Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author 'Prof. Robert P. Houser' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Oklahoma 620 Parrington Oval, Room 208 Norman, OK 73019-3051 USA ; _publ_contact_author_email houser@ou.edu _publ_contact_author_fax 1(405)3256111 _publ_contact_author_phone 1(405)3253551 loop_ _publ_author_name _publ_author_address 'Laura R. Whiteaker' . 'Lei Yang.' . U.P.Chaudhuri ; Department of Chemistry and Biochemistry University of Oklahoma 620 Parrington Oval, Room 208 Norman, OK 73019-3051 USA ; R.P.Houser ; Department of Chemistry and Biochemistry University of Oklahoma 620 Parrington Oval, Room 208 Norman, OK 73019-3051 USA ; _publ_section_title ; Multinuclear Copper Complexes of Pyridylmethylamide Ligands ; _publ_section_references ; Bruker (1998) SMART and SAINT, Bruker AXS, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2002) SADABS. Version 2.03. University of G\"ottingen, Germany Sheldrick, G. M. (2000) SHELXTL. Version 6.10. Bruker AXS, Inc., Madison, Wisconsin, USA. van der Sluis, P. and Spek, A. L. (1990) Acta Cryst., A46, 194-201. ; _publ_section_acknowledgements ; The authors wish to thank the National Science Foundation (CHE-0130835) and the University of Oklahoma for funds to acquire the diffractometer and computers used in this work. ; _publ_contact_author_name 'Prof. Robert P. Houser' data_bh4154 _database_code_depnum_ccdc_archive 'CCDC 285146' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C56 H54 Cu4 N8 O6) 2+, (Cl O4)2 1-, (C2 H3 N)2, (H2 O)3 ; _chemical_formula_sum 'C60 H66 Cl2 Cu4 N10 O17' _chemical_formula_weight 1524.29 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 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.218(8) _cell_length_b 17.377(3) _cell_length_c 26.792(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.224(5) _cell_angle_gamma 90.00 _cell_volume 19134(6) _cell_formula_units_Z 12 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.23 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9384 _exptl_absorpt_coefficient_mu 1.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(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 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104083 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18806 _reflns_number_gt 16688 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL (Sheldrick, 2002)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2002)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2002)' _computing_publication_material 