Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _database_code_CSD 170087 _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Feyissa, Gadissa Gelacha' ; Institut fur organische Chemie Universitat Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; 'Schulz,Manfred' ; Institut fur Organische Chemie Martin-Luther-Universitat Halle-Wittenberg Kurt-Mothestrasse 2 06099 Halle Bundesrepublik Deutschland ; 'Kluge,Ralph' ; Institut fur organische Chemie Martin-Luther-Universitat Halle-Wittenberg Kurt-Mothesstrasse 2 06099 Halle Bundesrepublik Deutschland ; 'Sieler, Joachim' ; Insitut fur Anorganische Chemie Universitat Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author_name 'Dr Feyissa Gadissa Gelalcha' _publ_contact_author_address ; Institut fur Organische Chemie Universitat Leipzig Johannisallee 29, D-04103 Leipzig Leipzig Sachsen D-04103 GERMANY ; _publ_contact_author_phone '0341 9736215' _publ_contact_author_fax '0341 9736249' _publ_contact_author_email 'sieler@rz.uni-leipzig.de' _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' _publ_section_title ; Molecular Self-Assembly: Synthesis and Structural Characterisation of bis[{1,6-bis[(4S)-4-i-propyl-1,3-oxazolin-1-yl]-pyridyl}-Copper(I)] trifluoromethane sulfonate - A Novel Binuclear Double Helicate ; _publ_contact_letter ; Please consider this submission for publication in "J.Chem.Soc.,Dalton Trans." as a deposition of a crystal structure. ; #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Molecular Self-Assembly: Synthesis and Characterisation of bis [{2,6- bis[(4S)-4-isopropyl-1,3-oxazolin-2-yl]-pyridyl}-Copper(I)-trifluoromethane sulphonate- a Dinuclear Double-Helical Complex ; #========================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H46 Cu2 F6 N6 O10 S2' _chemical_formula_weight 1027.99 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' _cell_length_a 14.560(3) _cell_length_b 10.193(2) _cell_length_c 30.500(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.48(3) _cell_angle_gamma 90.00 _cell_volume 4526.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1200 _cell_measurement_theta_min 1 _cell_measurement_theta_max 26 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.7454 _exptl_absorpt_correction_T_max 0.8967 _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_Diffractometer (BRUKER AXS)' _diffrn_measurement_method 'Omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19463 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 13556 _reflns_number_gt 10524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER AXS)' _computing_cell_refinement 'SAINT (BRUKER AXS)' _computing_data_reduction 'SAINT (BRUKER AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP(BRUKER AXS)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+19.8545P] 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 SHELXL _refine_ls_extinction_coef 0.00008(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 13556 _refine_ls_number_parameters 1122 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2101 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.010 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.69256(9) 0.61285(12) 0.86580(4) 0.0506(3) Uani 1 d . . . Cu2 Cu 0.83794(9) 0.49353(12) 0.90818(4) 0.0516(3) Uani 1 d . . . N1 N 0.6754(5) 0.6643(8) 0.9314(3) 0.045(2) Uani 1 d . . . N2 N 0.6915(5) 0.8128(8) 0.8585(3) 0.043(2) Uani 1 d . . . N3 N 0.7525(6) 0.3992(8) 0.9426(3) 0.046(2) Uani 1 d . . . N4 N 0.7943(6) 0.5325(9) 0.8210(3) 0.052(2) Uani 1 d . . . N5 N 0.9163(6) 0.6267(9) 0.8857(3) 0.059(2) Uani 1 d . . . N6 N 0.6180(6) 0.4732(9) 0.8365(3) 0.053(2) Uani 1 d . . . O1 O 0.6714(5) 0.9984(7) 0.8969(2) 0.0556(18) Uani 1 d . . . O2 O 0.6294(5) 0.3654(7) 0.9853(3) 0.060(2) Uani 1 d . . . O3 O 0.9871(7) 0.7445(11) 0.8337(4) 0.100(4) Uani 1 d . . . O4 O 0.6121(9) 0.3385(9) 0.7791(3) 0.088(3) Uani 1 d . . . C1 C 0.6593(6) 0.7939(10) 0.9353(3) 0.042(2) Uani 1 d . . . C2 C 0.6260(7) 0.8470(11) 0.9739(4) 0.056(3) Uani 1 d . . . H2 H 0.6124 0.9480 0.9757 0.126(17) Uiso 1 calc R . . C3 C 0.6109(8) 0.7696(13) 1.0093(4) 0.064(3) Uani 