# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'H. L. Kwong' _publ_contact_author_address ; Biology and Chemistry City University of Hong Kong 83 Tat Chee Ave. Kowloon Tong HONG KONG ; _publ_contact_author_email BHHOIK@CITYU.EDU.HK _publ_section_title ; Supramolecular Double Helical Cu(I) Complexes for Asymmetric Cyclopropanation ; loop_ _publ_author_name 'H. L. Kwong' 'Chui-Shan Tsang' 'Wai-Yeung Wong' 'Chi-Tung Yeung' 'Ho-Lun Yeung' data_wy1264wm _database_code_depnum_ccdc_archive 'CCDC 651264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H96 Cl2 Cu2 N6 O9' _chemical_formula_weight 1411.55 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.9614(9) _cell_length_b 14.0008(9) _cell_length_c 18.1790(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.0730(10) _cell_angle_gamma 90.00 _cell_volume 3793.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8212 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18953 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.1380 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12119 _reflns_number_gt 6302 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+0.0000P] 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 0.007(18) _refine_ls_number_reflns 12119 _refine_ls_number_parameters 833 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1456 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 C1 C 0.3405(7) -0.0680(13) 0.4878(6) 0.268(8) Uani 1 1 d . . . H1A H 0.3861 -0.0381 0.4618 0.402 Uiso 1 1 calc R . . H1B H 0.3238 -0.1279 0.4647 0.402 Uiso 1 1 calc R . . H1C H 0.3631 -0.0790 0.5382 0.402 Uiso 1 1 calc R . . C2 C 0.2698(7) -0.0119(8) 0.4861(4) 0.149(4) Uani 1 1 d . . . H2A H 0.2469 -0.0036 0.4349 0.179 Uiso 1 1 calc R . . H2B H 0.2894 0.0502 0.5047 0.179 Uiso 1 1 calc R . . C3 C 0.1945(5) -0.0437(6) 0.5281(3) 0.097(3) Uani 1 1 d . . . H3A H 0.1714 -0.1039 0.5080 0.116 Uiso 1 1 calc R . . H3B H 0.1464 0.0029 0.5220 0.116 Uiso 1 1 calc R . . C4 C 0.2234(4) -0.0564(4) 0.6116(3) 0.0649(19) Uani 1 1 d . . . H4A H 0.2623 -0.1118 0.6177 0.078 Uiso 1 1 calc R . . H4B H 0.2585 -0.0011 0.6286 0.078 Uiso 1 1 calc R . . C5 C 0.1489(3) -0.0684(4) 0.6599(3) 0.0503(16) Uani 1 1 d . . . H5A H 0.1138 -0.0092 0.6578 0.060 Uiso 1 1 calc R . . C6 C 0.0850(4) -0.1508(4) 0.6374(3) 0.0568(17) Uani 1 1 d . . . H6A H 0.0563 -0.1451 0.5870 0.068 Uiso 1 1 calc R . . C7 C 0.1364(4) -0.2452(4) 0.6520(3) 0.0614(17) Uani 1 1 d . . . H7A H 0.2010 -0.2402 0.6509 0.074 Uiso 1 1 calc R . . H7B H 0.1122 -0.2991 0.6232 0.074 Uiso 1 1 calc R . . C8 C 0.1032(4) -0.2373(4) 0.7297(3) 0.0610(17) Uani 1 1 d . . . H8A H 0.0902 -0.2978 0.7537 0.073 Uiso 1 1 calc R . . C9 C 0.1625(3) -0.1697(4) 0.7745(3) 0.0492(15) Uani 1 1 d . . . C10 C 0.1858(3) -0.0843(3) 0.7402(3) 0.0402(14) Uani 1 1 d . . . C11 C 0.0198(4) -0.1803(4) 0.6947(3) 0.0623(18) Uani 1 1 d . . . C12 C -0.0206(4) -0.1055(5) 0.7420(4) 0.084(2) Uani 1 1 d . . . H12A H -0.0699 -0.0749 0.7140 0.126 Uiso 1 1 calc R . . H12B H 0.0242 -0.0587 0.7573 0.126 Uiso 1 1 calc R . . H12C H -0.0416 -0.1354 0.7848 0.126 Uiso 1 1 calc R . . C13 C -0.0533(4) -0.2485(5) 0.6628(3) 0.081(2) Uani 1 1 d . . . H13A H -0.1038 -0.2124 0.6418 0.121 Uiso 1 1 calc R . . H13B H -0.0718 -0.2888 0.7015 0.121 Uiso 1 1 calc R . . H13C H -0.0303 -0.2873 0.6252 0.121 Uiso 1 1 calc R . . C14 C 0.1965(3) -0.1840(4) 0.8471(3) 0.0534(16) Uani 1 1 d . . . H14A H 0.1861 -0.2416 0.8704 0.064 Uiso 1 1 calc R . . C15 C 0.2456(3) -0.1132(4) 0.8852(3) 0.0469(15) Uani 1 1 d . . . H15A H 0.2649 -0.1208 0.9349 0.056 Uiso 1 1 calc R . . C16 C 0.2653(3) -0.0311(3) 0.8479(2) 0.0383(13) Uani 1 1 d . . . C17 C 0.3207(3) 0.0462(4) 0.8864(3) 0.0419(14) Uani 1 1 d . . . C18 C 0.3596(4) 0.0306(4) 0.9562(3) 0.0611(18) Uani 1 1 d . . . H18A H 0.3488 -0.0253 0.9815 0.073 Uiso 1 1 calc R . . C19 C 0.4161(4) 0.1011(5) 0.9881(3) 0.078(2) Uani 1 1 d . . . H19A H 0.4476 0.0900 1.0337 0.093 Uiso 1 1 calc R . . C20 C 0.4258(4) 0.1872(4) 0.9528(3) 0.0634(18) Uani 1 1 d . . . H20A H 0.4607 0.2357 0.9755 0.076 Uiso 1 1 calc R . . C21 C 0.3827(3) 0.2003(4) 0.8826(3) 0.0443(14) Uani 1 1 d . . . C22 C 0.3921(3) 0.2925(3) 0.8457(3) 0.0394(14) Uani 1 1 d . . . C23 C 0.4713(3) 0.3430(4) 0.8588(3) 0.0516(16) Uani 1 1 d . . . H23A H 0.5189 0.3166 0.8883 0.062 Uiso 1 1 calc R . . C24 C 0.4801(4) 0.4319(4) 0.8285(3) 0.0526(16) Uani 1 1 d . . . H24A H 0.5333 0.4660 0.8375 0.063 Uiso 1 1 calc R . . C25 C 0.4081(3) 0.4708(4) 0.7838(3) 0.0445(15) Uani 1 1 d . . . C26 C 0.3321(3) 0.4154(3) 0.7718(3) 0.0407(14) Uani 1 1 d . . . C27 C 0.2543(3) 0.4537(4) 0.7173(3) 0.0461(15) Uani 1 1 d . . . H27A H 0.2496 0.4113 0.6742 0.055 Uiso 1 1 calc R . . C28 C 0.2821(3) 0.5544(4) 0.6901(3) 0.0513(16) Uani 1 1 d . . . H28A H 0.2364 0.5865 0.6569 0.062 Uiso 1 1 calc R . . C29 C 0.3183(3) 0.6153(4) 0.7598(3) 0.0577(16) Uani 1 1 d . . . H29A H 0.3171 0.6838 0.7521 0.069 Uiso 1 1 calc R . . H29B H 0.2931 0.5978 0.8053 0.069 Uiso 1 1 calc R . . C30 C 0.4096(4) 0.5671(4) 0.7486(3) 0.0607(18) Uani 1 1 d . . . H30A H 0.4635 0.6058 0.7607 0.073 Uiso 1 1 calc R . . C31 C 0.3769(4) 0.5578(4) 0.6652(3) 0.0507(16) Uani 1 1 d . . . C32 C 0.4112(4) 0.4755(4) 0.6219(3) 0.0657(19) Uani 1 1 d . . . H32A H 0.4011 0.4166 0.6469 0.099 Uiso 1 1 calc R . . H32B H 0.4743 0.4834 0.6178 0.099 Uiso 1 1 calc R . . H32C H 0.3799 0.4742 0.5734 0.099 Uiso 1 1 calc R . . C33 C 0.3914(4) 0.6526(4) 0.6225(3) 0.081(2) Uani 1 1 d . . . H33A H 0.3699 0.6448 0.5715 0.122 Uiso 1 1 calc R . . H33B H 0.4542 0.6679 0.6261 0.122 Uiso 1 1 calc R . . H33C H 0.3590 0.7034 0.6437 0.122 Uiso 1 1 calc R . . C34 C 0.1623(3) 0.4567(4) 0.7467(3) 0.0537(16) Uani 1 1 d . . . H34A H 0.1553 0.4001 0.7765 0.064 Uiso 1 1 calc R . . H34B H 0.1596 0.5118 0.7788 0.064 Uiso 1 1 calc R . . C35 C 0.0852(3) 0.4617(4) 0.6880(3) 0.0595(18) Uani 1 1 d . . . H35A H 0.0899 0.4087 0.6542 0.071 Uiso 1 1 calc R . . H35B H 0.0903 0.5202 0.6601 0.071 Uiso 1 1 calc R . . C36 C -0.0072(4) 0.4590(6) 0.7170(4) 0.088(2) Uani 1 1 d . . . H36A H -0.0115 0.4025 0.7474 0.106 Uiso 1 1 calc R . . H36B H -0.0140 0.5144 0.7480 0.106 Uiso 1 1 calc R . . C37 C -0.0813(4) 0.4577(7) 0.6574(5) 0.135(4) Uani 1 1 d . . . H37A H -0.1377 0.4540 0.6787 0.203 Uiso 1 1 calc R . . H37B H -0.0748 0.4033 0.6262 0.203 Uiso 1 1 calc R . . H37C H -0.0795 0.5151 0.6287 0.203 Uiso 1 1 calc R . . C38 C 0.4931(5) -0.2008(5) 0.8683(4) 0.094(2) Uani 1 1 d . . . H38A H 0.4679 -0.2637 0.8697 0.141 Uiso 1 1 calc R . . H38B H 0.4718 -0.1627 0.9071 0.141 Uiso 1 1 calc R . . H38C H 0.5574 -0.2049 0.8751 0.141 Uiso 1 1 calc R . . C39 C 0.4656(4) -0.1555(4) 0.7951(3) 0.070(2) Uani 1 1 d . . . H39A H 0.4006 -0.1546 0.7881 0.084 Uiso 1 1 calc R . . H39B H 0.4868 -0.1954 0.7566 0.084 Uiso 1 1 calc R . . C40 C 0.4996(4) -0.0547(4) 0.7851(3) 0.0611(18) Uani 1 1 d . . . H40A H 0.4843 -0.0166 0.8268 0.073 Uiso 1 1 calc R . . H40B H 0.5645 -0.0568 0.7867 0.073 Uiso 1 1 calc R . . C41 C 0.4644(4) -0.0047(4) 0.7153(3) 0.0565(17) Uani 1 1 d . . . H41A H 0.4826 -0.0410 0.6737 0.068 Uiso 1 1 calc R . . H41B H 0.3994 -0.0059 0.7124 0.068 Uiso 1 1 calc R . . C42 C 0.4937(3) 0.0966(4) 0.7070(3) 0.0454(14) Uani 1 1 d . . . H42A H 0.4910 0.1285 0.7547 0.054 Uiso 1 1 calc R . . C43 C 0.5901(3) 0.1040(5) 