'SHELXTL (Sheldrick, 2002)' _refine_special_details ; Several solvent groups were severely disordered and were found to be best modeled using the Squeeze program. ; _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^)+(0.0680P)^2^+28.0000P] 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_number_reflns 18806 _refine_ls_number_parameters 1264 _refine_ls_number_restraints 513 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _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 Cu1A Cu 0.291576(6) 0.536594(15) 0.550945(10) 0.02306(7) Uani 1 1 d . . . Cu2A Cu 0.363212(7) 0.520320(16) 0.591457(10) 0.02561(7) Uani 1 1 d . . . Cu3A Cu 0.303136(7) 0.390539(16) 0.617725(11) 0.02712(8) Uani 1 1 d . . . Cu4A Cu 0.343909(7) 0.459603(17) 0.481514(10) 0.02612(7) Uani 1 1 d . . . O1A O 0.32333(4) 0.49285(9) 0.61352(6) 0.0251(3) Uani 1 1 d . . . H1AO H 0.3198 0.5336 0.6322 0.030 Uiso 1 1 d R . . O2A O 0.33048(4) 0.54130(9) 0.52418(6) 0.0255(3) Uani 1 1 d . . . H2AO H 0.3343 0.5906 0.5170 0.031 Uiso 1 1 d R . . N1A N 0.26443(5) 0.60352(11) 0.49769(7) 0.0256(4) Uani 1 1 d . . . C2A C 0.27012(6) 0.62192(14) 0.45166(9) 0.0298(5) Uani 1 1 d . . . H2A H 0.2888 0.6014 0.4422 0.036 Uiso 1 1 calc R . . C3A C 0.24951(6) 0.66979(15) 0.41780(9) 0.0336(5) Uani 1 1 d . . . H3A H 0.2540 0.6824 0.3856 0.040 Uiso 1 1 calc R . . C4A C 0.22223(7) 0.69906(15) 0.43168(9) 0.0355(5) Uani 1 1 d . . . H4A H 0.2077 0.7319 0.4089 0.043 Uiso 1 1 calc R . . C5A C 0.21635(6) 0.68024(15) 0.47870(9) 0.0334(5) Uani 1 1 d . . . H5A H 0.1977 0.6999 0.4887 0.040 Uiso 1 1 calc R . . C6A C 0.23804(6) 0.63214(13) 0.51129(9) 0.0268(5) Uani 1 1 d . . . C7A C 0.23346(6) 0.60929(13) 0.56358(9) 0.0282(5) Uani 1 1 d . . . H7AA H 0.2384 0.6536 0.5873 0.034 Uiso 1 1 calc R . . H7AB H 0.2106 0.5936 0.5611 0.034 Uiso 1 1 calc R . . N8A N 0.25523(5) 0.54553(11) 0.58298(7) 0.0254(4) Uani 1 1 d . . . C9A C 0.24969(6) 0.50138(13) 0.61958(9) 0.0275(5) Uani 1 1 d . . . O10A O 0.26652(4) 0.44197(9) 0.63585(6) 0.0300(4) Uani 1 1 d . . . C11A C 0.22201(7) 0.52109(15) 0.64537(10) 0.0364(6) Uani 1 1 d . . . H11A H 0.2250 0.5744 0.6585 0.044 Uiso 1 1 calc R . . H11B H 0.2012 0.5192 0.6193 0.044 Uiso 1 1 calc R . . C12A C 0.21974(6) 0.46798(14) 0.68900(10) 0.0320(5) Uani 1 1 d . . . C13A C 0.24114(7) 0.47580(15) 0.73650(10) 0.0361(6) Uani 1 1 d . . . H13A H 0.2572 0.5152 0.7416 0.043 Uiso 1 1 calc R . . C14A C 0.23928(7) 0.42653(17) 0.77654(10) 0.0400(6) Uani 1 1 d . . . H14A H 0.2539 0.4327 0.8090 0.048 Uiso 1 1 calc R . . C15A