# Copyright The Royal Society of Chemistry, 1998 ### Supplementary crystallographic data Bernhardt and Sharpe ### Manuscript reference 8/00297E/DAP (Dalton Transactions) ###[CuL1](ClO4)2 data_1178ps14 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H40 Cl4 Cu2 N8 O18' _chemical_formula_weight 877.42 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.215(4) _cell_length_b 14.9140(10) _cell_length_c 15.528(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.080(10) _cell_angle_gamma 90.00 _cell_volume 3432.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description 'prism' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method ? _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.632 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'ENRAF-NONIUS CAD4' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5861 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.96 _reflns_number_total 5636 _reflns_number_observed 3943 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'XTAL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+7.3283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5636 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_obs 0.0458 _refine_ls_wR_factor_all 0.1410 _refine_ls_wR_factor_obs 0.1210 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_restrained_S_all 1.022 _refine_ls_restrained_S_obs 1.064 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.30222(4) 0.11743(4) 0.48149(4) 0.0347(2) Uani 1 d . . N11 N 0.3806(4) 0.1704(4) 0.4049(4) 0.073(2) Uani 1 d . . H11A H 0.4122(4) 0.2170(4) 0.4329(4) 0.087 Uiso 1 d R . H11B H 0.4200(4) 0.1289(4) 0.3947(4) 0.087 Uiso 1 d R . N12 N 0.2020(3) 0.1306(3) 0.3723(3) 0.0476(11) Uani 1 d . . H12 H 0.1750(3) 0.1845(3) 0.3761(3) 0.057 Uiso 1 d R . N13 N 0.2189(3) 0.0752(3) 0.5566(3) 0.0392(10) Uani 1 d . . H13 H 0.1919(3) 0.1251(3) 0.5724(3) 0.047 Uiso 1 d R . N14 N 0.3991(3) 0.1044(4) 0.5918(3) 0.0593(13) Uani 1 d . . H14A H 0.4313(3) 0.0543(4) 0.5892(3) 0.071 Uiso 1 d R . H14B H 0.4367(3) 0.1517(4) 0.5980(3) 0.071 Uiso 1 d R . O11 O 0.0495(3) 0.1423(3) 0.4503(3) 0.0674(12) Uani 1 d . . H11 H 0.0566(3) 0.1522(3) 0.5033(3) 0.101 Uiso 1 d R . C11 C 0.3229(6) 0.2010(5) 0.3206(5) 0.084(3) Uani 1 d . . H11C H 0.3570(6) 0.2016(5) 0.2748(5) 0.101 Uiso 1 d R . H11D H 0.3007(6) 0.2611(5) 0.3266(5) 0.101 Uiso 1 d R . C12 C 0.2441(5) 0.1351(5) 0.2964(4) 0.070(2) Uani 1 d . . H12A H 0.2006(5) 0.1557(5) 0.2444(4) 0.085 Uiso 1 d R . H12B H 0.2656(5) 0.0764(5) 0.2840(4) 0.085 Uiso 1 d R . C13 C 0.1282(4) 0.0585(4) 0.3590(4) 0.061(2) Uani 1 d . . H13A H 0.0817(4) 0.0732(4) 0.3070(4) 0.073 Uiso 1 d R . H13B H 0.1539(4) 0.0011(4) 0.3485(4) 0.073 Uiso 1 d R . C14 C 0.0854(4) 0.0502(4) 0.4377(4) 0.058(2) Uani 1 d . . H14 H 0.0331(4) 0.0105(4) 0.4200(4) 0.070 Uiso 1 d R . C15 C 0.1449(4) 0.0110(4) 0.5196(4) 0.0535(15) Uani 1 d . . H15A H 0.1095(4) -0.0009(4) 0.5630(4) 0.064 Uiso 1 d R . H15B H 0.1704(4) -0.0452(4) 0.5053(4) 0.064 Uiso 1 d R . C16 C 0.2750(5) 0.0371(4) 0.6401(4) 0.062(2) Uani 1 d . . H16A H 0.2946(5) -0.0231(4) 0.6302(4) 0.074 