Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_kdk18 _database_code_CSD 150146 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H53 Cl8 Cu2 N7 O8' _chemical_formula_weight 1194.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5816(2) _cell_length_b 14.8247(2) _cell_length_c 18.0045(2) _cell_angle_alpha 112.4800(3) _cell_angle_beta 97.2565(2) _cell_angle_gamma 94.2666(2) _cell_volume 2565.53(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.302 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6961 _exptl_absorpt_correction_T_max 0.9378 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16251 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.00 _reflns_number_total 7939 _reflns_number_gt 6994 _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^)+(0.0383P)^2^+6.0492P] 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 7939 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.77009(4) 0.24043(3) 0.77214(2) 0.02503(12) Uani 1 1 d . . . Cu2 Cu 0.58823(4) 0.36720(3) 0.53824(3) 0.03082(13) Uani 1 1 d . . . Cl1 Cl 0.27932(9) 0.32872(7) 0.02614(6) 0.0404(2) Uani 1 1 d . . . Cl2 Cl 0.82502(8) 0.18813(7) 0.49555(5) 0.0348(2) Uani 1 1 d . . . O1 O 0.3220(4) 0.2983(4) 0.0889(3) 0.0921(14) Uani 1 1 d . . . O2 O 0.2707(5) 0.2542(3) -0.0524(3) 0.1030(16) Uani 1 1 d . . . O3 O 0.1531(3) 0.3544(3) 0.0347(2) 0.0630(9) Uani 1 1 d . . . O4 O 0.3615(3) 0.4128(3) 0.0318(2) 0.0673(10) Uani 1 1 d . . . O5 O 0.7006(3) 0.2142(2) 0.5124(2) 0.0611(9) Uani 1 1 d . . . O6 O 0.9206(3) 0.2609(2) 0.55651(19) 0.0567(8) Uani 1 1 d . . . O7 O 0.8364(3) 0.0934(2) 0.49804(18) 0.0527(8) Uani 1 1 d . . . O8 O 0.8407(4) 0.1840(3) 0.41711(19) 0.0742(11) Uani 1 1 d . . . N1 N 0.7632(3) 0.2800(2) 0.89856(16) 0.0252(6) Uani 1 1 d . . . N2 N 0.6469(3) 0.4506(2) 0.67389(17) 0.0260(6) Uani 1 1 d . . . N3 N 0.5883(3) 0.1886(2) 0.72207(17) 0.0276(6) Uani 1 1 d . . . N4 N 0.8773(3) 0.1283(2) 0.75003(18) 0.0299(7) Uani 1 1 d . . . N5 N 0.4343(3) 0.2858(2) 0.53361(19) 0.0318(7) Uani 1 1 d . . . N6 N 0.7005(3) 0.4493(2) 0.50654(19) 0.0362(7) Uani 1 1 d . . . N7 N 0.8898(2) 0.3745(2) 0.80577(16) 0.0219(6) Uani 1 1 d . . . C1 C 0.6297(3) 0.2676(3) 0.9148(2) 0.0314(8) Uani 1 1 d . . . H1A H 0.6252 0.3137 0.9709 0.038 Uiso 1 1 calc R . . H1B H 0.6081 0.1997 0.9111 0.038 Uiso 1 1 calc R . . C2 C 0.5307(3) 0.2867(3) 0.8545(2) 0.0333(8) Uani 1 1 d . . . H2A H 0.4507 0.2992 0.8778 0.040 Uiso 1 1 calc R . . H2B H 0.5642 0.3470 0.8481 0.040 Uiso 1 1 calc R . . C3 C 0.4988(3) 0.2034(3) 0.7717(2) 0.0311(8) Uani 1 1 d . . . C4 C 0.3836(4) 0.1406(3) 0.7475(3) 0.0490(11) Uani 1 1 d . . . H4A H 0.3214 0.1513 0.7826 0.059 Uiso 1 1 calc R . . C5 C 0.3594(4) 0.0626(4) 0.6724(3) 0.0588(13) Uani 1 1 d . . . H5A H 0.2821 0.0180 0.6563 0.071 Uiso 1 1 calc R . . C6 C 0.4492(4) 0.0499(3) 0.6209(3) 0.0465(10) Uani 1 1 d . . . H6A H 0.4339 -0.0022 0.5683 0.056 Uiso 1 1 calc R . . C7 C 0.5603(4) 0.1144(3) 0.6475(2) 0.0343(8) Uani 1 1 d . . . H7A H 0.6211 0.1066 0.6117 0.041 Uiso 1 1 calc R . . C8 C 0.8439(4) 0.2214(3) 0.9307(2) 0.0322(8) Uani 1 1 d . . . H8A H 0.8232 0.2281 0.9845 0.039 Uiso 1 1 calc R . . H8B H 0.9355 0.2480 0.9387 0.039 Uiso 1 1 calc R . . C9 C 0.8236(4) 0.1121(3) 0.8736(2) 0.0385(9) Uani 1 1 d . . . H9A H 0.8494 0.0738 0.9063 0.046 Uiso 1 1 calc R . . H9B H 0.7305 0.0920 0.8522 0.046 Uiso 1 1 calc R . . C10 C 0.8949(4) 0.0834(3) 0.8019(2) 0.0338(8) Uani 1 1 d . . . C11 C 0.9724(5) 0.0095(3) 0.7881(3) 0.0514(11) Uani 1 1 d . . . H11A H 0.9867 -0.0200 0.8263 0.062 Uiso 1 1 calc R . . C12 C 1.0290(5) -0.0219(3) 0.7193(3) 0.0559(12) Uani 1 1 d . . . H12A H 1.0807 -0.0737 0.7092 0.067 Uiso 1 1 calc R . . C13 C 1.0093(4) 0.0232(3) 0.6651(3) 0.0419(10) Uani 1 1 d . . . H13A H 1.0460 0.0026 0.6168 0.050 Uiso 1 1 calc R . . C14 C 0.9353(4) 0.0982(3) 0.6831(2) 0.0349(8) Uani 1 1 d . . . H14A H 0.9240 0.1308 0.6469 0.042 Uiso 1 1 calc R . . C15 C 0.8172(3) 0.3858(2) 0.9360(2) 0.0273(7) Uani 1 1 d . . . H15A H 0.8482 0.4051 0.9949 0.033 Uiso 1 1 calc R . . H15B H 0.7488 0.4259 0.9304 0.033 Uiso 1 1 calc R . . C16 C 0.9281(3) 0.4066(3) 0.8956(2) 0.0257(7) Uani 1 1 d . . . H16A H 0.9590 0.4781 0.9202 0.031 Uiso 1 1 calc R . . H16B H 1.0001 0.3719 0.9064 0.031 Uiso 1 1 calc R . . C17 C 0.5395(3) 0.4277(3) 0.7112(2) 0.0352(9) Uani 1 1 d . . . H17A H 0.5444 0.4808 0.7659 0.042 Uiso 1 1 calc R . . H17B H 0.5498 0.3658 0.7187 0.042 Uiso 1 1 calc R . . C18 C 0.4048(3) 0.4165(3) 0.6612(2) 0.0376(9) Uani 1 1 d . . . H18A H 0.3410 0.4301 0.6986 0.045 Uiso 1 1 calc R . . H18B H 0.4049 0.4665 0.6373 0.045 Uiso 1 1 calc R . . C19 C 0.3635(3) 0.3164(3) 0.5939(2) 0.0330(8) Uani 1 1 d . . . C20 C 0.2539(4) 0.2562(4) 0.5923(3) 0.0488(11) Uani 1 1 d . . . H20A H 0.2051 0.2778 0.6353 0.059 Uiso 1 1 calc R . . C21 C 0.2164(4) 0.1657(4) 0.5285(3) 0.0605(13) Uani 1 1 d . . . H21A H 0.1412 0.1249 0.5264 0.073 Uiso 1 1 calc R . . C22 C 0.2902(4) 0.1357(3) 0.4679(3) 0.0604(14) Uani 1 1 d . . . H22A H 0.2669 0.0735 0.4236 0.073 Uiso 1 1 calc R . . C23 C 0.3977(4) 0.1963(3) 0.4719(3) 0.0452(10) Uani 1 1 d . . . H23A H 0.4481 0.1747 0.4299 