C 0.21628(7) 0.36858(16) 0.76933(10) 0.0378(6) Uani 1 1 d . . . H15A H 0.2152 0.3345 0.7966 0.045 Uiso 1 1 calc R . . C16A C 0.19492(7) 0.36040(15) 0.72249(10) 0.0367(6) Uani 1 1 d . . . H16A H 0.1790 0.3209 0.7175 0.044 Uiso 1 1 calc R . . C17A C 0.19664(6) 0.40988(16) 0.68240(10) 0.0356(5) Uani 1 1 d . . . H17A H 0.1818 0.4038 0.6501 0.043 Uiso 1 1 calc R . . N1B N 0.39057(5) 0.54941(12) 0.65942(8) 0.0323(4) Uani 1 1 d . . . C2B C 0.38330(7) 0.53873(17) 0.70544(10) 0.0396(6) Uani 1 1 d . . . H2B H 0.3648 0.5085 0.7072 0.048 Uiso 1 1 calc R . . C3B C 0.40156(8) 0.5698(2) 0.74967(11) 0.0484(7) Uani 1 1 d . . . H3B H 0.3958 0.5615 0.7815 0.058 Uiso 1 1 calc R . . C4B C 0.42843(8) 0.61345(19) 0.74723(11) 0.0517(8) Uani 1 1 d . . . H4B H 0.4414 0.6357 0.7775 0.062 Uiso 1 1 calc R . . C5B C 0.43635(8) 0.62463(19) 0.70054(11) 0.0490(7) Uani 1 1 d . . . H5B H 0.4548 0.6547 0.6982 0.059 Uiso 1 1 calc R . . C6B C 0.41688(6) 0.59104(16) 0.65676(10) 0.0376(6) Uani 1 1 d . . . C7B C 0.42442(7) 0.59892(17) 0.60512(10) 0.0404(6) Uani 1 1 d . . . H7BA H 0.4246 0.6540 0.5958 0.049 Uiso 1 1 calc R . . H7BB H 0.4463 0.5774 0.6060 0.049 Uiso 1 1 calc R . . N8B N 0.40007(5) 0.55812(12) 0.56695(8) 0.0309(4) Uani 1 1 d . . . C9B C 0.40355(6) 0.55291(15) 0.51954(10) 0.0326(5) Uani 1 1 d . . . O10B O 0.38386(4) 0.51637(10) 0.48468(6) 0.0334(4) Uani 1 1 d . . . C11B C 0.43173(7) 0.5925(2) 0.50328(11) 0.0473(7) Uani 1 1 d . . . H11C H 0.4284 0.6488 0.5039 0.057 Uiso 1 1 calc R . . H11D H 0.4521 0.5804 0.5288 0.057 Uiso 1 1 calc R . . C12B C 0.43589(7) 0.57004(18) 0.45104(11) 0.0429(6) Uani 1 1 d . . . C13B C 0.41505(9) 0.5935(2) 0.40734(12) 0.0592(9) Uani 1 1 d . . . H13B H 0.3968 0.6246 0.4091 0.071 Uiso 1 1 calc R . . C14B C 0.42047(10) 0.5719(3) 0.36002(15) 0.0843(15) Uani 1 1 d . . . H14B H 0.4060 0.5886 0.3294 0.101 Uiso 1 1 calc R . . C15B C 0.44677(10) 0.5261(3) 0.35738(19) 0.0895(18) Uani 1 1 d . . . H15B H 0.4506 0.5123 0.3249 0.107 Uiso 1 1 calc R . . C16B C 0.46661(11) 0.5017(3) 0.3997(2) 0.0826(14) Uani 1 1 d . . . H16B H 0.4846 0.4697 0.3980 0.099 Uiso 1 1 calc R . . C17B C 0.46114(10) 0.5229(2) 0.44657(18) 0.0718(11) Uani 1 1 d . . . H17B H 0.4754 0.5042 0.4769 0.086 Uiso 1 1 calc R . . N1C N 0.28973(5) 0.29452(11) 0.64935(8) 0.0301(4) Uani 1 1 d . . . C2C C 0.26445(6) 0.28762(15) 0.67170(11) 0.0376(6) Uani 1 1 d . . . H2C H 0.2495 0.3291 0.6694 0.045 Uiso 1 1 calc R . . C3C C 0.25948(7) 0.22242(16) 0.69781(13) 0.0448(7) Uani 1 1 d . . . H3C H 0.2417 0.2193 0.7140 0.054 Uiso 1 1 calc R . . C4C C 0.28082(7) 0.16110(16) 0.70029(12) 0.0441(7) Uani 1 1 d . . . H4C H 0.2776 0.1151 0.7176 0.053 Uiso 1 1 calc R . . C5C C 0.30658(6) 0.16773(15) 0.67747(11) 0.0377(6) Uani 1 1 d . . . H5C H 0.3214 0.1263 0.6786 0.045 Uiso 1 1 calc R . . C6C C 0.31067(6) 0.23599(14) 0.65269(9) 0.0313(5) Uani 1 1 d . . . C7C C 0.33911(7) 0.24716(15) 0.62933(11) 0.0393(6) Uani 1 1 d . . . H7CA H 0.3595 0.2411 0.6560 0.047 Uiso 1 1 calc R . . H7CB H 0.3388 0.2074 0.6028 0.047 Uiso 1 1 calc R . . N8C N 0.33835(5) 0.32363(11) 0.60617(8) 0.0306(4) Uani 1 1 d . . . C9C C 0.36099(6) 0.33981(14) 0.58116(9) 0.0298(5) Uani 1 1 d . . . O10C O 0.36265(4) 0.40415(9) 0.55975(6) 0.0282(3) Uani 1 1 d . . . C11C C 0.38713(7) 0.27963(16) 0.57880(11) 0.0397(6) Uani 1 1 d . . . H11E H 0.3973 0.2634 0.6143 0.048 Uiso 1 1 calc R . . H11F H 0.3763 0.2339 0.5604 0.048 Uiso 1 1 calc R . . C12C C 0.41360(7) 0.30426(17) 0.55350(12) 0.0433(6) Uani 1 1 d . . . C13C C 0.41951(8) 0.2621(2) 0.51224(12) 0.0521(8) Uani 1 1 d . . . H13C H 0.4062 0.2191 0.4996 0.063 Uiso 1 1 calc R . . C14C C 0.44472(9) 0.2824(3) 0.48944(14) 0.0643(10) Uani 1 1 d . . . H14C H 0.4486 0.2532 0.4615 0.077 Uiso 1 1 calc R . . C15C C 0.46390(10) 0.3444(3) 0.50716(19) 0.0749(12) Uani 1 1 d . . . H15C H 0.4812 0.3579 0.4916 0.090 Uiso 1 1 calc R . . C16C C 0.45828(10) 0.3869(2) 0.5470(2) 0.0781(13) Uani 1 1 d . . . H16C H 0.4716 0.4302 0.5589 0.094 Uiso 1 1 calc R . . C17C C 0.43318(8) 0.3672(2) 0.57039(16) 0.0594(9) Uani 1 1 d . . . H17C H 0.4295 0.3972 0.5981 0.071 Uiso 1 1 calc R . . N1D N 0.35536(5) 0.39893(12) 0.42520(7) 0.0303(4) Uani 1 1 d . . . C2D C 0.38546(6) 0.38981(16) 0.41736(9) 0.0339(5) Uani 1 1 d . . . H2D H 0.4034 0.4106 0.4416 0.041 Uiso 1 1 calc R . . C3D C 0.39108(6) 0.35114(17) 0.37520(10) 0.0379(6) Uani 1 1 d . . . H3D H 0.4126 0.3447 0.3707 0.045 Uiso 1 1 calc R . . C4D C 0.36482(7) 0.32213(18) 0.33982(10) 0.0413(6) Uani 1 1 d . . . H4D H 0.3680 0.2959 0.3103 0.050 Uiso 1 1 calc R . . C5D C 0.33386(7) 0.33145(19) 0.34761(10) 0.0440(7) Uani 1 1 d . . . H5D H 0.3155 0.3121 0.3235 0.053 Uiso 1 1 calc R . . C6D C 0.33004(6) 0.36964(17) 0.39138(9) 0.0357(6) Uani 1 1 d . . . C7D C 0.29721(6) 0.3823(2) 0.40308(10) 0.0435(7) Uani 1 1 d . . . H7DA H 0.2849 0.4210 0.3792 0.052 Uiso 1 1 calc R . . H7DB H 0.2847 0.3336 0.3984 0.052 Uiso 1 1 calc R . . N8D N 0.30149(5) 0.40917(13) 0.45604(8) 0.0325(4) Uani 1 1 d . . . C9D C 0.27774(6) 0.39952(13) 0.47990(9) 0.0275(5) Uani 1 1 d . . . O10D O 0.28052(4) 0.41711(9) 0.52642(6) 0.0259(3) Uani 1 