0.6858(3) 0.0588(16) Uani 1 1 d . . . H43A H 0.6339 0.0700 0.7194 0.071 Uiso 1 1 calc R . . C44 C 0.5934(4) 0.0771(5) 0.6048(3) 0.073(2) Uani 1 1 d . . . H44A H 0.5464 0.0336 0.5858 0.088 Uiso 1 1 calc R . . H44B H 0.6519 0.0563 0.5919 0.088 Uiso 1 1 calc R . . C45 C 0.5724(3) 0.1853(4) 0.5887(3) 0.0589(17) Uani 1 1 d . . . H45A H 0.5996 0.2138 0.5468 0.071 Uiso 1 1 calc R . . C46 C 0.4755(3) 0.1983(4) 0.5908(3) 0.0496(15) Uani 1 1 d . . . C47 C 0.4323(3) 0.1520(4) 0.6492(3) 0.0464(15) Uani 1 1 d . . . C48 C 0.6188(3) 0.2074(4) 0.6673(3) 0.0567(17) Uani 1 1 d . . . C49 C 0.5879(4) 0.2906(4) 0.7090(3) 0.0619(18) Uani 1 1 d . . . H49A H 0.6225 0.2947 0.7560 0.093 Uiso 1 1 calc R . . H49B H 0.5256 0.2828 0.7165 0.093 Uiso 1 1 calc R . . H49C H 0.5957 0.3480 0.6815 0.093 Uiso 1 1 calc R . . C50 C 0.7241(3) 0.2140(5) 0.6658(4) 0.082(2) Uani 1 1 d . . . H50A H 0.7510 0.2273 0.7146 0.123 Uiso 1 1 calc R . . H50B H 0.7385 0.2643 0.6329 0.123 Uiso 1 1 calc R . . H50C H 0.7466 0.1544 0.6489 0.123 Uiso 1 1 calc R . . C51 C 0.4193(3) 0.2511(5) 0.5405(3) 0.0573(16) Uani 1 1 d . . . H51A H 0.4434 0.2817 0.5013 0.069 Uiso 1 1 calc R . . C52 C 0.3305(3) 0.2585(4) 0.5479(3) 0.0529(15) Uani 1 1 d . . . H52A H 0.2942 0.2948 0.5144 0.064 Uiso 1 1 calc R . . C53 C 0.2935(3) 0.2119(3) 0.6053(3) 0.0440(14) Uani 1 1 d . . . C54 C 0.1961(3) 0.2128(3) 0.6115(3) 0.0386(14) Uani 1 1 d . . . C55 C 0.1361(4) 0.2220(4) 0.5483(3) 0.067(2) Uani 1 1 d . . . H55A H 0.1574 0.2333 0.5025 0.080 Uiso 1 1 calc R . . C56 C 0.0458(4) 0.2143(5) 0.5542(3) 0.076(2) Uani 1 1 d . . . H56A H 0.0057 0.2201 0.5123 0.091 Uiso 1 1 calc R . . C57 C 0.0152(4) 0.1985(4) 0.6202(3) 0.0588(17) Uani 1 1 d . . . H57A H -0.0462 0.1923 0.6239 0.071 Uiso 1 1 calc R . . C58 C 0.0740(3) 0.1914(4) 0.6826(3) 0.0508(16) Uani 1 1 d . . . C59 C 0.0422(3) 0.1785(3) 0.7577(3) 0.0410(14) Uani 1 1 d . . . C60 C -0.0409(3) 0.1412(4) 0.7661(3) 0.0627(19) Uani 1 1 d . . . H60A H -0.0789 0.1221 0.7255 0.075 Uiso 1 1 calc R . . C61 C -0.0666(3) 0.1327(4) 0.8380(3) 0.0656(19) Uani 1 1 d . . . H61A H -0.1231 0.1085 0.8449 0.079 Uiso 1 1 calc R . . C62 C -0.0120(3) 0.1583(4) 0.8972(3) 0.0588(18) Uani 1 1 d . . . C63 C 0.0708(3) 0.1967(4) 0.8841(3) 0.0446(15) Uani 1 1 d . . . C64 C 0.1364(4) 0.2253(4) 0.9510(3) 0.0582(18) Uani 1 1 d . . . H64A H 0.1912 0.1873 0.9496 0.070 Uiso 1 1 calc R . . C65 C 0.0921(4) 0.1988(5) 1.0208(3) 0.076(2) Uani 1 1 d . . . H65A H 0.1282 0.2139 1.0669 0.091 Uiso 1 1 calc R . . C66 C -0.0070(4) 0.2401(5) 1.0156(3) 0.082(2) Uani 1 1 d . . . H66A H -0.0319 0.2477 1.0627 0.099 Uiso 1 1 calc R . . H66B H -0.0164 0.2965 0.9849 0.099 Uiso 1 1 calc R . . C67 C -0.0301(4) 0.1466(4) 0.9766(3) 0.068(2) Uani 1 1 d . . . H67A H -0.0889 0.1197 0.9850 0.082 Uiso 1 1 calc R . . C68 C 0.0498(4) 0.0990(5) 1.0186(3) 0.0727(19) Uani 1 1 d . . . C69 C 0.0950(5) 0.0171(5) 0.9838(4) 0.091(2) Uani 1 1 d . . . H69A H 0.1107 0.0356 0.9358 0.137 Uiso 1 1 calc R . . H69B H 0.0548 -0.0365 0.9792 0.137 Uiso 1 1 calc R . . H69C H 0.1482 -0.0002 1.0142 0.137 Uiso 1 1 calc R . . C70 C 0.0255(5) 0.0669(7) 1.0959(4) 0.135(4) Uani 1 1 d . . . H70A H -0.0018 0.0048 1.0923 0.202 Uiso 1 1 calc R . . H70B H -0.0157 0.1118 1.1142 0.202 Uiso 1 1 calc R . . H70C H 0.0791 0.0642 1.1291 0.202 Uiso 1 1 calc R . . C71 C 0.1622(4) 0.3321(4) 0.9500(3) 0.0667(19) Uani 1 1 d . . . H71A H 0.1783 0.3473 0.9008 0.080 Uiso 1 1 calc R . . H71B H 0.1091 0.3690 0.9580 0.080 Uiso 1 1 calc R . . C72 C 0.2356(5) 0.3651(6) 1.0032(5) 0.114(3) Uani 1 1 d . . . H72A H 0.2885 0.3271 0.9964 0.137 Uiso 1 1 calc R . . H72B H 0.2189 0.3526 1.0526 0.137 Uiso 1 1 calc R . . C73 C 0.2599(6) 0.4674(7) 0.9983(7) 0.185(5) Uani 1 1 d . . . H73A H 0.2394 0.4883 0.9487 0.222 Uiso 1 1 calc R . . H73B H 0.2242 0.5016 1.0317 0.222 Uiso 1 1 calc R . . C74 C 0.3348(11) 0.4948(10) 1.0102(12) 0.325(10) Uani 1 1 d . . . H74A H 0.3366 0.5626 1.0031 0.487 Uiso 1 1 calc R . . H74B H 0.3722 0.4640 0.9771 0.487 Uiso 1 1 calc R . . H74C H 0.3561 0.4798 1.0603 0.487 Uiso 1 1 calc R . . Cl1 Cl 0.85561(11) 0.00923(13) 0.52795(9) 0.0749(5) Uani 1 1 d . . . Cl2 Cl 0.28377(14) 0.76442(18) 0.07292(12) 0.1338(8) Uani 1 1 d . . . Cu1 Cu 0.28241(4) 0.10584(5) 0.73703(3) 0.05462(19) Uani 1 1 d . . . Cu2 Cu 0.21451(4) 0.25346(5) 0.79076(4) 0.0551(2) Uani 1 1 d . . . N1 N 0.2352(3) -0.0141(3) 0.7763(2) 0.0458(13) Uani 1 1 d . . . N2 N 0.3303(2) 0.1300(3) 0.8495(2) 0.0344(11) Uani 1 1 d . . . N3 N 0.3217(2) 0.3279(3) 0.8009(2) 0.0412(12) Uani 1 1 d . . . N4 N 0.3460(3) 0.1603(3) 0.6581(2) 0.0402(11) Uani 1 1 d . . . N5 N 0.1642(3) 0.1977(3) 0.6778(2) 0.0420(12) Uani 1 1 d . . . N6 N 0.0981(3) 0.2055(3) 0.8170(2) 0.0446(12) Uani 1 1 d . . . O1 O 0.8405(6) 0.1003(5) 0.4958(4) 0.189(3) Uani 1 1 d . . . O2 O 0.8529(5) 0.0177(5) 0.6033(3) 0.155(3) Uani 1 1 d . . . O3 O 0.7943(5) -0.0512(6) 0.4987(5) 0.218(4) Uani 1 1 d . . . O4 O 0.9411(4) -0.0159(7) 0.5136(4) 0.217(4) Uani 1 1 d . . . O5 O 0.2238(5) 0.7362(6) 0.0180(4) 0.234(3) Uani 1 1 d . . . O6 O 0.3095(6) 0.7008(5) 0.1221(3) 0.202(4) Uani 1 1 d . . . O7 O 0.3340(4) 0.8286(6) 0.0556(4) 0.378(3) Uani 1 1 d D . . O8 O 0.2112(10) 0.8112(14) 0.1112(10) 0.515(13) Uani 1 1 d D . . O9 O 0.6904(9) -0.3132(10) 0.7328(7) 0.310(6) Uiso 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 C1 0.176(9) 0.48(2) 0.164(10) -0.039(12) 0.085(8) 0.090(13) C2 0.201(9) 0.180(9) 0.067(5) -0.009(6) 0.009(6) -0.070(8) C3 0.096(5) 0.144(7) 0.049(4) 0.002(4) -0.002(4) -0.015(5) C4 0.078(4) 0.063(4) 0.052(4) -0.005(3) -0.006(3) -0.015(3) C5 0.060(3) 0.042(3) 0.047(3) -0.001(3) -0.010(3) 0.010(3) C6 0.065(3) 0.033(3) 0.070(4) -0.002(3) -0.009(3) -0.006(3) C7 0.084(4) 0.034(3) 0.063(3) 0.001(3) -0.011(3) 0.000(3) C8 0.077(4) 0.037(3) 0.065(4) 0.000(3) -0.015(3) -0.005(3) C9 0.048(3) 0.037(3) 0.060(3) 0.007(3) -0.011(3) -0.002(3) C10 0.048(3) 0.027(3) 0.045(3) -0.007(2) -0.003(2) 0.004(2) C11 0.059(3) 0.054(4) 0.070(4) -0.005(3) -0.014(3) -0.014(3) C12 0.058(4) 0.098(5) 0.096(5) -0.012(4) 0.005(4) 0.016(4) C13 0.073(4) 0.071(4) 0.093(4) -0.007(4) -0.021(3) -0.025(4) C14 0.065(3) 0.038(3) 0.058(4) 0.013(3) 0.007(3) -0.009(3) C15 0.063(3) 0.038(3) 0.039(3) 0.003(2) 0.004(3) -0.009(3) C16 0.038(3) 0.038(3) 0.038(3) -0.004(2) 0.000(2) 0.004(2) C17 0.046(3) 0.040(3) 0.039(3) -0.002(2) 0.003(2) 0.007(2) C18 0.102(4) 0.035(3) 0.043(3) 0.011(3) -0.009(3) 0.002(3) C19 0.107(4) 0.076(4) 0.044(3) 0.015(4) -0.031(3) -0.007(4) C20 0.079(4) 0.062(4) 0.044(3) 0.000(3) -0.026(3) -0.011(3) C21 0.050(3) 0.037(3) 0.045(3) 0.000(2) -0.001(2) 0.009(3) C22 0.035(3) 0.037(3) 0.045(3) -0.010(2) -0.004(2) 0.000(2) C23 0.043(3) 0.051(3) 0.058(3) 0.003(3) -0.009(3) -0.009(3) C24 0.048(3) 0.052(4) 0.055(3) -0.007(3) -0.004(3) -0.012(3) C25 0.038(3) 0.038(3) 0.057(3) -0.007(2) 0.000(2) -0.016(2) C26 0.046(3) 0.033(3) 0.042(3) 0.000(2) -0.004(2) 0.006(2) C27 0.036(3) 0.046(3) 0.056(3) 0.008(3) -0.003(2) 0.005(2) C28 0.045(3) 0.032(3) 0.076(4) 0.006(3) 0.000(3) 0.006(3) C29 0.067(3) 0.029(3) 0.077(4) -0.004(3) 0.005(3) -0.007(3) C30 0.058(3) 0.048(4) 0.076(4) 0.013(3) 0.004(3) -0.018(3) C31 0.061(3) 0.038(3) 0.053(3) 0.005(3) 0.003(3) -0.007(3) C32 0.059(3) 0.074(4) 0.065(4) 0.003(3) 0.009(3) -0.008(3) C33 0.105(5) 0.063(4) 0.079(4) 