Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Data-Type: text X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1330 data_global loop_ _publ_author_name 'Gao, En-Qing' 'Jiang, Zong-Hui' 'Liao, Dai-Zheng' 'Tang, Jin-Kui' 'Yan, Shi-Ping' 'Zhao, Qi-Hua' _journal_coden_Cambridge 186 #data_Liao _publ_contact_author ; Dai-Zheng Liao Department of Chemistry, Nankai University, Tianjin 300071,China ; _publ_contact_author_email ' coord@sun.nankai.edu.cn ' _publ_section_title ; A New One-dimensional coordination polymer and a new supramolecular dimer made of trinuclear Cu(II) complexes: Crystal Structure and Magnetic Properties ; data_1 _database_code_CSD 155651 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H40 Cl2 Cu3 N6 O17' _chemical_formula_weight 886.09 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 orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 21.2818(11) _cell_length_b 12.8206(7) _cell_length_c 12.6462(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3450.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6911 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.24 _exptl_crystal_description ? _exptl_crystal_colour greenish blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 2.065 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.6263 _exptl_absorpt_correction_T_max 0.6829 _exptl_absorpt_process_details ? _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_type 'ccd area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.04 _diffrn_reflns_number 13935 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5353 _reflns_number_gt 4552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART' _computing_cell_refinement 'SAINT' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.1306P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(17) _refine_ls_number_reflns 5353 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.54050(3) 0.25570(5) 0.90119(6) 0.04400(18) Uani 1 1 d . . . Cu2 Cu 0.65671(3) 0.16077(5) 0.55441(5) 0.04219(17) Uani 1 1 d . . . Cu3 Cu 0.40722(3) 0.32158(5) 1.23557(6) 0.04070(17) Uani 1 1 d . . . O1 O 0.6007(2) 0.1492(3) 0.8521(3) 0.0506(11) Uani 1 1 d . . . O2 O 0.5329(2) 0.1973(3) 1.0464(4) 0.0586(12) Uani 1 1 d . . . N1 N 0.54560(19) 0.3089(3) 0.7587(3) 0.0335(10) Uani 1 1 d . . . N2 N 0.4810(2) 0.3595(4) 0.9488(4) 0.0391(10) Uani 1 1 d . . . O3 O 0.65296(18) 0.1129(3) 0.7046(3) 0.0472(10) Uani 1 1 d . . . O4 O 0.59411(19) 0.2633(3) 0.6006(3) 0.0470(10) Uani 1 1 d . . . N3 N 0.6727(2) 0.2363(4) 0.4162(4) 0.0473(12) Uani 1 1 d . . . N4 N 0.7346(2) 0.0751(4) 0.5233(4) 0.0434(11) Uani 1 1 d . . . O5 O 0.4817(2) 0.2377(4) 1.1950(3) 0.0604(12) Uani 1 1 d . . . O6 O 0.42041(18) 0.3903(3) 1.0985(3) 0.0447(9) Uani 1 1 d . . . O7 O 0.5491(2) 0.5284(3) 0.8309(4) 0.0581(11) Uani 1 1 d . . . H7A H 0.5668 0.5574 0.7813 0.087 Uiso 1 1 calc R . . N5 N 0.3175(2) 0.3686(4) 1.2421(5) 0.0572(13) Uani 1 1 d . . . N6 N 0.3905(3) 0.2331(4) 1.3636(4) 0.0520(13) Uani 1 1 d . . . O8 O 0.5800(3) 0.0455(5) 0.5061(5) 0.0849(17) Uani 1 1 d . . . C1 C 0.6146(3) 0.1628(4) 0.7571(5) 0.0411(14) Uani 1 1 d . . . C2 C 0.5820(2) 0.2530(4) 0.6987(4) 0.0341(12) Uani 1 1 d . . . C3 C 0.5094(3) 0.3964(4) 0.7141(4) 0.0395(12) Uani 1 1 d . . . H3A H 0.4705 0.3697 0.6847 0.047 Uiso 1 1 calc R . . H3B H 0.5332 0.4276 0.6569 0.047 Uiso 1 1 calc R . . C4 C 0.4943(3) 0.4789(4) 0.7945(5) 0.0453(14) Uani 1 1 d . . . H4A H 0.4702 0.5325 0.7569 0.054 Uiso 1 1 calc R . . C5 C 0.4535(3) 0.4447(4) 0.8876(5) 0.0468(14) Uani 1 1 d . . . H5A H 0.4468 0.5040 0.9340 0.056 Uiso 1 1 calc R . . H5B H 0.4128 0.4229 0.8611 0.056 Uiso 1 1 calc R . . C6 C 0.4620(2) 0.3414(4) 1.0437(5) 0.0359(12) Uani 1 1 d . . . C7 C 0.4955(3) 0.2507(5) 1.1004(5) 0.0490(15) Uani 1 1 d . . . C8 C 0.7358(3) 0.2014(5) 0.3804(5) 0.0508(15) Uani 1 1 d . . . H8A H 0.7680 0.2434 0.4142 0.061 Uiso 1 1 calc R . . H8B H 0.7394 0.2105 0.3045 0.061 Uiso 1 1 calc R . . C9 C 0.7452(3) 0.0884(5) 0.4084(5) 0.0516(14) Uani 1 1 d . . . H9A H 0.7158 0.0454 0.3690 0.062 Uiso 1 1 calc R . . H9B H 0.7875 0.0669 0.3901 0.062 Uiso 1 1 calc R . . C10 C 0.6727(5) 0.3517(6) 0.4296(8) 0.087(3) Uani 1 1 d . . . H10A H 0.6806 0.3844 0.3626 0.130 Uiso 1 1 calc R . . H10B H 0.7050 0.3712 0.4788 0.130 Uiso 1 1 calc R . . H10C H 0.6326 0.3739 0.4561 0.130 Uiso 1 1 calc R . . C11 C 0.6247(4) 0.2045(8) 0.3354(7) 0.086(3) Uani 1 1 d . . . H11A H 0.6327 0.2405 0.2703 0.128 Uiso 1 1 calc R . . H11B H 0.5835 0.2219 0.3606 0.128 Uiso 1 1 calc R . . H11C H 0.6273 0.1306 0.3239 0.128 Uiso 1 1 calc R . . C12 C 0.7874(3) 0.1133(7) 0.5877(6) 0.074(2) Uani 1 1 d . . . H12A H 0.8242 0.0725 0.5729 0.111 Uiso 1 1 calc R . . H12B H 0.7770 0.1073 0.6613 0.111 Uiso 1 1 calc R . . H12C H 0.7955 0.1851 0.5709 0.111 Uiso 1 1 calc R . . C13 C 0.7254(3) -0.0374(4) 0.5482(7) 0.0660(19) Uani 1 1 d . . . H13A H 0.7632 -0.0751 0.5324 0.099 Uiso 1 1 calc R . . H13B H 0.6915 -0.0645 0.5063 0.099 Uiso 1 1 calc R . . H13C