0.054 Uiso 1 1 calc R . . C24 C 0.6767(5) 0.5566(3) 0.6925(3) 0.0455(10) Uani 1 1 d . . . H24A H 0.7699 0.5770 0.7131 0.055 Uiso 1 1 calc R . . H24B H 0.6304 0.5941 0.7366 0.055 Uiso 1 1 calc R . . C25 C 0.6402(4) 0.5845(3) 0.6185(3) 0.0443(10) Uani 1 1 d . . . H25A H 0.5488 0.5586 0.5949 0.053 Uiso 1 1 calc R . . H25B H 0.6485 0.6572 0.6384 0.053 Uiso 1 1 calc R . . C26 C 0.7193(4) 0.5470(3) 0.5521(3) 0.0434(10) Uani 1 1 d . . . C27 C 0.8103(4) 0.6097(4) 0.5372(3) 0.0570(13) Uani 1 1 d . . . H27A H 0.8249 0.6784 0.5701 0.068 Uiso 1 1 calc R . . C28 C 0.8777(4) 0.5701(5) 0.4744(4) 0.0704(17) Uani 1 1 d . . . H28A H 0.9380 0.6116 0.4628 0.084 Uiso 1 1 calc R . . C29 C 0.8579(4) 0.4708(5) 0.4285(3) 0.0603(14) Uani 1 1 d . . . H29A H 0.9048 0.4429 0.3853 0.072 Uiso 1 1 calc R . . C30 C 0.7699(4) 0.4122(4) 0.4456(3) 0.0474(11) Uani 1 1 d . . . H30A H 0.7568 0.3433 0.4138 0.057 Uiso 1 1 calc R . . C31 C 0.7622(3) 0.4078(3) 0.69510(19) 0.0252(7) Uani 1 1 d . . . H31A H 0.8303 0.4206 0.6660 0.030 Uiso 1 1 calc R . . H31B H 0.7395 0.3355 0.6748 0.030 Uiso 1 1 calc R . . C32 C 0.8177(3) 0.4476(2) 0.7868(2) 0.0248(7) Uani 1 1 d . . . H32A H 0.8757 0.5098 0.8026 0.030 Uiso 1 1 calc R . . H32B H 0.7467 0.4619 0.8188 0.030 Uiso 1 1 calc R . . C33 C 1.0066(3) 0.3564(2) 0.7650(2) 0.0241(7) Uani 1 1 d . . . H33A H 0.9793 0.3406 0.7062 0.029 Uiso 1 1 calc R . . H33B H 1.0386 0.2973 0.7695 0.029 Uiso 1 1 calc R . . C34 C 1.1175(3) 0.4389(2) 0.79697(19) 0.0246(7) Uani 1 1 d . . . C35 C 1.2252(3) 0.4349(3) 0.8489(2) 0.0291(8) Uani 1 1 d . . . H35A H 1.2264 0.3810 0.8651 0.035 Uiso 1 1 calc R . . C36 C 1.3302(3) 0.5079(3) 0.8771(2) 0.0323(8) Uani 1 1 d . . . H36A H 1.4024 0.5035 0.9121 0.039 Uiso 1 1 calc R . . C37 C 1.3299(3) 0.5869(3) 0.8543(2) 0.0371(9) Uani 1 1 d . . . H37A H 1.4019 0.6369 0.8736 0.045 Uiso 1 1 calc R . . C38 C 1.2250(4) 0.5931(3) 0.8035(3) 0.0397(9) Uani 1 1 d . . . H38A H 1.2247 0.6476 0.7880 0.048 Uiso 1 1 calc R . . C39 C 1.1191(3) 0.5196(3) 0.7748(2) 0.0334(8) Uani 1 1 d . . . H39A H 1.0473 0.5245 0.7397 0.040 Uiso 1 1 calc R . . 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 0.0210(2) 0.0286(2) 0.0210(2) 0.00583(17) 0.00256(16) 0.00033(17) Cu2 0.0270(2) 0.0372(3) 0.0257(2) 0.0117(2) 0.00024(17) -0.00016(19) Cl1 0.0379(5) 0.0444(6) 0.0406(5) 0.0177(4) 0.0092(4) 0.0057(4) Cl2 0.0316(5) 0.0367(5) 0.0278(5) 0.0038(4) 0.0046(4) 0.0054(4) O1 0.066(2) 0.139(4) 0.106(3) 0.094(3) -0.005(2) 0.010(2) O2 0.151(4) 0.067(3) 0.079(3) 0.004(2) 0.066(3) 0.001(3) O3 0.0389(17) 0.070(2) 0.081(2) 