0.024(3) 0.022(4) -0.017(4) C34 0.050(3) 0.050(3) 0.059(3) 0.007(3) -0.007(3) 0.007(3) C35 0.047(3) 0.056(4) 0.074(4) 0.000(3) -0.006(3) 0.011(3) C36 0.058(4) 0.120(6) 0.083(5) -0.022(4) -0.009(4) 0.004(4) C37 0.052(4) 0.167(9) 0.181(8) -0.045(7) -0.020(5) 0.002(5) C38 0.123(6) 0.073(5) 0.085(5) 0.025(4) 0.009(4) 0.016(4) C39 0.094(4) 0.042(4) 0.072(4) 0.010(3) 0.001(4) 0.016(3) C40 0.062(3) 0.068(4) 0.052(3) 0.002(3) -0.002(3) 0.018(3) C41 0.055(3) 0.053(4) 0.060(3) 0.014(3) -0.008(3) 0.007(3) C42 0.047(3) 0.041(3) 0.046(3) 0.012(3) -0.004(2) 0.011(3) C43 0.043(3) 0.073(4) 0.060(3) 0.008(3) 0.007(2) 0.022(3) C44 0.043(3) 0.094(5) 0.084(4) -0.020(3) 0.017(3) 0.011(3) C45 0.045(3) 0.074(4) 0.060(4) 0.009(3) 0.018(3) 0.007(3) C46 0.068(3) 0.042(3) 0.040(3) -0.002(3) 0.012(3) 0.001(3) C47 0.045(3) 0.046(3) 0.049(3) -0.001(3) 0.005(3) 0.006(3) C48 0.050(3) 0.062(4) 0.057(3) 0.000(3) 0.002(3) 0.005(3) C49 0.064(3) 0.047(4) 0.075(4) 0.008(3) 0.004(3) -0.008(3) C50 0.041(3) 0.106(5) 0.099(5) -0.005(4) 0.009(3) -0.010(3) C51 0.065(3) 0.070(4) 0.039(3) 0.010(3) 0.012(3) -0.009(3) C52 0.068(3) 0.046(3) 0.045(3) 0.018(3) 0.009(3) 0.005(3) C53 0.049(3) 0.038(3) 0.043(3) -0.002(2) -0.006(2) 0.003(2) C54 0.045(3) 0.033(3) 0.037(3) 0.006(2) -0.002(2) 0.004(2) C55 0.057(3) 0.086(5) 0.053(4) 0.003(3) -0.012(3) 0.007(3) C56 0.062(4) 0.108(6) 0.053(4) 0.006(4) -0.020(3) 0.004(4) C57 0.043(3) 0.059(4) 0.071(4) 0.001(3) -0.014(3) 0.001(3) C58 0.039(3) 0.042(3) 0.069(4) -0.001(3) -0.009(3) 0.005(3) C59 0.033(2) 0.038(3) 0.052(3) 0.001(2) 0.007(2) 0.003(2) C60 0.046(3) 0.068(4) 0.074(4) -0.006(3) 0.002(3) -0.005(3) C61 0.036(3) 0.085(5) 0.078(4) 0.008(3) 0.018(3) -0.010(3) C62 0.047(3) 0.071(4) 0.061(4) 0.003(3) 0.016(3) -0.005(3) C63 0.047(3) 0.040(3) 0.049(3) 0.004(3) 0.015(2) 0.009(3) C64 0.054(3) 0.057(4) 0.064(4) -0.003(3) 0.008(3) -0.001(3) C65 0.083(4) 0.095(5) 0.052(4) 0.012(3) 0.015(3) 0.008(4) C66 0.072(4) 0.101(5) 0.079(4) -0.015(4) 0.035(3) 0.025(4) C67 0.055(3) 0.069(4) 0.086(4) -0.002(3) 0.033(3) -0.001(3) C68 0.080(4) 0.069(4) 0.074(4) 0.028(4) 0.027(3) -0.008(4) C69 0.106(5) 0.071(5) 0.096(5) 0.011(4) 0.007(4) 0.014(4) C70 0.130(6) 0.185(9) 0.094(6) 0.036(5) 0.035(5) -0.049(6) C71 0.070(4) 0.067(4) 0.065(4) -0.005(3) 0.021(3) -0.001(3) C72 0.113(6) 0.099(6) 0.128(6) -0.038(5) -0.009(5) -0.017(5) C73 0.080(6) 0.137(8) 0.328(13) -0.119(8) -0.043(7) -0.013(6) C74 0.316(18) 0.135(13) 0.55(3) 0.075(14) 0.202(18) 0.052(13) Cl1 0.0701(10) 0.0799(11) 0.0725(10) -0.0142(9) -0.0058(8) 0.0038(9) Cl2 0.1233(14) 0.1506(18) 0.1162(14) 0.0687(14) -0.0532(12) -0.0607(15) Cu1 0.0634(4) 0.0545(4) 0.0450(3) 0.0106(4) -0.0010(3) -0.0073(4) Cu2 0.0438(3) 0.0528(4) 0.0670(4) 0.0082(4) -0.0042(3) -0.0080(4) N1 0.049(2) 0.061(3) 0.026(2) -0.005(2) -0.0021(19) 0.010(2) N2 0.0325(19) 0.027(2) 0.043(2) 0.0018(18) -0.0009(17) -0.0016(18) N3 0.032(2) 0.046(3) 0.045(3) -0.001(2) 0.0008(19) 0.005(2) N4 0.045(2) 0.035(2) 0.040(2) -0.0018(18) -0.0001(19) 0.002(2) N5 0.044(2) 0.027(2) 0.053(3) 0.007(2) -0.010(2) 0.009(2) N6 0.049(2) 0.034(2) 0.051(3) 0.000(2) 0.002(2) 0.005(2) O1 0.283(8) 0.114(5) 0.158(5) 0.038(5) -0.053(5) 0.018(6) O2 0.232(7) 0.155(6) 0.074(4) 0.015(4) 0.003(4) 0.029(5) O3 0.168(6) 0.200(7) 0.280(9) -0.090(6) -0.008(6) -0.094(5) O4 0.110(4) 0.352(11) 0.191(7) -0.040(7) 0.024(5) 0.081(6) O5 0.227(5) 0.296(8) 0.153(5) 0.102(5) -0.123(4) -0.178(5) O6 0.352(9) 0.119(5) 0.113(5) 0.051(4) -0.097(5) -0.041(6) O7 0.161(4) 0.548(8) 0.383(6) 0.402(5) -0.203(4) -0.231(5) O8 0.70(3) 0.38(2) 0.44(2) -0.051(17) -0.07(2) 0.271(19) _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 C1 C2 1.316(15) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.484(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.553(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.489(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C10 1.530(6) . ? C5 C6 1.530(7) . ? C5 H5A 0.9800 . ? C6 C7 1.541(7) . ? C6 C11 1.544(8) . ? C6 H6A 0.9800 . ? C7 C8 1.541(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.489(7) . ? C8 C11 1.568(8) . ? C8 H8A 0.9800 . ? C9 C14 1.387(7) . ? C9 C10 1.406(7) . ? C10 N1 1.363(6) . ? C11 C12 1.515(8) . ? C11 C13 1.527(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.382(7) . ? C14 H14A 0.9300 . ? C15 C16 1.380(7) . ? C15 H15A 0.9300 . ? C16 N1 1.360(6) . ? C16 C17 1.499(7) . ? C17 C18 1.365(7) . ? C17 N2 1.366(6) . ? C18 C19 1.391(8) . ? C18 H18A 0.9300 . ? C19 C20 1.380(9) . ? C19 H19A 0.9300 . ? C20 C21 1.389(7) . ? C20 H20A 0.9300 . ? C21 N2 1.364(6) . ? C21 C22 1.467(7) . ? C22 N3 1.367(6) . ? C22 C23 1.383(6) . ? C23 C24 1.371(7) . ? C23 H23A 0.9300 . ? C24 C25 1.402(7) . ? C24 H24A 0.9300 . ? C25 C26 1.378(6) . ? C25 C30 1.494(7) . ? C26 N3 1.348(6) . ? C26 C27 1.557(6) . ? C27 C34 1.521(7) . ? C27 C28 1.562(7) . ? C27 H27A 0.9800 . ? C28 C31 1.528(7) . ? C28 C29 1.583(7) . ? C28 H28A 0.9800 . ? C29 C30 1.554(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.556(7) . ? C30 H30A 0.9800 . ? C31 C32 1.510(8) . ? C31 C33 1.562(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.503(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.523(8) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.480(9) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.499(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.516(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.503(7) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.497(7) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.528(6) . ? C42 C47 1.541(6) . ? C42 H42A 0.9800 . ? C43 C44 1.526(7) . ? C43 C48 1.555(8) . ? C43 H43A 0.9800 . ? C44 C45 1.569(8) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.465(7) . ? C45 C48 1.562(7) . ? C45 H45A 0.9800 . ? C46 C51 1.399(7) . ? C46 C47 1.444(7) . ? C47 N4 1.321(6) . ? C48 C49 1.486(8) . ? C48 C50 1.580(7) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.351(7) . ? C51 H51A 0.9300 . ? C52 C53 1.387(7) . ? C52 H52A 0.9300 . ? C53 N4 1.389(6) . ? C53 C54 1.470(7) . ? C54 N5 1.354(6) . ? C54 C55 1.400(7) . ? C55 C56 1.368(8) . ? C55 H55A 0.9300 . ? C56 C57 1.341(8) . ? C56 H56A 0.9300 . ? C57 C58 1.376(7) . ? C57 H57A 0.9300 . ? C58 N5 1.361(6) . ? C58 C59 1.497(7) . ? C59 N6 1.358(6) . ? C59 C60 1.370(7) . ? C60 C61 1.399(8) . ? C60 H60A 0.9300 . ? C61 C62 1.341(8) . ? C61 H61A 0.9300 . ? C62 C63 1.390(7) . ? C62 C67 1.501(8) . ? C63 N6 1.326(6) . ? C63 C64 1.546(7) . ? C64 C65 1.528(8) . ? C64 C71 1.544(8) . ? C64 H64A 0.9800 . ? C65 C68 1.534(9) . ? C65 C66 1.586(8) . ? C65 H65A 0.9800 . ? C66 C67 1.514(9) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.515(8) . ? C67 H67A 0.9800 . ? C68 C69 1.498(9) . ? C68 C70 1.549(9) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 C72 1.472(9) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.483(12) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.186(18) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? Cl1 O3 1.325(7) . ? Cl1 O4 1.374(7) . ? Cl1 O2 1.378(5) . ? Cl1 O1 1.412(7) . ? Cl2 O7 1.230(7) . ? Cl2 O6 1.296(6) . ? Cl2 O5 1.341(6) . ? Cl2 O8 1.492(15) . ? Cu1 N4 1.946(4) . ? Cu1 N1 1.980(4) . ? Cu1 N2 2.133(4) . ? Cu1 N5 2.367(4) . ? Cu1 Cu2 2.5363(10) . ? Cu2 N3 1.907(4) . ? Cu2 N6 1.965(4) . ? Cu2 N5 2.262(4) . ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 117.0(10) . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.3 . . ? C2 C3 C4 112.2(6) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 115.6(5) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C4 C5 C10 110.6(4) . . ? C4 C5 C6 114.2(4) . . ? C10 C5 C6 108.1(4) . . ? C4 C5 H5A 107.9 . . ? C10 C5 H5A 107.9 . . ? C6 C5 H5A 107.9 . . ? C5 C6 C7 108.1(4) . . ? C5 C6 C11 116.0(4) . . ? C7 C6 C11 89.4(4) . . ? C5 C6 H6A 113.6 . . ? C7 C6 H6A 113.6 . . ? C11 C6 H6A 113.6 . . ? C6 C7 C8 84.2(4) . . ? C6 C7 H7A 114.6 . . ? C8 C7 H7A 114.6 . . ? C6 C7 H7B 114.6 . . ? C8 C7 H7B 114.6 . . ? H7A C7 H7B 111.7 . . ? C9 C8 C7 108.8(4) . . ? C9 C8 C11 108.3(5) . . ? C7 C8 C11 88.6(4) . . ? C9 C8 H8A 116.0 . . ? C7 C8 H8A 116.0 . . ? C11 C8 H8A 116.0 . . ? C14 C9 C10 117.4(4) . . ? C14 C9 C8 125.4(5) . . ? C10 C9 C8 117.2(4) . . ? N1 C10 C9 123.0(4) . . ? N1 C10 C5 119.3(4) . . ? C9 C10 C5 117.6(4) . . ? C12 C11 C13 109.9(5) . . ? C12 C11 C6 120.3(5) . . ? C13 C11 C6 112.7(5) . . ? C12 C11 C8 117.7(5) . . ? C13 C11 C8 110.7(5) . . ? C6 C11 C8 83.2(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C9 120.5(5) . . ? C15 C14 H14A 119.7 . . ? C9 C14 H14A 119.7 . . ? C16 C15 C14 118.5(5) . . ? C16 C15 H15A 120.7 . . ? C14 C15 H15A 120.7 . . ? N1 C16 C15 123.3(4) . . ? N1 C16 C17 116.3(4) . . ? C15 C16 C17 120.4(4) . . ? C18 C17 N2 122.6(5) . . ? C18 C17 C16 119.4(5) . . ? N2 C17 C16 118.0(4) . . ? C17 C18 C19 117.9(5) . . ? C17 C18 H18A 121.1 . . ? C19 C18 H18A 121.1 . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C21 118.9(5) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? N2 C21 C20 120.8(5) . . ? N2 C21 C22 120.5(4) . . ? C20 C21 C22 118.7(5) . . ? N3 C22 C23 121.4(4) . . ? N3 C22 C21 119.4(4) . . ? C23 C22 C21 119.1(4) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.3(5) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 117.0(5) . . ? C26 C25 C30 119.0(4) . . ? C24 C25 C30 124.0(4) . . ? N3 C26 C25 124.9(4) . . ? N3 C26 C27 117.2(4) . . ? C25 C26 C27 117.8(4) . . ? C34 C27 C26 115.7(4) . . ? C34 C27 C28 111.2(4) . . ? C26 C27 C28 107.9(4) . . ? C34 C27 H27A 107.2 . . ? C26 C27 H27A 107.2 . . ? C28 C27 H27A 107.2 . . ? C31 C28 C27 113.7(4) . . ? C31 C28 C29 87.7(4) . . ? C27 C28 C29 108.4(4) . . ? C31 C28 H28A 114.7 . . ? C27 C28 H28A 114.7 . . ? C29 C28 H28A 114.7 . . ? C30 C29 C28 84.5(4) . . ? C30 C29 H29A 114.6 . . ? C28 C29 H29A 114.6 . . ? C30 C29 H29B 114.6 . . ? C28 C29 H29B 114.6 . . ? H29A C29 H29B 111.7 . . ? C25 C30 C29 106.8(4) . . ? C25 C30 C31 109.1(4) . . ? C29 C30 C31 87.7(4) . . ? C25 C30 H30A 116.5 . . ? C29 C30 H30A 116.5 . . ? C31 C30 H30A 116.5 . . ? C32 C31 C28 119.9(4) . . ? C32 C31 C30 118.7(4) . . ? C28 C31 C30 86.2(4) . . ? C32 C31 C33 108.7(4) . . ? C28 C31 C33 110.3(4) . . ? C30 C31 C33 111.5(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C27 114.4(4) . . ? C35 C34 H34A 108.7 . . ? C27 C34 H34A 108.7 . . ? C35 C34 H34B 108.7 . . ? C27 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C34 C35 C36 114.6(5) . . ? C34 C35 H35A 108.6 . . ? C36 C35 H35A 108.6 . . ? C34 C35 H35B 108.6 . . ? C36 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 113.0(6) . . ? C37 C36 H36A 109.0 . . ? C35 C36 H36A 109.0 . . ? C37 C36 H36B 109.0 . . ? C35 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C38 C39 C40 115.5(5) . . ? C38 C39 H39A 108.4 . . ? C40 C39 H39A 108.4 . . ? C38 C39 H39B 108.4 . . ? C40 C39 H39B 108.4 . . ? H39A C39 H39B 107.5 . . ? C41 C40 C39 116.0(5) . . ? C41 C40 H40A 108.3 . . ? C39 C40 H40A 108.3 . . ? C41 C40 H40B 108.3 . . ? C39 C40 H40B 108.3 . . ? H40A C40 H40B 107.4 . . ? C42 C41 C40 116.3(4) . . ? C42 C41 H41A 108.2 . . ? C40 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? C40 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 112.4(4) . . ? C41 C42 C47 112.6(4) . . ? C43 C42 C47 108.3(4) . . ? C41 C42 H42A 107.8 . . ? C43 C42 H42A 107.8 . . ? C47 C42 H42A 107.8 . . ? C44 C43 C42 109.7(4) . . ? C44 C43 C48 89.3(4) . . ? C42 C43 C48 113.7(4) . . ? C44 C43 H43A 113.9 . . ? C42 C43 H43A 113.9 . . ? C48 C43 H43A 113.9 . . ? C43 C44 C45 85.3(4) . . ? C43 C44 H44A 114.4 . . ? C45 C44 H44A 114.4 . . ? C43 C44 H44B 114.4 . . ? C45 C44 H44B 114.4 . . ? H44A C44 H44B 111.6 . . ? C46 C45 C48 108.2(4) . . ? C46 C45 C44 107.3(5) . . ? C48 C45 C44 87.5(4) . . ? C46 C45 H45A 116.7 . . ? C48 C45 H45A 116.7 . . ? C44 C45 H45A 116.7 . . ? C51 C46 C47 115.9(5) . . ? C51 C46 C45 126.0(5) . . ? C47 C46 C45 118.1(5) . . ? N4 C47 C46 123.8(4) . . ? N4 C47 C42 119.4(4) . . ? C46 C47 C42 116.6(4) . . ? C49 C48 C43 121.0(4) . . ? C49 C48 C45 119.3(5) . . ? C43 C48 C45 84.6(4) . . ? C49 C48 C50 108.5(5) . . ? C43 C48 C50 110.7(5) . . ? C45 C48 C50 111.0(4) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C46 120.9(5) . . ? C52 C51 H51A 119.5 . . ? C46 C51 H51A 119.5 . . ? C51 C52 C53 120.1(5) . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C52 C53 N4 121.7(4) . . ? C52 C53 C54 121.2(4) . . ? N4 C53 C54 117.1(4) . . ? N5 C54 C55 119.6(4) . . ? N5 C54 C53 119.8(4) . . ? C55 C54 C53 120.4(5) . . ? C56 C55 C54 119.6(5) . . ? C56 C55 H55A 120.2 . . ? C54 C55 H55A 120.2 . . ? C57 C56 C55 120.1(5) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C58 120.3(5) . . ? C56 C57 H57A 119.8 . . ? C58 C57 H57A 119.8 . . ? N5 C58 C57 120.6(5) . . ? N5 C58 C59 117.5(4) . . ? C57 C58 C59 121.9(5) . . ? N6 C59 C60 121.3(5) . . ? N6 C59 C58 117.9(4) . . ? C60 C59 C58 120.9(4) . . ? C59 C60 C61 117.6(5) . . ? C59 C60 H60A 121.2 . . ? C61 C60 H60A 121.2 . . ? C62 C61 C60 122.0(5) . . ? C62 C61 H61A 119.0 . . ? C60 C61 H61A 119.0 . . ? C61 C62 C63 117.0(5) . . ? C61 C62 C67 126.5(5) . . ? C63 C62 C67 116.5(5) . . ? N6 C63 C62 123.1(5) . . ? N6 C63 C64 118.2(4) . . ? C62 C63 C64 118.7(5) . . ? C65 C64 C71 111.8(5) . . ? C65 C64 C63 107.3(4) . . ? C71 C64 C63 112.6(4) . . ? C65 C64 H64A 108.3 . . ? C71 C64 H64A 108.3 . . ? C63 C64 H64A 108.3 . . ? C64 C65 C68 114.1(5) . . ? C64 C65 C66 109.5(5) . . ? C68 C65 C66 87.1(5) . . ? C64 C65 H65A 114.4 . . ? C68 C65 H65A 114.4 . . ? C66 C65 H65A 114.4 . . ? C67 C66 C65 83.5(5) . . ? C67 C66 H66A 114.7 . . ? C65 C66 H66A 114.7 . . ? C67 C66 H66B 114.7 . . ? C65 C66 H66B 114.7 . . ? H66A C66 H66B 111.8 . . ? C62 C67 C66 107.6(5) . . ? C62 C67 C68 109.3(5) . . ? C66 C67 C68 90.4(5) . . ? C62 C67 H67A 115.5 . . ? C66 C67 H67A 115.5 . . ? C68 C67 H67A 115.5 . . ? C69 C68 C67 119.3(5) . . ? C69 C68 C65 120.5(5) . . ? C67 C68 C65 85.3(5) . . ? C69 C68 C70 108.1(6) . . ? C67 C68 C70 110.3(5) . . ? C65 C68 C70 111.7(6) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 C64 118.0(6) . . ? C72 C71 H71A 107.8 . . ? C64 C71 H71A 107.8 . . ? C72 C71 H71B 107.8 . . ? C64 C71 H71B 107.8 . . ? H71A C71 H71B 107.2 . . ? C71 C72 C73 115.9(7) . . ? C71 C72 H72A 108.3 . . ? C73 C72 H72A 108.3 . . ? C71 C72 H72B 108.3 . . ? C73 C72 H72B 108.3 . . ? H72A C72 H72B 107.4 . . ? C74 C73 C72 122.2(11) . . ? C74 C73 H73A 106.8 . . ? C72 C73 H73A 106.8 . . ? C74 C73 H73B 106.8 . . ? C72 C73 H73B 106.8 . . ? H73A C73 H73B 106.6 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O3 Cl1 O4 112.6(6) . . ? O3 Cl1 O2 111.9(5) . . ? O4 Cl1 O2 