1 d . . . H3 H 0.5877 0.8113 1.0387 0.126(17) Uiso 1 calc R . . C4 C 0.6263(7) 0.6339(12) 1.0067(4) 0.054(3) Uani 1 d . . . H4 H 0.6132 0.5701 1.0329 0.126(17) Uiso 1 calc R . . C5 C 0.6607(7) 0.5896(10) 0.9662(3) 0.044(2) Uani 1 d . . . C6 C 0.6726(7) 0.8675(10) 0.8948(4) 0.046(3) Uani 1 d . . . C7 C 0.7076(7) 0.9177(10) 0.8259(3) 0.047(2) Uani 1 d . . . H7 H 0.7783 0.9233 0.8196 0.067(9) Uiso 1 calc R . . C8 C 0.6782(8) 1.0413(11) 0.8510(4) 0.057(3) Uani 1 d . . . H8A H 0.7273 1.1160 0.8478 0.122(14) Uiso 1 calc R . . H8B H 0.6146 1.0759 0.8393 0.122(14) Uiso 1 calc R . . C9 C 0.6565(8) 0.9005(12) 0.7827(4) 0.061(3) Uani 1 d . . . H9 H 0.5857 0.8964 0.7888 0.067(9) Uiso 1 calc R . . C10 C 0.6858(10) 0.7739(12) 0.7585(4) 0.072(4) Uani 1 d . . . H10A H 0.6485 0.7657 0.7290 0.150(10) Uiso 1 calc R . . H10B H 0.6723 0.6921 0.7784 0.150(10) Uiso 1 calc R . . H10C H 0.7563 0.7781 0.7517 0.150(10) Uiso 1 calc R . . C11 C 0.6761(10) 1.0179(13) 0.7531(4) 0.078(4) Uani 1 d . . . H11A H 0.6400 1.0069 0.7234 0.150(10) Uiso 1 calc R . . H11B H 0.7468 1.0229 0.7469 0.150(10) Uiso 1 calc R . . H11C H 0.6549 1.1044 0.7687 0.150(10) Uiso 1 calc R . . C12 C 0.6838(7) 0.4452(11) 0.9632(3) 0.046(3) Uani 1 d . . . C13 C 0.7547(7) 0.2556(10) 0.9527(4) 0.052(3) Uani 1 d . . . H13 H 0.7562 0.2036 0.9230 0.067(9) Uiso 1 calc R . . C14 C 0.6621(9) 0.2333(12) 0.9739(4) 0.065(3) Uani 1 d . . . H14A H 0.6165 0.1872 0.9520 0.122(14) Uiso 1 calc R . . H14B H 0.6690 0.1749 1.0021 0.122(14) Uiso 1 calc R . . C15 C 0.8384(10) 0.2197(13) 0.9792(5) 0.079(4) Uani 1 d . . . H15 H 0.8953 0.2459 0.9601 0.067(9) Uiso 1 calc R . . C16 C 0.8447(12) 0.0700(14) 0.9860(6) 0.102(5) Uani 1 d . . . H16A H 0.9037 0.0478 1.0046 0.150(10) Uiso 1 calc R . . H16B H 0.8485 0.0232 0.9554 0.150(10) Uiso 1 calc R . . H16C H 0.7863 0.0371 1.0026 0.150(10) Uiso 1 calc R . . C17 C 0.8479(17) 0.2914(19) 1.0205(7) 0.163(11) Uani 1 d . . . H17A H 0.9079 0.2609 1.0368 0.150(10) Uiso 1 calc R . . H17B H 0.7907 0.2725 1.0402 0.150(10) Uiso 1 calc R . . H17C H 0.8518 0.3924 1.0140 0.150(10) Uiso 1 calc R . . C18 C 0.8780(8) 0.5814(14) 0.8103(4) 0.072(4) Uani 1 d . . . C19 C 0.9152(10) 0.5624(19) 0.7702(5) 0.098(6) Uani 1 d . . . H19 H 0.9787 0.6052 0.7626 0.126(17) Uiso 1 calc R . . C20 C 0.8705(13) 0.488(2) 0.7398(5) 0.112(7) Uani 1 d . . . H20 H 0.9000 0.4722 0.7090 0.126(17) Uiso 1 calc R . . C21 C 0.7859(13) 0.4332(16) 0.7494(4) 0.093(5) Uani 1 d . . . H21 H 0.7502 0.3734 0.7270 0.126(17) Uiso 1 calc R . . C22 C 0.7516(9) 0.4623(11) 0.7904(4) 0.061(3) Uani 1 d . . . C23 C 0.9257(7) 0.6509(12) 0.8453(5) 0.061(3) Uani 1 d . . . C24 C 0.9833(8) 0.7131(12) 0.9100(5) 0.072(4) Uani 1 d . . . H24 H 0.9475 0.7675 0.9336 0.067(9) Uiso 1 calc R . . C25 C 1.0181(12) 0.805(2) 0.8756(8) 0.129(8) Uani 1 d . . . H25A H 0.9898 0.8992 0.8794 0.122(14) Uiso 1 calc R . . H25B H 1.0900 0.8121 0.8769 0.122(14) Uiso 1 calc R . . C26 C 1.0559(8) 0.6282(14) 0.9333(5) 0.079(4) Uani 1 d . . . H26 H 1.0218 0.5606 0.9534 0.067(9) Uiso 1 calc R . . C27 C 1.1122(9) 0.5535(17) 0.9014(6) 0.102(5) Uani 1 d . . . H27A H 1.1610 0.4967 0.9184 0.150(10) Uiso 1 calc R . . H27B H 1.1460 0.6194 0.8806 0.150(10) Uiso 1 calc R . . H27C H 1.0694 0.4918 0.8828 0.150(10) Uiso 1 calc R . . C28 C 1.1169(10) 0.7166(19) 0.9631(7) 0.123(7) Uani 1 d . . . H28A H 1.1665 0.6587 0.9791 0.150(10) Uiso 1 calc R . . H28B H 1.0757 0.7634 0.9864 0.150(10) Uiso 1 calc R . . H28C H 1.1498 0.7875 0.9438 0.150(10) Uiso 1 calc R . . C29 C 0.6578(9) 0.4248(11) 0.8036(4) 0.057(3) Uani 1 d . . . C30 C 0.5256(8) 0.4152(14) 0.8405(5) 0.079(4) Uani 1 d . . . H30 H 0.5249 0.3528 0.8678 0.067(9) Uiso 1 calc R . . C31 C 0.5224(14) 0.3304(14) 0.7981(5) 0.101(6) Uani 1 d . . . H31A H 0.5063 0.2327 0.8057 0.122(14) Uiso 1 calc R . . H31B H 0.4725 0.3667 0.7762 0.122(14) Uiso 1 calc R . . C32 C 0.4513(9) 0.520(2) 0.8461(6) 0.111(6) Uani 1 d . . . H32 H 0.4723 0.5751 0.8735 0.067(9) Uiso 1 calc R . . C33 C 0.3594(17) 0.480(4) 0.8555(11) 0.247(19) Uani 1 d . . . H33A H 0.3166 0.5626 0.8567 0.150(10) Uiso 1 calc R . . H33B H 0.3583 0.4314 0.8859 0.150(10) Uiso 