_b 13.9410(6) _cell_length_c 21.463(1) _cell_angle_alpha 90 _cell_angle_beta 109.377(1) _cell_angle_gamma 90 _cell_volume 4073.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _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, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 2119.57 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H112 Cl6 Cu6 N18 O32 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2188.00 _exptl_absorpt_coefficient_mu 1.828 _exptl_absorpt_correction_type numerical #------------------------------------------------------------------------------ _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method 'CCD' _diffrn_reflns_number 35456 _reflns_number_total 11925 _reflns_number_gt 6913 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04795 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 29.76 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu 0 12 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 12 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 64 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 36 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 108 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 224 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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) 0.12784(4) 0.04482(4) 0.32618(3) 0.0209(2) 1.000 . Uani d ? Cu(2) 0.02543(4) -0.10828(4) 0.36534(3) 0.0209(2) 1.000 . Uani d ? Cu(3) -0.40197(5) -0.02486(5) -0.00323(3) 0.0344(2) 1.000 . Uani d ? Cu(3*) -0.59801(8) 0.02495(7) 0.00318(5) 0.0333(3) 1.000 . Uani d ? Cl(1) 0.16177(9) 0.4206(1) 0.49734(7) 0.0291(3) 1.000 . Uani d ? Cl(2) 0.9300(2) 0.1585(2) 0.8688(2) 0.0910(9) 1.000 . Uani d ? Cl(3) 0.5105(1) 0.0412(1) 0.79081(9) 0.0540(5) 1.000 . Uani d ? O(1) 0.0931(2) 0.0099(2) 0.4039(2) 0.0212(9) 1.000 . Uani d ? O(2) 0.0225(2) -0.0431(3) 0.2859(2) 0.026(1) 1.000 . Uani d ? O(3) -0.4909(3) 0.0832(3) -0.0215(2) 0.041(1) 1.000 . Uani d ? O(4) 0.0782(3) 0.3838(5) 0.4491(3) 0.090(2) 1.000 . Uani d ? O(5) 0.1919(6) 0.5130(4) 0.4861(2) 0.098(2) 1.000 . Uani d ? O(6) 0.1523(5) 0.4189(4) 0.5605(2) 0.095(2) 1.000 . Uani d ? O(7) 0.2370(4) 0.3620(6) 0.4964(4) 0.149(3) 1.000 . Uani d ? O(8) 0.8535(8) 0.0989(7) 0.8513(5) 0.197(5) 1.000 . Uani d ? O(9) 0.9897(6) 0.1626(6) 0.8313(4) 0.133(3) 1.000 . Uani d ? O(10) 0.9137(5) 0.2433(4) 0.8946(3) 0.095(2) 1.000 . Uani d ? O(11) 0.9932(9) 0.0959(8) 0.9407(9) 0.269(7) 1.000 . Uani d ? O(12) 0.6038(3) 0.0893(4) 0.8093(2) 0.058(2) 1.000 . Uani d ? O(13) 0.4844(4) 0.0040(5) 0.7286(3) 0.087(2) 1.000 . Uani d ? O(14) 0.5155(7) -0.0384(8) 0.8316(3) 0.197(4) 1.000 . Uani d ? O(15) 0.4417(6) 0.1014(7) 0.7956(8) 0.287(6) 1.000 . Uani d ? O(16) 0.0232(5) 0.2381(4) 0.0477(3) 0.091(2) 1.000 . Uani d ? N(1) 0.0812(3) 0.2014(3) 0.2894(2) 0.018(1) 1.000 . Uani d ? N(2) 0.1832(3) 0.0484(3) 0.2504(2) 0.031(1) 1.000 . Uani d ? N(3) 0.2539(3) 0.1138(3) 0.3764(2) 0.027(1) 1.000 . Uani d ? N(4) -0.1325(3) -0.1142(3) 0.3702(2) 0.020(1) 1.000 . Uani d ? N(5) 0.0530(3) -0.1801(3) 0.4519(2) 0.028(1) 1.000 . Uani d ? N(6) -0.0101(3) -0.2404(3) 0.3247(2) 0.027(1) 1.000 . Uani d ? N(7) -0.2735(3) 0.0199(3) 0.0888(2) 0.025(1) 1.000 . Uani d ? N(8) -0.3228(4) -0.1470(3) 0.0077(2) 0.037(1) 