108.7(5) . . ? O3 Cl1 O1 109.3(5) . . ? O4 Cl1 O1 105.6(6) . . ? O2 Cl1 O1 108.5(4) . . ? O7 Cl2 O6 121.9(5) . . ? O7 Cl2 O5 114.1(5) . . ? O6 Cl2 O5 116.7(5) . . ? O7 Cl2 O8 106.6(8) . . ? O6 Cl2 O8 99.4(8) . . ? O5 Cl2 O8 90.6(8) . . ? N4 Cu1 N1 144.29(16) . . ? N4 Cu1 N2 119.98(15) . . ? N1 Cu1 N2 83.63(14) . . ? N4 Cu1 N5 81.18(15) . . ? N1 Cu1 N5 110.38(15) . . ? N2 Cu1 N5 121.59(14) . . ? N4 Cu1 Cu2 101.73(12) . . ? N1 Cu1 Cu2 112.59(12) . . ? N2 Cu1 Cu2 67.28(10) . . ? N5 Cu1 Cu2 54.82(10) . . ? N3 Cu2 N6 156.77(17) . . ? N3 Cu2 N5 119.08(16) . . ? N6 Cu2 N5 82.60(16) . . ? N3 Cu2 Cu1 96.93(12) . . ? N6 Cu2 Cu1 102.05(12) . . ? N5 Cu2 Cu1 58.79(10) . . ? C16 N1 C10 117.0(4) . . ? C16 N1 Cu1 113.3(3) . . ? C10 N1 Cu1 129.3(3) . . ? C21 N2 C17 119.0(4) . . ? C21 N2 Cu1 131.9(3) . . ? C17 N2 Cu1 107.1(3) . . ? C26 N3 C22 117.0(4) . . ? C26 N3 Cu2 125.7(3) . . ? C22 N3 Cu2 117.2(3) . . ? C47 N4 C53 117.4(4) . . ? C47 N4 Cu1 127.1(3) . . ? C53 N4 Cu1 115.5(3) . . ? C54 N5 C58 119.8(4) . . ? C54 N5 Cu2 129.7(3) . . ? C58 N5 Cu2 102.6(3) . . ? C54 N5 Cu1 100.4(3) . . ? C58 N5 Cu1 129.9(3) . . ? Cu2 N5 Cu1 66.39(10) . . ? C63 N6 C59 119.1(4) . . ? C63 N6 Cu2 127.4(3) . . ? C59 N6 Cu2 113.5(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.956 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.073 # Attachment 'wy1547wm2.cif' data_wy1547wm _database_code_depnum_ccdc_archive 'CCDC 651265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H82 Cu2 F12 N10 P2' _chemical_formula_weight 1624.60 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.5877(8) _cell_length_b 13.2827(7) _cell_length_c 19.0425(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.6540(10) _cell_angle_gamma 90.00 _cell_volume 3861.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9081 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19386 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13289 _reflns_number_gt 9804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+0.0000P] 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 constr _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 -0.002(12) _refine_ls_number_reflns 13289 _refine_ls_number_parameters 973 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.2069(4) 0.4884(4) 0.5610(3) 0.0538(14) Uani 1 1 d . . . H1A H 0.2190 0.4175 0.5616 0.081 Uiso 1 1 calc R . . H1B H 0.2245 0.5185 0.5203 0.081 Uiso 1 1 calc R . . H1C H 0.1453 0.4988 0.5577 0.081 Uiso 1 1 calc R . . C2 C 0.2375(5) 0.4779(5) 0.6934(3) 0.076(2) Uani 1 1 d . . . H2A H 0.2430 0.4071 0.6855 0.114 Uiso 1 1 calc R . . H2B H 0.1789 0.4926 0.6987 0.114 Uiso 1 1 calc R . . H2C H 0.2781 0.4974 0.7361 0.114 Uiso 1 1 calc R . . C3 C 0.2575(4) 0.5363(4) 0.6293(3) 0.0520(14) Uani 1 1 d . . . C4 C 0.2500(4) 0.6522(4) 0.6408(3) 0.0532(13) Uani 1 1 d . . . H4A H 0.2056 0.6738 0.6674 0.064 Uiso 1 1 calc R . . C5 C 0.2514(3) 0.7074(4) 0.5728(3) 0.0434(12) Uani 1 1 d . . . C6 C 0.3179(3) 0.6817(3) 0.5366(3) 0.0417(12) Uani 1 1 d . . . C7 C 0.3780(3) 0.5935(4) 0.5652(3) 0.0484(12) Uani 1 1 d . . . H7A H 0.3638 0.5382 0.5307 0.058 Uiso 1 1 calc R . . C8 C 0.3574(4) 0.5565(4) 0.6370(3) 0.0534(14) Uani 1 1 d . . . H8A H 0.3962 0.5038 0.6615 0.064 Uiso 1 1 calc R . . C9 C 0.3449(4) 0.6487(5) 0.6835(3) 0.0610(15) Uani 1 1 d . . . H9A H 0.3502 0.6337 0.7340 0.073 Uiso 1 1 calc R . . H9B H 0.3799 0.7067 0.6764 0.073 Uiso 1 1 calc R . . C10 C 0.4740(4) 0.6168(5) 0.5720(4) 0.0698(18) Uani 1 1 d . . . H10A H 0.4844 0.6395 0.5266 0.105 Uiso 1 1 calc R . . H10B H 0.5078 0.5571 0.5864 0.105 Uiso 1 1 calc R . . H10C H 0.4908 0.6685 0.6073 0.105 Uiso 1 1 calc R . . C11 C 0.1953(3) 0.7828(4) 0.5443(3) 0.0473(13) Uani 1 1 d . . . H11A H 0.1490 0.8001 0.5659 0.057 Uiso 1 1 calc R . . C12 C 0.2071(3) 0.8332(4) 0.4840(3) 0.0453(12) Uani 1 1 d . . . H12A H 0.1690 0.8845 0.4645 0.054 Uiso 1 1 calc R . . C13 C 0.2763(3) 0.8064(3) 0.4527(3) 0.0371(11) Uani 1 1 d . . . C14 C 0.2960(3) 0.8619(4) 0.3898(3) 0.0427(12) Uani 1 1 d . . . C15 C 0.2846(4) 0.9655(4) 0.3849(3) 0.0506(14) Uani 1 1 d . . . H15A H 0.2646 1.0010 0.4205 0.061 Uiso 1 1 calc R . . C16 C 0.3035(4) 1.0146(4) 0.3261(4) 0.0637(16) Uani 1 1 d . . . H16A H 0.2951 1.0837 0.3210 0.076 Uiso 1 1 calc R . . C17 C 0.3350(4) 0.9607(4) 0.2752(3) 0.0578(15) Uani 1 1 d . . . H17A H 0.3495 0.9933 0.2360 0.069 Uiso 1 1 calc R . . C18 C 0.3449(3) 0.8575(4) 0.2828(3) 0.0436(12) Uani 1 1 d . . . C19 C 0.3766(3) 0.7931(4) 0.2285(3) 0.0436(12) Uani 1 1 d . . . C20 C 0.4205(4) 0.8327(5) 0.1780(3) 0.0574(16) Uani 1 1 d . . . H20A H 0.4300 0.9016 0.1754 0.069 Uiso 1 1 calc R . . C21 C 0.4494(4) 0.7672(5) 0.1321(3) 0.0636(17) Uani 1 1 d . . . H21A H 0.4798 0.7913 0.0983 0.076 Uiso 1 1 calc R . . C22 C 0.4325(4) 0.6629(5) 0.1364(3) 0.0576(14) Uani 1 1 d . . . H22A H 0.4514 0.6172 0.1058 0.069 Uiso 1 1 calc R . . C23 C 0.3870(3) 0.6313(4) 0.1877(3) 0.0412(12) Uani 1 1 d . . . C24 C 0.3640(3) 0.5228(4) 0.1928(3) 0.0421(12) Uani 1 1 d . . . C25 C 0.4268(4) 0.4483(5) 0.1938(3) 0.0586(15) Uani 1 1 d . . . H25A H 0.4846 0.4655 0.1933 0.070 Uiso 1 1 calc R . . C26 C 0.4034(4) 0.3510(5) 0.1955(3) 0.0623(16) Uani 1 1 d . . . H26A H 0.4453 0.3007 0.1978 0.075 Uiso 1 1 calc R . . C27 C 0.3176(4) 0.3261(4) 0.1937(3) 0.0588(15) Uani 1 1 d . . . H27A H 0.3004 0.2589 0.1927 0.071 Uiso 1 1 calc R . . C28 C 0.2561(4) 0.4033(4) 0.1935(3) 0.0453(12) Uani 1 1 d . . . C29 C 0.1611(4) 0.3835(4) 0.1886(3) 0.0478(13) Uani 1 1 d . . . C30 C 0.1287(5) 0.2863(4) 0.1874(5) 0.081(2) Uani 1 1 d . . . H30A H 0.1662 0.2316 0.1892 0.098 Uiso 1 1 calc R . . C31 C 0.0394(5) 0.2712(5) 0.1835(5) 0.091(3) Uani 1 1 d . . . H31A H 0.0168 0.2064 0.1834 0.109 Uiso 1 1 calc R . . C32 C -0.0143(4) 0.3527(4) 0.1798(4) 0.0649(17) Uani 1 1 d . . . C33 C 0.0218(3) 0.4494(4) 0.1828(3) 0.0447(12) Uani 1 1 d . . . C34 C -0.0382(3) 0.5382(4) 0.1855(3) 0.0453(12) Uani 1 1 d . . . H34A H -0.0185 0.5716 0.2318 0.054 Uiso 1 1 calc R . . C35 C -0.0392(4) 0.6174(5) 0.1268(3) 0.0624(16) Uani 1 1 d . . . H35A H 0.0193 0.6413 0.1284 0.094 Uiso 1 1 calc R . . H35B H -0.0759 0.6727 0.1344 0.094 Uiso 1 1 calc R . . H35C H -0.0616 0.5878 0.0807 0.094 Uiso 1 1 calc R . . C36 C -0.1320(3) 0.5003(5) 0.1828(3) 0.0536(14) Uani 1 1 d . . . H36A H -0.1756 0.5534 0.1829 0.064 Uiso 1 1 calc R . . C37 C -0.1557(4) 0.4225(5) 0.1205(4) 0.0722(18) Uani 1 1 d . . . H37A H -0.2181 0.4119 0.1037 0.087 Uiso 1 1 calc R . . H37B H -0.1259 0.4331 0.0811 0.087 Uiso 1 1 calc R . . C38 C -0.1110(4) 0.3453(5) 0.1769(4) 0.0717(19) Uani 1 1 d . . . H38A H -0.1356 0.2771 0.1721 0.086 Uiso 1 1 calc R . . C39 C -0.1370(4) 0.4108(4) 0.2357(3) 0.0590(15) Uani 1 1 d . . . C40 C -0.0778(4) 0.4123(5) 0.3093(4) 0.0716(18) Uani 1 1 d . . . H40A H -0.0189 0.4268 0.3047 0.107 Uiso 1 1 calc R . . H40B H -0.0796 0.3479 0.3317 0.107 Uiso 1 1 calc R . . H40C H -0.0975 0.4633 0.3381 0.107 Uiso 1 1 calc R . . C41 C -0.2323(4) 0.3887(5) 0.2433(5) 0.086(2) Uani 1 1 d . . . H41A H -0.2325 0.3336 0.2758 0.130 Uiso 1 1 calc R . . H41B H -0.2670 0.3714 0.1972 0.130 Uiso 1 1 calc R . . H41C H -0.2565 0.4473 0.2614 0.130 Uiso 1 1 calc R . . C42 C 0.3141(6) 0.3599(6) -0.1198(4) 0.103(3) Uani 1 1 d . . . H42A H 0.3745 0.3729 -0.1207 0.155 Uiso 1 1 calc R . . H42B H 0.2792 