Uiso 1 d R . H16B H 0.2412(5) 0.0351(4) 0.6860(4) 0.074 Uiso 1 d R . C17 C 0.3560(5) 0.0996(5) 0.6659(4) 0.068(2) Uani 1 d . . H17A H 0.3363(5) 0.1587(5) 0.6794(4) 0.081 Uiso 1 d R . H17B H 0.3980(5) 0.0767(5) 0.7177(4) 0.081 Uiso 1 d R . Cu2 Cu 0.73406(4) 0.12270(4) 0.00046(4) 0.0360(2) Uani 1 d . . N21 N 0.6001(3) 0.1004(3) -0.0325(3) 0.0456(11) Uani 1 d . . H21A H 0.5890(3) 0.0410(3) -0.0356(3) 0.055 Uiso 1 d R . H21B H 0.5735(3) 0.1241(3) 0.0085(3) 0.055 Uiso 1 d R . N22 N 0.7198(3) 0.1624(3) -0.1260(3) 0.0403(10) Uani 1 d . . H22 H 0.7153(3) 0.2233(3) -0.1273(3) 0.048 Uiso 1 d R . N23 N 0.8685(3) 0.1464(3) 0.0322(3) 0.0395(10) Uani 1 d . . H23 H 0.8761(3) 0.2061(3) 0.0435(3) 0.047 Uiso 1 d R . N24 N 0.7493(3) 0.0888(4) 0.1289(3) 0.0530(12) Uani 1 d . . H24A H 0.7069(3) 0.1160(4) 0.1517(3) 0.064 Uiso 1 d R . H24B H 0.7434(3) 0.0291(4) 0.1340(3) 0.064 Uiso 1 d R . C21 C 0.5639(4) 0.1425(4) -0.1194(4) 0.0504(14) Uani 1 d . . H21C H 0.5565(4) 0.2065(4) -0.1124(4) 0.060 Uiso 1 d R . H21D H 0.5057(4) 0.1169(4) -0.1468(4) 0.060 Uiso 1 d R . C22 C 0.6304(4) 0.1253(4) -0.1752(4) 0.0489(14) Uani 1 d . . H22A H 0.6111(4) 0.1546(4) -0.2321(4) 0.059 Uiso 1 d R . H22B H 0.6355(4) 0.0614(4) -0.1849(4) 0.059 Uiso 1 d R . C23 C 0.7927(4) 0.1374(5) -0.1713(4) 0.061(2) Uani 1 d . . H23A H 0.7787(4) 0.1611(5) -0.2310(4) 0.073 Uiso 1 d R . H23B H 0.7958(4) 0.0726(5) -0.1750(4) 0.073 Uiso 1 d R . C24 C 0.8842(4) 0.1733(5) -0.1219(4) 0.063(2) Uani 1 d . . H24 H 0.9273(4) 0.1640(5) -0.1594(4) 0.076 Uiso 1 d R . C25 C 0.9207(4) 0.1237(4) -0.0342(4) 0.060(2) Uani 1 d . . H25A H 0.9178(4) 0.0595(4) -0.0446(4) 0.072 Uiso 1 d R . H25B H 0.9834(4) 0.1398(4) -0.0115(4) 0.072 Uiso 1 d R . C26 C 0.9030(4) 0.0979(4) 0.1171(4) 0.0511(14) Uani 1 d . . H26A H 0.9050(4) 0.0339(4) 0.1068(4) 0.061 Uiso 1 d R . H26B H 0.9635(4) 0.1183(4) 0.1441(4) 0.061 Uiso 1 d R . C27 C 0.8409(4) 0.1180(4) 0.1766(4) 0.0559(15) Uani 1 d . . H27A H 0.8593(4) 0.0851(4) 0.2317(4) 0.067 Uiso 1 d R . H27B H 0.8412(4) 0.1815(4) 0.1899(4) 0.067 Uiso 1 d R . O21 O 0.8752(3) 0.2737(3) -0.1096(3) 0.0701(13) Uani 1 d . . H21 H 0.9255(3) 0.2967(3) -0.0992(3) 0.105 Uiso 1 d R . Cl1 Cl 1.04335(10) 0.17201(10) -0.30206(9) 0.0520(4) Uani 1 d . . O1A O 1.0384(3) 0.2437(3) -0.2398(3) 0.0755(14) Uani 1 d . . O1B1 O 1.0721(8) 0.0802(7) -0.2780(7) 0.066(3) Uiso 0.478(12) d P 1 O1C1 O 0.9455(8) 0.1702(8) -0.3529(8) 0.081(4) Uiso 0.478(12) d P 1 O1D1 O 1.0926(9) 0.2098(9) -0.3633(9) 0.094(4) Uiso 0.478(12) d P 1 O1B2 O 1.0326(8) 0.0799(7) -0.2601(7) 0.073(3) Uiso 0.522(12) d P 2 O1C2 O 0.9884(6) 0.1787(6) -0.3863(6) 0.066(3) Uiso 0.522(12) d P 2 O1D2 O 1.1366(9) 0.1803(9) -0.3088(10) 0.110(5) Uiso 0.522(12) d P 2 Cl2 Cl 0.64654(9) 0.13950(8) 0.54743(8) 0.0402(3) Uani 1 d . . O2A O 0.6708(5) 0.0521(4) 0.5884(5) 0.121(2) Uani 1 d . . O2B1 O 0.5704(9) 0.1963(8) 0.5558(9) 0.077(4) Uiso 0.428(14) d P 1 O2C1 O 0.7236(11) 0.1969(12) 0.5766(13) 0.122(7) Uiso 0.428(14) d P 1 O2D1 O 0.6382(16) 0.1318(13) 0.4558(14) 0.146(8) Uiso 0.428(14) d P 1 O2B2 O 0.6143(9) 0.2036(8) 0.6010(9) 0.112(4) Uiso 