1 calc R . . H33C H 0.3360 0.4160 0.8308 0.150(10) Uiso 1 calc R . . C34 C 0.4497(10) 0.6179(18) 0.8080(7) 0.122(7) Uani 1 d . . . H34A H 0.3982 0.6881 0.8133 0.150(10) Uiso 1 calc R . . H34B H 0.4362 0.5678 0.7786 0.150(10) Uiso 1 calc R . . H34C H 0.5137 0.6650 0.8060 0.150(10) Uiso 1 calc R . . Cu3 Cu 0.18428(11) 0.91657(14) 0.63987(5) 0.0647(4) Uani 1 d . . . Cu4 Cu 0.32913(10) 1.03609(15) 0.59972(5) 0.0669(4) Uani 1 d . . . O5 O 0.4718(10) 0.8345(13) 0.6919(5) 0.128(4) Uani 1 d . . . O6 O 0.0691(9) 1.2064(9) 0.7125(3) 0.091(3) Uani 1 d . . . O7 O 0.1747(5) 0.5301(7) 0.6088(3) 0.062(2) Uani 1 d . . . O8 O 0.1317(6) 1.1593(8) 0.5153(3) 0.068(2) Uani 1 d . . . N7 N 0.2757(7) 1.0253(10) 0.6868(3) 0.062(3) Uani 1 d . . . N8 N 0.0995(7) 1.0533(10) 0.6623(3) 0.064(3) Uani 1 d . . . N9 N 0.1910(6) 0.7199(9) 0.6465(3) 0.051(2) Uani 1 d . . . N10 N 0.1742(6) 0.8654(8) 0.5725(3) 0.046(2) Uani 1 d . . . N11 N 0.4037(7) 0.9132(12) 0.6303(4) 0.079(3) Uani 1 d . . . N12 N 0.2482(6) 1.1274(8) 0.5622(3) 0.052(2) Uani 1 d . . . C36 C 0.3872(10) 1.0398(15) 0.7441(5) 0.081(4) Uani 1 d . . . H36 H 0.4520 1.0134 0.7566 0.126(17) Uiso 1 calc R . . C35 C 0.3556(9) 0.9945(15) 0.7017(4) 0.069(3) Uani 1 d . . . C37 C 0.3288(12) 1.1187(17) 0.7674(4) 0.087(4) Uani 1 d . . . H37 H 0.3496 1.1521 0.7986 0.126(17) Uiso 1 calc R . . C38 C 0.2462(12) 1.1547(15) 0.7519(4) 0.086(5) Uani 1 d . . . H38 H 0.2041 1.2201 0.7692 0.126(17) Uiso 1 calc R . . C39 C 0.2186(10) 1.1021(13) 0.7120(4) 0.067(4) Uani 1 d . . . C40 C 0.4083(10) 0.9157(14) 0.6739(6) 0.084(5) Uani 1 d . . . C41 C 0.5085(12) 0.7626(18) 0.6565(6) 0.105(6) Uani 1 d . . . H41A H 0.4950 0.6622 0.6606 0.122(14) Uiso 1 calc R . . H41B H 0.5800 0.7756 0.6554 0.122(14) Uiso 1 calc R . . C42 C 0.4667(13) 0.8087(18) 0.6157(8) 0.116(7) Uani 1 d . . . H42 H 0.4258 0.7318 0.6035 0.067(9) Uiso 1 calc R . . C43 C 0.525(2) 0.858(3) 0.5777(9) 0.169(14) Uani 1 d . . . H43 H 0.4835 0.8991 0.5530 0.067(9) Uiso 1 calc R . . C44 C 0.592(2) 0.961(3) 0.5965(13) 0.25(2) Uani 1 d . . . H44A H 0.5545 1.0385 0.6104 0.150(10) Uiso 1 calc R . . H44B H 0.6334 0.9976 0.5712 0.150(10) Uiso 1 calc R . . H44C H 0.6338 0.9177 0.6207 0.150(10) Uiso 1 calc R . . C45 C 0.591(2) 0.766(4) 0.5588(13) 0.32(3) Uani 1 d . . . H45A H 0.6286 0.8132 0.5341 0.150(10) Uiso 1 calc R . . H45B H 0.5559 0.6854 0.5453 0.150(10) Uiso 1 calc R . . H45C H 0.6365 0.7329 0.5834 0.150(10) Uiso 1 calc R . . C46 C 0.1274(10) 1.1184(13) 0.6939(4) 0.069(3) Uani 1 d . . . C47 C -0.0185(15) 1.1851(17) 0.6912(7) 0.113(6) Uani 1 d . . . H47A H -0.0448 1.2736 0.6787 0.122(14) Uiso 1 calc R . . H47B H -0.0660 1.1455 0.7132 0.122(14) Uiso 1 calc R . . C48 C 0.0004(10) 1.0881(16) 0.6537(5) 0.087(5) Uani 1 d . . . H48 H -0.0030 1.1402 0.6241 0.067(9) Uiso 1 calc R . . C49 C -0.0628(10) 0.972(2) 0.6498(7) 0.112(6) Uani 1 d . . . H49 H -0.0359 0.9117 0.6252 0.067(9) Uiso 1 calc R . . C50 C -0.0611(12) 0.891(2) 0.6922(7) 0.125(7) Uani 1 d . . . H50A H -0.1046 0.8098 0.6887 0.150(10) Uiso 1 calc R . . H50B H -0.0838 0.9497 0.7183 0.150(10) Uiso 1 calc R . . H50C H 0.0062 0.8592 0.6986 0.150(10) Uiso 1 calc R . . C51 C -0.1566(15) 1.008(3) 0.6357(9) 0.199(13) Uani 1 d . . . H51A H -0.1976 0.9239 0.6339 0.150(10) Uiso 1 calc R . . H51B H -0.1541 1.0532 0.6047 0.150(10) Uiso 1 calc R . . H51C H -0.1848 1.0743 0.6584 0.150(10) Uiso 1 calc R . . C52 C 0.1587(7) 0.7346(11) 0.5689(4) 0.054(3) Uani 1 d . . . C53 C 0.1289(9) 0.6769(14) 0.5299(4) 0.074(4) Uani 1 d . . . H53 H 0.1203 0.5749 0.5277 0.126(17) Uiso 1 calc R . . C54 C 0.1109(11) 0.7558(15) 0.4946(5) 0.085(4) Uani 1 d . . . H54 H 0.0839 0.7150 0.4656 0.126(17) Uiso 1 calc R . . C55 C 0.1279(9) 0.8873(13) 0.4969(4) 0.067(3) Uani 1 d . . . H55 H 0.1173 0.9488 0.4697 0.126(17) Uiso 1 calc R . . C56 C 0.1599(7) 0.9369(11) 0.5366(3) 0.051(3) Uani 1 d . . . C57 C 0.1757(7) 0.6625(11) 0.6102(5) 0.055(3) Uani 1 d . . . C58 C 0.1834(8) 0.4892(12) 0.6547(4) 0.062(3) Uani 1 d . . . H58A H 0.2345 0.4172 0.6583 0.122(14) Uiso 1 calc R . . H58B H 0.1210 0.4516 0.6662 0.122(14) Uiso 1 calc R . . C59 C 0.2104(7) 0.6164(11) 