0.3695 -0.1670 0.155 Uiso 1 1 calc R . . H42C H 0.3079 0.2919 -0.1047 0.155 Uiso 1 1 calc R . . C43 C 0.3492(5) 0.4327(6) 0.0035(4) 0.092(2) Uani 1 1 d . . . H43A H 0.4064 0.4462 -0.0058 0.139 Uiso 1 1 calc R . . H43B H 0.3491 0.3675 0.0254 0.139 Uiso 1 1 calc R . . H43C H 0.3346 0.4830 0.0353 0.139 Uiso 1 1 calc R . . C44 C 0.2827(5) 0.4345(5) -0.0660(3) 0.0716(19) Uani 1 1 d . . . C45 C 0.1627(5) 0.4872(6) -0.1319(4) 0.087(2) Uani 1 1 d . . . H45A H 0.1590 0.4534 -0.1775 0.104 Uiso 1 1 calc R . . H45B H 0.1128 0.5310 -0.1323 0.104 Uiso 1 1 calc R . . C46 C 0.2517(5) 0.5360(5) -0.1019(3) 0.0659(17) Uani 1 1 d . . . H46A H 0.2842 0.5609 -0.1374 0.079 Uiso 1 1 calc R . . C47 C 0.2387(4) 0.6096(5) -0.0451(3) 0.0544(14) Uani 1 1 d . . . C48 C 0.1897(4) 0.5766(4) 0.0041(3) 0.0522(14) Uani 1 1 d . . . C49 C 0.1569(5) 0.4674(5) -0.0007(3) 0.0666(17) Uani 1 1 d . . . H49A H 0.1871 0.4327 0.0428 0.080 Uiso 1 1 calc R . . C50 C 0.1854(5) 0.4162(5) -0.0646(3) 0.0756(19) Uani 1 1 d . . . H50A H 0.1659 0.3464 -0.0733 0.091 Uiso 1 1 calc R . . C51 C 0.0594(5) 0.4577(7) -0.0033(4) 0.105(3) Uani 1 1 d . . . H51A H 0.0432 0.3879 -0.0060 0.157 Uiso 1 1 calc R . . H51B H 0.0276 0.4924 -0.0448 0.157 Uiso 1 1 calc R . . H51C H 0.0455 0.4869 0.0392 0.157 Uiso 1 1 calc R . . C52 C 0.2705(4) 0.7053(5) -0.0381(3) 0.0597(16) Uani 1 1 d . . . H52A H 0.3050 0.7290 -0.0691 0.072 Uiso 1 1 calc R . . C53 C 0.2512(4) 0.7680(4) 0.0154(3) 0.0577(15) Uani 1 1 d . . . H53A H 0.2727 0.8334 0.0211 0.069 Uiso 1 1 calc R . . C54 C 0.1989(3) 0.7296(4) 0.0599(3) 0.0460(12) Uani 1 1 d . . . C55 C 0.1720(3) 0.7947(4) 0.1159(3) 0.0484(13) Uani 1 1 d . . . C56 C 0.1606(4) 0.8968(4) 0.1086(3) 0.0603(16) Uani 1 1 d . . . H56A H 0.1727 0.9291 0.0685 0.072 Uiso 1 1 calc R . . C57 C 0.1312(4) 0.9515(5) 0.1602(4) 0.0649(17) Uani 1 1 d . . . H57A H 0.1244 1.0209 0.1559 0.078 Uiso 1 1 calc R . . C58 C 0.1121(4) 0.9009(4) 0.2188(3) 0.0605(16) Uani 1 1 d . . . H58A H 0.0916 0.9359 0.2544 0.073 Uiso 1 1 calc R . . C59 C 0.1239(3) 0.7987(4) 0.2237(3) 0.0446(12) Uani 1 1 d . . . C60 C 0.1087(3) 0.7387(4) 0.2859(3) 0.0451(12) Uani 1 1 d . . . C61 C 0.0472(3) 0.7650(5) 0.3272(3) 0.0547(15) Uani 1 1 d . . . H61A H 0.0147 0.8239 0.3179 0.066 Uiso 1 1 calc R . . C62 C 0.0361(4) 0.7018(5) 0.3817(3) 0.0553(15) Uani 1 1 d . . . H62A H -0.0046 0.7177 0.4096 0.066 Uiso 1 1 calc R . . C63 C 0.0851(3) 0.6150(5) 0.3950(3) 0.0509(14) Uani 1 1 d . . . H63A H 0.0775 0.5710 0.4313 0.061 Uiso 1 1 calc R . . C64 C 0.1462(3) 0.5951(4) 0.3526(3) 0.0408(11) Uani 1 1 d . . . C65 C 0.2071(3) 0.5082(4) 0.3666(2) 0.0375(11) Uani 1 1 d . . . C66 C 0.1788(3) 0.4121(4) 0.3797(3) 0.0480(13) Uani 1 1 d . . . H66A H 0.1203 0.4010 0.3814 0.058 Uiso 1 1 calc R . . C67 C 0.2364(4) 0.3344(4) 0.3900(3) 0.0513(13) Uani 1 1 d . . . H67A H 0.2180 0.2693 0.3970 0.062 Uiso 1 1 calc R . . C68 C 0.3240(4) 0.3548(4) 0.3898(3) 0.0490(14) Uani 1 1 d . . . H68A H 0.3651 0.3031 0.3967 0.059 Uiso 1 1 calc R . . C69 C 0.3494(3) 0.4514(4) 0.3793(3) 0.0384(11) Uani 1 1 d . . . C70 C 0.4432(3) 0.4795(4) 0.3841(3) 0.0387(11) Uani 1 1 d . . . C71 C 0.5091(4) 0.4092(4) 0.3946(3) 0.0571(15) Uani 1 1 d . . . H71A H 0.4961 0.3416 0.3999 0.069 Uiso 1 1 calc R . . C72 C 0.5957(4) 0.4391(4) 0.3973(3) 0.0542(14) Uani 1 1 d . . . H72A H 0.6410 0.3922 0.4045 0.065 Uiso 1 1 calc R . . C73 C 0.6122(3) 0.5390(4) 0.3889(3) 0.0431(12) Uani 1 1 d . . . C74 C 0.5429(3) 0.6086(4) 0.3802(2) 0.0375(11) Uani 1 1 d . . . C75 C 0.5622(3) 0.7191(4) 0.3711(3) 0.0424(12) Uani 1 1 d . . . H75A H 0.5321 0.7398 0.3231 0.051 Uiso 1 1 calc R . . C76 C 0.5309(4) 0.7866(4) 0.4254(3) 0.0545(14) Uani 1 1 d . . . H76A H 0.4691 0.7775 0.4218 0.082 Uiso 1 1 calc R . . H76B H 0.5426 0.8556 0.4157 0.082 Uiso 1 1 calc R . . H76C H 0.5613 0.7692 0.4728 0.082 Uiso 1 1 calc R . . C77 C 0.6614(3) 0.7337(4) 0.3763(3) 0.0528(14) Uani 1 1 d . . . H77A H 0.6798 0.8038 0.3730 0.063 Uiso 1 1 calc R . . C78 C 0.7017(3) 0.5817(4) 0.3929(3) 0.0513(13) Uani 1 1 d . . . H78A H 0.7502 0.5334 0.4015 0.062 Uiso 1 1 calc R . . C79 C 0.7119(4) 0.6754(5) 0.4430(3) 0.0605(15) Uani 1 1 d . . . H79A H 0.7719 0.6974 0.4596 0.073 Uiso 1 1 calc R . . H79B H 0.6809 0.6704 0.4822 0.073 Uiso 1 1 calc R . . C80 C 0.7003(3) 0.6589(5) 0.3290(3) 0.0520(12) Uani 1 1 d . . . C81 C 0.6460(4) 0.6351(5) 0.2552(3) 0.0620(16) Uani 1 1 d . . . H81A H 0.6512 0.6892 0.2229 0.093 Uiso 1 1 calc R . . H81B H 0.5857 0.6273 0.2584 0.093 Uiso 1 1 calc R . . H81C H 0.6668 0.5739 0.2377 0.093 Uiso 1 1 calc R . . C82 C 0.7956(4) 0.6880(5) 0.3217(4) 0.078(2) Uani 1 1 d . . . H82A H 0.7930 0.7353 0.2832 0.117 Uiso 1 1 calc R . . H82B H 0.8263 0.6287 0.3118 0.117 Uiso 1 1 calc R . . H82C H 0.8260 0.7179 0.3656 0.117 Uiso 1 1 calc R . . Cu1 Cu 0.34239(4) 0.65884(4) 0.34046(3) 0.04508(17) Uani 1 1 d . . . Cu2 Cu 0.17942(4) 0.59870(5) 0.19276(4) 0.0564(2) Uani 1 1 d . . . F1 F 0.0276(5) 0.0014(4) 0.3784(4) 0.161(3) Uani 1 1 d . . . F2 F -0.0276(5) 0.1379(9) 0.3331(4) 0.231(4) Uani 1 1 d . . . F3 F 0.1082(5) 0.1167(7) 0.3442(6) 0.219(4) Uani 1 1 d . . . F4 F 0.0615(5) 0.2216(4) 0.4115(7) 0.237(6) Uani 1 1 d . . . F5 F 0.1188(6) 0.0835(7) 0.4526(5) 0.249(5) Uani 1 1 d . . . F6 F -0.0272(4) 0.1159(5) 0.4381(4) 0.180(3) Uani 1 1 d . . . F7 F 0.3390(13) 0.0053(9) 0.0452(10) 0.371(10) Uani 1 1 d . . . F8 F 0.3891(11) 0.0972(9) 0.1344(6) 0.321(7) Uani 1 1 d . . . F9 F 0.3187(17) 0.136(2) 0.009(2) 0.57(2) Uani 1 1 d . . . F10 F 0.4718(12) 0.0207(12) 0.0784(10) 0.363(11) Uani 1 1 d . . . F11 F 0.4417(12) 0.1067(12) -0.0065(8) 0.349(9) Uani 1 1 d . . . F12 F 0.417(2) 0.1897(7) 0.0692(10) 0.56(2) Uani 1 1 d . . . N1 N 0.3302(2) 0.7291(3) 0.4778(2) 0.0394(9) Uani 1 1 d . . . N2 N 0.3250(2) 0.8086(3) 0.3391(2) 0.0366(9) Uani 1 1 d . . . N3 N 0.3599(3) 0.6943(3) 0.2340(2) 0.0414(10) Uani 1 1 d . . . N4 N 0.2801(3) 0.5011(3) 0.1927(2) 0.0412(9) Uani 1 1 d . . . N5 N 0.1084(3) 0.4637(3) 0.1867(2) 0.0430(10) Uani 1 1 d . . . N6 N 0.4600(2) 0.5785(3) 0.3756(2) 0.0347(9) Uani 1 1 d . . . N7 N 0.2918(3) 0.5273(3) 0.3667(2) 0.0373(9) Uani 1 1 d . . . N8 N 0.1565(2) 0.6551(3) 0.29873(19) 0.0375(8) Uani 1 1 d . . . N9 N 0.1536(3) 0.7452(3) 0.1730(2) 0.0432(10) Uani 1 1 d . . . N10 N 0.1705(3) 0.6343(3) 0.0563(2) 0.0505(11) Uani 1 1 d . . . P1 P 0.04253(11) 0.11138(14) 0.39676(13) 0.0771(6) Uani 1 1 d . . . P2 P 0.4014(4) 0.0942(2) 0.0542(3) 0.200(2) 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 C1 0.061(4) 0.051(3) 0.050(3) -0.001(3) 0.014(3) 0.003(3) C2 0.124(6) 0.055(4) 0.062(4) 0.005(3) 0.049(4) 0.009(4) C3 0.077(4) 0.045(3) 0.039(3) 0.003(2) 0.021(3) 0.004(3) C4 0.073(4) 0.048(3) 0.044(3) -0.005(3) 0.027(3) -0.006(3) C5 0.049(3) 0.039(3) 0.044(3) -0.007(2) 0.015(2) 0.002(2) C6 0.044(3) 0.035(3) 0.045(3) -0.007(2) 0.007(2) 0.004(2) C7 0.051(3) 0.046(3) 0.049(3) 0.005(3) 0.010(2) 0.012(3) C8 0.076(4) 0.042(3) 0.042(3) 0.008(2) 0.012(3) 0.009(3) C9 0.082(4) 0.061(4) 0.038(3) -0.002(3) 0.008(3) -0.004(3) C10 0.057(4) 0.068(4) 0.085(4) 0.023(3) 0.016(3) 0.017(3) C11 0.043(3) 0.044(3) 0.060(4) -0.007(3) 0.022(3) 0.005(2) C12 0.043(3) 0.039(3) 0.055(3) -0.001(2) 0.012(3) 0.008(2) C13 0.037(3) 0.030(2) 0.044(3) -0.004(2) 0.007(2) 0.002(2) C14 0.037(3) 0.040(3) 0.048(3) 0.003(2) 0.001(2) 0.004(2) C15 