H 0.7156 -0.0451 0.6218 0.099 Uiso 1 1 calc R . . C14 C 0.3239(5) 0.2543(10) 1.3908(12) 0.146(6) Uani 1 1 d . . . H14A H 0.2996 0.1930 1.3719 0.175 Uiso 1 1 calc R . . H14B H 0.3212 0.2617 1.4670 0.175 Uiso 1 1 calc R . . C15 C 0.2959(5) 0.3370(12) 1.3475(9) 0.129(5) Uani 1 1 d . . . H15A H 0.3014 0.3957 1.3949 0.155 Uiso 1 1 calc R . . H15B H 0.2512 0.3227 1.3433 0.155 Uiso 1 1 calc R . . C16 C 0.4340(6) 0.2572(7) 1.4497(7) 0.097(3) Uani 1 1 d . . . H16A H 0.4248 0.2136 1.5094 0.146 Uiso 1 1 calc R . . H16B H 0.4296 0.3291 1.4694 0.146 Uiso 1 1 calc R . . H16C H 0.4764 0.2446 1.4266 0.146 Uiso 1 1 calc R . . C17 C 0.3966(5) 0.1194(5) 1.3427(8) 0.090(3) Uani 1 1 d . . . H17A H 0.3885 0.0813 1.4066 0.134 Uiso 1 1 calc R . . H17B H 0.4384 0.1045 1.3186 0.134 Uiso 1 1 calc R . . H17C H 0.3669 0.0991 1.2895 0.134 Uiso 1 1 calc R . . C18 C 0.3098(3) 0.4863(6) 1.2332(8) 0.078(2) Uani 1 1 d . . . H18A H 0.2660 0.5039 1.2368 0.117 Uiso 1 1 calc R . . H18B H 0.3268 0.5097 1.1670 0.117 Uiso 1 1 calc R . . H18C H 0.3318 0.5196 1.2903 0.117 Uiso 1 1 calc R . . C19 C 0.2818(4) 0.3230(7) 1.1567(9) 0.092(3) Uani 1 1 d . . . H19A H 0.2390 0.3463 1.1607 0.138 Uiso 1 1 calc R . . H19B H 0.2831 0.2484 1.1623 0.138 Uiso 1 1 calc R . . H19C H 0.2996 0.3440 1.0903 0.138 Uiso 1 1 calc R . . Cl1 Cl 0.64740(8) 0.42392(13) 1.06474(16) 0.0629(4) Uani 1 1 d . . . O9 O 0.6363(3) 0.3772(5) 0.9634(4) 0.0826(16) Uani 1 1 d . . . O10 O 0.5985(5) 0.4047(17) 1.1293(11) 0.289(11) Uani 1 1 d . . . O11 O 0.6697(10) 0.5159(8) 1.0620(12) 0.315(11) Uani 1 1 d . . . O12 O 0.6940(6) 0.3647(8) 1.1159(8) 0.164(4) Uani 1 1 d . . . Cl2 Cl 0.87332(10) 0.83496(14) 0.79894(18) 0.0735(5) Uani 1 1 d . . . O16 O 0.8522(4) 0.7808(9) 0.8916(11) 0.171(4) Uani 1 1 d . . . O15 O 0.8271(5) 0.9024(7) 0.7732(7) 0.163(4) Uani 1 1 d . . . O14 O 0.9290(4) 0.8829(7) 0.8259(8) 0.151(4) Uani 1 1 d . . . O13 O 0.8863(4) 0.7585(7) 0.7256(8) 0.154(4) Uani 1 1 d . . . O17 O 0.9777(4) 0.9850(6) 0.6239(10) 0.186(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0532(4) 0.0438(3) 0.0350(3) 0.0085(3) 0.0151(3) 0.0184(3) Cu2 0.0475(4) 0.0474(4) 0.0317(3) 0.0000(3) 0.0074(3) 0.0122(3) Cu3 0.0405(3) 0.0481(3) 0.0335(4) 0.0010(3) 0.0088(3) 0.0014(3) O1 0.063(3) 0.051(2) 0.038(2) 0.0118(18) 0.0163(19) 0.025(2) O2 0.066(3) 0.056(2) 0.054(3) 0.016(2) 0.027(2) 0.028(2) N1 0.036(2) 0.035(2) 0.030(3) -0.0007(18) 0.0047(17) 0.0064(18) N2 0.041(2) 0.041(2) 0.036(3) 0.0066(19) 0.008(2) 0.010(2) O3 0.056(2) 0.052(2) 0.034(2) 0.0010(18) 0.0102(18) 0.0188(19) O4 0.054(2) 0.054(2) 0.034(2) 0.0031(18) 0.0070(18) 0.0133(18) N3 0.050(3) 0.061(3) 0.031(3) 0.007(2) 0.005(2) 0.009(2) N4 0.051(3) 0.047(3) 0.032(3) -0.003(2) 0.007(2) 0.007(2) O5 0.064(3) 0.081(3) 0.037(3) 0.017(2) 0.019(2) 0.026(2) O6 0.051(2) 0.046(2) 0.037(2) 0.0007(17) 0.0125(17) 0.0112(18) O7 0.071(3) 0.054(2) 0.049(3) 0.006(2) -0.002(2) -0.014(2) N5 0.051(3) 0.075(3) 0.046(3) -0.009(3) 0.008(3) 0.007(3) N6 0.062(3) 0.040(3) 0.053(3) 0.004(2) 0.021(3) -0.001(2) O8 0.083(4) 0.094(4) 0.079(4) -0.027(3) 0.022(3) -0.024(3) C1 0.043(3) 0.036(3) 0.043(4) 0.002(2) 0.003(3) 0.009(2) C2 0.040(3) 0.035(3) 0.028(3) 0.003(2) 0.000(2) 0.008(2) C3 0.051(3) 0.031(2) 0.036(3) 0.008(2) 0.004(2) 0.007(2) C4 0.057(4) 0.035(3) 0.044(3) 0.004(3) 0.015(3) 0.002(3) C5 0.050(3) 0.042(3) 0.048(4) 0.012(3) 0.015(3) 0.015(2) C6 0.033(3) 0.044(3) 0.030(3) 0.001(2) 0.008(2) 0.007(2) C7 0.044(3) 0.059(4) 0.043(4) 0.015(3) 0.013(3) 0.016(3) C8 0.057(4) 0.054(3) 0.041(4) -0.004(3) 0.014(3) -0.002(3) C9 0.057(3) 0.058(3) 0.040(3) -0.009(3) 0.015(3) 0.006(3) C10 0.124(7) 0.052(4) 0.086(6) 0.030(4) 0.038(5) 0.038(4) C11 0.061(5) 0.146(8) 0.050(5) 0.023(5) -0.006(4) 0.001(5) C12 0.067(4) 0.097(6) 0.058(5) -0.015(4) -0.012(4) 0.010(4) C13 0.085(5) 0.046(3) 0.067(5) 0.001(4) 0.022(4) 0.017(3) C14 0.095(7) 0.168(11) 0.175(13) 0.112(11) 0.082(8) 0.050(7) C15 0.068(6) 0.230(14) 0.089(8) 0.060(8) 0.045(5) 0.036(7) C16 0.159(9) 0.080(6) 0.053(5) 0.025(4) -0.020(5) -0.038(6) C17 0.137(8) 0.038(4) 0.094(7) 0.006(4) 0.025(6) 0.005(4) C18 0.065(4) 0.074(5) 0.094(6) -0.026(5) -0.013(5) 0.026(4) C19 0.065(5) 0.101(6) 0.111(8) -0.036(6) -0.025(5) -0.020(4) Cl1 0.0747(11) 0.0586(9) 0.0555(10) -0.0017(8) -0.0106(9) 0.0072(8) O9 0.074(3) 0.122(4) 0.053(3) -0.014(3) 0.000(3) -0.016(3) O10 0.116(8) 0.56(3) 0.185(13) -0.219(17) 0.050(7) -0.028(11) O11 0.65(3) 0.112(7) 0.179(13) 0.060(8) -0.202(17) -0.131(12) O12 0.227(10) 0.153(7) 0.112(7) -0.022(6) -0.075(7) 0.048(7) Cl2 0.0721(12) 0.0627(10) 0.0856(15) -0.0116(10) 0.0102(10) 0.0106(9) O16 0.155(8) 0.183(9) 0.177(11) 0.069(8) 0.043(8) 0.017(7) O15 0.215(9) 0.148(7) 0.125(8) -0.015(6) -0.022(6) 0.114(7) O14 0.140(7) 0.160(7) 0.155(9) -0.034(7) -0.001(6) -0.070(6) O13 0.158(7) 0.156(7) 0.149(9) -0.089(7) -0.023(6) 0.050(6) O17 0.181(8) 0.101(5) 0.277(15) 0.022(7) 0.169(10) 0.022(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 N1 1.930(4) . ? Cu1 N2 1.933(4) . ? Cu1 