0.572(14) d P 2 O2C2 O 0.7127(6) 0.1823(6) 0.5084(6) 0.070(3) Uiso 0.572(14) d P 2 O2D2 O 0.5740(10) 0.1102(8) 0.4755(9) 0.121(5) Uiso 0.572(14) d P 2 Cl3 Cl 0.52997(9) 0.12662(9) 0.21468(9) 0.0453(3) Uani 1 d . . O3A O 0.6217(3) 0.1493(3) 0.2547(3) 0.0680(12) Uani 1 d . . O3B O 0.4806(3) 0.2140(3) 0.1971(3) 0.0703(13) Uani 1 d . . O3C O 0.4917(3) 0.0687(3) 0.2731(3) 0.0709(13) Uani 1 d . . O3D O 0.5290(4) 0.0738(4) 0.1367(3) 0.094(2) Uani 1 d . . Cl4 Cl 0.74323(15) -0.13103(10) -0.00316(12) 0.0750(6) Uani 1 d . . O4A O 0.7557(4) -0.0503(3) -0.0529(3) 0.084(2) Uani 1 d . . O4B O 0.7294(4) -0.2165(3) -0.0498(4) 0.098(2) Uani 1 d . . O4C O 0.6616(6) -0.1128(4) 0.0300(6) 0.143(3) Uani 1 d . . O4D O 0.8120(6) -0.1406(5) 0.0706(5) 0.163(4) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0291(3) 0.0357(3) 0.0409(3) 0.0031(3) 0.0114(2) -0.0023(3) N11 0.061(3) 0.073(4) 0.097(5) 0.010(3) 0.046(3) -0.004(3) N12 0.055(3) 0.050(3) 0.038(2) 0.000(2) 0.013(2) 0.016(2) N13 0.041(2) 0.036(2) 0.045(2) 0.001(2) 0.019(2) 0.002(2) N14 0.045(3) 0.057(3) 0.068(3) -0.006(3) -0.004(2) 0.001(2) O11 0.046(2) 0.080(3) 0.073(3) -0.005(2) 0.007(2) 0.017(2) C11 0.122(7) 0.068(5) 0.089(5) 0.031(4) 0.081(5) 0.029(5) C12 0.103(6) 0.069(5) 0.045(4) 0.010(3) 0.028(4) 0.028(4) C13 0.058(4) 0.059(4) 0.055(4) -0.017(3) -0.010(3) 0.003(3) C14 0.036(3) 0.058(4) 0.082(4) -0.021(3) 0.019(3) -0.008(3) C15 0.046(3) 0.045(3) 0.079(4) -0.003(3) 0.035(3) -0.009(3) C16 0.087(5) 0.057(4) 0.046(3) 0.020(3) 0.026(3) 0.016(3) C17 0.086(5) 0.057(4) 0.050(4) -0.006(3) -0.007(3) 0.016(4) Cu2 0.0369(3) 0.0381(4) 0.0329(3) 0.0000(3) 0.0080(2) -0.0019(3) N21 0.043(2) 0.048(3) 0.046(3) -0.001(2) 0.012(2) -0.006(2) N22 0.050(3) 0.033(2) 0.038(2) 0.002(2) 0.009(2) -0.007(2) N23 0.038(2) 0.037(2) 0.043(2) 0.004(2) 0.008(2) -0.001(2) N24 0.058(3) 0.067(3) 0.037(2) -0.003(2) 0.016(2) -0.003(3) C21 0.040(3) 0.048(3) 0.058(4) -0.006(3) -0.001(3) -0.002(3) C22 0.057(3) 0.044(3) 0.040(3) 0.001(3) -0.002(3) -0.007(3) C23 0.071(4) 0.076(4) 0.041(3) -0.004(3) 0.025(3) -0.011(3) C24 0.054(4) 0.083(5) 0.060(4) 0.009(3) 0.029(3) -0.011(3) C25 0.046(3) 0.070(4) 0.067(4) 0.001(3) 0.021(3) 0.005(3) C26 0.046(3) 0.050(3) 0.051(3) 0.005(3) -0.002(3) 0.000(3) C27 0.067(4) 0.060(4) 0.036(3) 0.000(3) 0.000(3) 0.000(3) O21 0.058(3) 0.071(3) 0.077(3) 0.021(2) 0.008(2) -0.025(2) Cl1 0.0599(9) 0.0483(8) 0.0502(8) -0.0103(7) 0.0179(7) -0.0015(7) O1A 0.097(4) 0.074(3) 0.062(3) -0.025(2) 0.032(3) -0.006(3) Cl2 0.0472(7) 0.0354(7) 0.0402(7) 0.0005(5) 0.0143(5) 0.0072(5) O2A 0.174(6) 0.063(4) 0.131(5) 0.041(4) 0.044(5) 0.021(4) Cl3 0.0480(7) 0.0424(7) 0.0500(7) 0.0007(6) 0.0207(6) -0.0014(6) O3A 0.049(2) 0.076(3) 0.079(3) 0.012(3) 0.013(2) 0.005(2) O3B 0.054(3) 0.066(3) 0.093(3) 0.022(3) 0.020(2) 0.016(2) O3C 0.083(3) 0.064(3) 0.080(3) 0.015(2) 0.047(3) -0.003(2) O3D 0.115(4) 0.101(4) 0.078(3) -0.039(3) 0.048(3) -0.039(3) Cl4 0.1090(15) 0.0281(7) 0.0727(11) 0.0058(7) -0.0115(10) -0.0072(8) O4A 0.133(5) 0.042(3) 0.084(3) 0.013(2) 0.036(3) 0.002(3) O4B 0.129(5) 0.048(3) 0.112(4) -0.017(3) 