1.000 . Uani d ? N(9) -0.3081(4) 0.0242(4) -0.0486(2) 0.043(2) 1.000 . Uani d ? C(1) 0.0702(4) 0.1885(4) 0.2194(3) 0.026(1) 1.000 . Uani d ? C(2) 0.1563(4) 0.1362(4) 0.2091(3) 0.031(2) 1.000 . Uani d ? C(3) 0.2904(4) 0.0376(5) 0.2848(3) 0.044(2) 1.000 . Uani d ? C(4) 0.3256(4) 0.1074(4) 0.3400(3) 0.035(2) 1.000 . Uani d ? C(5) 0.2283(4) 0.2126(4) 0.3888(3) 0.027(1) 1.000 . Uani d ? C(6) 0.1675(3) 0.2614(3) 0.3252(2) 0.022(1) 1.000 . Uani d ? C(7) -0.1247(4) -0.1631(4) 0.4327(3) 0.027(1) 1.000 . Uani d ? C(8) -0.0217(4) -0.1519(4) 0.4821(2) 0.028(1) 1.000 . Uani d ? C(9) 0.0577(4) -0.2848(4) 0.4415(3) 0.035(2) 1.000 . Uani d ? C(10) 0.0602(4) -0.3048(4) 0.3731(3) 0.040(2) 1.000 . Uani d ? C(11) -0.1148(4) -0.2647(4) 0.3127(3) 0.030(2) 1.000 . Uani d ? C(12) -0.1759(4) -0.1757(4) 0.3120(2) 0.025(1) 1.000 . Uani d ? C(13) -0.2472(4) -0.0750(4) 0.1187(3) 0.029(1) 1.000 . Uani d ? C(14) -0.2372(4) -0.1496(4) 0.0697(3) 0.033(2) 1.000 . Uani d ? C(15) -0.2971(6) -0.1506(5) -0.0536(3) 0.053(2) 1.000 . Uani d ? C(16) -0.2524(6) -0.0570(5) -0.0635(3) 0.051(2) 1.000 . Uani d ? C(17) -0.2459(5) 0.0987(5) -0.0063(3) 0.042(2) 1.000 . Uani d ? C(18) -0.1981(4) 0.0611(4) 0.0639(3) 0.033(2) 1.000 . Uani d ? C(19) -0.0096(3) 0.2428(3) 0.2967(2) 0.021(1) 1.000 . Uani d ? C(20) -0.1881(4) -0.0230(4) 0.3654(2) 0.023(1) 1.000 . Uani d ? C(21) -0.3069(3) 0.0886(4) 0.1298(2) 0.024(1) 1.000 . Uani d ? C(22) -0.0932(3) 0.1733(3) 0.2793(2) 0.017(1) 1.000 . Uani d ? C(23) -0.1031(3) 0.1098(4) 0.3267(2) 0.020(1) 1.000 . Uani d ? C(24) -0.1791(3) 0.0437(3) 0.3123(2) 0.018(1) 1.000 . Uani d ? C(25) -0.2458(3) 0.0406(3) 0.2485(2) 0.020(1) 1.000 . Uani d ? C(26) -0.2370(3) 0.1011(4) 0.1996(2) 0.019(1) 1.000 . Uani d ? C(27) -0.1617(3) 0.1691(3) 0.2156(2) 0.020(1) 1.000 . Uani d ? H(1) 0.0120 0.1527 0.1988 0.032 1.000 . Uiso c ? H(2) 0.0645 0.2499 0.1993 0.032 1.000 . Uiso c ? H(3) 0.2114 0.1780 0.2204 0.038 1.000 . Uiso c ? H(4) 0.1391 0.1184 0.1639 0.038 1.000 . Uiso c ? H(5) 0.1612 -0.0032 0.2245 0.037 1.000 . Uiso c ? H(6) 0.3035 -0.0256 0.3020 0.053 1.000 . Uiso c ? H(7) 0.3241 0.0485 0.2543 0.053 1.000 . Uiso c ? H(8) 0.3325 0.1687 0.3227 0.043 1.000 . Uiso c ? H(9) 0.3874 0.0869 0.3694 0.043 1.000 . Uiso c ? H(10) 0.2804 0.0844 0.4157 0.032 1.000 . Uiso c ? H(11) 0.1917 0.2110 0.4183 0.032 1.000 . Uiso c ? H(12) 0.2871 0.2481 0.4082 0.032 1.000 . Uiso c ? H(13) 0.2069 0.2709 0.2980 0.026 1.000 . Uiso c ? H(14) 0.1453 0.3217 0.3353 0.026 1.000 . Uiso c ? H(15) -0.1707 -0.1358 0.4506 0.032 1.000 . Uiso c ? H(16) -0.1388 -0.2294 0.4243 0.032 1.000 . Uiso c ? H(17) -0.0151 -0.1915 0.5193 0.034 1.000 . Uiso c ? H(18) -0.0115 -0.0868 0.4958 0.034 1.000 . Uiso c ? H(19) 0.1121 -0.1611 0.4792 0.034 1.000 . Uiso c ? H(20) 0.1154 -0.3100 0.4732 0.042 1.000 . Uiso c ? H(21) 0.0016 -0.3146 0.4467 0.042 1.000 . Uiso c ? H(22) 0.0423 -0.3697 0.3619 0.048 1.000 . Uiso c ? H(23) 0.1246 -0.2938 0.3721 0.048 1.000 . Uiso c ? H(24) 0.0019 -0.2426 0.2862 0.033 1.000 . Uiso c ? H(25) -0.1403 -0.2961 0.2712 0.036 1.000 . Uiso c ? H(26) -0.1189 -0.3065 0.3466 0.036 1.000 . Uiso c ? H(27) -0.2395 -0.1951 0.3111 0.030 1.000 . Uiso c ? H(28) -0.1814 -0.1396 0.2734 0.030 1.000 . Uiso c ? H(29) -0.1864 -0.0701 0.1537 0.035 1.000 . Uiso c ? H(30) -0.2969 -0.0953 0.1358 0.035 1.000 . Uiso c ? H(31) -0.2331 -0.2114 0.0890 0.040 1.000 . Uiso c ? H(32) -0.1790 -0.1371 0.0596 0.040 1.000 . Uiso c ? H(33) -0.3623 -0.1969 0.0077 0.045 1.000 . Uiso c ? H(34) -0.2513 -0.2009 -0.0503 0.064 1.000 . Uiso c ? H(35) -0.3548 -0.1623 -0.0902 0.064 1.000 . Uiso c ? H(36) -0.2542 -0.0525 -0.1081 0.061 1.000 . Uiso c ? H(37) -0.1862 -0.0542 -0.0350 0.061 1.000 . Uiso c ? H(38) -0.3437 0.0517 -0.0871 0.051 1.000 . Uiso c ? H(39) -0.1961 0.1168 -0.0239 0.050 1.000 . Uiso c ? H(40) -0.2853 0.1529 -0.0053 0.050 1.000 . Uiso c ? H(41) -0.1657 0.1124 0.0918 0.039 1.000 . Uiso c ? H(42) -0.1515 0.0129 0.0639 0.039 1.000 . Uiso c ? H(43) 0.0042 0.2623 0.3412 0.025 1.000 . Uiso c ? H(44) -0.0285 0.2971 0.2685 0.025 1.000 . Uiso c ? H(45) -0.2556 -0.0380 0.3561 0.027 1.000 . Uiso c ? H(46) -0.1639 0.0092 0.4067 0.027 1.000 . Uiso c ? H(47) -0.3159 0.1494 0.1087 0.028 1.000 . Uiso c ? H(48) -0.3680 0.0665 0.1321 0.028 1.000 . Uiso c ? H(49) -0.0567 0.1118 0.3701 0.023 1.000 . Uiso c ? H(50) -0.2986 -0.0039 0.2382 0.024 1.000 . Uiso c ? H(51) -0.1571 0.2129 0.1829 0.023 1.000 . Uiso c ? H(52) 0.1033 0.0358 0.4399 0.025 1.000 . Uiso c ? H(53) -0.0125 -0.0503 0.2474 0.032 1.000 . Uiso c ? H(54) -0.4856 0.1371 -0.0353 0.050 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) 0.0216(3) 0.0162(3) 0.0288(3) -0.0022(2) 0.0135(3) -0.0007(3) Cu(2) 0.0229(3) 0.0156(3) 0.0257(3) -0.0031(3) 0.0098(3) -0.0018(3) Cu(3) 0.0431(4) 0.0222(4) 0.0278(4) -0.0008(3) -0.0017(3) -0.0029(3) Cl(1) 0.0255(7) 0.0266(7) 0.0342(7) -0.0038(5) 0.0084(6) -0.0072(6) Cl(2) 0.063(1) 0.065(1) 0.162(2) -0.018(1) 0.060(2) -0.065(2) Cl(3) 0.0376(9) 0.081(1) 0.050(1) -0.0196(9) 0.0244(8) -0.017(1) O(1) 0.025(2) 0.017(2) 0.024(2) -0.005(1) 0.011(1) -0.006(1) O(2) 0.029(2) 0.026(2) 0.023(2) -0.007(2) 0.008(2) -0.003(2) O(3) 0.046(2) 0.019(2) 0.048(3) -0.001(2) -0.001(2) 0.007(2) O(4) 0.042(3) 0.148(6) 0.069(4) -0.027(3) 0.005(3) -0.054(4) O(5) 0.198(7) 0.045(3) 0.042(3) -0.034(4) 0.029(4) 0.005(3) O(6) 0.160(6) 0.088(4) 0.050(3) -0.091(4) 0.051(4) -0.028(3) O(7) 0.048(4) 0.161(8) 0.203(8) 0.040(4) -0.007(4) -0.125(7) O(8) 0.21(1) 0.18(1) 0.23(1) -0.142(9) 0.124(9) -0.144(9) O(9) 0.165(7) 0.141(7) 0.124(6) 0.022(6) 0.092(6) -0.031(6) O(10) 0.167(6) 0.052(4) 0.081(4) 0.006(4) 0.062(4) -0.021(3) O(11) 0.16(1) 0.118(9) 0.57(3) 0.070(8) 0.19(1) 0.05(1) O(12) 0.036(2) 0.088(4) 0.050(3) -0.021(2) 0.017(2) 0.010(3) O(13) 0.092(4) 0.114(5) 0.049(3) -0.021(4) 0.015(3) -0.012(3) O(14) 0.175(8) 0.32(1) 0.065(4) -0.178(9) -0.010(5) 0.065(7) O(15) 0.094(6) 0.19(1) 0.64(2) -0.097(6) 0.20(1) -0.31(1) O(16) 0.127(5) 0.043(3) 0.063(4) 0.001(3) -0.024(3) 0.000(3) N(1) 0.017(2) 0.017(2) 0.024(2) -0.001(2) 0.010(2) -0.002(2) N(2) 0.034(3) 0.025(3) 0.044(3) 0.000(2) 0.026(2) -0.003(2) N(3) 0.018(2) 0.025(2) 0.036(3) -0.003(2) 0.008(2) 0.011(2) N(4) 0.025(2) 0.017(2) 0.019(2) -0.001(2) 0.008(2) 0.001(2) N(5) 0.025(2) 0.021(2) 0.031(3) -0.003(2) 0.000(2) -0.001(2) N(6) 0.031(2) 0.020(2) 0.031(3) 0.000(2) 0.010(2) -0.007(2) N(7) 0.030(2) 0.024(2) 0.021(2) -0.001(2) 0.008(2) -0.002(2) N(8) 0.048(3) 0.022(3) 0.037(3) 0.001(2) 0.007(2) -0.003(2) N(9) 0.077(4) 0.027(3) 0.022(3) 0.001(3) 