O1 1.973(4) . ? Cu1 O2 1.989(5) . ? Cu1 O9 2.684(6) . ? Cu2 O4 1.961(4) . ? Cu2 O3 1.998(4) . ? Cu2 N3 2.027(5) . ? Cu2 N4 2.028(4) . ? Cu2 O8 2.285(5) . ? Cu3 O6 1.964(4) . ? Cu3 O5 1.984(4) . ? Cu3 N5 2.004(5) . ? Cu3 N6 2.009(5) . ? Cu3 O7 2.453(4) 2_665 ? O1 C1 1.250(7) . ? O2 C7 1.253(7) . ? N1 C2 1.299(7) . ? N1 C3 1.473(6) . ? N2 C6 1.288(7) . ? N2 C5 1.462(7) . ? O3 C1 1.231(7) . ? O4 C2 1.273(6) . ? N3 C8 1.486(7) . ? N3 C10 1.489(9) . ? N3 C11 1.500(9) . ? N4 C12 1.471(8) . ? N4 C9 1.481(8) . ? N4 C13 1.490(8) . ? O5 C7 1.242(7) . ? O6 C6 1.287(6) . ? O7 C4 1.406(8) . ? N5 C19 1.444(10) . ? N5 C15 1.467(11) . ? N5 C18 1.522(9) . ? N6 C16 1.462(11) . ? N6 C14 1.484(10) . ? N6 C17 1.487(9) . ? C1 C2 1.538(7) . ? C3 C4 1.502(7) . ? C4 C5 1.528(8) . ? C6 C7 1.541(7) . ? C8 C9 1.505(8) . ? C14 C15 1.334(14) . ? Cl1 O11 1.272(10) . ? Cl1 O10 1.345(12) . ? Cl1 O12 1.406(9) . ? Cl1 O9 1.434(6) . ? Cl2 O15 1.349(7) . ? Cl2 O13 1.377(7) . ? Cl2 O14 1.378(8) . ? Cl2 O16 1.434(11) . ? 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 N1 Cu1 N2 94.84(18) . . ? N1 Cu1 O1 85.07(17) . . ? N2 Cu1 O1 179.6(2) . . ? N1 Cu1 O2 178.0(2) . . ? N2 Cu1 O2 85.32(17) . . ? O1 Cu1 O2 94.75(16) . . ? N1 Cu1 O9 91.49(18) . . ? N2 Cu1 O9 90.4(2) . . ? O1 Cu1 O9 90.0(2) . . ? O2 Cu1 O9 90.5(2) . . ? O4 Cu2 O3 83.99(16) . . ? O4 Cu2 N3 92.90(18) . . ? O3 Cu2 N3 166.8(2) . . ? O4 Cu2 N4 167.61(19) . . ? O3 Cu2 N4 92.91(17) . . ? N3 Cu2 N4 87.39(18) . . ? O4 Cu2 O8 91.59(19) . . ? O3 Cu2 O8 91.5(2) . . ? N3 Cu2 O8 101.4(2) . . ? N4 Cu2 O8 100.5(2) . . ? O6 Cu3 O5 84.30(16) . . ? O6 Cu3 N5 92.1(2) . . ? O5 Cu3 N5 159.3(2) . . ? O6 Cu3 N6 171.8(2) . . ? O5 Cu3 N6 92.54(19) . . ? N5 Cu3 N6 88.1(2) . . ? O6 Cu3 O7 91.60(17) . 2_665 ? O5 Cu3 O7 104.47(19) . 2_665 ? N5 Cu3 O7 96.0(2) . 2_665 ? N6 Cu3 O7 96.52(19) . 2_665 ? C1 O1 Cu1 111.1(4) . . ? C7 O2 Cu1 110.5(4) . . ? C2 N1 C3 120.5(4) . . ? C2 N1 Cu1 112.6(3) . . ? C3 N1 Cu1 126.6(3) . . ? C6 N2 C5 120.1(4) . . ? C6 N2 Cu1 111.9(4) . . ? C5 N2 Cu1 127.8(4) . . ? C1 O3 Cu2 112.3(4) . . ? C2 O4 Cu2 111.0(3) . . ? C8 N3 C10 109.4(5) . . ? C8 N3 C11 109.0(5) . . ? C10 N3 C11 110.4(7) . . ? C8 N3 Cu2 105.7(4) . . ? C10 N3 Cu2 112.1(4) . . ? C11 N3 Cu2 110.1(4) . . ? C12 N4 C9 112.9(5) . . ? C12 N4 C13 107.8(6) . . ? C9 N4 C13 109.8(5) . . ? C12 N4 Cu2 109.7(4) . . ? C9 N4 Cu2 104.6(4) . . ? C13 N4 Cu2 112.1(4) . . ? C7 O5 Cu3 111.4(4) . . ? C6 O6 Cu3 110.8(3) . . ? C19 N5 C15 113.7(8) . . ? C19 N5 C18 106.9(7) . . ? C15 N5 C18 107.9(8) . . ? C19 N5 Cu3 110.4(5) . . ? C15 N5 Cu3 104.6(5) . . ? C18 N5 Cu3 113.4(4) . . ? C16 N6 C14 113.3(9) . . ? C16 N6 C17 106.5(7) . . ? C14 N6 C17 107.7(8) . . ? C16 N6 Cu3 111.6(4) . . ? C14 N6 Cu3 104.7(5) . . ? C17 N6 Cu3 113.2(5) . . ? O3 C1 O1 127.0(5) . . ? O3 C1 C2 115.6(5) . . ? O1 C1 C2 117.4(5) . . ? O4 C2 N1 129.3(5) . . ? O4 C2 C1 117.0(4) . . ? N1 C2 C1 113.7(5) . . ? N1 C3 C4 112.9(5) . . ? O7 C4 C3 111.3(5) . . ? O7 C4 C5 110.4(5) . . ? C3 C4 C5 116.1(4) . . ? N2 C5 C4 113.2(4) . . ? O6 C6 N2 129.1(5) . . ? O6 C6 C7 115.8(5) . . ? N2 C6 C7 115.1(4) . . ? O5 C7 O2 127.0(6) . . ? O5 C7 C6 116.1(5) . . ? O2 C7 C6 116.9(5) . . ? N3 C8 C9 109.8(5) . . ? N4 C9 C8 108.7(5) . . ? C15 C14 N6 118.4(8) . . ? C14 C15 N5 117.0(9) . . ? O11 Cl1 O10 118.4(13) . . ? O11 Cl1 O12 104.5(9) . . ? O10 Cl1 O12 99.6(10) . . ? O11 Cl1 O9 115.1(7) . . ? O10 Cl1 O9 109.8(6) . . ? O12 Cl1 O9 107.5(5) . . ? Cl1 O9 Cu1 129.0(3) . . ? O15 Cl2 O13 116.1(6) . . ? O15 Cl2 O14 113.6(6) . . ? O13 Cl2 O14 108.1(6) . . ? O15 Cl2 O16 106.2(6) . . ? O13 Cl2 O16 105.6(7) . . ? O14 Cl2 O16 106.5(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.990 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.077 #==END data_2 _database_code_CSD 155652 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H88 Cl4 Cu6 N12 O36' _chemical_formula_weight 1884.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.2579(13) _cell_length_b 17.1410(11) _cell_length_c 22.1609(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.6130(10) _cell_angle_gamma 90.00 _cell_volume 7509.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5595 _cell_measurement_theta_min 4.774 _cell_measurement_theta_max 52.632 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3864 _exptl_absorpt_coefficient_mu 1.905 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5553 _exptl_absorpt_correction_T_max 0.7019 _exptl_absorpt_process_details ? _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_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.5 _diffrn_reflns_number 30423 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13088 _reflns_number_gt 8736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+2.6795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13088 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.53461(3) 0.44227(3) 0.16456(3) 0.04408(16) Uani 1 1 d . . . Cu2 Cu 0.65387(3) 0.20037(3) 0.27942(3) 0.04913(17) Uani 