0.0300(19) 0.0079(16) 0.0105(16) O4 0.0434(18) 0.059(2) 0.100(3) 0.039(2) -0.0011(18) -0.0092(16) O5 0.0317(16) 0.056(2) 0.080(2) 0.0091(17) 0.0098(15) 0.0083(14) O6 0.0369(16) 0.058(2) 0.0526(19) 0.0000(15) 0.0078(14) -0.0089(14) O7 0.070(2) 0.0388(16) 0.0456(17) 0.0109(14) 0.0098(15) 0.0145(15) O8 0.126(3) 0.069(2) 0.0386(18) 0.0224(17) 0.034(2) 0.039(2) N1 0.0247(15) 0.0282(15) 0.0208(14) 0.0080(12) 0.0051(11) -0.0008(12) N2 0.0250(15) 0.0274(15) 0.0227(14) 0.0075(12) 0.0005(12) 0.0047(12) N3 0.0241(15) 0.0296(16) 0.0269(15) 0.0097(13) 0.0016(12) 0.0021(12) N4 0.0296(16) 0.0289(16) 0.0292(16) 0.0093(13) 0.0051(13) 0.0037(13) N5 0.0192(15) 0.0381(18) 0.0359(17) 0.0133(14) 0.0007(13) 0.0044(13) N6 0.0339(17) 0.047(2) 0.0311(17) 0.0223(16) -0.0025(14) 0.0016(15) N7 0.0165(13) 0.0255(15) 0.0220(14) 0.0085(12) 0.0017(11) 0.0011(11) C1 0.0309(19) 0.036(2) 0.0254(18) 0.0090(16) 0.0107(15) -0.0004(16) C2 0.0248(18) 0.036(2) 0.038(2) 0.0112(17) 0.0100(16) 0.0052(15) C3 0.0213(18) 0.033(2) 0.038(2) 0.0131(17) 0.0043(15) 0.0030(15) C4 0.025(2) 0.063(3) 0.049(3) 0.013(2) 0.0066(18) -0.0062(19) C5 0.034(2) 0.062(3) 0.056(3) 0.004(2) -0.002(2) -0.021(2) C6 0.040(2) 0.043(2) 0.039(2) 0.0002(19) -0.0006(19) -0.0056(19) C7 0.031(2) 0.037(2) 0.029(2) 0.0078(17) 0.0007(15) 0.0015(16) C8 0.033(2) 0.036(2) 0.0286(19) 0.0146(16) 0.0043(15) 0.0029(16) C9 0.052(2) 0.036(2) 0.036(2) 0.0207(18) 0.0122(18) 0.0094(18) C10 0.038(2) 0.0255(19) 0.040(2) 0.0150(17) 0.0090(17) 0.0010(16) C11 0.063(3) 0.049(3) 0.061(3) 0.033(2) 0.026(2) 0.028(2) C12 0.061(3) 0.045(3) 0.071(3) 0.026(2) 0.025(3) 0.025(2) C13 0.041(2) 0.037(2) 0.041(2) 0.0052(18) 0.0162(18) 0.0071(18) C14 0.033(2) 0.033(2) 0.035(2) 0.0077(17) 0.0104(16) 0.0041(16) C15 0.0274(18) 0.0268(18) 0.0209(17) 0.0039(14) 0.0014(14) -0.0029(14) C16 0.0217(17) 0.0299(18) 0.0216(17) 0.0081(14) -0.0007(13) -0.0017(14) C17 0.0250(19) 0.054(2) 0.0231(18) 0.0102(17) 0.0043(15) 0.0102(17) C18 0.0214(18) 0.053(2) 0.033(2) 0.0104(18) 0.0039(15) 0.0109(17) C19 0.0210(18) 0.041(2) 0.038(2) 0.0174(18) -0.0011(15) 0.0098(16) C20 0.028(2) 0.073(3) 0.056(3) 0.036(3) 0.0101(19) 0.010(2) C21 0.032(2) 0.058(3) 0.086(4) 0.028(3) 0.001(2) -0.008(2) C22 0.036(2) 0.038(2) 0.087(4) 0.008(2) -0.003(2) -0.001(2) C23 0.029(2) 0.037(2) 0.050(3) -0.0010(19) -0.0035(18) 0.0039(17) C24 0.061(3) 0.034(2) 0.037(2) 0.0131(18) -0.004(2) 0.007(2) C25 0.055(3) 0.031(2) 0.045(2) 0.0163(19) -0.006(2) 0.0104(19) C26 0.034(2) 0.054(3) 0.050(3) 0.036(2) -0.0109(18) 0.0000(19) C27 0.047(3) 0.054(3) 0.078(3) 