0.013(2) -0.005(2) C(1) 0.028(3) 0.028(3) 0.025(3) -0.001(2) 0.011(2) 0.003(2) C(2) 0.038(3) 0.032(3) 0.031(3) -0.004(3) 0.021(3) 0.000(3) C(3) 0.041(4) 0.038(4) 0.068(4) 0.013(3) 0.039(3) 0.013(3) C(4) 0.023(3) 0.032(3) 0.054(4) 0.001(2) 0.016(3) 0.010(3) C(5) 0.025(3) 0.023(3) 0.029(3) -0.010(2) 0.005(2) -0.001(2) C(6) 0.021(3) 0.016(3) 0.029(3) -0.006(2) 0.009(2) -0.002(2) C(7) 0.035(3) 0.021(3) 0.027(3) -0.004(2) 0.014(2) 0.005(2) C(8) 0.039(3) 0.024(3) 0.020(3) -0.003(2) 0.008(2) 0.003(2) C(9) 0.032(3) 0.022(3) 0.047(4) 0.002(2) 0.007(3) 0.004(3) C(10) 0.040(3) 0.019(3) 0.057(4) 0.004(3) 0.012(3) -0.006(3) C(11) 0.036(3) 0.018(3) 0.033(3) -0.007(2) 0.009(3) -0.008(2) C(12) 0.027(3) 0.022(3) 0.023(3) -0.007(2) 0.005(2) -0.003(2) C(13) 0.036(3) 0.025(3) 0.024(3) 0.002(2) 0.006(2) -0.001(2) C(14) 0.041(3) 0.026(3) 0.031(3) 0.003(3) 0.010(3) -0.001(3) C(15) 0.094(5) 0.033(4) 0.032(4) 0.007(4) 0.020(4) -0.009(3) C(16) 0.090(5) 0.038(4) 0.029(3) 0.007(4) 0.026(3) -0.003(3) C(17) 0.066(4) 0.032(4) 0.037(3) -0.003(3) 0.030(3) -0.003(3) C(18) 0.037(3) 0.033(3) 0.034(3) -0.006(3) 0.019(3) -0.005(3) C(19) 0.018(2) 0.015(3) 0.029(3) 0.001(2) 0.007(2) -0.003(2) C(20) 0.024(3) 0.024(3) 0.023(3) 0.001(2) 0.012(2) -0.002(2) C(21) 0.021(3) 0.027(3) 0.022(3) 0.002(2) 0.005(2) 0.001(2) C(22) 0.017(2) 0.014(2) 0.020(2) 0.005(2) 0.006(2) -0.003(2) C(23) 0.019(2) 0.020(3) 0.020(2) 0.004(2) 0.006(2) -0.004(2) C(24) 0.020(2) 0.016(2) 0.022(3) 0.002(2) 0.011(2) -0.002(2) C(25) 0.019(2) 0.017(3) 0.025(3) -0.003(2) 0.009(2) -0.007(2) C(26) 0.017(2) 0.019(3) 0.019(2) 0.003(2) 0.002(2) -0.005(2) C(27) 0.023(3) 0.015(2) 0.023(3) 0.007(2) 0.010(2) 0.002(2) #------------------------------------------------------------------------------ _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)]' _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 6913 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_all 0.0753 _refine_ls_wR_factor_ref 0.0703 _refine_ls_goodness_of_fit_all 1.815 _refine_ls_goodness_of_fit_ref 2.214 _refine_ls_shift/su_max 0.0490 _refine_ls_shift/su_mean 0.0033 _refine_diff_density_min -1.29 _refine_diff_density_max 1.46 #------------------------------------------------------------------------------ _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) Cu(2) 2.8757(8) . . yes Cu(1) O(1) 1.957(3) . . yes Cu(1) O(2) 1.920(3) . . yes Cu(1) N(1) 2.342(4) . . yes Cu(1) N(2) 2.037(4) . . yes Cu(1) N(3) 2.024(4) . . yes Cu(2) O(1) 1.954(3) . . yes Cu(2) O(2) 1.919(4) . . yes Cu(2) N(4) 2.317(4) . . yes Cu(2) N(5) 2.030(4) . . yes Cu(2) N(6) 2.029(4) . . yes Cu(3) Cu(3) 2.961(2) . 3_455 yes Cu(3) O(3) 1.933(4) . . yes Cu(3) O(3) 1.969(4) . 3_455 yes Cu(3) N(7) 2.301(4) . . yes Cu(3) N(8) 2.020(5) . . yes Cu(3) N(9) 2.033(5) . . yes Cl(1) O(4) 1.400(5) . . yes Cl(1) O(5) 1.406(5) . . yes Cl(1) O(6) 1.408(5) . . yes Cl(1) O(7) 1.365(5) . . yes Cl(2) O(8) 1.332(7) . . yes Cl(2) O(9) 1.362(7) . . yes Cl(2) O(10) 1.358(5) . . yes Cl(2) O(11) 1.74(2) . . yes Cl(3) O(12) 1.438(4) . . yes Cl(3) O(13) 1.364(5) . . yes Cl(3) O(14) 1.401(8) . . yes Cl(3) O(15) 1.330(7) . . yes O(1) H(52) 0.82 . . no O(2) H(53) 0.82 . . no O(3) H(54) 0.82 . . no N(1) C(1) 1.468(6) . . yes N(1) C(6) 1.485(6) . . yes N(1) C(19) 