0.058(4) 0.040(3) 0.054(3) 0.000(3) 0.014(3) 0.004(3) C16 0.074(4) 0.034(3) 0.081(5) 0.008(3) 0.010(3) 0.007(3) C17 0.070(4) 0.046(3) 0.059(4) 0.018(3) 0.015(3) 0.007(3) C18 0.039(3) 0.043(3) 0.046(3) 0.011(2) 0.002(2) -0.001(2) C19 0.045(3) 0.044(3) 0.040(3) 0.004(2) 0.006(2) -0.001(2) C20 0.055(4) 0.058(4) 0.062(4) 0.022(3) 0.020(3) -0.003(3) C21 0.066(4) 0.076(4) 0.055(4) 0.020(3) 0.027(3) -0.001(3) C22 0.052(3) 0.078(4) 0.046(3) 0.004(3) 0.017(3) 0.005(3) C23 0.036(3) 0.053(3) 0.034(3) 0.003(2) 0.006(2) 0.004(2) C24 0.048(3) 0.046(3) 0.033(3) 0.000(2) 0.009(2) 0.008(2) C25 0.044(3) 0.066(4) 0.065(4) -0.009(3) 0.011(3) 0.012(3) C26 0.057(4) 0.061(4) 0.068(4) -0.007(3) 0.010(3) 0.019(3) C27 0.069(4) 0.046(3) 0.061(4) -0.005(3) 0.011(3) 0.010(3) C28 0.060(3) 0.041(3) 0.035(3) 0.000(2) 0.011(2) 0.011(3) C29 0.057(3) 0.043(3) 0.046(3) -0.007(2) 0.014(3) 0.002(2) C30 0.076(5) 0.033(3) 0.136(7) -0.015(4) 0.026(5) 0.005(3) C31 0.078(5) 0.038(3) 0.159(8) -0.025(4) 0.028(5) -0.010(3) C32 0.056(4) 0.046(3) 0.095(5) -0.019(3) 0.019(3) -0.010(3) C33 0.047(3) 0.041(3) 0.046(3) -0.001(2) 0.010(2) -0.005(2) C34 0.042(3) 0.043(3) 0.051(3) -0.005(2) 0.008(2) -0.002(2) C35 0.051(3) 0.065(4) 0.071(4) 0.019(3) 0.010(3) 0.000(3) C36 0.042(3) 0.061(3) 0.057(4) -0.001(3) 0.009(3) -0.002(3) C37 0.060(4) 0.075(4) 0.076(4) -0.023(4) 0.000(3) -0.012(3) C38 0.062(4) 0.048(3) 0.105(5) -0.019(4) 0.016(4) -0.017(3) C39 0.049(3) 0.056(3) 0.074(4) 0.004(3) 0.018(3) -0.007(3) C40 0.064(4) 0.080(4) 0.075(4) 0.024(4) 0.024(3) 0.003(3) C41 0.065(4) 0.070(4) 0.130(7) 0.028(4) 0.032(4) -0.005(3) C42 0.171(9) 0.084(5) 0.071(5) -0.010(4) 0.062(5) 0.021(6) C43 0.124(7) 0.086(5) 0.064(5) 0.004(4) 0.010(4) 0.037(5) C44 0.095(5) 0.077(4) 0.045(4) 0.000(3) 0.019(3) 0.014(4) C45 0.099(6) 0.118(6) 0.048(4) -0.016(4) 0.026(4) 0.001(5) C46 0.088(5) 0.078(4) 0.038(3) 0.010(3) 0.029(3) 0.011(4) C47 0.061(3) 0.062(4) 0.042(3) 0.010(3) 0.016(3) 0.004(3) C48 0.068(4) 0.055(4) 0.033(3) 0.006(3) 0.009(3) 0.002(3) C49 0.097(5) 0.060(4) 0.046(3) -0.005(3) 0.020(3) -0.018(3) C50 0.107(6) 0.075(4) 0.046(4) -0.014(3) 0.019(4) -0.016(4) C51 0.108(6) 0.130(7) 0.086(6) -0.038(5) 0.041(5) -0.053(6) C52 0.068(4) 0.064(4) 0.051(4) 0.017(3) 0.022(3) 0.002(3) C53 0.068(4) 0.052(3) 0.052(4) 0.018(3) 0.010(3) 0.004(3) C54 0.048(3) 0.045(3) 0.044(3) 0.010(3) 0.006(2) 0.008(2) C55 0.046(3) 0.049(3) 0.049(3) 0.008(3) 0.006(3) 0.006(2) C56 0.082(4) 0.044(3) 0.052(4) 0.009(3) 0.005(3) 0.006(3) C57 0.078(4) 0.043(3) 0.073(4) 0.011(3) 0.013(3) 0.017(3) C58 0.067(4) 0.050(3) 0.059(4) -0.007(3) 0.001(3) 0.019(3) C59 0.035(3) 0.049(3) 0.045(3) -0.003(2) -0.004(2) 0.006(2) C60 0.038(3) 0.055(3) 0.042(3) -0.012(3) 0.006(2) -0.003(2) C61 0.040(3) 0.064(4) 0.058(4) -0.014(3) 0.007(3) 0.013(3) C62 0.039(3) 0.078(4) 0.050(3) -0.013(3) 0.014(3) 0.002(3) C63 0.035(3) 0.074(4) 0.045(3) -0.004(3) 0.010(2) -0.002(3) C64 0.035(2) 0.044(3) 0.043(3) -0.006(3) 0.006(2) -0.007(2) C65 0.034(3) 0.047(3) 0.032(3) -0.004(2) 0.007(2) -0.008(2) C66 0.045(3) 0.055(3) 0.043(3) 0.006(3) 0.007(2) -0.013(3) C67 0.057(3) 0.045(3) 0.051(3) 0.009(3) 0.007(3) -0.012(3) C68 0.056(4) 0.038(3) 0.052(3) 0.002(3) 0.007(3) -0.002(3) C69 0.044(3) 0.039(3) 0.034(3) -0.001(2) 0.011(2) -0.002(2) C70 0.042(3) 0.037(3) 0.038(3) 0.008(2) 0.009(2) 0.001(2) C71 0.057(4) 0.039(3) 0.075(4) 0.020(3) 0.013(3) 0.014(3) C72 0.047(3) 0.047(3) 0.069(4) 0.018(3) 0.012(3) 0.010(2) C73 0.037(3) 0.050(3) 0.042(3) 0.002(2) 0.006(2) 0.006(2) C74 0.039(3) 0.040(3) 0.033(3) 0.003(2) 0.007(2) 0.002(2) C75 0.030(3) 0.039(3) 0.058(3) -0.003(2) 0.008(2) 0.002(2) C76 0.053(3) 0.044(3) 0.069(4) -0.007(3) 0.018(3) -0.002(2) C77 0.035(3) 0.050(3) 0.076(4) -0.011(3) 0.017(3) -0.012(2) C78 0.031(3) 0.047(3) 0.074(4) 0.003(3) 0.006(2) 0.011(2) C79 0.043(3) 0.068(4) 0.066(4) -0.005(3) -0.001(3) 0.000(3) C80 0.035(3) 0.056(3) 0.068(3) 0.005(3) 0.018(2) 0.001(3) C81 0.059(3) 0.073(4) 0.056(3) 0.001(3) 0.017(3) 0.005(3) C82 0.048(3) 0.069(4) 0.126(6) -0.004(4) 0.043(4) -0.004(3) Cu1 0.0461(4) 0.0344(3) 0.0568(4) 0.0082(3) 0.0152(3) 0.0028(3) Cu2 0.0548(4) 0.0399(4) 0.0785(5) 0.0053(4) 0.0232(4) 0.0065(3) F1 0.202(7) 0.073(3) 0.211(7) -0.040(4) 0.045(5) -0.026(4) F2 0.161(6) 0.323(13) 0.190(7) 0.074(8) -0.008(5) 0.066(8) F3 0.173(6) 0.219(9) 0.306(11) 0.002(8) 0.143(7) -0.011(6) F4 0.127(5) 0.058(3) 0.542(18) -0.016(6) 0.104(8) -0.027(3) F5 0.248(9) 0.184(7) 0.235(9) -0.064(7) -0.144(7) 0.101(7) F6 0.168(5) 0.162(6) 0.251(8) -0.045(6) 0.143(6) -0.049(5) F7 0.51(3) 0.168(10) 0.43(2) 0.019(12) 0.097(19) -0.177(14) F8 0.61(2) 0.179(8) 0.224(10) 0.019(8) 0.200(13) 0.053(13) F9 0.49(3) 0.41(3) 0.71(5) 0.37(4) -0.10(3) -0.02(3) F10 0.50(2) 0.256(13) 0.43(2) 0.198(14) 0.32(2) 0.160(16) F11 0.57(3) 0.290(14) 0.269(13) 0.073(12) 0.271(18) 0.028(18) F12 1.38(7) 0.076(6) 0.330(18) 0.001(8) 0.43(3) -0.030(16) N1 0.041(2) 0.036(2) 0.042(2) 0.0008(19) 0.0117(18) 0.0007(18) N2 0.034(2) 0.041(2) 0.033(2) 0.0037(19) 0.0049(17) 0.0014(18) N3 0.041(2) 0.046(3) 0.037(2) 0.0065(19) 0.0081(19) 0.0035(18) N4 0.045(2) 0.047(2) 0.032(2) -0.0011(18) 0.0106(18) 0.0030(19) N5 0.053(3) 0.038(2) 0.038(2) -0.0018(19) 0.009(2) 0.002(2) N6 0.036(2) 0.031(2) 0.036(2) 0.0011(17) 0.0061(17) 0.0007(16) N7 0.040(2) 0.044(2) 0.028(2) 0.0036(18) 0.0071(18) -0.0023(18) N8 0.038(2) 0.041(2) 0.034(2) -0.003(2) 0.0077(16) -0.001(2) N9 0.040(2) 0.042(2) 0.046(3) -0.005(2) 0.0027(19) 0.0021(19) N10 0.057(3) 0.057(3) 0.037(2) -0.002(2) 0.009(2) 0.003(2) P1 0.0509(9) 0.0516(9) 0.1321(17) 0.0012(11) 0.0261(11) 0.0035(8) P2 0.399(7) 0.0662(18) 0.182(4) 0.037(2) 0.173(5) 0.027(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 C1 C3 1.519(8) . ? C2 C3 1.529(8) . ? C3 C8 1.559(8) . ? C3 C4 1.562(7) . ? C4 C5 1.492(7) . ? C4 C9 1.538(8) . ? C5 C11 1.367(7) . ? C5 C6 1.398(7) . ? C6 N1 1.332(6) . ? C6 C7 1.530(7) . ? C7 C10 1.508(7) . ? C7 C8 1.545(7) . ? C8 C9 1.546(8) . ? C11 C12 1.373(7) . ? C12 C13 1.380(6) . ? C13 N1 1.352(6) . ? C13 C14 1.490(7) . ? C14 N2 1.347(6) . ? C14 C15 1.388(7) . ? C15 C16 1.377(8) . ? C16 C17 1.373(8) . ? C17 C18 1.384(8) . ? C18 N2 1.343(6) . ? C18 C19 1.500(7) . ? C19 N3 1.346(6) . ? C19 C20 1.392(7) . ? C20 C21 1.372(9) . ? C21 C22 1.416(9) . ? C22 C23 1.383(7) . ? C23 N3 1.344(6) . ? C23 C24 1.493(7) . ? C24 N4 1.339(6) . ? C24 C25 1.390(7) . ? C25 C26 1.345(9) . ? C26 C27 1.372(8) . ? C27 C28 1.403(7) . ? C28 N4 1.353(6) . ? C28 C29 1.488(7) . ? C29 N5 1.341(7) . ? C29 C30 1.384(8) . ? C30 C31 1.394(9) . ? C31 C32 1.361(9) . ? C32 C33 1.399(7) . ? C32 C38 1.500(8) . ? C33 N5 1.351(6) . ? C33 C34 1.512(7) . ? C34 C35 1.533(7) . ? C34 C36 1.538(7) . ? C36 C37 1.561(8) . ? C36 C39 1.570(8) . ? C37 C38 1.544(10) . ? C38 C39 1.536(9) . ? C39 C40 1.515(9) . ? C39 C41 1.549(8) . ? C42 C44 1.573(9) . ? C43 C44 1.509(10) . ? C44 C50 1.540(10) . ? C44 C46 1.544(9) . ? C45 C46 1.533(10) . ? C45 C50 1.572(10) . ? C46 C47 1.502(9) . ? C47 C52 1.361(8) . ? C47 C48 1.394(7) . ? C48 N10 1.336(6) . ? C48 C49 1.535(8) . ? C49 C51 1.516(10) . ? C49 C50 1.536(8) . ? C52 C53 1.396(8) . ? C53 C54 1.385(7) . ? C54 N10 1.339(7) . ? C54 C55 1.498(7) . ? C55 N9 1.350(7) . ? C55 C56 1.371(7) . ? C56 C57 1.372(8) . ? C57 C58 1.386(8) . ? C58 C59 1.370(8) . ? C59 N9 1.354(6) . ? C59 C60 1.486(8) . ? C60 N8 1.333(7) . ? C60 C61 1.402(7) . ? C61 C62 1.372(8) . ? C62 C63 1.378(8) . ? C63 C64 1.393(7) . ? C64 N8 1.335(6) . ? C64 C65 1.483(7) . ? C65 N7 1.345(6) . ? C65 C66 1.390(7) . ? C66 C67 1.356(8) . ? C67 C68 1.393(7) . ? C68 C69 1.369(7) . ? C69 N7 1.340(6) . ? C69 C70 1.494(7) . ? C70 N6 1.357(6) . ? C70 C71 1.372(7) . ? C71 C72 1.399(8) . ? C72 C73 1.368(7) . ? C73 C74 1.405(7) . ? C73 C78 1.494(7) . ? C74 N6 1.339(6) . ? C74 C75 1.515(7) . ? C75 C76 1.520(7) . ? C75 C77 1.541(7) . ? C77 C80 1.546(8) . ? C77 C79 1.557(8) . ? C78 C79 1.557(8) . ? C78 C80 1.587(8) . ? C80 C81 1.520(8) . ? C80 C82 1.569(7) . ? Cu1 N2 2.007(4) . ? Cu1 N7 2.020(4) . ? Cu1 N6 2.111(4) . ? Cu1 N3 2.152(4) . ? Cu2 N9 2.007(4) . ? Cu2 N4 2.036(4) . ? Cu2 N5 2.099(4) . ? Cu2 N8 2.247(4) . ? F1 P1 1.509(5) . ? F2 P1 1.501(7) . ? F3 P1 1.572(7) . ? F4 P1 1.508(6) . ? F5 P1 1.473(7) . ? F6 P1 1.466(5) . ? F7 P2 1.518(12) . ? F8 P2 1.577(11) . ? F9 P2 1.51(2) . ? F10 P2 1.471(14) . ? F11 P2 1.432(9) . ? F12 P2 1.311(12) . ? 