0.6797(4) 0.055(3) Uani 1 d . . . H59 H 0.2812 0.6147 0.6865 0.067(9) Uiso 1 calc R . . C60 C 0.1578(8) 0.6337(11) 0.7227(4) 0.059(3) Uani 1 d . . . H60 H 0.0873 0.6403 0.7155 0.067(9) Uiso 1 calc R . . C61 C 0.1875(11) 0.7572(14) 0.7457(5) 0.079(4) Uani 1 d . . . H61A H 0.1751 0.8382 0.7252 0.150(10) Uiso 1 calc R . . H61B H 0.2579 0.7516 0.7532 0.150(10) Uiso 1 calc R . . H61C H 0.1502 0.7679 0.7748 0.150(10) Uiso 1 calc R . . C62 C 0.1742(10) 0.5145(14) 0.7526(5) 0.085(4) Uani 1 d . . . H62A H 0.1535 0.4288 0.7362 0.150(10) Uiso 1 calc R . . H62B H 0.1360 0.5253 0.7814 0.150(10) Uiso 1 calc R . . H62C H 0.2443 0.5081 0.7606 0.150(10) Uiso 1 calc R . . C63 C 0.1836(9) 1.0793(11) 0.5397(4) 0.057(3) Uani 1 d . . . C64 C 0.1628(10) 1.2933(13) 0.5252(5) 0.077(4) Uani 1 d . . . H64A H 0.1144 1.3435 0.5443 0.122(14) Uiso 1 calc R . . H64B H 0.1745 1.3466 0.4963 0.122(14) Uiso 1 calc R . . C65 C 0.2530(8) 1.2717(10) 0.5510(4) 0.054(3) Uani 1 d . . . H65 H 0.2523 1.3276 0.5799 0.067(9) Uiso 1 calc R . . C66 C 0.3392(11) 1.2998(15) 0.5259(5) 0.084(4) Uani 1 d . . . H66 H 0.3937 1.2705 0.5465 0.067(9) Uiso 1 calc R . . C67 C 0.3507(14) 1.226(2) 0.4848(6) 0.131(7) Uani 1 d . . . H67A H 0.4132 1.2516 0.4703 0.150(10) Uiso 1 calc R . . H67B H 0.2963 1.2477 0.4632 0.150(10) Uiso 1 calc R . . H67C H 0.3506 1.1246 0.4916 0.150(10) Uiso 1 calc R . . C68 C 0.3509(13) 1.4488(15) 0.5196(6) 0.105(5) Uani 1 d . . . H68A H 0.4113 1.4671 0.5020 0.150(10) Uiso 1 calc R . . H68B H 0.3553 1.4948 0.5504 0.150(10) Uiso 1 calc R . . H68C H 0.2943 1.4861 0.5021 0.150(10) Uiso 1 calc R . . S1 S 0.9198(3) 0.1967(4) 0.8494(2) 0.1106(17) Uani 1 d . . . O9 O 0.8972(7) 0.0800(11) 0.8739(4) 0.105(3) Uani 1 d . . . O10 O 0.8881(12) 0.1899(18) 0.8004(5) 0.180(8) Uani 1 d . . . O11 O 0.9030(10) 0.3135(12) 0.8695(4) 0.134(5) Uani 1 d . . . C69 C 1.0363(19) 0.1890(18) 0.8376(8) 0.153(11) Uani 1 d . . . F1 F 1.0614(7) 0.0809(9) 0.8172(3) 0.121(3) Uani 1 d . . . F2 F 1.0636(10) 0.2892(10) 0.8155(4) 0.165(6) Uani 1 d . . . F3 F 1.0753(10) 0.1717(18) 0.8793(6) 0.187(7) Uani 1 d . . . S2 S 0.4263(2) 1.0163(4) 0.89388(11) 0.0756(9) Uani 1 d . . . O12 O 0.4521(7) 1.0940(16) 0.8589(4) 0.147(6) Uani 1 d . . . O13 O 0.4643(8) 0.8875(12) 0.8940(4) 0.107(3) Uani 1 d . . . O14 O 0.4312(10) 1.0677(14) 0.9359(4) 0.144(5) Uani 1 d . . . C70 C 0.3091(14) 0.984(4) 0.8849(8) 0.163(12) Uani 1 d . . . F4 F 0.2711(9) 0.922(3) 0.9161(5) 0.309(16) Uani 1 d . . . F5 F 0.2856(10) 0.936(2) 0.8477(5) 0.201(9) Uani 1 d . . . F6 F 0.2675(11) 1.105(2) 0.8818(7) 0.245(10) Uani 1 d . . . S3 S 0.4227(3) 1.3538(4) 0.65665(14) 0.0839(11) Uani 1 d . . . O15 O 0.4011(9) 1.3741(15) 0.7021(4) 0.130(5) Uani 1 d . . . O16 O 0.4073(7) 1.4690(11) 0.6299(4) 0.106(4) Uani 1 d . . . O17 O 0.3888(9) 1.2367(11) 0.6377(4) 0.130(5) Uani 1 d . . . C71 C 0.5449(13) 1.336(2) 0.6590(6) 0.111(6) Uani 1 d . . . F7 F 0.5660(9) 1.2303(12) 0.6831(4) 0.152(5) Uani 1 d . . . F8 F 0.5754(8) 1.3285(18) 0.6181(4) 0.178(6) Uani 1 d . . . F9 F 0.5836(7) 1.4414(12) 0.6763(4) 0.136(4) Uani 1 d . . . S4 S -0.0687(2) 0.5106(5) 0.60430(12) 0.0863(11) Uani 1 d . . . O18 O -0.0568(10) 0.4582(18) 0.5632(5) 0.162(7) Uani 1 d . . . O19 O -0.0385(8) 0.457(2) 0.6429(4) 0.177(8) Uani 1 d . . . O20 O -0.0439(9) 0.6465(14) 0.6023(5) 0.131(4) Uani 1 d . . . C72 C -0.1895(17) 0.510(4) 0.6081(7) 0.169(12) Uani 1 d . . . F10 F -0.2177(8) 0.5807(19) 0.6440(5) 0.174(6) Uani 1 d . . . F11 F -0.2338(8) 0.545(3) 0.5780(4) 0.240(11) Uani 1 d . . . F12 F -0.2165(12) 0.388(3) 0.6196(10) 0.287(15) 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 0.0613(8) 0.0410(7) 0.0494(7) -0.0100(6) 0.0025(6) 0.0028(6) Cu2 0.0479(7) 0.0456(8) 0.0612(8) 0.0057(6) 0.0058(6) -0.0008(6) N1 0.035(4) 0.045(5) 0.054(5) -0.003(4) 0.002(4) -0.001(3) N2 0.038(4) 0.038(5) 0.053(5) -0.001(4) -0.003(4) 0.003(4) N3 0.056(5) 0.037(5) 0.046(5) 0.004(4) -0.003(4) 0.001(4) N4 0.062(6) 0.052(6) 0.041(5) 0.009(5) 0.003(4) 0.022(5) N5 0.046(5) 0.049(6) 0.083(7) 0.021(6) 0.002(5) 0.011(4) N6 0.061(5) 0.044(5) 0.053(5) 0.006(5) -0.011(4) -0.002(4) O1 0.064(4) 0.030(4) 