0.048(3) -0.020(3) -0.009(2) C28 0.031(2) 0.115(5) 0.105(5) 0.090(4) 0.002(3) 0.001(3) C29 0.034(2) 0.101(4) 0.071(3) 0.060(3) 0.011(2) 0.010(3) C30 0.036(2) 0.077(3) 0.043(2) 0.038(2) 0.0061(19) 0.012(2) C31 0.0208(17) 0.0335(19) 0.0198(17) 0.0099(15) 0.0001(13) 0.0045(14) C32 0.0188(16) 0.0275(18) 0.0226(17) 0.0060(14) -0.0016(13) -0.0003(13) C33 0.0177(16) 0.0298(18) 0.0215(17) 0.0069(14) 0.0018(13) 0.0034(14) C34 0.0202(17) 0.0281(18) 0.0212(17) 0.0047(14) 0.0050(13) 0.0027(14) C35 0.0234(18) 0.036(2) 0.0290(19) 0.0141(16) 0.0050(15) 0.0038(15) C36 0.0195(17) 0.044(2) 0.0265(18) 0.0081(17) 0.0005(14) 0.0002(15) C37 0.0248(19) 0.038(2) 0.034(2) -0.0004(17) 0.0100(16) -0.0087(16) C38 0.039(2) 0.039(2) 0.048(2) 0.0216(19) 0.0186(19) 0.0028(18) C39 0.0224(18) 0.047(2) 0.037(2) 0.0239(18) 0.0029(15) 0.0035(16) _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 N3 1.979(3) . ? Cu1 N4 2.024(3) . ? Cu1 N7 2.106(3) . ? Cu1 N1 2.135(3) . ? Cu2 N6 1.925(3) . ? Cu2 N5 1.927(3) . ? Cu2 N2 2.252(3) . ? Cu2 O5 2.551(3) . ? Cl1 O1 1.405(4) . ? Cl1 O2 1.410(4) . ? Cl1 O3 1.427(3) . ? Cl1 O4 1.428(3) . ? Cl2 O8 1.421(3) . ? Cl2 O6 1.429(3) . ? Cl2 O7 1.435(3) . ? Cl2 O5 1.436(3) . ? N1 C8 1.480(4) . ? N1 C15 1.483(4) . ? N1 C1 1.491(4) . ? N2 C17 1.473(5) . ? N2 C24 1.476(5) . ? N2 C31 1.491(4) . ? N3 C7 1.350(5) . ? N3 C3 1.355(5) . ? N4 C10 1.343(5) . ? N4 C14 1.358(5) . ? N5 C19 1.351(5) . ? N5 C23 1.353(5) . ? N6 C26 1.349(5) . ? N6 C30 1.359(5) . ? N7 C32 1.487(4) . ? N7 C16 1.491(4) . ? N7 C33 1.506(4) . ? C1 C2 1.531(5) . ? C2 C3 1.505(5) . ? C3 C4 1.390(5) . ? C4 C5 1.379(6) . ? C5 C6 1.384(6) . ? C6 C7 1.366(5) . ? C8 C9 1.533(5) . ? C9 C10 1.513(5) . ? C10 C11 1.382(5) . ? C11 C12 1.377(6) . ? C12 C13 1.381(6) . ? C13 C14 1.368(5) . ? C15 C16 1.528(5) . ? C17 C18 1.548(5) . ? C18 C19 1.502(5) . ? C19 C20 1.400(6) . ? C20 C21 1.381(7) . ? C21 C22 1.375(7) . ? C22 C23 1.373(6) . ? C24 C25 1.552(5) . ? C25 C26 1.501(6) . ? C26 C27 1.410(6) . ? C27 C28 1.375(8) . ? C28 C29 1.369(8) . ? C29 C30 1.369(6) . ? C31 C32 1.542(4) . ? C33 C34 1.511(5) . ? C34 C39 1.398(5) . ? C34 C35 1.400(5) . ? C35 C36 1.385(5) . ? C36 C37 1.382(6) . ? C37 C38 1.379(6) . ? C38 C39 1.397(5) . ? 