0.018(4) -0.011(3) O4C 0.209(9) 0.083(4) 0.171(7) 0.026(4) 0.116(7) 0.023(5) O4D 0.183(8) 0.121(6) 0.130(6) 0.039(5) -0.078(6) -0.056(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N14 2.001(5) . ? Cu1 N13 2.008(4) . ? Cu1 N12 2.017(5) . ? Cu1 N11 2.026(5) . ? N11 C11 1.475(9) . ? N12 C12 1.466(8) . ? N12 C13 1.535(8) . ? N13 C15 1.491(7) . ? N13 C16 1.493(7) . ? N14 C17 1.448(9) . ? O11 C14 1.506(7) . ? C11 C12 1.530(11) . ? C13 C14 1.514(9) . ? C14 C15 1.503(9) . ? C16 C17 1.525(9) . ? Cu2 N21 2.014(4) . ? Cu2 N22 2.016(4) . ? Cu2 N24 2.019(4) . ? Cu2 N23 2.024(4) . ? N21 C21 1.478(7) . ? N22 C23 1.488(7) . ? N22 C22 1.506(7) . ? N23 C25 1.476(7) . ? N23 C26 1.492(7) . ? N24 C27 1.488(7) . ? C21 C22 1.495(8) . ? C23 C24 1.526(9) . ? C24 O21 1.520(8) . ? C24 C25 1.539(9) . ? C26 C27 1.493(8) . ? Cl1 O1C2 1.387(9) . ? Cl1 O1D1 1.451(13) . ? Cl1 O1D2 1.452(13) . ? Cl1 O1A 1.455(4) . ? Cl1 O1B1 1.460(10) . ? Cl1 O1C1 1.519(11) . ? Cl1 O1B2 1.545(11) . ? Cl2 O2D1 1.40(2) . ? Cl2 O2B2 1.426(12) . ? Cl2 O2C2 1.437(9) . ? Cl2 O2C1 1.44(2) . ? Cl2 O2D2 1.449(13) . ? Cl2 O2A 1.461(5) . ? Cl2 O2B1 1.463(13) . ? Cl3 O3A 1.434(5) . ? Cl3 O3D 1.442(5) . ? Cl3 O3C 1.466(4) . ? Cl3 O3B 1.498(4) . ? Cl4 O4D 1.373(6) . ? Cl4 O4B 1.458(5) . ? Cl4 O4A 1.466(5) . ? Cl4 O4C 1.472(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N14 Cu1 N13 84.9(2) . . ? N14 Cu1 N12 178.4(2) . . ? N13 Cu1 N12 93.6(2) . . ? N14 Cu1 N11 97.1(2) . . ? N13 Cu1 N11 175.0(2) . . ? N12 Cu1 N11 84.4(2) . . ? C11 N11 Cu1 109.3(4) . . ? C12 N12 C13 111.3(5) . . ? C12 N12 Cu1 107.2(4) . . ? C13 N12 Cu1 115.9(3) . . ? C15 N13 C16 108.9(4) . . ? C15 N13 Cu1 119.9(3) . . ? C16 N13 Cu1 108.2(3) . . ? C17 N14 Cu1 107.8(4) . . ? N11 C11 C12 107.2(5) . . ? N12 C12 C11 107.0(5) . . ? C14 C13 N12 112.5(5) . . ? C15 C14 O11 114.3(5) . . ? C15 C14 C13 115.4(5) . . ? O11 C14 C13 105.4(5) . . ? N13 C15 C14 109.5(5) . . ? N13 C16 C17 105.3(5) . . ? N14 C17 C16 107.8(5) . . ? N21 Cu2 N22 85.5(2) . . ? N21 Cu2 N24 95.3(2) . . ? N22 Cu2 N24 177.4(2) . . ? N21 Cu2 N23 179.2(2) . . ? N22 Cu2 N23 93.8(2) . . ? N24 Cu2 N23 85.4(2) . . ? C21 N21 Cu2 107.9(3) . . ? C23 N22 C22 110.7(4) . . ? C23 N22 Cu2 117.3(4) . . ? C22 N22 Cu2 105.7(3) . . ? C25 N23 C26 111.7(4) . . ? C25 N23 Cu2 117.6(4) . . ? C26 N23 Cu2 105.3(3) . . ? C27 N24 Cu2 107.7(3) . . ? N21 C21 C22 107.2(4) . . ? C21 C22 N22 107.2(4) . . ? N22 C23 C24 111.6(5) . . ? O21 C24 C23 108.2(5) . . ? O21 C24 C25 112.7(5) . . ? C23 C24 C25 112.4(5) . . ? N23 C25 C24 111.4(5) . . ? N23 C26 C27 107.8(4) . . ? N24 C27 C26 106.6(4) . . ? O1C2 Cl1 O1D2 108.4(7) . . ? O1C2 Cl1 O1A 117.6(4) . . ? O1D1 Cl1 O1A 105.2(5) . . ? O1D2 Cl1 O1A 100.6(6) . . ? O1D1 Cl1 O1B1 111.3(7) . . ? O1A Cl1 O1B1 125.2(5) . . ? O1D1 Cl1 O1C1 104.9(7) . . ? O1A Cl1 O1C1 99.6(5) . . ? O1B1 Cl1 O1C1 108.5(6) . . ? O1C2 Cl1 O1B2 111.3(5) . . ? O1D2 Cl1 O1B2 107.7(7) . . ? O1A Cl1 O1B2 110.3(5) . . ? O2B2 Cl2 O2C2 108.3(6) . . ? O2D1 Cl2 O2C1 104.4(11) . . ? O2B2 Cl2 O2D2 110.4(8) . . ? O2C2 Cl2 O2D2 107.1(7) . . ? O2D1 Cl2 O2A 108.9(8) . . ? O2B2 Cl2 O2A 