0.073(5) -0.001(4) -0.003(4) -0.003(4) O2 0.068(5) 0.042(4) 0.071(5) 0.006(4) 0.030(4) -0.010(4) O3 0.065(6) 0.093(8) 0.142(10) 0.066(7) 0.022(6) -0.003(5) O4 0.135(9) 0.053(6) 0.075(6) -0.012(5) -0.045(6) -0.007(6) C1 0.033(5) 0.042(6) 0.051(6) -0.012(5) -0.003(4) 0.002(4) C2 0.053(7) 0.048(7) 0.068(8) -0.015(6) 0.001(6) 0.015(5) C3 0.076(8) 0.068(8) 0.047(7) -0.012(6) 0.000(6) -0.002(6) C4 0.047(6) 0.061(8) 0.052(6) -0.006(6) 0.006(5) -0.005(5) C5 0.047(6) 0.042(6) 0.044(6) -0.004(5) 0.004(4) -0.010(5) C6 0.041(6) 0.035(6) 0.063(7) -0.008(5) -0.008(5) 0.006(4) C7 0.041(5) 0.040(6) 0.060(6) -0.003(5) -0.008(5) 0.005(5) C8 0.072(7) 0.045(7) 0.055(7) 0.004(6) 0.000(5) 0.002(6) C9 0.066(7) 0.052(7) 0.065(7) 0.003(6) -0.005(6) 0.014(6) C10 0.103(10) 0.049(7) 0.062(8) -0.002(6) -0.017(7) 0.013(7) C11 0.119(11) 0.060(8) 0.056(7) 0.009(7) -0.001(7) 0.007(8) C12 0.050(6) 0.053(7) 0.035(5) -0.012(5) -0.002(5) -0.004(5) C13 0.061(7) 0.027(5) 0.069(7) -0.002(5) 0.001(6) -0.011(5) C14 0.078(8) 0.046(7) 0.071(8) 0.000(6) -0.002(7) -0.002(6) C15 0.087(9) 0.051(7) 0.100(11) 0.016(7) -0.035(8) -0.009(7) C16 0.120(13) 0.058(9) 0.128(14) 0.024(9) -0.036(11) 0.001(8) C17 0.24(3) 0.084(13) 0.158(19) 0.011(13) -0.135(19) -0.005(15) C18 0.053(7) 0.089(10) 0.075(8) 0.037(7) 0.025(6) 0.027(7) C19 0.085(10) 0.155(17) 0.054(8) 0.032(10) 0.015(7) 0.053(10) C20 0.110(13) 0.171(19) 0.055(9) 0.022(11) 0.033(9) 0.083(13) C21 0.134(14) 0.105(12) 0.040(7) -0.019(8) -0.002(8) 0.069(11) C22 0.075(8) 0.048(7) 0.060(7) 0.003(6) -0.004(6) 0.030(6) C23 0.029(5) 0.065(8) 0.089(10) 0.022(7) -0.005(6) 0.011(5) C24 0.054(7) 0.043(7) 0.119(11) -0.003(7) 0.012(7) -0.007(6) C25 0.080(11) 0.097(13) 0.21(2) 0.077(15) -0.019(13) -0.019(10) C26 0.052(7) 0.071(9) 0.113(11) 0.017(8) -0.010(7) -0.008(7) C27 0.060(8) 0.090(11) 0.156(15) 0.003(11) -0.011(9) 0.023(8) C28 0.059(9) 0.122(15) 0.188(19) -0.019(14) -0.042(10) -0.023(9) C29 0.099(9) 0.031(6) 0.042(6) -0.002(5) -0.030(6) 0.001(6) C30 0.060(8) 0.070(8) 0.105(10) 0.027(8) -0.023(7) -0.027(7) C31 0.155(16) 0.050(8) 0.096(11) 0.012(8) -0.074(12) -0.042(10) C32 0.049(8) 0.151(17) 0.134(14) 0.019(14) -0.016(8) -0.023(10) C33 0.13(2) 0.31(5) 0.30(4) 0.14(4) -0.01(2) -0.05(3) C34 0.058(9) 0.091(12) 0.22(2) 0.007(15) -0.015(11) 0.006(9) Cu3 0.0857(10) 0.0465(8) 0.0618(9) -0.0111(7) -0.0139(7) 0.0051(8) Cu4 0.0671(9) 0.0588(9) 0.0745(10) 0.0022(8) -0.0148(7) 0.0063(7) O5 0.135(11) 0.097(9) 0.151(12) 0.012(9) -0.049(9) 0.023(8) O6 0.140(9) 0.049(6) 0.085(7) -0.020(5) 0.031(7) 0.010(6) O7 0.076(5) 0.037(5) 0.074(5) -0.011(4) -0.001(4) 0.006(4) O8 0.076(5) 0.068(6) 0.059(5) 0.010(4) -0.026(4) 0.008(4) N7 0.062(6) 0.060(6) 0.064(6) 0.023(6) -0.020(5) -0.027(5) N8 0.091(7) 0.050(6) 0.052(6) -0.010(5) 0.007(5) -0.002(5) N9 0.048(5) 0.036(5) 0.068(6) -0.007(5) 0.005(4) -0.005(4) N10 0.048(5) 0.045(5) 0.045(5) -0.007(4) 0.002(4) 0.000(4) N11 0.069(7) 0.066(7) 0.102(9) -0.013(7) -0.027(6) 0.005(6) N12 0.069(6) 0.039(5) 0.047(5) 0.004(4) -0.003(4) 0.004(4) C36 0.073(9) 0.084(10) 0.085(10) 0.014(9) -0.029(8) -0.029(8) C35 0.069(8) 0.071(9) 0.068(8) 0.024(7) 0.001(7) -0.017(7) C37 0.121(13) 0.095(11) 0.046(7) 0.009(8) -0.002(8) -0.030(11) C38 0.123(13) 0.092(11) 0.044(7) 0.001(7) -0.009(8) -0.041(9) C39 0.108(10) 0.049(7) 0.044(6) 0.005(6) 0.010(7) -0.038(8) C40 0.079(9) 0.062(8) 0.111(12) 0.036(9) -0.061(9) -0.015(8) C41 0.102(12) 0.085(12) 0.128(15) 0.022(11) -0.054(12) 0.017(10) C42 0.096(12) 0.094(12) 0.158(19) -0.064(13) -0.030(13) 0.027(10) C43 0.17(2) 0.20(3) 0.132(18) -0.06(2) -0.034(18) 0.13(2) C44 0.17(3) 0.25(4) 0.34(5) 0.16(4) 0.10(3) 0.08(3) C45 0.19(3) 0.31(5) 0.46(7) -0.16(5) -0.06(4) 0.16(4) C46 0.092(10) 0.048(7) 0.069(8) 0.020(7) 0.002(7) 0.002(7) C47 0.136(16) 0.075(11) 0.128(15) -0.003(11) 0.021(13) 0.026(11) C48 0.090(10) 0.096(12) 0.076(9) 0.024(8) 0.003(7) 0.038(9) C49 0.050(8) 0.114(15) 0.172(18) 0.002(13) -0.002(9) 0.002(9) C50 0.096(13) 0.104(14) 0.176(19) 0.034(14) 0.023(12) -0.010(10) C51 0.110(16) 0.26(3) 0.23(3) -0.05(3) -0.048(17) 0.02(2) C52 0.050(6) 0.042(7) 0.070(8) -0.018(6) 0.008(5) 0.000(5) C53 0.086(9) 0.066(9) 