1.488(6) . . yes N(2) C(2) 1.485(7) . . yes N(2) C(3) 1.484(7) . . yes N(2) H(5) 0.90 . . no N(3) C(4) 1.493(7) . . yes N(3) C(5) 1.474(7) . . yes N(3) H(10) 0.90 . . no N(4) C(7) 1.476(6) . . yes N(4) C(12) 1.472(6) . . yes N(4) C(20) 1.489(6) . . yes N(5) C(8) 1.484(7) . . yes N(5) C(9) 1.481(7) . . yes N(5) H(19) 0.90 . . no N(6) C(10) 1.488(7) . . yes N(6) C(11) 1.485(7) . . yes N(6) H(24) 0.90 . . no N(7) C(13) 1.464(7) . . yes N(7) C(18) 1.479(7) . . yes N(7) C(21) 1.486(6) . . yes N(8) C(14) 1.486(7) . . yes N(8) C(15) 1.482(8) . . yes N(8) H(33) 0.90 . . no N(9) C(16) 1.483(8) . . yes N(9) C(17) 1.472(8) . . yes N(9) H(38) 0.90 . . no C(1) C(2) 1.519(7) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(3) C(4) 1.485(9) . . yes C(3) H(6) 0.95 . . no C(3) H(7) 0.95 . . no C(4) H(8) 0.95 . . no C(4) H(9) 0.95 . . no C(5) C(6) 1.518(7) . . yes C(5) H(11) 0.95 . . no C(5) H(12) 0.95 . . no C(6) H(13) 0.95 . . no C(6) H(14) 0.95 . . no C(7) C(8) 1.520(7) . . yes C(7) H(15) 0.95 . . no C(7) H(16) 0.95 . . no C(8) H(17) 0.95 . . no C(8) H(18) 0.95 . . no C(9) C(10) 1.506(9) . . yes C(9) H(20) 0.95 . . no C(9) H(21) 0.95 . . no C(10) H(22) 0.95 . . no C(10) H(23) 0.95 . . no C(11) C(12) 1.520(7) . . yes C(11) H(25) 0.95 . . no C(11) H(26) 0.95 . . no C(12) H(27) 0.95 . . no C(12) H(28) 0.95 . . no C(13) C(14) 1.520(7) . . yes C(13) H(29) 0.95 . . no C(13) H(30) 0.95 . . no C(14) H(31) 0.95 . . no C(14) H(32) 0.95 . . no C(15) C(16) 1.50(1) . . yes C(15) H(34) 0.95 . . no C(15) H(35) 0.95 . . no C(16) H(36) 0.95 . . no C(16) H(37) 0.95 . . no C(17) C(18) 1.527(8) . . yes C(17) H(39) 0.95 . . no C(17) H(40) 0.95 . . no C(18) H(41) 0.95 . . no C(18) H(42) 0.95 . . no C(19) C(22) 1.495(6) . . yes C(19) H(43) 0.95 . . no C(19) H(44) 0.95 . . no C(20) C(24) 1.510(7) . . yes C(20) H(45) 0.95 . . no C(20) H(46) 0.95 . . no C(21) C(26) 1.513(7) . . yes C(21) H(47) 0.95 . . no C(21) H(48) 0.95 . . no C(22) C(23) 1.393(7) . . yes C(22) C(27) 1.397(7) . . yes C(23) C(24) 1.386(7) . . yes C(23) H(49) 0.95 . . no C(24) C(25) 1.388(7) . . yes C(25) C(26) 1.384(7) . . yes C(25) H(50) 0.95 . . no C(26) C(27) 1.396(7) . . yes C(27) H(51) 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 Cu(2) Cu(1) O(1) 42.63(9) . . . yes Cu(2) Cu(1) O(2) 41.5(1) . . . yes Cu(2) Cu(1) N(1) 132.23(9) . . . yes Cu(2) Cu(1) N(2) 128.9(1) . . . yes Cu(2) Cu(1) N(3) 130.9(1) . . . yes O(1) Cu(1) O(2) 80.6(1) . . . yes O(1) Cu(1) N(1) 113.1(1) . . . yes O(1) Cu(1) N(2) 165.2(2) . . . yes O(1) Cu(1) N(3) 95.9(2) . . . yes O(2) Cu(1) N(1) 110.3(1) . . . yes O(2) Cu(1) N(2) 96.8(2) . . . yes O(2) Cu(1) N(3) 168.7(2) . . . yes N(1) Cu(1) N(2) 81.5(2) . . . yes N(1) Cu(1) N(3) 81.0(2) . . . yes N(2) Cu(1) N(3) 83.8(2) . . . yes Cu(1) Cu(2) O(1) 42.70(9) . . . yes Cu(1) Cu(2) O(2) 41.5(1) . . . yes Cu(1) Cu(2) N(4) 130.4(1) . . . yes Cu(1) Cu(2) N(5) 132.1(1) . . . yes Cu(1) Cu(2) N(6) 129.0(1) . . . yes O(1) Cu(2) O(2) 80.7(1) . . . yes O(1) Cu(2) N(4) 111.8(1) . . . yes O(1) Cu(2) N(5) 96.3(2) . . . yes O(1) Cu(2) N(6) 165.2(2) . . . yes O(2) Cu(2) N(4) 108.9(1) . . . yes O(2) Cu(2) N(5) 170.4(2) . . . yes O(2) Cu(2) N(6) 96.9(2) . . . yes N(4) Cu(2) N(5) 80.7(2) . . . yes N(4) Cu(2) N(6) 82.8(2) . . . yes N(5) Cu(2) N(6) 83.7(2) . . . yes Cu(3) Cu(3) O(3) 41.1(1) 3_455 . . yes Cu(3) Cu(3) O(3) 40.2(1) 3_455 . 