115.5(6) . . ? O2C2 Cl2 O2A 116.6(4) . . ? O2C1 Cl2 O2A 106.6(8) . . ? O2D2 Cl2 O2A 98.0(6) . . ? O2D1 Cl2 O2B1 104.2(10) . . ? O2C1 Cl2 O2B1 103.4(8) . . ? O2A Cl2 O2B1 127.2(6) . . ? O3A Cl3 O3D 108.4(3) . . ? O3A Cl3 O3C 110.8(3) . . ? O3D Cl3 O3C 105.6(3) . . ? O3A Cl3 O3B 105.8(3) . . ? O3D Cl3 O3B 114.4(3) . . ? O3C Cl3 O3B 111.8(3) . . ? O4D Cl4 O4B 108.7(4) . . ? O4D Cl4 O4A 111.1(4) . . ? O4B Cl4 O4A 118.5(3) . . ? O4D Cl4 O4C 105.7(6) . . ? O4B Cl4 O4C 107.2(4) . . ? O4A Cl4 O4C 104.7(4) . . ? _refine_diff_density_max 0.814 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.093 #=END ####[Cu3(L2)Cl2](ClO4)2.2H2O data_1224ps17 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H38 Cl4 Cu3 N6 O13' _chemical_formula_weight 842.93 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.480(10) _cell_length_b 11.710(3) _cell_length_c 25.590(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.43(2) _cell_angle_gamma 90.00 _cell_volume 6309.0(42) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description 'prism' _exptl_crystal_colour blue _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method ? _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 2.408 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'ENRAF-NONIUS CAD4' _diffrn_measurement_method 'omega-2 theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5711 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5555 _reflns_number_observed 3109 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'XTAL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+15.2446P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5555 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_obs 0.0678 _refine_ls_wR_factor_all 0.2124 _refine_ls_wR_factor_obs 0.1724 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.180 _refine_ls_restrained_S_all 1.067 _refine_ls_restrained_S_obs 1.180 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu -0.04273(5) -0.04768(10) 0.06639(4) 0.0549(3) Uani 1 d . . Cu2 Cu 0.08966(5) -0.21570(10) 0.11407(4) 0.0577(4) Uani 1 d . . Cu3 Cu 0.07429(5) 0.06106(10) 0.15875(4) 0.0540(3) Uani 1 d . . Cl1 Cl 0.04664(11) 0.0652(2) 0.06584(8) 0.0548(6) Uani 1 d . . Cl2 Cl -0.04050(12) 0.0038(3) 0.16729(9) 0.0696(7) Uani 1 d . . O1 O 0.0067(3) -0.1827(5) 0.0748(2) 0.059(2) Uani 1 d . . O2 O 0.1645(4) -0.2190(7) 0.0598(3) 0.086(2) Uani 1 d . . H2A H 0.1987(4) -0.1648(7) 0.0709(3) 0.129 Uiso 1 d R . O3 O 0.1115(3) -0.0873(5) 0.1593(2) 0.058(2) Uani 1 d . . N1 N -0.1050(4) 0.0723(7) 0.0388(3) 0.066(2) Uani 1 d . . H1A H -0.0995(4) 0.1334(7) 0.0606(3) 0.079 Uiso 1 d R . H1B H -0.1007(4) 0.0947(7) 0.0061(3) 0.079 Uiso 1 d R . N2 N -0.1172(4) -0.1555(7) 0.0539(3) 0.066(2) Uani 1 d . . H2 H -0.1293(4) -0.1684(7) 0.0855(3) 0.079 Uiso 1 d R . N3 N 0.0732(5) -0.3767(7) 0.0854(4) 0.075(2) Uani 1 d . . N4 N 0.1615(4) -0.2974(8) 0.1644(3) 0.072(2) Uani 1 d . . N5 N 0.1142(3) 0.0637(7) 0.2362(3) 0.058(2) Uani 1 d . . H5 H 0.0843(3) 0.0442(7) 0.2554(3) 0.070 Uiso 1 d R . N6 N 0.0682(4) 0.2283(7) 0.1655(3) 0.065(2) Uani 1 d . . H6A H 0.0954(4) 