0.071(9) -0.025(7) -0.009(7) -0.009(7) C54 0.113(12) 0.076(10) 0.065(9) -0.033(8) -0.015(8) 0.001(8) C55 0.091(9) 0.072(9) 0.039(6) -0.010(6) -0.012(6) -0.002(7) C56 0.057(6) 0.053(7) 0.044(6) -0.012(5) -0.003(5) 0.000(5) C57 0.033(6) 0.041(7) 0.092(9) -0.009(6) -0.002(5) -0.002(4) C58 0.068(7) 0.040(6) 0.078(8) 0.000(6) 0.001(6) -0.002(6) C59 0.049(6) 0.043(6) 0.073(7) 0.002(6) -0.003(5) 0.000(5) C60 0.061(7) 0.045(7) 0.069(7) 0.018(6) 0.008(6) -0.010(5) C61 0.106(11) 0.064(9) 0.068(9) -0.004(7) 0.008(8) -0.004(8) C62 0.091(10) 0.055(8) 0.108(11) 0.020(8) -0.013(8) -0.002(7) C63 0.075(8) 0.051(8) 0.045(6) -0.005(5) 0.001(6) 0.006(6) C64 0.094(10) 0.049(8) 0.087(10) 0.010(7) -0.002(8) -0.006(7) C65 0.077(8) 0.034(6) 0.052(6) -0.003(5) 0.005(6) 0.007(5) C66 0.095(11) 0.077(10) 0.080(10) 0.004(8) 0.027(8) 0.006(8) C67 0.148(16) 0.125(16) 0.121(15) -0.002(13) 0.072(13) 0.007(13) C68 0.124(13) 0.072(11) 0.119(13) 0.024(9) 0.017(10) -0.018(9) S1 0.080(3) 0.076(3) 0.177(5) 0.011(3) 0.042(3) 0.016(2) O9 0.101(7) 0.090(8) 0.123(9) 0.018(6) 0.035(6) 0.004(6) O10 0.221(16) 0.195(16) 0.123(11) 0.066(11) -0.102(11) -0.041(13) O11 0.183(13) 0.084(8) 0.137(10) 0.001(7) 0.058(9) 0.070(8) C69 0.23(3) 0.066(12) 0.16(2) -0.019(13) 0.15(2) 0.014(14) F1 0.139(8) 0.080(6) 0.145(8) 0.002(6) 0.064(7) 0.023(5) F2 0.266(15) 0.074(6) 0.158(10) -0.004(7) 0.119(10) -0.054(8) F3 0.152(11) 0.227(18) 0.181(13) 0.008(13) -0.063(10) 0.019(11) S2 0.077(2) 0.087(3) 0.062(2) 0.017(2) 0.0015(15) -0.0041(19) O12 0.086(7) 0.215(15) 0.141(10) 0.127(11) -0.028(7) -0.035(8) O13 0.106(8) 0.095(8) 0.120(9) 0.010(7) 0.008(7) 0.012(7) O14 0.176(13) 0.139(12) 0.118(10) -0.045(9) -0.023(9) 0.025(10) C70 0.093(13) 0.29(4) 0.104(15) 0.12(2) 0.014(12) 0.034(18) F4 0.108(9) 0.62(5) 0.196(14) 0.21(2) -0.020(9) -0.106(16) F5 0.156(12) 0.30(2) 0.147(11) 0.087(14) -0.060(10) -0.112(14) F6 0.128(11) 0.31(3) 0.29(2) 0.07(2) -0.010(13) 0.106(15) S3 0.069(2) 0.093(3) 0.089(3) 0.019(2) -0.0146(19) -0.0150(19) O15 0.122(9) 0.188(14) 0.079(7) 0.013(8) 0.009(6) 0.041(9) O16 0.106(8) 0.103(8) 0.109(8) 0.048(7) -0.038(6) -0.007(6) O17 0.160(11) 0.077(7) 0.152(11) 0.023(7) -0.073(9) -0.074(8) C71 0.097(13) 0.143(18) 0.091(13) -0.015(13) -0.025(10) 0.017(13) F7 0.171(11) 0.115(8) 0.167(10) 0.003(8) -0.070(9) 0.069(8) F8 0.117(9) 0.30(2) 0.120(9) -0.003(11) 0.035(7) 0.009(10) F9 0.098(7) 0.143(10) 0.167(10) 0.011(8) -0.048(6) -0.037(7) S4 0.075(2) 0.116(3) 0.068(2) 0.030(2) 0.0004(17) -0.003(2) O18 0.131(11) 0.214(18) 0.143(11) -0.077(12) 0.042(9) -0.010(11) O19 0.079(7) 0.31(2) 0.145(11) 0.141(14) 0.009(7) 0.028(10) O20 0.120(10) 0.115(11) 0.158(12) -0.006(9) -0.009(8) -0.008(8) C72 0.135(19) 0.31(4) 0.064(11) 0.020(19) 0.003(12) 0.03(3) F10 0.103(8) 0.27(2) 0.147(11) 0.037(12) 0.007(7) 0.048(10) F11 0.119(9) 0.48(3) 0.118(9) 0.001(14) -0.066(8) 0.063(15) F12 0.127(12) 0.29(3) 0.44(4) 0.14(3) 0.018(16) -0.079(15) _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 N6 1.996(9) . ? Cu1 N2 2.050(8) . ? Cu1 N1 2.084(8) . ? Cu1 N4 2.184(8) . ? Cu1 Cu2 2.754(2) . ? Cu2 N3 1.896(8) . ? Cu2 N5 1.904(10) . ? Cu2 O11 2.382(10) . ? N1 C5 1.326(13) . ? N1 C1 1.347(13) . ? N2 C6 1.270(13) . ? N2 C7 1.481(13) . ? N3 C12 1.275(12) . ? N3 C13 1.496(13) . ? N4 C22 1.325(15) . ? N4 C18 1.359(15) . ? N5 C23 1.267(15) . ? N5 C24 1.504(16) . ? N6 C29 1.263(14) . ? N6 C30 1.475(15) . ? O1 C6 1.336(12) . ? O1 C8 1.470(13) . ? O2 C12 1.324(12) . ? O2 C14 1.471(14) . ? O3 C23 1.356(14) . ? O3 C25 1.48(2) . ? O4 C29 1.330(13) . ? O4 C31 1.44(2) . ? C1 C2 1.387(15) . ? C1 C6 1.461(15) . ? C2 C3 1.357(17) . ? C3 C4 1.404(17) . ? C4 C5 1.412(14) . ? C5 C12 1.512(15) . ? C7 C9 1.517(15) . ? C7 C8 1.537(15) . ? C9 C11 1.527(17) . ? C9 C10 1.549(17) . ? C13 C15 1.502(16) . ? C13 C14 1.517(16) . ? C15 C17 1.46(2) . ? C15 C16 1.542(19) . ? C18 C19 1.356(18) . ? C18 C23 1.453(19) . ? C19 C20 1.36(3) . ? C20 C21 1.39(3) . ? C21 C22 1.383(17) . ? C22 C29 1.477(18) . ? C24 C25 1.50(2) . ? C24 C26 1.537(18) . ? C26 C27 1.49(2) . ? C26 C28 1.55(2) . ? C30 C32 1.53(2) . ? C30 C31 1.55(2) . ? C32 C33 1.43(3) . ? C32 C34 