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 N3 Cu1 N4 110.12(12) . . ? N3 Cu1 N7 136.02(11) . . ? N4 Cu1 N7 109.95(11) . . ? N3 Cu1 N1 101.84(11) . . ? N4 Cu1 N1 100.90(11) . . ? N7 Cu1 N1 87.66(10) . . ? N6 Cu2 N5 157.68(13) . . ? N6 Cu2 N2 96.70(12) . . ? N5 Cu2 N2 100.97(12) . . ? N6 Cu2 O5 103.08(13) . . ? N5 Cu2 O5 86.52(11) . . ? N2 Cu2 O5 102.06(11) . . ? O1 Cl1 O2 113.2(3) . . ? O1 Cl1 O3 107.8(2) . . ? O2 Cl1 O3 107.1(3) . . ? O1 Cl1 O4 111.0(2) . . ? O2 Cl1 O4 108.7(2) . . ? O3 Cl1 O4 108.9(2) . . ? O8 Cl2 O6 109.9(2) . . ? O8 Cl2 O7 109.34(19) . . ? O6 Cl2 O7 109.9(2) . . ? O8 Cl2 O5 110.2(2) . . ? O6 Cl2 O5 108.40(19) . . ? O7 Cl2 O5 109.0(2) . . ? Cl2 O5 Cu2 135.9(2) . . ? C8 N1 C15 110.9(3) . . ? C8 N1 C1 109.8(3) . . ? C15 N1 C1 110.0(3) . . ? C8 N1 Cu1 110.2(2) . . ? C15 N1 Cu1 103.18(19) . . ? C1 N1 Cu1 112.6(2) . . ? C17 N2 C24 113.4(3) . . ? C17 N2 C31 110.7(3) . . ? C24 N2 C31 112.1(3) . . ? C17 N2 Cu2 106.4(2) . . ? C24 N2 Cu2 109.4(2) . . ? C31 N2 Cu2 104.27(19) . . ? C7 N3 C3 118.4(3) . . ? C7 N3 Cu1 119.6(2) . . ? C3 N3 Cu1 118.3(2) . . ? C10 N4 C14 118.5(3) . . ? C10 N4 Cu1 120.9(2) . . ? C14 N4 Cu1 120.7(2) . . ? C19 N5 C23 119.1(3) . . ? C19 N5 Cu2 120.0(3) . . ? C23 N5 Cu2 120.9(3) . . ? C26 N6 C30 119.0(4) . . ? C26 N6 Cu2 117.8(3) . . ? C30 N6 Cu2 122.9(3) . . ? C32 N7 C16 110.8(3) . . ? C32 N7 C33 112.3(3) . . ? C16 N7 C33 109.9(2) . . ? C32 N7 Cu1 110.76(19) . . ? C16 N7 Cu1 102.95(19) . . ? C33 N7 Cu1 109.76(19) . . ? N1 C1 C2 112.2(3) . . ? C3 C2 C1 114.0(3) . . ? N3 C3 C4 120.5(4) . . ? N3 C3 C2 118.0(3) . . ? C4 C3 C2 121.5(3) . . ? C5 C4 C3 120.0(4) . . ? C4 C5 C6 119.2(4) . . ? C7 C6 C5 118.2(4) . . ? N3 C7 C6 123.5(4) . . ? N1 C8 C9 112.4(3) . . ? C10 C9 C8 116.5(3) . . ? N4 C10 C11 120.5(4) . . ? N4 C10 C9 118.6(3) . . ? C11 C10 C9 120.8(3) . . ? C12 C11 C10 120.7(4) . . ? C11 C12 C13 118.9(4) . . ? C14 C13 C12 118.1(4) . . ? N4 C14 C13 123.3(4) . . ? N1 C15 C16 111.3(3) . . ? N7 C16 C15 112.3(3) . . ? N2 C17 C18 114.3(3) . . ? C19 C18 C17 113.9(3) . . ? N5 C19 C20 120.3(4) . . ? N5 C19 C18 118.2(3) . . ? C20 C19 C18 121.5(4) . . ? C21 C20 C19 120.2(4) . . ? C22 C21 C20 118.6(4) . . ? C23 C22 C21 119.6(4) . . ? N5 C23 C22 122.3(4) . . ? N2 C24 C25 114.1(3) . . ? C26 C25 C24 115.1(3) . . ? N6 C26 C27 120.5(4) . . ? N6 C26 C25 117.1(4) . . ? C27 C26 C25 122.4(4) . . ? C28 C27 C26 119.0(5) . . ? C29 C28 C27 120.0(5) . . ? C30 C29 C28 119.2(5) . . ? N6 C30 C29 122.3(5) . . ? N2 C31 C32 115.2(3) . . ? N7 C32 C31 110.7(3) . . ? N7 C33 C34 116.9(3) . . ? C39 C34 C35 117.7(3) . . ? C39 C34 C33 122.3(3) . . ? C35 C34 C33 120.0(3) . . ? C36 C35 C34 121.3(3) . . ? C37 C36 C35 120.1(3) . . ? C38 C37 C36 119.9(3) . . ? C37 C38 C39 120.2(4) . . ? C38 C39 C34 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.443 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.068