0.2629(7) 0.1480(3) 0.078 Uiso 1 d R . H6B H 0.0285(4) 0.2512(7) 0.1510(3) 0.078 Uiso 1 d R . C1 C -0.1696(5) 0.0220(11) 0.0367(5) 0.076(3) Uani 1 d . . H1C H -0.1797(5) 0.0225(11) 0.0720(5) 0.092 Uiso 1 d R . H1D H -0.2016(5) 0.0663(11) 0.0131(5) 0.092 Uiso 1 d R . C2 C -0.1692(5) -0.0975(10) 0.0177(4) 0.074(3) Uani 1 d . . H2C H -0.1624(5) -0.0990(10) -0.0186(4) 0.089 Uiso 1 d R . H2D H -0.2093(5) -0.1347(10) 0.0187(4) 0.089 Uiso 1 d R . C3 C -0.0933(5) -0.2635(9) 0.0355(4) 0.068(3) Uani 1 d . . H3A H -0.0874(5) -0.2563(9) -0.0009(4) 0.082 Uiso 1 d R . H3B H -0.1228(5) -0.3254(9) 0.0373(4) 0.082 Uiso 1 d R . C4 C -0.0297(5) -0.2842(8) 0.0719(4) 0.063(3) Uani 1 d . . H4 H -0.0369(5) -0.3034(8) 0.1076(4) 0.076 Uiso 1 d R . C5 C 0.0081(5) -0.3765(9) 0.0525(4) 0.074(3) Uani 1 d . . H5A H -0.0114(5) -0.4504(9) 0.0553(4) 0.089 Uiso 1 d R . H5B H 0.0096(5) -0.3634(9) 0.0154(4) 0.089 Uiso 1 d R . C6 C 0.0792(7) -0.4454(10) 0.1354(5) 0.099(4) Uani 1 d . . H6C H 0.0943(7) -0.5216(10) 0.1297(5) 0.119 Uiso 1 d R . H6D H 0.0376(7) -0.4528(10) 0.1444(5) 0.119 Uiso 1 d R . C7 C 0.1246(6) -0.3896(11) 0.1825(5) 0.090(4) Uani 1 d . . H7A H 0.1003(6) -0.3583(11) 0.2073(5) 0.109 Uiso 1 d R . H7B H 0.1529(6) -0.4474(11) 0.2012(5) 0.109 Uiso 1 d R . C8 C 0.1237(7) -0.4061(11) 0.0557(5) 0.096(4) Uani 1 d . . H8A H 0.1081(7) -0.3916(11) 0.0181(5) 0.115 Uiso 1 d R . H8B H 0.1339(7) -0.4866(11) 0.0601(5) 0.115 Uiso 1 d R . C9 C 0.1823(6) -0.3351(12) 0.0743(5) 0.092(4) Uani 1 d . . H9 H 0.2152(6) -0.3587(12) 0.0549(5) 0.111 Uiso 1 d R . C10 C 0.2093(6) -0.3398(10) 0.1336(5) 0.087(4) Uani 1 d . . H10A H 0.2205(6) -0.4181(10) 0.1438(5) 0.104 Uiso 1 d R . H10B H 0.2475(6) -0.2938(10) 0.1420(5) 0.104 Uiso 1 d R . C11 C 0.1874(5) -0.2145(10) 0.2074(4) 0.080(3) Uani 1 d . . H11A H 0.2248(5) -0.1776(10) 0.1992(4) 0.097 Uiso 1 d R . H11B H 0.1997(5) -0.2541(10) 0.2411(4) 0.097 Uiso 1 d R . C12 C 0.1378(5) -0.1245(9) 0.2113(4) 0.067(3) Uani 1 d . . H12 H 0.1045(5) -0.1596(9) 0.2271(4) 0.081 Uiso 1 d R . C13 C 0.1639(5) -0.0228(9) 0.2437(4) 0.070(3) Uani 1 d . . H13A H 0.1754(5) -0.0435(9) 0.2811(4) 0.084 Uiso 1 d R . H13B H 0.2016(5) 0.0054(9) 0.2324(4) 0.084 Uiso 1 d R . C14 C 0.1355(5) 0.1809(8) 0.2509(4) 0.065(3) Uani 1 d . . H14A H 0.1748(5) 0.1966(8) 0.2389(4) 0.078 Uiso 1 d R . H14B H 0.1428(5) 0.1909(8) 0.2892(4) 0.078 Uiso 1 d R . C15 C 0.0836(5) 0.2599(9) 0.2229(4) 0.071(3) Uani 1 d . . H15A H 0.0463(5) 0.2516(9) 0.2386(4) 0.086 Uiso 1 d R . H15B H 0.0977(5) 0.3387(9) 0.2269(4) 0.086 Uiso 1 d R . Cl3 Cl 0.22929(15) 0.2842(3) 0.12900(12) 0.0814(8) Uani 1 d . . O4 O 0.2143(8) 0.1740(10) 0.1420(6) 0.184(6) Uani 1 d . . O5 O 0.1951(9) 0.3153(15) 0.0815(6) 0.238(9) Uani 1 d . . O6 O 0.2907(6) 0.2984(17) 0.1333(6) 0.216(8) Uani 1 d . . O7 O 0.2070(6) 0.3511(8) 0.1683(4) 0.132(4) Uani 1 d . . Cl4 Cl -0.0978(2) 0.3630(3) 0.11017(15) 0.0998(10) Uani 1 d . . O8 O -0.1457(6) 0.2802(9) 0.1058(6) 0.158(5) Uani 1 d . . O9 O -0.0673(8) 0.3750(14) 0.1644(4) 0.198(6) Uani 1 d . . O10 O -0.0506(4) 0.3280(9) 0.0815(4) 0.113(3) Uani 1 d . . O11 O -0.1259(5) 