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 C1 C3 C2 108.5(5) . . ? C1 C3 C8 119.2(5) . . ? C2 C3 C8 111.9(5) . . ? C1 C3 C4 119.5(5) . . ? C2 C3 C4 110.8(4) . . ? C8 C3 C4 85.3(4) . . ? C5 C4 C9 107.0(4) . . ? C5 C4 C3 110.4(4) . . ? C9 C4 C3 87.3(5) . . ? C11 C5 C6 117.5(5) . . ? C11 C5 C4 125.7(5) . . ? C6 C5 C4 116.7(5) . . ? N1 C6 C5 123.1(4) . . ? N1 C6 C7 118.7(4) . . ? C5 C6 C7 118.2(4) . . ? C10 C7 C6 113.5(5) . . ? C10 C7 C8 111.7(5) . . ? C6 C7 C8 109.7(4) . . ? C7 C8 C9 109.1(4) . . ? C7 C8 C3 110.7(4) . . ? C9 C8 C3 87.2(4) . . ? C4 C9 C8 86.6(4) . . ? C5 C11 C12 120.4(5) . . ? C11 C12 C13 118.9(5) . . ? N1 C13 C12 121.8(4) . . ? N1 C13 C14 116.5(4) . . ? C12 C13 C14 121.7(4) . . ? N2 C14 C15 122.0(5) . . ? N2 C14 C13 118.0(4) . . ? C15 C14 C13 120.0(5) . . ? C16 C15 C14 118.6(5) . . ? C17 C16 C15 119.5(5) . . ? C16 C17 C18 119.4(5) . . ? N2 C18 C17 121.6(5) . . ? N2 C18 C19 115.8(4) . . ? C17 C18 C19 122.6(5) . . ? N3 C19 C20 123.5(5) . . ? N3 C19 C18 114.0(4) . . ? C20 C19 C18 122.4(5) . . ? C21 C20 C19 118.1(6) . . ? C20 C21 C22 119.6(5) . . ? C23 C22 C21 117.8(6) . . ? N3 C23 C22 123.2(5) . . ? N3 C23 C24 116.5(4) . . ? C22 C23 C24 120.2(5) . . ? N4 C24 C25 122.1(5) . . ? N4 C24 C23 117.1(4) . . ? C25 C24 C23 120.7(5) . . ? C26 C25 C24 119.4(6) . . ? C25 C26 C27 120.0(5) . . ? C26 C27 C28 119.1(6) . . ? N4 C28 C27 120.7(5) . . ? N4 C28 C29 116.3(4) . . ? C27 C28 C29 122.8(5) . . ? N5 C29 C30 121.4(5) . . ? N5 C29 C28 117.2(5) . . ? C30 C29 C28 121.4(5) . . ? C29 C30 C31 119.5(6) . . ? C32 C31 C30 119.0(6) . . ? C31 C32 C33 119.4(5) . . ? C31 C32 C38 123.5(6) . . ? C33 C32 C38 117.0(5) . . ? N5 C33 C32 121.3(5) . . ? N5 C33 C34 120.5(4) . . ? C32 C33 C34 118.2(5) . . ? C33 C34 C35 115.2(4) . . ? C33 C34 C36 109.5(4) . . ? C35 C34 C36 109.3(4) . . ? C34 C36 C37 108.6(5) . . ? C34 C36 C39 113.4(5) . . ? C37 C36 C39 87.2(5) . . ? C38 C37 C36 84.7(5) . . ? C32 C38 C39 110.3(5) . . ? C32 C38 C37 107.0(6) . . ? C39 C38 C37 88.9(5) . . ? C40 C39 C38 118.7(5) . . ? C40 C39 C41 109.4(5) . . ? C38 C39 C41 111.1(5) . . ? C40 C39 C36 118.9(5) . . ? C38 C39 C36 84.7(4) . . ? C41 C39 C36 112.1(5) . . ? C43 C44 C50 119.2(6) . . ? C43 C44 C46 120.0(6) . . ? C50 C44 C46 85.7(5) . . ? C43 C44 C42 108.2(6) . . ? C50 C44 C42 110.4(6) . . ? C46 C44 C42 111.8(5) . . ? C46 C45 C50 84.9(5) . . ? C47 C46 C45 107.4(5) . . ? C47 C46 C44 109.0(5) . . ? C45 C46 C44 88.5(6) . . ? C52 C47 C48 117.8(6) . . ? C52 C47 C46 125.4(5) . . ? C48 C47 C46 116.8(6) . . ? N10 C48 C47 123.7(5) . . ? N10 C48 C49 117.7(5) . . ? C47 C48 C49 118.6(5) . . ? C51 C49 C48 113.7(6) . . ? C51 C49 C50 112.7(5) . . ? C48 C49 C50 108.6(5) . . ? C49 C50 C44 112.8(5) . . ? C49 C50 C45 109.0(6) . . ? C44 C50 C45 87.3(5) . . ? C47 C52 C53 120.0(5) . . ? C54 C53 C52 117.8(6) . . ? N10 C54 C53 123.1(5) . . ? N10 C54 C55 116.4(4) . . ? C53 C54 C55 120.4(5) . . ? N9 C55 C56 121.3(5) . . ? N9 C55 C54 115.3(4) . . ? C56 C55 C54 123.2(5) . . ? C55 C56 C57 120.5(6) . . ? C56 C57 C58 118.4(6) . . ? C59 C58 C57 119.1(6) . . ? N9 C59 C58 122.2(5) . . ? N9 C59 C60 114.8(5) . . ? C58 C59 C60 123.0(5) . . ? N8 C60 C61 121.7(5) . . ? N8 C60 C59 114.9(4) . . ? C61 C60 C59 123.4(5) . . ? C62 C61 C60 118.5(5) . . ? C61 C62 C63 120.1(5) . . ? C62 C63 C64 118.1(5) . . ? N8 C64 C63 122.4(5) . . ? N8 C64 C65 115.5(4) . . ? C63 C64 C65 122.1(5) . . ? N7 C65 C66 121.4(5) . . ? N7 C65 C64 116.5(4) . . ? C66 C65 C64 122.2(4) . . ? C67 C66 C65 120.0(5) . . ? C66 C67 C68 118.2(5) . . ? C69 C68 C67 119.7(5) . . ? N7 C69 C68 121.9(5) . . ? N7 C69 C70 115.8(4) . . ? C68 C69 C70 122.2(5) . . ? N6 C70 C71 121.3(4) . . ? N6 C70 C69 116.4(4) . . ? C71 C70 C69 122.2(4) . . ? C70 C71 C72 120.1(5) . . ? C73 C72 C71 118.3(5) . . ? C72 C73 C74 119.6(5) . . ? C72 C73 C78 123.9(5) . . ? C74 C73 C78 116.4(5) . . ? N6 C74 C73 121.3(5) . . ? N6 C74 C75 119.5(4) . . ? C73 C74 C75 119.0(4) . . ? C74 C75 C76 113.3(4) . . ? C74 C75 C77 109.5(4) . . ? C76 C75 C77 109.7(4) . . ? C75 C77 C80 112.9(4) . . ? C75 C77 C79 109.0(5) . . ? C80 C77 C79 87.8(4) . . ? C73 C78 C79 108.2(4) . . ? C73 C78 C80 109.8(4) . . ? C79 C78 C80 86.4(4) . . ? C78 C79 C77 85.7(4) . . ? C81 C80 C77 117.5(4) . . ? C81 C80 C82 109.3(5) . . ? C77 C80 C82 112.6(5) . . ? C81 C80 C78 119.5(5) . . ? C77 C80 C78 85.1(4) . . ? C82 C80 C78 111.1(5) . . ? N2 Cu1 N7 143.28(17) . . ? N2 Cu1 N6 127.72(15) . . ? N7 Cu1 N6 80.90(15) . . ? N2 Cu1 N3 79.24(16) . . ? N7 Cu1 N3 123.54(16) . . ? N6 Cu1 N3 98.18(15) . . ? N9 Cu2 N4 137.97(17) . . ? N9 Cu2 N5 137.28(17) . . ? N4 Cu2 N5 81.58(16) . . ? N9 Cu2 N8 77.48(17) . . ? N4 Cu2 N8 118.33(15) . . ? N5 Cu2 N8 99.03(15) . . ? C6 N1 C13 118.2(4) . . ? C18 N2 C14 118.9(4) . . ? C18 N2 Cu1 115.9(3) . . ? C14 N2 Cu1 125.2(3) . . ? C23 N3 C19 117.7(4) . . ? C23 N3 Cu1 126.7(3) . . ? C19 N3 Cu1 110.5(3) . . ? C24 N4 C28 118.7(4) . . ? C24 N4 Cu2 128.0(4) . . ? C28 N4 Cu2 113.3(3) . . ? C29 N5 C33 119.4(4) . . ? C29 N5 Cu2 111.4(3) . . ? C33 N5 Cu2 129.3(3) . . ? C74 N6 C70 119.3(4) . . ? C74 N6 Cu1 129.4(3) . . ? C70 N6 Cu1 110.6(3) . . ? C69 N7 C65 118.7(4) . . ? C69 N7 Cu1 114.5(3) . . ? C65 N7 Cu1 126.5(3) . . ? C60 N8 C64 119.3(4) . . ? C60 N8 Cu2 107.3(3) . . ? C64 N8 Cu2 123.9(3) . . ? C55 N9 C59 118.5(5) . . ? C55 N9 Cu2 123.8(3) . . ? C59 N9 Cu2 117.4(3) . . ? C48 N10 C54 117.3(5) . . ? F6 P1 F5 101.6(6) . . ? F6 P1 F2 85.8(5) . . ? F5 P1 F2 172.6(6) . . ? F6 P1 F4 89.9(4) . . ? F5 P1 F4 90.6(6) . . ? F2 P1 F4 90.3(6) . . ? F6 P1 F1 93.9(4) . . ? F5 P1 F1 89.3(5) . . ? F2 P1 F1 89.3(6) . . ? F4 P1 F1 176.1(5) . . ? F6 P1 F3 171.5(6) . . ? F5 P1 F3 86.4(6) . . ? F2 P1 F3 86.4(5) . . ? F4 P1 F3 86.9(5) . . ? F1 P1 F3 89.2(4) . . ? F12 P2 F11 88.5(10) . . ? F12 P2 F10 119(2) . . ? F11 P2 F10 84.8(9) . . ? F12 P2 F9 82.1(14) . . ? F11 P2 F9 87.4(14) . . ? F10 P2 F9 157.3(19) . . ? F12 P2 F7 149.4(18) . . ? F11 P2 F7 112.1(10) . . ? F10 P2 F7 86.5(9) . . ? F9 P2 F7 76.7(13) . . ? F12 P2 F8 79.4(8) . . ? F11 P2 F8 159.5(11) . . ? F10 P2 F8 86.7(8) . . ? F9 P2 F8 106.9(18) . . ? F7 P2 F8 85.9(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.726 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.060