1 1 d . . . Cu3 Cu 0.46756(3) 0.72219(3) 0.08472(3) 0.04673(17) Uani 1 1 d . . . N1 N 0.59232(18) 0.4192(2) 0.24371(16) 0.0409(8) Uani 1 1 d . . . N2 N 0.54596(18) 0.5473(2) 0.19565(17) 0.0428(9) Uani 1 1 d . . . N3 N 0.74075(19) 0.1886(2) 0.34352(18) 0.0508(10) Uani 1 1 d . . . N4 N 0.6679(2) 0.0906(2) 0.2517(2) 0.0584(11) Uani 1 1 d . . . N5 N 0.4772(2) 0.8288(2) 0.12253(19) 0.0553(11) Uani 1 1 d . . . N6 N 0.4002(2) 0.7686(2) 0.01385(18) 0.0519(10) Uani 1 1 d . . . O1 O 0.52549(15) 0.32593(17) 0.15810(15) 0.0487(8) Uani 1 1 d . . . O2 O 0.46950(16) 0.49125(18) 0.09344(15) 0.0527(8) Uani 1 1 d . . . O3 O 0.57792(16) 0.22286(17) 0.20771(15) 0.0499(8) Uani 1 1 d . . . O4 O 0.64852(16) 0.31262(17) 0.29668(14) 0.0495(8) Uani 1 1 d . . . O5 O 0.44535(17) 0.61239(17) 0.05780(15) 0.0539(8) Uani 1 1 d . . . O6 O 0.51722(17) 0.67394(17) 0.16245(14) 0.0517(8) Uani 1 1 d . . . O7 O 0.6115(2) 0.4462(3) 0.1008(2) 0.0947(14) Uani 1 1 d . . . O8 O 0.5733(2) 0.1721(3) 0.3408(2) 0.0927(14) Uani 1 1 d . . . O9 O 0.5637(2) 0.7164(2) 0.04373(19) 0.0742(11) Uani 1 1 d . . . C1 C 0.5675(2) 0.2953(2) 0.2013(2) 0.0417(10) Uani 1 1 d . . . C2 C 0.6077(2) 0.3456(3) 0.2527(2) 0.0423(10) Uani 1 1 d . . . C3 C 0.5159(2) 0.6005(2) 0.1580(2) 0.0414(10) Uani 1 1 d . . . C4 C 0.4733(2) 0.5650(3) 0.0979(2) 0.0478(11) Uani 1 1 d . . . C5 C 0.6164(2) 0.4834(3) 0.2809(2) 0.0444(11) Uani 1 1 d . . . C6 C 0.5899(2) 0.5556(3) 0.2548(2) 0.0429(10) Uani 1 1 d . . . C7 C 0.6072(3) 0.6246(3) 0.2864(2) 0.0513(12) Uani 1 1 d . . . H7A H 0.5896 0.6718 0.2695 0.062 Uiso 1 1 calc R . . C8 C 0.6515(3) 0.6220(3) 0.3439(2) 0.0631(14) Uani 1 1 d . . . H8A H 0.6642 0.6682 0.3653 0.076 Uiso 1 1 calc R . . C9 C 0.6769(3) 0.5524(3) 0.3696(2) 0.0751(18) Uani 1 1 d . . . H9A H 0.7058 0.5518 0.4084 0.090 Uiso 1 1 calc R . . C10 C 0.6598(3) 0.4829(3) 0.3380(2) 0.0588(13) Uani 1 1 d . . . H10A H 0.6777 0.4360 0.3555 0.071 Uiso 1 1 calc R . . C11 C 0.7566(3) 0.1045(3) 0.3448(3) 0.0681(15) Uani 1 1 d . . . H11C H 0.7311 0.0774 0.3706 0.082 Uiso 1 1 calc R . . H11D H 0.8044 0.0966 0.3621 0.082 Uiso 1 1 calc R . . C12 C 0.7387(3) 0.0724(3) 0.2801(3) 0.0698(16) Uani 1 1 d . . . H12C H 0.7681 0.0951 0.2556 0.084 Uiso 1 1 calc R . . H12D H 0.7453 0.0164 0.2812 0.084 Uiso 1 1 calc R . . C13 C 0.7938(3) 0.2345(4) 0.3236(3) 0.0744(17) Uani 1 1 d . . . H13D H 0.8356 0.2293 0.3536 0.112 Uiso 1 1 calc R . . H13E H 0.7807 0.2885 0.3200 0.112 Uiso 1 1 calc R . . H13F H 0.7995 0.2158 0.2843 0.112 Uiso 1 1 calc R . . C14 C 0.7354(3) 0.2162(4) 0.4048(3) 0.0698(16) Uani 1 1 d . . . H14D H 0.7779 0.2092 0.4334 0.105 Uiso 1 1 calc R . . H14E H 0.7010 0.1870 0.4186 0.105 Uiso 1 1 calc R . . H14F H 0.7236 0.2706 0.4025 0.105 Uiso 1 1 calc R . . C15 C 0.6585(4) 0.0851(4) 0.1825(3) 0.087(2) Uani 1 1 d . . . H15A H 0.6654 0.0322 0.1711 0.131 Uiso 1 1 calc R . . H15B H 0.6905 0.1185 0.1691 0.131 Uiso 1 1 calc R . . H15C H 0.6134 0.1011 0.1631 0.131 Uiso 1 1 calc R . . C16 C 0.6230(3) 0.0343(3) 0.2724(4) 0.0816(19) Uani 1 1 d . . . H16A H 0.6313 -0.0170 0.2583 0.122 Uiso 1 1 calc R . . H16B H 0.5767 0.0485 0.2558 0.122 Uiso 1 1 calc R . . H16C H 0.6314 0.0345 0.3168 0.122 Uiso 1 1 calc R . . C17 C 0.3914(4) 0.8510(4) 0.0296(3) 0.102(3) Uani 1 1 d . . . H17B H 0.3830 0.8818 -0.0081 0.122 Uiso 1 1 calc R . . H17C H 0.3519 0.8554 0.0475 0.122 Uiso 1 1 calc R . . C18 C 0.4481(4) 0.8823(3) 0.0716(3) 0.094(2) Uani 1 1 d . . . H18A H 0.4347 0.9302 0.0890 0.113 Uiso 1 1 calc R . . H18B H 0.4828 0.8953 0.0492 0.113 Uiso 1 1 calc R . . C19 C 0.4225(3) 0.7589(5) -0.0444(3) 0.090(2) Uani 1 1 d . . . H19A H 0.3896 0.7815 -0.0776 0.135 Uiso 1 1 calc R . . H19B H 0.4273 0.7043 -0.0523 0.135 Uiso 1 1 calc R . . H19C H 0.4652 0.7845 -0.0415 0.135 Uiso 1 1 calc R . . C20 C 0.3338(3) 0.7285(4) 0.0044(3) 0.092(2) Uani 1 1 d . . . H20D H 0.3028 0.7520 -0.0298 0.137 Uiso 1 1 calc R . . H20E H 0.3162 0.7334 0.0411 0.137 Uiso 1 1 calc R . . H20F H 0.3394 0.6743 -0.0042 0.137 Uiso 1 1 calc R . . C21 C 0.5487(3) 0.8507(3) 0.1497(3) 0.0746(17) Uani 1 1 d . . . H21A H 0.5500 0.9023 0.1669 0.112 Uiso 1 1 calc R . . H21B H 0.5743 0.8498 0.1180 0.112 Uiso 1 1 calc R . . H21C H 0.5678 0.8143 0.1816 0.112 Uiso 1 1 calc R . . C22 C 0.4394(3) 0.8311(4) 0.1730(3) 0.0824(18) Uani 1 1 d . . . H22A H 0.4437 0.8820 0.1916 0.124 Uiso 1 1 calc R . . H22B H 0.4576 0.7927 0.2037 0.124 Uiso 1 1 calc R . . H22C H 0.3925 0.8201 0.1564 0.124 Uiso 1 1 calc R . . Cu1' Cu 0.46417(3) 0.45348(3) 0.32535(3) 0.05231(17) Uani 1 1 d . . . Cu2' Cu 0.51280(3) 0.72735(3) 0.42483(3) 0.05173(18) Uani 1 1 d . . . Cu3' Cu 0.36131(3) 0.21171(3) 0.20248(3) 0.05356(18) Uani 1 1 d . . . N1' N 0.4395(2) 0.5595(2) 0.30388(18) 0.0507(10) Uani 1 1 d . . . N2' N 0.40889(18) 0.4329(2) 0.24503(17) 0.0443(9) Uani 1 1 d . . . N3' N 0.5054(2) 0.8379(2) 0.39303(19) 0.0563(10) Uani 1 1 d . . . N4' N 0.5808(2) 0.7669(3) 0.49903(19) 0.0621(12) Uani 1 1 d . . . N5' N 0.2709(2) 0.1989(2) 0.1437(2) 0.0565(11) Uani 