0.4654(8) 0.0882(5) 0.142(4) Uani 1 d . . O12 O 0.2418(5) -0.0464(9) 0.1021(6) 0.144(4) Uani 1 d . . O13A O -0.0168(12) -0.2550(23) 0.2061(10) 0.176(12) Uiso 0.55(3) d P . O13B O -0.1240(26) -0.4010(44) 0.1936(23) 0.296(28) Uiso 0.45(3) d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0529(6) 0.0602(7) 0.0493(6) -0.0045(5) 0.0039(5) 0.0101(5) Cu2 0.0655(7) 0.0576(7) 0.0466(6) 0.0004(5) 0.0031(5) 0.0163(6) Cu3 0.0596(7) 0.0612(7) 0.0384(6) -0.0037(5) 0.0026(5) 0.0069(6) Cl1 0.0603(13) 0.0674(14) 0.0361(10) 0.0009(10) 0.0082(9) 0.0014(11) Cl2 0.069(2) 0.099(2) 0.0430(12) -0.0109(13) 0.0176(11) -0.0051(14) O1 0.060(4) 0.055(4) 0.057(4) -0.006(3) 0.001(3) 0.011(3) O2 0.077(5) 0.109(6) 0.074(5) 0.016(4) 0.018(4) 0.028(5) O3 0.062(4) 0.065(4) 0.040(3) -0.002(3) -0.005(3) 0.018(3) N1 0.065(5) 0.071(5) 0.057(5) 0.004(4) 0.002(4) 0.025(4) N2 0.066(5) 0.068(5) 0.064(5) 0.002(4) 0.015(4) 0.001(4) N3 0.094(7) 0.059(5) 0.069(6) -0.001(4) 0.008(5) 0.017(5) N4 0.072(6) 0.073(6) 0.065(5) 0.013(5) 0.002(4) 0.030(5) N5 0.052(4) 0.083(6) 0.039(4) 0.002(4) 0.007(3) 0.000(4) N6 0.077(6) 0.061(5) 0.057(5) -0.002(4) 0.013(4) 0.010(4) C1 0.054(6) 0.111(10) 0.067(7) 0.006(6) 0.018(5) 0.019(6) C2 0.051(6) 0.106(9) 0.063(6) -0.001(6) 0.005(5) 0.002(6) C3 0.064(6) 0.072(7) 0.065(6) -0.006(5) 0.004(5) -0.014(5) C4 0.068(6) 0.060(6) 0.059(6) -0.001(5) 0.009(5) 0.002(5) C5 0.081(8) 0.064(7) 0.075(7) -0.005(5) 0.007(6) -0.004(6) C6 0.147(12) 0.063(7) 0.086(9) 0.019(7) 0.015(8) 0.025(8) C7 0.118(10) 0.082(8) 0.065(7) 0.012(6) 0.003(7) 0.028(8) C8 0.116(11) 0.087(9) 0.087(9) -0.006(7) 0.029(8) 0.042(8) C9 0.082(8) 0.114(10) 0.083(8) -0.014(8) 0.022(7) 0.042(8) C10 0.094(8) 0.077(8) 0.080(8) 0.001(6) -0.008(6) 0.035(7) C11 0.081(8) 0.094(8) 0.059(7) 0.005(6) -0.007(6) 0.020(7) C12 0.067(6) 0.079(7) 0.048(5) 0.006(5) -0.007(5) 0.017(6) C13 0.065(6) 0.096(8) 0.043(5) 0.000(5) -0.002(5) 0.004(6) C14 0.065(6) 0.072(7) 0.058(6) -0.019(5) 0.011(5) -0.014(5) C15 0.077(7) 0.072(7) 0.070(7) -0.017(6) 0.024(6) 0.001(6) Cl3 0.080(2) 0.087(2) 0.075(2) -0.003(2) 0.008(2) -0.008(2) O4 0.257(16) 0.098(8) 0.230(16) -0.008(9) 0.127(13) 0.011(9) O5 0.291(19) 0.238(16) 0.126(11) -0.020(10) -0.098(12) 0.069(15) O6 0.110(9) 0.355(23) 0.202(15) -0.036(14) 0.074(10) -0.067(12) O7 0.176(10) 0.104(7) 0.126(9) -0.019(6) 0.052(8) 0.007(7) Cl4 0.122(3) 0.087(2) 0.096(2) 0.014(2) 0.035(2) 0.011(2) O8 0.150(10) 0.102(8) 0.249(16) 0.010(9) 0.099(10) -0.012(7) O9 0.289(18) 0.233(15) 0.068(7) 0.003(8) 0.024(9) 0.010(14) O10 0.102(7) 0.138(8) 0.102(7) 0.007(6) 0.023(5) 0.018(6) O11 0.157(10) 0.084(7) 0.203(12) 0.048(7) 0.079(9) 0.031(6) O12 0.118(8) 0.112(8) 0.198(13) -0.006(8) 0.018(8) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.894(6) . ? Cu1 N1 1.972(7) . ? Cu1 N2 2.013(8) . ? Cu1 Cl1 2.333(3) . ? Cu1 Cl2 2.642(3) . ? Cu2 O3 1.898(6) . ? Cu2 O1 1.903(6) . ? Cu2 N3 2.028(9) . ? Cu2 N4 2.042(8) . ? Cu2 O2 2.323(7) . ? Cu3 O3 1.911(6) . ? Cu3 N6 1.973(8) . ? Cu3 N5 1.999(7) . ? Cu3 Cl1 2.334(2) . ? Cu3 Cl2 2.606(3) . ? O1 C4 1.417(11) . ? O2 C9 1.440(14) . ? O3 