3_455 yes Cu(3) Cu(3) N(7) 114.0(1) 3_455 . . yes Cu(3) Cu(3) N(8) 134.8(1) 3_455 . . yes Cu(3) Cu(3) N(9) 138.0(2) 3_455 . . yes O(3) Cu(3) O(3) 81.3(2) . . 3_455 yes O(3) Cu(3) N(7) 104.7(2) . . . yes O(3) Cu(3) N(8) 172.9(2) . . . yes O(3) Cu(3) N(9) 98.3(2) . . . yes O(3) Cu(3) N(7) 111.2(2) 3_455 . . yes O(3) Cu(3) N(8) 94.9(2) 3_455 . . yes O(3) Cu(3) N(9) 167.5(2) 3_455 . . yes N(7) Cu(3) N(8) 82.3(2) . . . yes N(7) Cu(3) N(9) 81.1(2) . . . yes N(8) Cu(3) N(9) 84.2(2) . . . yes O(4) Cl(1) O(5) 116.7(4) . . . yes O(4) Cl(1) O(6) 111.7(3) . . . yes O(4) Cl(1) O(7) 105.3(4) . . . yes O(5) Cl(1) O(6) 108.4(3) . . . yes O(5) Cl(1) O(7) 104.7(5) . . . yes O(6) Cl(1) O(7) 109.6(5) . . . yes O(8) Cl(2) O(9) 119.1(5) . . . yes O(8) Cl(2) O(10) 114.8(6) . . . yes O(8) Cl(2) O(11) 94.5(7) . . . yes O(9) Cl(2) O(10) 115.7(5) . . . yes O(9) Cl(2) O(11) 107.2(5) . . . yes O(10) Cl(2) O(11) 100.7(6) . . . yes O(12) Cl(3) O(13) 112.1(3) . . . yes O(12) Cl(3) O(14) 110.4(4) . . . yes O(12) Cl(3) O(15) 109.8(4) . . . yes O(13) Cl(3) O(14) 104.5(5) . . . yes O(13) Cl(3) O(15) 110.2(7) . . . yes O(14) Cl(3) O(15) 109.7(8) . . . yes Cu(1) O(1) Cu(2) 94.7(1) . . . yes Cu(1) O(1) H(52) 132.7 . . . no Cu(2) O(1) H(52) 132.7 . . . no Cu(1) O(2) Cu(2) 97.0(1) . . . yes Cu(1) O(2) H(53) 131.5 . . . no Cu(2) O(2) H(53) 131.5 . . . no Cu(3) O(3) Cu(3) 98.7(2) . . 3_455 yes Cu(3) O(3) H(54) 130.6 . . . no Cu(3) O(3) H(54) 130.7 3_455 . . no Cu(1) N(1) C(1) 98.8(3) . . . yes Cu(1) N(1) C(6) 104.7(3) . . . yes Cu(1) N(1) C(19) 119.4(3) . . . yes C(1) N(1) C(6) 112.7(4) . . . yes C(1) N(1) C(19) 110.8(4) . . . yes C(6) N(1) C(19) 110.0(4) . . . yes Cu(1) N(2) C(2) 113.8(3) . . . yes Cu(1) N(2) C(3) 102.7(3) . . . yes Cu(1) N(2) H(5) 108.8 . . . no C(2) N(2) C(3) 113.8(4) . . . yes C(2) N(2) H(5) 108.8 . . . no C(3) N(2) H(5) 108.8 . . . no Cu(1) N(3) C(4) 110.4(3) . . . yes Cu(1) N(3) C(5) 107.8(3) . . . yes Cu(1) N(3) H(10) 108.1 . . . no C(4) N(3) C(5) 114.1(4) . . . yes C(4) N(3) H(10) 108.1 . . . no C(5) N(3) H(10) 108.1 . . . no Cu(2) N(4) C(7) 106.1(3) . . . yes Cu(2) N(4) C(12) 97.5(3) . . . yes Cu(2) N(4) C(20) 118.8(3) . . . yes C(7) N(4) C(12) 112.6(4) . . . yes C(7) N(4) C(20) 109.5(4) . . . yes C(12) N(4) C(20) 111.8(4) . . . yes Cu(2) N(5) C(8) 108.6(3) . . . yes Cu(2) N(5) C(9) 110.7(3) . . . yes Cu(2) N(5) H(19) 107.8 . . . no C(8) N(5) C(9) 113.8(4) . . . yes C(8) N(5) H(19) 107.8 . . . no C(9) N(5) H(19) 107.8 . . . no Cu(2) N(6) C(10) 103.4(3) . . . yes Cu(2) N(6) C(11) 112.3(3) . . . yes Cu(2) N(6) H(24) 109.1 . . . no C(10) N(6) C(11) 113.7(4) . . . yes C(10) N(6) H(24) 109.1 . . . no C(11) N(6) H(24) 109.1 . . . no Cu(3) N(7) C(13) 98.6(3) . . . yes Cu(3) N(7) C(18) 106.0(3) . . . yes Cu(3) N(7) C(21) 110.9(3) . . . yes C(13) N(7) C(18) 113.2(4) . . . yes C(13) N(7) C(21) 114.2(4) . . . yes C(18) N(7) C(21) 112.8(4) . . . yes Cu(3) N(8) C(14) 113.3(3) . . . yes Cu(3) N(8) C(15) 103.0(4) . . . yes Cu(3) N(8) H(33) 108.6 . . . no C(14) N(8) C(15) 114.6(5) . . . yes C(14) N(8) H(33) 108.6 . . . no C(15) N(8) H(33) 108.6 . . . no Cu(3) N(9) C(16) 110.0(4) . . . yes Cu(3) N(9) C(17) 