1 1 d . . . N6' N 0.3497(2) 0.1022(3) 0.2334(3) 0.0760(15) Uani 1 1 d . . . O1' O 0.5170(2) 0.4984(2) 0.40262(17) 0.0718(11) Uani 1 1 d . . . O2' O 0.48148(16) 0.34005(19) 0.32728(15) 0.0539(8) Uani 1 1 d . . . O3' O 0.5357(2) 0.6163(2) 0.44574(17) 0.0689(10) Uani 1 1 d . . . O4' O 0.46242(18) 0.68424(19) 0.34474(15) 0.0578(9) Uani 1 1 d . . . O5' O 0.43902(16) 0.23623(18) 0.27291(16) 0.0554(9) Uani 1 1 d . . . O6' O 0.36168(17) 0.32548(19) 0.18710(15) 0.0556(8) Uani 1 1 d . . . O8' O 0.4190(2) 0.7205(2) 0.46549(19) 0.0790(12) Uani 1 1 d . . . O9' O 0.4320(2) 0.1854(3) 0.1374(2) 0.1064(18) Uani 1 1 d . . . C1' C 0.5104(3) 0.5715(3) 0.4025(2) 0.0604(14) Uani 1 1 d . . . C2' C 0.4668(2) 0.6105(3) 0.3449(2) 0.0494(11) Uani 1 1 d . . . C3' C 0.3995(2) 0.3592(3) 0.2320(2) 0.0466(11) Uani 1 1 d . . . C4' C 0.4435(2) 0.3078(3) 0.2823(2) 0.0483(11) Uani 1 1 d . . . C5' C 0.3950(2) 0.5695(3) 0.2454(2) 0.0443(10) Uani 1 1 d . . . C6' C 0.3763(2) 0.4995(3) 0.2132(2) 0.0455(11) Uani 1 1 d . . . C7' C 0.3309(3) 0.4994(3) 0.1567(2) 0.0568(13) Uani 1 1 d . . . H7'A H 0.3186 0.4529 0.1356 0.068 Uiso 1 1 calc R . . C8' C 0.3045(3) 0.5691(3) 0.1323(3) 0.0672(15) Uani 1 1 d . . . H8'A H 0.2733 0.5696 0.0947 0.081 Uiso 1 1 calc R . . C9' C 0.3234(3) 0.6388(3) 0.1627(2) 0.0621(14) Uani 1 1 d . . . H9'A H 0.3059 0.6856 0.1447 0.074 Uiso 1 1 calc R . . C10' C 0.3682(3) 0.6396(3) 0.2195(2) 0.0526(12) Uani 1 1 d . . . H10B H 0.3803 0.6865 0.2401 0.063 Uiso 1 1 calc R . . C11' C 0.5327(4) 0.8853(3) 0.4478(3) 0.104(3) Uani 1 1 d . . . H11A H 0.5456 0.9359 0.4345 0.124 Uiso 1 1 calc R . . H11B H 0.4974 0.8935 0.4704 0.124 Uiso 1 1 calc R . . C12' C 0.5899(4) 0.8515(4) 0.4886(4) 0.111(3) Uani 1 1 d . . . H12A H 0.5977 0.8785 0.5280 0.134 Uiso 1 1 calc R . . H12B H 0.6296 0.8587 0.4714 0.134 Uiso 1 1 calc R . . C13' C 0.5437(4) 0.8440(5) 0.3435(3) 0.104(2) Uani 1 1 d . . . H13A H 0.5406 0.8963 0.3277 0.156 Uiso 1 1 calc R . . H13B H 0.5250 0.8084 0.3107 0.156 Uiso 1 1 calc R . . H13C H 0.5903 0.8311 0.3599 0.156 Uiso 1 1 calc R . . C14' C 0.4359(3) 0.8615(4) 0.3647(3) 0.0830(18) Uani 1 1 d . . . H14A H 0.4357 0.9143 0.3503 0.125 Uiso 1 1 calc R . . H14B H 0.4084 0.8578 0.3948 0.125 Uiso 1 1 calc R . . H14C H 0.4180 0.8277 0.3305 0.125 Uiso 1 1 calc R . . C15' C 0.6480(3) 0.7275(5) 0.5051(3) 0.097(2) Uani 1 1 d . . . H15D H 0.6792 0.7476 0.5407 0.145 Uiso 1 1 calc R . . H15E H 0.6652 0.7375 0.4687 0.145 Uiso 1 1 calc R . . H15F H 0.6428 0.6723 0.5097 0.145 Uiso 1 1 calc R . . C16' C 0.5581(4) 0.7494(5) 0.5559(3) 0.100(2) Uani 1 1 d . . . H16D H 0.5909 0.7684 0.5908 0.151 Uiso 1 1 calc R . . H16E H 0.5533 0.6940 0.5595 0.151 Uiso 1 1 calc R . . H16F H 0.5154 0.7743 0.5546 0.151 Uiso 1 1 calc R . . C17' C 0.2780(5) 0.0845(5) 0.2054(6) 0.172(5) Uani 1 1 d . . . H17A H 0.2729 0.0283 0.2023 0.206 Uiso 1 1 calc R . . H17D H 0.2506 0.1028 0.2333 0.206 Uiso 1 1 calc R . . C18' C 0.2525(3) 0.1159(4) 0.1481(3) 0.0828(19) Uani 1 1 d . . . H18C H 0.2036 0.1112 0.1387 0.099 Uiso 1 1 calc R . . H18D H 0.2694 0.0863 0.1173 0.099 Uiso 1 1 calc R . . C19' C 0.3982(6) 0.0481(5) 0.2186(5) 0.156(5) Uani 1 1 d . . . H19D H 0.3907 -0.0027 0.2340 0.234 Uiso 1 1 calc R . . H19E H 0.4431 0.0653 0.2374 0.234 Uiso 1 1 calc R . . H19F H 0.3933 0.0457 0.1746 0.234 Uiso 1 1 calc R . . C20' C 0.3553(4) 0.0998(4) 0.3013(4) 0.110(3) Uani 1 1 d . . . H20A H 0.3494 0.0471 0.3138 0.166 Uiso 1 1 calc R . . H20B H 0.3210 0.1324 0.3119 0.166 Uiso 1 1 calc R . . H20C H 0.3991 0.1183 0.3220 0.166 Uiso 1 1 calc R . . C21' C 0.2728(3) 0.2188(4) 0.0800(3) 0.0790(18) Uani 1 1 d . . . H21D H 0.2287 0.2116 0.0539 0.118 Uiso 1 1 calc R . . H21E H 0.3047 0.1857 0.0661 0.118 Uiso 1 1 calc R . . H21F H 0.2863 0.2723 0.0781 0.118 Uiso 1 1 calc R . . C22' C 0.2209(3) 0.2472(4) 0.1651(3) 0.0791(19) Uani 1 1 d . . . H22D H 0.1776 0.2413 0.1374 0.119 Uiso 1 1 calc R . . H22E H 0.2346 0.3009 0.1660 0.119 Uiso 1 1 calc R . . H22F H 0.2178 0.2310 0.2058 0.119 Uiso 1 1 calc R . . Cl1 Cl 0.36358(11) 0.07216(9) 0.98517(8) 0.0839(5) Uani 1 1 d . . . O11 O 0.3052(7) 0.0973(7) 0.9478(6) 0.321(9) Uani 1 1 d . . . O12 O 0.3952(6) 0.1416(4) 1.0000(5) 0.221(5) Uani 1 1 d . . . O13 O 0.3450(4) 0.0372(3) 1.0338(3) 0.149(3) Uani 1 1 d . . . O14 O 0.3980(4) 0.0217(3) 0.9535(3) 0.142(3) Uani 1 1 d . . . Cl2 Cl 0.76488(7) 0.33174(9) 0.16771(7) 0.0691(4) Uani 1 1 d . . . O15 O 0.7827(4) 0.3138(6) 0.1129(3) 0.186(4) Uani 1 1 d . . . O16 O 0.7326(5) 0.3972(5) 0.1618(6) 0.278(7) Uani 1 1 d . . . O17 O 0.7202(3) 0.2719(4) 0.1775(3) 0.145(3) Uani 1 1 d . . . O18 O 0.8247(3) 0.3353(4) 0.2135(2) 0.126(2) Uani 1 1 d . . . Cl3 Cl 0.66222(11) 0.06654(9) 0.50122(8) 0.0843(5) Uani 1 1 d . . . O19 O 0.7325(4) 0.0784(7) 0.5168(5) 0.245(6) Uani 1 1 d . . . O20 O 0.6507(6) 0.0323(5) 0.4461(4) 0.214(5) Uani 1 1 d . . . O21 O 0.6337(6) 0.1374(4) 0.4957(5) 0.227(5) Uani 1 1 d . . . O22 O 0.6369(4) 0.0203(3) 0.5433(3) 0.136(2) Uani 1 1 d . . . Cl4 Cl 0.26771(12) 