1.53(2) . ? Cu3 N8 1.987(10) . ? Cu3 N9 2.017(9) . ? Cu3 N10 2.124(8) . ? Cu3 N7 2.241(9) . ? Cu3 Cu4 2.734(2) . ? Cu4 N12 1.882(9) . ? Cu4 N11 1.898(12) . ? O5 C40 1.354(16) . ? O5 C41 1.41(2) . ? O6 C46 1.363(16) . ? O6 C47 1.44(2) . ? O7 C57 1.351(14) . ? O7 C58 1.465(14) . ? O8 C63 1.336(13) . ? O8 C64 1.470(15) . ? N7 C35 1.284(15) . ? N7 C39 1.381(16) . ? N8 C46 1.235(16) . ? N8 C48 1.507(17) . ? N9 C57 1.270(15) . ? N9 C59 1.487(14) . ? N10 C56 1.329(14) . ? N10 C52 1.357(14) . ? N11 C40 1.332(18) . ? N11 C42 1.476(19) . ? N12 C63 1.259(14) . ? N12 C65 1.511(14) . ? C36 C37 1.37(2) . ? C36 C35 1.444(18) . ? C35 C40 1.40(2) . ? C37 C38 1.34(2) . ? C38 C39 1.385(17) . ? C39 C46 1.443(18) . ? C41 C42 1.46(2) . ? C42 C43 1.53(4) . ? C43 C45 1.47(3) . ? C43 C44 1.54(4) . ? C47 C48 1.54(2) . ? C48 C49 1.50(2) . ? C49 C51 1.48(2) . ? C49 C50 1.53(2) . ? C52 C53 1.393(16) . ? C52 C57 1.477(17) . ? C53 C54 1.37(2) . ? C54 C55 1.366(19) . ? C55 C56 1.389(15) . ? C56 C63 1.495(16) . ? C58 C59 1.553(16) . ? C59 C60 1.535(15) . ? C60 C61 1.503(17) . ? C60 C62 1.536(17) . ? C64 C65 1.542(18) . ? C65 C66 1.504(17) . ? C66 C67 1.48(2) . ? C66 C68 1.54(2) . ? S1 O11 1.363(12) . ? S1 O9 1.445(11) . ? S1 O10 1.560(13) . ? S1 C69 1.74(2) . ? C69 F2 1.29(2) . ? C69 F1 1.318(17) . ? C69 F3 1.40(3) . ? S2 O12 1.384(10) . ? S2 O14 1.387(12) . ? S2 O13 1.425(12) . ? S2 C70 1.76(2) . ? C70 F4 1.27(2) . ? C70 F5 1.28(3) . ? C70 F6 1.38(4) . ? S3 O17 1.412(10) . ? S3 O15 1.439(11) . ? S3 O16 1.448(10) . ? S3 C71 1.790(18) . ? C71 F9 1.32(2) . ? C71 F8 1.33(2) . ? C71 F7 1.34(2) . ? S4 O19 1.365(11) . ? S4 O18 1.374(13) . ? S4 O20 1.432(14) . ? S4 C72 1.76(2) . ? C72 F11 1.17(2) . ? C72 F12 1.35(4) . ? C72 F10 1.38(3) . ? 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 N6 Cu1 N2 131.1(3) . . ? N6 Cu1 N1 122.7(3) . . ? N2 Cu1 N1 81.5(3) . . ? N6 Cu1 N4 79.7(4) . . ? N2 Cu1 N4 108.0(3) . . ? N1 Cu1 N4 141.5(3) . . ? N6 Cu1 Cu2 107.9(3) . . ? N2 Cu1 Cu2 119.7(2) . . ? N1 Cu1 Cu2 76.0(2) . . ? N4 Cu1 Cu2 66.8(2) . . ? N3 Cu2 N5 163.4(4) . . ? N3 Cu2 O11 98.6(4) . . ? N5 Cu2 O11 97.4(5) . . ? N3 Cu2 Cu1 88.8(2) . . ? N5 Cu2 Cu1 88.7(3) . . ? O11 Cu2 Cu1 114.5(4) . . ? C5 N1 C1 117.5(9) . . ? C5 N1 Cu1 130.2(7) . . ? C1 N1 Cu1 110.8(7) . . ? C6 N2 C7 107.7(9) . . ? C6 N2 Cu1 110.1(7) . . ? C7 N2 Cu1 142.1(7) . . ? C12 N3 C13 105.9(9) . . ? C12 N3 Cu2 127.4(7) . . ? C13 N3 Cu2 126.7(7) . . ? C22 N4 C18 116.5(10) . . ? C22 N4 Cu1 109.1(7) . . ? C18 N4 Cu1 128.8(9) . . ? C23 N5 C24 106.9(10) . . ? C23 N5 Cu2 124.0(9) . . ? C24 N5 Cu2 128.9(8) . . ? C29 N6 C30 109.5(10) . . ? C29 N6 Cu1 112.5(8) . . ? C30 N6 Cu1 137.9(9) . . ? C6 O1 C8 104.5(9) . . ? C12 O2 C14 104.2(8) . . ? C23 O3 C25 105.4(12) . . ? C29 O4 C31 105.2(11) . . ? N1 C1 C2 121.4(10) . . ? N1 C1 C6 113.8(9) . . ? C2 C1 C6 124.6(10) . . ? C3 C2 C1 120.6(11) . . ? C2 C3 C4 120.0(11) . . ? C3 C4 C5 115.0(11) . . ? N1 C5 C4 125.3(10) . . ? N1 C5 C12 118.2(9) . . ? C4 C5 C12 116.4(10) . . ? N2 C6 O1 118.9(11) . . ? N2 C6 C1 122.8(10) . . ? O1 C6 C1 118.1(10) . . ? N2 C7 C9 114.9(9) . . ? N2 C7 C8 102.2(8) . . ? C9 C7 C8 113.0(9) . . ? O1 C8 C7 104.6(8) . . ? C7 C9 C11 109.3(10) . . ? C7 C9 C10 112.0(9) . . ? C11 C9 C10 108.5(10) . . ? N3 C12 O2 120.0(10) . . ? N3 C12 C5 124.3(9) . . ? O2 C12 C5 115.7(9) . . ? N3 C13 C15 111.4(9) . . ? N3 C13 C14 102.6(9) . . ? C15 C13 C14 117.0(11) . . ? O2 C14 C13 104.7(9) . . ? C17 C15 C13 114.3(14) . . ? C17 C15 C16 112.0(14) . . ? C13 C15 C16 111.1(11) . . ? C19 C18 N4 122.0(15) . . ? C19 C18 C23 122.7(14) . . ? N4 C18 C23 115.3(10) . . ? C18 C19 C20 120.1(16) . . ? C19 C20 C21 120.2(13) . . ? C22 C21 C20 115.6(15) . . ? N4 C22 C21 125.5(14) . . ? N4 C22 C29 112.1(10) . . ? C21 C22 C29 122.2(13) . . ? N5 C23 O3 117.9(13) . . ? N5 C23 C18 124.4(11) . . ? O3 C23 C18 117.6(13) . . ? C25 C24 N5 104.1(13) . . ? C25 C24 C26 116.2(11) . . ? N5 C24 C26 109.8(10) . . ? O3 C25 C24 103.9(14) . . ? C27 C26 C24 111.5(12) . . ? C27 C26 C28 111.3(12) . . ? C24 C26 C28 109.4(12) . . ? N6 C29 O4 118.3(13) . . ? N6 C29 C22 123.2(10) . . ? O4 C29 C22 118.4(12) . . ? N6 C30 