C12 1.408(11) . ? N1 C1 1.499(13) . ? N2 C2 1.469(12) . ? N2 C3 1.475(13) . ? N3 C5 1.482(13) . ? N3 C8 1.483(15) . ? N3 C6 1.496(15) . ? N4 C7 1.467(15) . ? N4 C11 1.490(13) . ? N4 C10 1.497(14) . ? N5 C13 1.457(12) . ? N5 C14 1.472(12) . ? N6 C15 1.486(12) . ? C1 C2 1.48(2) . ? C3 C4 1.513(13) . ? C4 C5 1.495(14) . ? C6 C7 1.54(2) . ? C8 C9 1.51(2) . ? C9 C10 1.52(2) . ? C11 C12 1.517(14) . ? C12 C13 1.496(14) . ? C14 C15 1.515(14) . ? Cl3 O6 1.312(11) . ? Cl3 O5 1.339(13) . ? Cl3 O4 1.387(12) . ? Cl3 O7 1.431(10) . ? Cl4 O8 1.403(11) . ? Cl4 O11 1.407(10) . ? Cl4 O9 1.420(12) . ? Cl4 O10 1.423(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N1 164.1(3) . . ? O1 Cu1 N2 84.5(3) . . ? N1 Cu1 N2 85.9(3) . . ? O1 Cu1 Cl1 91.7(2) . . ? N1 Cu1 Cl1 95.4(3) . . ? N2 Cu1 Cl1 169.5(3) . . ? O1 Cu1 Cl2 100.2(2) . . ? N1 Cu1 Cl2 93.8(3) . . ? N2 Cu1 Cl2 99.1(3) . . ? Cl1 Cu1 Cl2 91.21(9) . . ? O3 Cu2 O1 104.7(2) . . ? O3 Cu2 N3 163.9(3) . . ? O1 Cu2 N3 85.4(3) . . ? O3 Cu2 N4 85.5(3) . . ? O1 Cu2 N4 159.9(4) . . ? N3 Cu2 N4 81.3(4) . . ? O3 Cu2 O2 105.1(3) . . ? O1 Cu2 O2 112.0(3) . . ? N3 Cu2 O2 82.0(4) . . ? N4 Cu2 O2 81.0(3) . . ? O3 Cu3 N6 159.6(3) . . ? O3 Cu3 N5 84.9(3) . . ? N6 Cu3 N5 85.4(3) . . ? O3 Cu3 Cl1 92.7(2) . . ? N6 Cu3 Cl1 93.5(2) . . ? N5 Cu3 Cl1 169.4(2) . . ? O3 Cu3 Cl2 99.6(2) . . ? N6 Cu3 Cl2 99.6(3) . . ? N5 Cu3 Cl2 98.5(2) . . ? Cl1 Cu3 Cl2 92.10(9) . . ? Cu1 Cl1 Cu3 91.48(9) . . ? Cu3 Cl2 Cu1 79.11(7) . . ? C4 O1 Cu1 113.7(5) . . ? C4 O1 Cu2 107.9(5) . . ? Cu1 O1 Cu2 132.5(3) . . ? C9 O2 Cu2 92.4(6) . . ? C12 O3 Cu2 109.6(6) . . ? C12 O3 Cu3 112.1(5) . . ? Cu2 O3 Cu3 131.6(3) . . ? C1 N1 Cu1 106.9(6) . . ? C2 N2 C3 117.7(8) . . ? C2 N2 Cu1 106.9(6) . . ? C3 N2 Cu1 105.8(6) . . ? C5 N3 C8 114.4(9) . . ? C5 N3 C6 113.5(10) . . ? C8 N3 C6 111.4(9) . . ? C5 N3 Cu2 106.4(6) . . ? C8 N3 Cu2 107.9(8) . . ? C6 N3 Cu2 102.2(7) . . ? C7 N4 C11 113.1(9) . . ? C7 N4 C10 113.1(9) . . ? C11 N4 C10 114.2(9) . . ? C7 N4 Cu2 99.0(6) . . ? C11 N4 Cu2 106.6(6) . . ? C10 N4 Cu2 109.6(6) . . ? C13 N5 C14 115.6(7) . . ? C13 N5 Cu3 106.2(5) . . ? C14 N5 Cu3 108.5(6) . . ? C15 N6 Cu3 109.2(6) . . ? C2 C1 N1 108.6(8) . . ? N2 C2 C1 106.5(9) . . ? N2 C3 C4 105.7(8) . . ? O1 C4 C5 107.1(8) . . ? O1 C4 C3 108.7(8) . . ? C5 C4 C3 113.3(9) . . ? N3 C5 C4 109.0(8) . . ? N3 C6 C7 112.1(10) . . ? N4 C7 C6 111.3(10) . . ? N3 C8 C9 111.2(10) . . ? O2 C9 C8 106.1(10) . . ? O2 C9 C10 108.8(10) . . ? C8 C9 C10 115.2(12) . . ? N4 C10 C9 110.4(9) . . ? N4 C11 C12 109.7(8) . . ? O3 C12 C13 108.4(8) . . ? O3 C12 C11 107.9(8) . . ? C13 C12 C11 113.5(8) . . ? N5 C13 C12 107.2(8) . . ? N5 C14 C15 106.6(8) . . ? N6 C15 C14 108.3(8) . . ? O6 Cl3 O5 113.8(12) . . ? O6 Cl3 O4 112.0(11) . . ? O5 Cl3 O4 111.0(11) . . ? O6 Cl3 O7 110.1(9) . . ? O5 Cl3 O7 106.8(9) . . ? O4 Cl3 O7 102.4(7) . . ? O8 Cl4 O11 107.9(8) . . ? O8 Cl4 O9 109.5(9) . . ? O11 Cl4 O9 112.6(9) . . ? O8 Cl4 O10 110.3(7) . . ? O11 Cl4 O10 109.4(7) . . ? O9 Cl4 O10 107.2(8) . . ? _refine_diff_density_max 1.013 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.128 #=END