0.35482(11) 0.32547(8) 0.0996(6) Uani 1 1 d . . . O23 O 0.3190(5) 0.4181(4) 0.3456(5) 0.212(4) Uani 1 1 d . . . O24 O 0.2385(3) 0.3416(4) 0.3740(3) 0.1212(19) Uani 1 1 d . . . O25 O 0.3028(3) 0.2877(3) 0.3128(2) 0.1039(16) Uani 1 1 d . . . O26 O 0.2205(6) 0.3778(6) 0.2747(3) 0.279(7) Uani 1 1 d . . . O27 O 0.2166(6) 0.9737(7) 0.0313(4) 0.256(5) Uani 1 1 d . . . O28 O 0.3883(4) 0.5728(5) 0.4967(4) 0.221(5) Uani 1 1 d . . . O29 O 0.3818(3) 0.4273(3) 0.9909(2) 0.1018(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0463(3) 0.0309(3) 0.0494(3) 0.0017(2) -0.0019(2) 0.0029(2) Cu2 0.0466(3) 0.0335(3) 0.0595(4) 0.0052(3) -0.0053(3) 0.0027(2) Cu3 0.0563(4) 0.0325(3) 0.0450(3) 0.0003(2) -0.0027(3) 0.0082(2) N1 0.047(2) 0.0312(19) 0.043(2) 0.0066(16) 0.0067(16) 0.0030(16) N2 0.045(2) 0.035(2) 0.046(2) 0.0005(17) 0.0057(17) 0.0065(16) N3 0.044(2) 0.047(2) 0.056(2) 0.0077(19) -0.0007(18) 0.0009(18) N4 0.059(3) 0.040(2) 0.069(3) 0.002(2) -0.002(2) 0.0065(19) N5 0.067(3) 0.037(2) 0.056(2) 0.0015(19) 0.000(2) 0.0076(19) N6 0.060(3) 0.044(2) 0.043(2) -0.0037(18) -0.0052(19) 0.0086(19) O1 0.0435(18) 0.0347(16) 0.0589(19) 0.0025(15) -0.0083(15) 0.0006(13) O2 0.054(2) 0.0342(17) 0.061(2) -0.0034(15) -0.0061(16) 0.0029(14) O3 0.0483(19) 0.0313(17) 0.063(2) 0.0065(15) -0.0042(15) -0.0031(13) O4 0.0542(19) 0.0350(17) 0.0520(18) 0.0040(14) -0.0044(15) 0.0034(14) O5 0.062(2) 0.0374(17) 0.0517(18) 0.0007(15) -0.0102(16) 0.0038(15) O6 0.064(2) 0.0322(17) 0.0509(18) 0.0007(14) -0.0041(15) 0.0061(15) O7 0.093(3) 0.097(3) 0.107(3) 0.011(3) 0.048(3) 0.014(3) O8 0.070(3) 0.110(4) 0.101(3) 0.032(3) 0.025(2) 0.018(3) O9 0.063(2) 0.073(3) 0.088(3) -0.005(2) 0.019(2) 0.0006(19) C1 0.037(2) 0.035(2) 0.051(3) 0.004(2) 0.006(2) -0.0023(19) C2 0.038(2) 0.043(3) 0.046(2) 0.003(2) 0.010(2) -0.001(2) C3 0.047(3) 0.031(2) 0.045(2) 0.002(2) 0.009(2) 0.0061(19) C4 0.048(3) 0.037(3) 0.055(3) 0.001(2) 0.004(2) 0.004(2) C5 0.054(3) 0.040(2) 0.039(2) 0.002(2) 0.009(2) 0.003(2) C6 0.050(3) 0.041(2) 0.038(2) -0.001(2) 0.009(2) 0.005(2) C7 0.067(3) 0.037(3) 0.050(3) -0.005(2) 0.015(2) 0.005(2) C8 0.094(4) 0.048(3) 0.044(3) -0.010(2) 0.007(3) 0.000(3) C9 0.112(5) 0.059(4) 0.044(3) -0.003(3) -0.006(3) -0.006(3) C10 0.083(4) 0.045(3) 0.042(3) 0.006(2) -0.001(2) 0.002(3) C11 0.061(3) 0.058(3) 0.078(4) 0.020(3) 0.001(3) 0.013(3) C12 0.069(4) 0.051(3) 0.087(4) 0.004(3) 0.010(3) 0.014(3) C13 0.044(3) 0.083(4) 0.091(4) 0.018(3) 0.003(3) -0.015(3) C14 0.066(4) 0.074(4) 0.061(3) 0.004(3) -0.005(3) -0.001(3) C15 0.108(5) 0.068(4) 0.076(4) -0.017(3) -0.002(4) 0.019(4) C16 0.074(4) 0.050(3) 0.120(5) -0.001(4) 0.019(4) -0.014(3) C17 0.148(7) 0.057(4) 0.075(4) -0.005(3) -0.028(4) 0.035(4) C18 0.126(6) 0.036(3) 0.095(5) 0.012(3) -0.032(4) 0.005(3) C19 0.089(5) 0.124(6) 0.053(3) 0.009(4) 0.007(3) 0.011(4) C20 0.068(4) 0.109(5) 0.086(5) 0.027(4) -0.010(3) 0.004(4) C21 0.077(4) 0.059(3) 0.080(4) -0.014(3) 0.000(3) -0.005(3) C22 0.102(5) 0.065(4) 0.088(4) -0.022(3) 0.035(4) 0.009(3) Cu1' 0.0561(4) 0.0390(3) 0.0559(4) -0.0019(3) -0.0005(3) -0.0038(3) Cu2' 0.0606(4) 0.0440(3) 0.0450(3) -0.0031(3) -0.0007(3) -0.0066(3) Cu3' 0.0455(3) 0.0386(3) 0.0713(4) -0.0106(3) 0.0012(3) -0.0006(2) N1' 0.059(3) 0.047(2) 0.043(2) -0.0011(18) 0.0043(18) -0.0080(19) N2' 0.041(2) 0.039(2) 0.051(2) -0.0014(18) 0.0050(17) -0.0022(16) N3' 0.060(3) 0.049(2) 0.056(2) 0.002(2) 0.005(2) -0.008(2) N4' 0.072(3) 0.057(3) 0.050(2) -0.005(2) -0.002(2) -0.010(2) N5' 0.046(2) 0.058(3) 0.062(3) -0.017(2) 0.006(2) 0.0004(19) N6' 0.072(3) 0.038(2) 0.106(4) -0.008(3) -0.007(3) 0.001(2) O1' 0.098(3) 0.044(2) 0.060(2) 0.0019(17) -0.013(2) 0.0065(19) O2' 0.0502(19) 0.0446(18) 0.061(2) -0.0001(16) -0.0016(16) -0.0030(15) O3' 0.086(3) 0.055(2) 0.054(2) -0.0023(18) -0.0092(19) -0.0016(19) O4' 0.071(2) 0.0403(19) 0.054(2) -0.0028(16) -0.0038(17) -0.0016(16) O5' 0.0483(19) 0.0393(19) 0.074(2) -0.0094(17) 0.0031(16) 0.0041(14) O6' 0.058(2) 0.0417(18) 0.060(2) -0.0061(16) -0.0014(17) -0.0052(15) O8' 0.069(3) 0.085(3) 0.082(3) 0.015(2) 0.016(2) -0.009(2) O9' 0.061(3) 0.151(5) 0.115(4) -0.076(3) 0.035(2) -0.036(3) C1' 0.071(4) 0.050(3) 0.053(3) -0.002(3) -0.002(3) 0.000(3) C2' 0.057(3) 0.046(3) 0.044(3) 0.001(2) 0.006(2) -0.001(2) C3' 0.044(3) 0.045(3) 0.053(3) -0.004(2) 0.016(2) -0.003(2) C4' 0.038(3) 0.045(3) 0.062(3) -0.002(2) 0.012(2) -0.002(2) C5' 0.046(3) 0.041(2) 0.047(3) 0.002(2) 0.011(2) -0.004(2) C6' 0.044(3) 0.046(3) 0.048(3) 0.000(2) 0.012(2) -0.005(2) C7' 0.069(3) 0.046(3) 0.051(3) 0.000(2) 0.001(2) -0.003(2) C8' 0.073(4) 0.068(4) 0.053(3) 0.004(3) -0.003(3) 0.000(3) C9' 0.070(4) 0.055(3) 0.059(3) 0.013(3) 0.009(3) -0.003(3) C10' 0.064(3) 0.044(3) 0.051(3) 0.005(2) 0.014(2) -0.006(2) C11' 0.141(7) 0.049(4) 0.098(5) -0.009(4) -0.024(5) -0.015(4) C12' 0.125(6) 0.069(4) 0.112(6) -0.012(4) -0.034(5) -0.025(4) C13' 0.105(6) 0.112(6) 0.110(6) 0.041(5) 0.053(5) 0.003(5) C14' 0.075(4) 0.073(4) 0.099(5) 0.018(4) 0.013(4) 0.008(3) C15' 0.067(4) 0.131(6) 