107.9(3) . . . yes Cu(3) N(9) H(38) 108.2 . . . no C(16) N(9) C(17) 114.2(5) . . . yes C(16) N(9) H(38) 108.2 . . . no C(17) N(9) H(38) 108.2 . . . no N(1) C(1) C(2) 113.0(4) . . . yes N(1) C(1) H(1) 108.6 . . . no N(1) C(1) H(2) 108.6 . . . no C(2) C(1) H(1) 108.6 . . . no C(2) C(1) H(2) 108.6 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 111.9(4) . . . yes N(2) C(2) H(3) 108.8 . . . no N(2) C(2) H(4) 108.9 . . . no C(1) C(2) H(3) 108.9 . . . no C(1) C(2) H(4) 108.9 . . . no H(3) C(2) H(4) 109.5 . . . no N(2) C(3) C(4) 110.8(5) . . . yes N(2) C(3) H(6) 109.1 . . . no N(2) C(3) H(7) 109.1 . . . no C(4) C(3) H(6) 109.1 . . . no C(4) C(3) H(7) 109.1 . . . no H(6) C(3) H(7) 109.5 . . . no N(3) C(4) C(3) 110.1(4) . . . yes N(3) C(4) H(8) 109.3 . . . no N(3) C(4) H(9) 109.3 . . . no C(3) C(4) H(8) 109.3 . . . no C(3) C(4) H(9) 109.3 . . . no H(8) C(4) H(9) 109.5 . . . no N(3) C(5) C(6) 111.2(4) . . . yes N(3) C(5) H(11) 109.0 . . . no N(3) C(5) H(12) 109.0 . . . no C(6) C(5) H(11) 109.0 . . . no C(6) C(5) H(12) 109.0 . . . no H(11) C(5) H(12) 109.5 . . . no N(1) C(6) C(5) 110.4(4) . . . yes N(1) C(6) H(13) 109.2 . . . no N(1) C(6) H(14) 109.2 . . . no C(5) C(6) H(13) 109.3 . . . no C(5) C(6) H(14) 109.2 . . . no H(13) C(6) H(14) 109.5 . . . no N(4) C(7) C(8) 110.4(4) . . . yes N(4) C(7) H(15) 109.2 . . . no N(4) C(7) H(16) 109.2 . . . no C(8) C(7) H(15) 109.3 . . . no C(8) C(7) H(16) 109.3 . . . no H(15) C(7) H(16) 109.5 . . . no N(5) C(8) C(7) 110.6(4) . . . yes N(5) C(8) H(17) 109.2 . . . no N(5) C(8) H(18) 109.2 . . . no C(7) C(8) H(17) 109.2 . . . no C(7) C(8) H(18) 109.2 . . . no H(17) C(8) H(18) 109.5 . . . no N(5) C(9) C(10) 110.2(5) . . . yes N(5) C(9) H(20) 109.3 . . . no N(5) C(9) H(21) 109.3 . . . no C(10) C(9) H(20) 109.3 . . . no C(10) C(9) H(21) 109.3 . . . no H(20) C(9) H(21) 109.5 . . . no N(6) C(10) C(9) 109.8(5) . . . yes N(6) C(10) H(22) 109.4 . . . no N(6) C(10) H(23) 109.4 . . . no C(9) C(10) H(22) 109.4 . . . no C(9) C(10) H(23) 109.4 . . . no H(22) C(10) H(23) 109.5 . . . no N(6) C(11) C(12) 111.7(4) . . . yes N(6) C(11) H(25) 108.9 . . . no N(6) C(11) H(26) 108.9 . . . no C(12) C(11) H(25) 108.9 . . . no C(12) C(11) H(26) 108.9 . . . no H(25) C(11) H(26) 109.5 . . . no N(4) C(12) C(11) 112.7(4) . . . yes N(4) C(12) H(27) 108.7 . . . no N(4) C(12) H(28) 108.7 . . . no C(11) C(12) H(27) 108.7 . . . no C(11) C(12) H(28) 108.7 . . . no H(27) C(12) H(28) 109.5 . . . no N(7) C(13) C(14) 112.7(4) . . . yes N(7) C(13) H(29) 108.7 . . . no N(7) C(13) H(30) 108.7 . . . no C(14) C(13) H(29) 108.7 . . . no C(14) C(13) H(30) 108.7 . . . no H(29) C(13) H(30) 109.5 . . . no N(8) C(14) C(13) 111.2(4) . . . yes N(8) C(14) H(31) 109.0 . . . no N(8) C(14) H(32) 109.0 . . . no C(13) C(14) H(31) 109.1 . . . no C(13) C(14) H(32) 109.1 . . . no H(31) C(14) H(32) 109.5 . . . no N(8) C(15) C(16) 110.0(5) . . . yes N(8) C(15) H(34) 109.3 . . . no N(8) C(15) H(35) 109.4 . . . no C(16) C(15) H(34) 109.3 . . . no C(16) C(15) H(35) 109.3 . . . no H(34) C(15) H(35) 109.5 . . . no N(9) C(16) C(15) 110.1(6) . . . yes N(9) C(16) H(36) 109.3 . . . no N(9) C(16) H(37) 109.3 . . . no C(15) C(16) H(36) 109.3 . . . no C(15) C(16) H(37) 109.3 . . . no H(36) C(16) H(37) 109.4 . . . no