C32 112.0(12) . . ? N6 C30 C31 100.1(12) . . ? C32 C30 C31 117.7(12) . . ? O4 C31 C30 106.5(10) . . ? C33 C32 C34 109.3(17) . . ? C33 C32 C30 119(2) . . ? C34 C32 C30 112.1(14) . . ? N8 Cu3 N9 133.8(4) . . ? N8 Cu3 N10 117.9(4) . . ? N9 Cu3 N10 81.7(4) . . ? N8 Cu3 N7 78.5(4) . . ? N9 Cu3 N7 113.5(4) . . ? N10 Cu3 N7 140.9(4) . . ? N8 Cu3 Cu4 109.0(3) . . ? N9 Cu3 Cu4 116.8(3) . . ? N10 Cu3 Cu4 74.0(2) . . ? N7 Cu3 Cu4 67.0(3) . . ? N12 Cu4 N11 168.0(4) . . ? N12 Cu4 Cu3 90.6(3) . . ? N11 Cu4 Cu3 85.8(4) . . ? C40 O5 C41 105.6(14) . . ? C46 O6 C47 105.3(11) . . ? C57 O7 C58 104.7(9) . . ? C63 O8 C64 106.3(9) . . ? C35 N7 C39 119.4(12) . . ? C35 N7 Cu3 129.6(10) . . ? C39 N7 Cu3 106.2(7) . . ? C46 N8 C48 108.5(11) . . ? C46 N8 Cu3 116.4(10) . . ? C48 N8 Cu3 134.5(9) . . ? C57 N9 C59 107.3(9) . . ? C57 N9 Cu3 111.2(8) . . ? C59 N9 Cu3 141.5(8) . . ? C56 N10 C52 116.6(9) . . ? C56 N10 Cu3 132.2(7) . . ? C52 N10 Cu3 109.2(7) . . ? C40 N11 C42 106.8(14) . . ? C40 N11 Cu4 120.0(10) . . ? C42 N11 Cu4 133.1(12) . . ? C63 N12 C65 107.0(9) . . ? C63 N12 Cu4 126.9(8) . . ? C65 N12 Cu4 126.1(7) . . ? C37 C36 C35 117.2(13) . . ? N7 C35 C40 115.1(12) . . ? N7 C35 C36 121.3(14) . . ? C40 C35 C36 123.6(13) . . ? C38 C37 C36 122.3(13) . . ? C37 C38 C39 117.2(16) . . ? N7 C39 C38 122.4(14) . . ? N7 C39 C46 114.1(10) . . ? C38 C39 C46 123.4(15) . . ? N11 C40 O5 114.9(17) . . ? N11 C40 C35 126.4(12) . . ? O5 C40 C35 118.7(15) . . ? O5 C41 C42 109.0(14) . . ? C41 C42 N11 103.4(16) . . ? C41 C42 C43 121.4(17) . . ? N11 C42 C43 110.0(17) . . ? C45 C43 C42 117(3) . . ? C45 C43 C44 100(3) . . ? C42 C43 C44 107(2) . . ? N8 C46 O6 118.5(13) . . ? N8 C46 C39 122.1(13) . . ? O6 C46 C39 119.4(13) . . ? O6 C47 C48 105.7(13) . . ? C49 C48 N8 114.4(12) . . ? C49 C48 C47 116.9(15) . . ? N8 C48 C47 101.4(13) . . ? C51 C49 C48 112.9(19) . . ? C51 C49 C50 112.9(18) . . ? C48 C49 C50 110.6(15) . . ? N10 C52 C53 122.3(12) . . ? N10 C52 C57 113.2(10) . . ? C53 C52 C57 124.5(11) . . ? C54 C53 C52 118.8(12) . . ? C55 C54 C53 120.1(12) . . ? C54 C55 C56 117.5(12) . . ? N10 C56 C55 124.6(11) . . ? N10 C56 C63 116.4(9) . . ? C55 C56 C63 118.9(11) . . ? N9 C57 O7 119.3(12) . . ? N9 C57 C52 122.8(10) . . ? O7 C57 C52 117.9(11) . . ? O7 C58 C59 104.5(9) . . ? N9 C59 C60 114.0(9) . . ? N9 C59 C58 102.3(8) . . ? C60 C59 C58 112.9(9) . . ? C61 C60 C59 110.6(10) . . ? C61 C60 C62 110.0(10) . . ? C59 C60 C62 109.9(10) . . ? N12 C63 O8 118.9(10) . . ? N12 C63 C56 125.7(11) . . ? O8 C63 C56 115.4(10) . . ? O8 C64 C65 103.4(10) . . ? C66 C65 N12 109.9(10) . . ? C66 C65 C64 115.1(11) . . ? N12 C65 C64 102.4(9) . . ? C67 C66 C65 115.8(14) . . ? C67 C66 C68 112.6(14) . . ? C65 C66 C68 110.2(12) . . ? O11 S1 O9 116.3(8) . . ? O11 S1 O10 114.7(10) . . ? O9 S1 O10 113.1(9) . . ? O11 S1 C69 108.2(10) . . ? O9 S1 C69 107.2(9) . . ? O10 S1 C69 94.7(12) . . ? S1 O11 Cu2 165.9(10) . . ? F2 C69 F1 109.1(13) . . ? F2 C69 F3 117(2) . . ? F1 C69 F3 102(2) . . ? F2 C69 S1 112.2(19) . . ? F1 C69 S1 114.3(18) . . ? F3 C69 S1 102.0(12) . . ? O12 S2 O14 119.1(10) . . ? O12 S2 O13 114.8(9) . . ? O14 S2 O13 109.3(8) . . ? O12 S2 C70 104.9(8) . . ? O14 S2 C70 104.9(12) . . ? O13 S2 C70 101.6(13) . . ? F4 C70 F5 111(3) . . ? F4 C70 F6 108(2) . . ? F5 C70 F6 99.5(17) . . ? F4 C70 S2 113.9(14) . . ? F5 C70 S2 117.5(17) . . ? F6 C70 S2 105(2) . . ? O17 S3 O15 115.9(9) . . ? O17 S3 O16 113.8(7) . . ? O15 S3 O16 113.1(8) . . ? O17 S3 C71 105.9(10) . . ? O15 S3 C71 101.6(8) . . ? O16 S3 C71 104.7(9) . . ? F9 C71 F8 106.0(19) . . ? F9 C71 F7 109.8(14) . . ? F8 C71 F7 113.2(18) . . ? F9 C71 S3 110.7(14) . . ? F8 C71 S3 108.0(12) . . ? F7 C71 S3 109.1(15) . . ? O19 S4 O18 126.1(12) . . ? O19 S4 O20 109.9(11) . . ? O18 S4 O20 107.7(10) . . ? O19 S4 C72 104.8(9) . . ? O18 S4 C72 101.1(11) . . ? O20 S4 C72 104.9(15) . . ? F11 C72 F12 109(3) . . ? F11 C72 F10 107(3) . . ? F12 C72 F10 101(2) . . ? F11 C72 S4 119.3(18) . . ? F12 C72 S4 108(2) . . ? F10 C72 S4 111(2) . . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.892 _refine_diff_density_max 0.767 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.082