0.080(4) -0.021(4) -0.009(3) 0.001(4) C16' 0.097(5) 0.153(7) 0.047(3) -0.018(4) 0.009(3) -0.033(5) C17' 0.146(8) 0.076(5) 0.239(12) 0.034(7) -0.079(8) -0.054(6) C18' 0.060(4) 0.075(4) 0.106(5) -0.018(4) 0.003(4) -0.012(3) C19' 0.255(13) 0.076(5) 0.159(9) 0.020(6) 0.092(9) 0.084(7) C20' 0.140(7) 0.064(4) 0.138(7) 0.013(5) 0.054(6) -0.002(4) C21' 0.063(4) 0.098(5) 0.070(4) -0.011(4) 0.002(3) 0.008(3) C22' 0.046(3) 0.086(4) 0.098(5) -0.031(4) 0.001(3) 0.014(3) Cl1 0.1287(15) 0.0462(8) 0.0778(10) 0.0034(8) 0.0247(10) -0.0025(9) O11 0.293(14) 0.252(12) 0.319(15) -0.049(11) -0.144(13) 0.078(11) O12 0.356(12) 0.106(5) 0.276(10) -0.075(6) 0.235(10) -0.090(6) O13 0.210(7) 0.093(4) 0.185(7) 0.026(4) 0.131(6) 0.021(4) O14 0.259(8) 0.074(3) 0.121(4) -0.006(3) 0.101(5) 0.016(4) Cl2 0.0603(8) 0.0601(8) 0.0816(10) -0.0068(7) 0.0037(7) -0.0025(7) O15 0.150(6) 0.310(11) 0.102(5) -0.032(6) 0.037(4) -0.075(6) O16 0.182(8) 0.127(6) 0.444(17) -0.098(8) -0.105(9) 0.067(6) O17 0.122(5) 0.189(6) 0.125(5) -0.018(4) 0.026(4) -0.091(5) O18 0.094(4) 0.178(6) 0.092(3) 0.028(4) -0.012(3) -0.057(4) Cl3 0.1237(15) 0.0535(9) 0.0787(10) -0.0006(8) 0.0286(10) -0.0115(9) O19 0.145(7) 0.306(12) 0.245(10) 0.150(10) -0.044(7) -0.079(8) O20 0.353(13) 0.183(7) 0.139(6) -0.060(5) 0.121(7) -0.143(8) O21 0.330(12) 0.104(5) 0.334(12) 0.063(6) 0.260(10) 0.054(6) O22 0.219(7) 0.092(4) 0.120(4) 0.005(3) 0.087(5) -0.026(4) Cl4 0.1517(18) 0.0772(12) 0.0776(11) 0.0099(9) 0.0417(12) 0.0502(12) O23 0.342(12) 0.086(5) 0.275(10) 0.003(6) 0.211(10) 0.005(6) O24 0.101(4) 0.146(5) 0.131(5) -0.015(4) 0.055(3) 0.002(4) O25 0.126(4) 0.079(3) 0.108(4) 0.002(3) 0.027(3) 0.043(3) O26 0.457(16) 0.258(10) 0.084(4) -0.025(5) -0.022(6) 0.276(11) O27 0.293(13) 0.276(12) 0.197(9) 0.006(8) 0.051(9) -0.020(10) O28 0.134(6) 0.215(8) 0.272(9) 0.181(8) -0.051(6) -0.034(5) O29 0.102(4) 0.107(4) 0.086(3) -0.033(3) -0.003(3) 0.002(3) _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 N2 1.923(4) . ? Cu1 N1 1.925(3) . ? Cu1 O1 2.005(3) . ? Cu1 O2 2.005(3) . ? Cu1 O7 2.321(4) . ? Cu2 O4 1.969(3) . ? Cu2 O3 1.993(3) . ? Cu2 N3 2.016(4) . ? Cu2 N4 2.020(4) . ? Cu2 O8 2.392(4) . ? Cu3 O6 1.977(3) . ? Cu3 O5 1.996(3) . ? Cu3 N5 2.002(4) . ? Cu3 N6 2.006(4) . ? Cu3 O9 2.324(4) . ? N1 C2 1.304(5) . ? N1 C5 1.398(6) . ? N2 C3 1.295(5) . ? N2 C6 1.421(6) . ? N3 C14 1.465(7) . ? N3 C13 1.475(6) . ? N3 C11 1.475(6) . ? N4 C16 1.467(7) . ? N4 C12 1.468(7) . ? N4 C15 1.506(7) . ? N5 C18 1.473(7) . ? N5 C22 1.488(7) . ? N5 C21 1.490(7) . ? N6 C19 1.467(7) . ? N6 C17 1.475(7) . ? N6 C20 1.485(7) . ? O1 C1 1.249(5) . ? O2 C4 1.269(5) . ? O3 C1 1.263(5) . ? O4 C2 1.266(5) . ? O5 C4 1.245(5) . ? O6 C3 1.263(5) . ? C1 C2 1.517(6) . ? C3 C4 1.544(6) . ? C5 C10 1.374(6) . ? C5 C6 1.421(6) . ? C6 C7 1.380(6) . ? C7 C8 1.390(7) . ? C8 C9 1.373(7) . ? C9 C10 1.386(7) . ? C11 C12 1.503(8) . ? C17 C18 1.418(9) . ? Cu1' N1' 1.916(4) . ? Cu1' N2' 1.917(4) . ? Cu1' O1' 1.967(4) . ? Cu1' O2' 1.974(3) . ? Cu2' O4' 1.987(3) . ? Cu2' O3' 1.990(4) . ? Cu2' N3' 2.016(4) . ? Cu2' N4' 2.018(4) . ? Cu2' O8' 2.276(4) . ? Cu3' O6' 1.980(3) . ? Cu3' O5' 2.005(3) . ? Cu3' N5' 2.015(4) . ? Cu3' N6' 2.029(5) . ? Cu3' O9' 2.288(4) . ? N1' C2' 1.295(6) . ? N1' C5' 1.419(6) . ? N2' C3' 1.301(6) . ? N2' C6' 1.426(6) . ? N3' C11' 1.465(7) . ? N3' C14' 1.469(7) . ? N3' C13' 1.479(7) . ? N4' C16' 1.463(8) . ? N4' C12' 1.486(8) . ? N4' C15' 1.500(8) . ? N5' C21' 1.461(7) . ? N5' C22' 1.464(7) . ? N5' C18' 1.478(7) . ? N6' C19' 1.441(9) . ? N6' C17' 1.480(9) . ? N6' C20' 1.484(9) . ? O1' C1' 1.261(6) . ? O2' C4' 1.247(5) . ? O3' C1' 1.247(6) . ? O4' C2' 1.267(6) . ? O5' C4' 1.245(5) . ? O6' C3' 1.257(5) . ? C1' C2' 1.539(7) . ? C3' C4' 1.542(7) . ? C5' C10' 1.390(6) . ? C5' C6' 1.404(6) . ? C6' C7' 1.382(6) . ? C7' C8' 1.371(7) . ? C8' C9' 1.384(7) . ? C9' C10' 1.382(7) . ? C11' C12' 1.426(9) . ? C17' C18' 1.371(11) . ? Cl1 O13 1.355(6) . ? Cl1 O11 1.357(10) . ? Cl1 O12 1.358(7) . ? Cl1 O14 1.392(6) . ? Cl2 O16 1.292(7) . ? Cl2 O15 1.375(7) . ? Cl2 O18 1.403(5) . ? Cl2 O17 1.415(5) . ? Cl3 O20 1.329(7) . ? Cl3 O21 1.339(7) . ? Cl3 O22 1.404(5) . ? Cl3 O19 1.404(8) . ? Cl4 O24 1.356(5) . ? Cl4 O26 1.366(7) . ? Cl4 O25 1.412(5) . ? Cl4 O23 1.500(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 N2 Cu1 N1 82.21(15) . . ? N2 Cu1 O1 163.43(15) . . ? N1 Cu1 O1 83.61(13) . . ? N2 Cu1 O2 84.05(14) . . ? N1 Cu1 O2 165.19(14) . . ? O1 Cu1 O2 109.02(12) . . ? N2 Cu1 O7 98.45(16) . . ? N1 Cu1 O7 101.87(16) . . ? O1 Cu1 O7 92.83(15) . . ? O2 Cu1 O7 85.60(16) . . ? O4 Cu2 O3 84.27(12) . . ? O4 Cu2 N3 92.16(14) . . ? O3 Cu2 N3 169.80(15) . . ? O4 Cu2 N4 170.81(17) . . ? O3 Cu2 N4 94.18(15) . . ? N3 Cu2 N4 87.83(16) . . ? O4 Cu2 O8 90.81(16) . . ? O3 Cu2 O8 89.36(15) . . ? N3 Cu2 O8 100.26(16) . . ? N4 Cu2 O8 98.24(18) . . ? O6 Cu3 O5 84.52(12) . . ? O6 Cu3 N5 91.88(14) . . ? O5 Cu3 N5 168.76(17) . . ? O6 Cu3 N6 167.95(17) . . ? O5 Cu3 N6 94.00(14) . . ? N5 Cu3 N6 87.30(16) . . ? O6 