N(9) C(17) C(18) 110.5(5) . . . yes N(9) C(17) H(39) 109.2 . . . no N(9) C(17) H(40) 109.2 . . . no C(18) C(17) H(39) 109.2 . . . no C(18) C(17) H(40) 109.2 . . . no H(39) C(17) H(40) 109.5 . . . no N(7) C(18) C(17) 110.1(4) . . . yes N(7) C(18) H(41) 109.3 . . . no N(7) C(18) H(42) 109.3 . . . no C(17) C(18) H(41) 109.3 . . . no C(17) C(18) H(42) 109.3 . . . no H(41) C(18) H(42) 109.5 . . . no N(1) C(19) C(22) 112.8(4) . . . yes N(1) C(19) H(43) 108.6 . . . no N(1) C(19) H(44) 108.6 . . . no C(22) C(19) H(43) 108.6 . . . no C(22) C(19) H(44) 108.6 . . . no H(43) C(19) H(44) 109.5 . . . no N(4) C(20) C(24) 113.4(4) . . . yes N(4) C(20) H(45) 108.5 . . . no N(4) C(20) H(46) 108.5 . . . no C(24) C(20) H(45) 108.5 . . . no C(24) C(20) H(46) 108.5 . . . no H(45) C(20) H(46) 109.5 . . . no N(7) C(21) C(26) 114.8(4) . . . yes N(7) C(21) H(47) 108.1 . . . no N(7) C(21) H(48) 108.1 . . . no C(26) C(21) H(47) 108.1 . . . no C(26) C(21) H(48) 108.1 . . . no H(47) C(21) H(48) 109.5 . . . no C(19) C(22) C(23) 120.0(4) . . . yes C(19) C(22) C(27) 121.5(4) . . . yes C(23) C(22) C(27) 118.5(4) . . . yes C(22) C(23) C(24) 121.6(4) . . . yes C(22) C(23) H(49) 119.2 . . . no C(24) C(23) H(49) 119.2 . . . no C(20) C(24) C(23) 120.0(4) . . . yes C(20) C(24) C(25) 121.4(4) . . . yes C(23) C(24) C(25) 118.6(4) . . . yes C(24) C(25) C(26) 121.4(4) . . . yes C(24) C(25) H(50) 119.3 . . . no C(26) C(25) H(50) 119.3 . . . no C(21) C(26) C(25) 118.8(4) . . . yes C(21) C(26) C(27) 122.0(4) . . . yes C(25) C(26) C(27) 119.1(4) . . . yes C(22) C(27) C(26) 120.6(4) . . . yes C(22) C(27) H(51) 119.7 . . . no C(26) C(27) H(51) 119.7 . . . 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(3) O(14) 3.349(7) . 1_454 no Cl(3) N(9) 3.578(5) . 1_656 no O(1) O(5) 3.215(7) . 2_546 no O(1) O(7) 3.370(7) . 2_546 no O(1) C(8) 3.554(6) . 3_556 no O(2) O(9) 2.975(8) . 3_656 no O(3) O(16) 2.873(7) . 4_455 no O(3) O(10) 3.057(7) . 4_354 no O(5) N(3) 3.123(7) . 2_556 no O(5) C(9) 3.373(9) . 1_565 no O(5) C(20) 3.565(8) . 4 no O(5) C(10) 3.590(8) . 1_565 no O(6) N(3) 3.135(7) . 2_556 no O(6) C(4) 3.334(8) . 2_556 no O(6) C(9) 3.549(8) . 3_556 no O(6) C(3) 3.552(8) . 2_556 no O(6) C(7) 3.596(8) . 3_556 no O(7) N(5) 2.920(7) . 2_556 no O(7) C(5) 3.081(8) . . no O(7) C(9) 3.480(8) . 2_556 no O(8) N(2) 2.914(9) . 3_656 no O(8) O(12) 3.41(1) . . no O(8) C(16) 3.50(1) . 1_656 no O(8) C(2) 3.51(1) . 3_656 no O(8) C(3) 3.53(1) . 3_656 no O(9) O(15) 3.40(1) . 4 no O(9) C(14) 3.50(1) . 3_656 no O(10) O(16) 3.141(8) . 1_656 no O(10) O(15) 3.15(1) . 4 no O(10) N(8) 3.207(7) . 2_556 no O(10) C(14) 3.256(8) . 2_556 no O(10) C(13) 3.437(8) . 2_556 no O(11) O(16) 2.96(2) . 1_656 no O(12) N(9) 3.027(6) . 1_656 no O(12) C(11) 3.361(7) . 2_556 no O(12) C(3) 3.405(8) . 3_656 no O(12) C(16) 3.486(8) . 1_656 no O(13) C(10) 3.370(9) . 2_556 no O(13) C(3) 3.406(8) . 3_656 no O(14) N(9) 3.084(8) . 1_656 no O(14) C(16) 3.37(1) . 1_656 no O(14) C(15) 3.38(1) . 1_656 no O(14) C(21) 3.45(1) . 3_556 no O(15) C(25) 3.322(8) . 3_556 no O(16) N(8) 3.171(8) . 2_455 no O(16) C(21) 3.476(7) . 4 no O(16) C(1) 3.585(8) . . no C(4) C(19) 3.513(7) . 4 no C(6) C(24) 3.574(7) . 4 no #------------------------------------------------------------------------------ #===END