Cu3 O9 90.71(15) . . ? O5 Cu3 O9 89.80(15) . . ? N5 Cu3 O9 100.91(16) . . ? N6 Cu3 O9 101.26(17) . . ? C2 N1 C5 129.1(4) . . ? C2 N1 Cu1 114.5(3) . . ? C5 N1 Cu1 116.1(3) . . ? C3 N2 C6 129.4(4) . . ? C3 N2 Cu1 115.2(3) . . ? C6 N2 Cu1 115.2(3) . . ? C14 N3 C13 108.1(4) . . ? C14 N3 C11 111.0(4) . . ? C13 N3 C11 111.0(4) . . ? C14 N3 Cu2 113.0(3) . . ? C13 N3 Cu2 108.5(3) . . ? C11 N3 Cu2 105.3(3) . . ? C16 N4 C12 109.9(5) . . ? C16 N4 C15 109.2(5) . . ? C12 N4 C15 108.6(5) . . ? C16 N4 Cu2 112.3(4) . . ? C12 N4 Cu2 104.8(3) . . ? C15 N4 Cu2 111.9(3) . . ? C18 N5 C22 112.0(5) . . ? C18 N5 C21 110.0(5) . . ? C22 N5 C21 107.7(4) . . ? C18 N5 Cu3 105.2(3) . . ? C22 N5 Cu3 108.7(3) . . ? C21 N5 Cu3 113.4(3) . . ? C19 N6 C17 113.1(5) . . ? C19 N6 C20 105.5(5) . . ? C17 N6 C20 108.8(5) . . ? C19 N6 Cu3 110.9(4) . . ? C17 N6 Cu3 107.0(3) . . ? C20 N6 Cu3 111.5(3) . . ? C1 O1 Cu1 109.1(3) . . ? C4 O2 Cu1 109.7(3) . . ? C1 O3 Cu2 111.2(3) . . ? C2 O4 Cu2 110.0(3) . . ? C4 O5 Cu3 111.4(3) . . ? C3 O6 Cu3 110.5(3) . . ? O1 C1 O3 124.7(4) . . ? O1 C1 C2 120.1(4) . . ? O3 C1 C2 115.2(4) . . ? O4 C2 N1 130.1(4) . . ? O4 C2 C1 118.5(4) . . ? N1 C2 C1 111.4(4) . . ? O6 C3 N2 130.7(4) . . ? O6 C3 C4 117.3(4) . . ? N2 C3 C4 112.0(4) . . ? O5 C4 O2 125.7(4) . . ? O5 C4 C3 116.1(4) . . ? O2 C4 C3 118.2(4) . . ? C10 C5 N1 127.5(4) . . ? C10 C5 C6 119.3(4) . . ? N1 C5 C6 113.2(4) . . ? C7 C6 N2 126.4(4) . . ? C7 C6 C5 120.5(4) . . ? N2 C6 C5 113.2(4) . . ? C6 C7 C8 118.7(4) . . ? C9 C8 C7 121.0(5) . . ? C8 C9 C10 120.6(5) . . ? C5 C10 C9 119.9(5) . . ? N3 C11 C12 109.5(4) . . ? N4 C12 C11 110.0(5) . . ? C18 C17 N6 113.2(5) . . ? C17 C18 N5 113.5(5) . . ? N1' Cu1' N2' 82.88(16) . . ? N1' Cu1' O1' 84.74(15) . . ? N2' Cu1' O1' 167.57(15) . . ? N1' Cu1' O2' 166.98(15) . . ? N2' Cu1' O2' 84.49(14) . . ? O1' Cu1' O2' 107.81(14) . . ? O4' Cu2' O3' 84.28(14) . . ? O4' Cu2' N3' 93.04(15) . . ? O3' Cu2' N3' 167.52(18) . . ? O4' Cu2' N4' 168.27(18) . . ? O3' Cu2' N4' 92.80(16) . . ? N3' Cu2' N4' 87.37(17) . . ? O4' Cu2' O8' 91.39(15) . . ? O3' Cu2' O8' 91.76(16) . . ? N3' Cu2' O8' 100.51(17) . . ? N4' Cu2' O8' 100.07(18) . . ? O6' Cu3' O5' 84.01(13) . . ? O6' Cu3' N5' 91.91(16) . . ? O5' Cu3' N5' 167.16(16) . . ? O6' Cu3' N6' 166.9(2) . . ? O5' Cu3' N6' 93.46(17) . . ? N5' Cu3' N6' 87.77(19) . . ? O6' Cu3' O9' 93.41(18) . . ? O5' Cu3' O9' 92.25(15) . . ? N5' Cu3' O9' 100.16(17) . . ? N6' Cu3' O9' 99.5(2) . . ? C2' N1' C5' 130.4(4) . . ? C2' N1' Cu1' 114.7(3) . . ? C5' N1' Cu1' 114.9(3) . . ? C3' N2' C6' 129.7(4) . . ? C3' N2' Cu1' 114.3(3) . . ? C6' N2' Cu1' 115.2(3) . . ? C11' N3' C14' 110.8(5) . . ? C11' N3' C13' 114.4(6) . . ? C14' N3' C13' 105.9(5) . . ? C11' N3' Cu2' 104.2(3) . . ? C14' N3' Cu2' 113.5(3) . . ? C13' N3' Cu2' 108.3(4) . . ? C16' N4' C12' 114.0(6) . . ? C16' N4' C15' 106.3(5) . . ? C12' N4' C15' 108.2(6) . . ? C16' N4' Cu2' 110.2(4) . . ? C12' N4' Cu2' 106.7(4) . . ? C15' N4' Cu2' 111.5(4) . . ? C21' N5' C22' 110.3(5) . . ? C21' N5' C18' 110.4(5) . . ? C22' N5' C18' 108.7(5) . . ? C21' N5' Cu3' 112.8(3) . . ? C22' N5' Cu3' 108.9(3) . . ? C18' N5' Cu3' 105.6(3) . . ? C19' N6' C17' 115.4(8) . . ? C19' N6' C20' 107.9(6) . . ? C17' N6' C20' 105.7(8) . . ? C19' N6' Cu3' 112.5(5) . . ? C17' N6' Cu3' 102.9(4) . . ? C20' N6' Cu3' 112.3(4) . . ? C1' O1' Cu1' 110.4(3) . . ? C4' O2' Cu1' 110.1(3) . . ? C1' O3' Cu2' 112.0(3) . . ? C2' O4' Cu2' 110.3(3) . . ? C4' O5' Cu3' 110.7(3) . . ? C3' O6' Cu3' 109.9(3) . . ? O3' C1' O1' 125.8(5) . . ? O3' C1' C2' 115.8(5) . . ? O1' C1' C2' 118.4(4) . . ? O4' C2' N1' 130.9(4) . . ? O4' C2' C1' 117.5(4) . . ? N1' C2' C1' 111.6(4) . . ? O6' C3' N2' 131.0(5) . . ? O6' C3' C4' 117.8(4) . . ? N2' C3' C4' 111.2(4) . . ? O5' C4' O2' 125.5(5) . . ? O5' C4' C3' 115.6(4) . . ? O2' C4' C3' 118.9(4) . . ? C10' C5' C6' 119.4(4) . . ? C10' C5' N1' 126.5(4) . . ? C6' C5' N1' 114.1(4) . . ? C7' C6' C5' 120.9(4) . . ? C7' C6' N2' 126.3(4) . . ? C5' C6' N2' 112.8(4) . . ? C8' C7' C6' 118.7(5) . . ? C7' C8' C9' 121.2(5) . . ? C10' C9' C8' 120.6(5) . . ? C9' C10' C5' 119.1(5) . . ? C12' C11' N3' 114.1(6) . . ? C11' C12' N4' 112.5(5) . . ? C18' C17' N6' 116.4(8) . . ? C17' C18' N5' 112.9(6) . . ? O13 Cl1 O11 105.6(8) . . ? O13 Cl1 O12 113.2(5) . . ? O11 Cl1 O12 99.9(7) . . ? O13 Cl1 O14 112.4(3) . . ? O11 Cl1 O14 110.7(7) . . ? O12 Cl1 O14 113.9(5) . . ? O16 Cl2 O15 109.3(8) . . ? O16 Cl2 O18 112.0(5) . . ? O15 Cl2 O18 107.3(4) . . ? O16 Cl2 O17 108.6(6) . . ? O15 Cl2 O17 105.9(4) . . ? O18 Cl2 O17 113.6(4) . . ? O20 Cl3 O21 109.3(7) . . ? O20 Cl3 O22 110.2(4) . . ? O21 Cl3 O22 111.1(4) . . ? O20 Cl3 O19 104.8(7) . . ? O21 Cl3 O19 106.6(7) . . ? O22 Cl3 O19 114.5(5) . . ? O24 Cl4 O26 110.7(6) . . ? O24 Cl4 O25 110.3(4) . . ? O26 Cl4 O25 111.3(4) . . ? O24 Cl4 O23 106.2(4) . . ? O26 Cl4 O23 110.6(7) . . ? O25 Cl4 O23 107.6(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.986 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.090 #==END