1 d . . . C11D C 0.24494(6) 0.36707(16) 0.44991(10) 0.0356(6) Uani 1 1 d . . . H11G H 0.2373 0.3985 0.4186 0.043 Uiso 1 1 calc R . . H11H H 0.2484 0.3140 0.4388 0.043 Uiso 1 1 calc R . . C12D C 0.21861(6) 0.36540(15) 0.47940(10) 0.0334(5) Uani 1 1 d . . . C13D C 0.20663(7) 0.29556(18) 0.49196(13) 0.0472(7) Uani 1 1 d . . . H13D H 0.2156 0.2488 0.4830 0.057 Uiso 1 1 calc R . . C14D C 0.18161(8) 0.2936(2) 0.51762(14) 0.0589(9) Uani 1 1 d . . . H14D H 0.1734 0.2457 0.5262 0.071 Uiso 1 1 calc R . . C15D C 0.16863(8) 0.3614(3) 0.53059(13) 0.0660(11) Uani 1 1 d . . . H15D H 0.1519 0.3601 0.5490 0.079 Uiso 1 1 calc R . . C16D C 0.17990(8) 0.4318(2) 0.51688(15) 0.0630(10) Uani 1 1 d . . . H16D H 0.1705 0.4785 0.5249 0.076 Uiso 1 1 calc R . . C17D C 0.20492(7) 0.43304(18) 0.49149(13) 0.0461(7) Uani 1 1 d . . . H17D H 0.2128 0.4809 0.4822 0.055 Uiso 1 1 calc R . . Cu1B Cu 0.536322(7) 0.903014(17) 0.763336(13) 0.03244(8) Uani 1 1 d . . . Cu2B Cu 0.513021(8) 1.01454(2) 0.675091(13) 0.03838(9) Uani 1 1 d . . . O1B O 0.49887(4) 0.91625(10) 0.70079(7) 0.0350(4) Uani 1 1 d . . . H1BO H 0.4987 0.8778 0.6782 0.042 Uiso 1 1 d R . . N1E N 0.56973(5) 0.85909(13) 0.82110(10) 0.0393(5) Uani 1 1 d . . . C2E C 0.56975(7) 0.86057(18) 0.87109(12) 0.0473(7) Uani 1 1 d . . . H2E H 0.5533 0.8887 0.8820 0.057 Uiso 1 1 calc R . . C3E C 0.59301(8) 0.8225(2) 0.90723(14) 0.0566(8) Uani 1 1 d . . . H3E H 0.5926 0.8243 0.9425 0.068 Uiso 1 1 calc R . . C4E C 0.61703(8) 0.7816(2) 0.89115(16) 0.0622(9) Uani 1 1 d . . . H4E H 0.6331 0.7542 0.9152 0.075 Uiso 1 1 calc R . . C5E C 0.61734(7) 0.78116(18) 0.84011(14) 0.0524(8) Uani 1 1 d . . . H5E H 0.6338 0.7541 0.8285 0.063 Uiso 1 1 calc R . . C6E C 0.59325(6) 0.82078(15) 0.80538(12) 0.0424(6) Uani 1 1 d . . . C7E C 0.59261(6) 0.82313(16) 0.74949(12) 0.0432(6) Uani 1 1 d . . . H7EA H 0.6143 0.8379 0.7445 0.052 Uiso 1 1 calc R . . H7EB H 0.5872 0.7715 0.7343 0.052 Uiso 1 1 calc R . . N8E N 0.56840(5) 0.87863(13) 0.72410(10) 0.0377(5) Uani 1 1 d . . . C9E C 0.56994(6) 0.91038(16) 0.68061(12) 0.0412(6) Uani 1 1 d . A . O10E O 0.55004(5) 0.96087(12) 0.65796(8) 0.0442(5) Uani 1 1 d . . . C11E C 0.59675(7) 0.88704(18) 0.65357(14) 0.0571(9) Uani 1 1 d D . . H11I H 0.5910 0.8366 0.6367 0.069 Uiso 0.532(6) 1 calc PR A 1 H11J H 0.6174 0.8805 0.6796 0.069 Uiso 0.532(6) 1 calc PR A 1 H11K H 0.5934 0.8342 0.6432 0.069 Uiso 0.468(6) 1 d PR A 2 H11L H 0.6173 0.8902 0.6779 0.069 Uiso 0.468(6) 1 d PR A 2 C12E C 0.60219(8) 0.9452(2) 0.61339(16) 0.0427(14) Uani 0.532(6) 1 d PDU A 1 C13E C 0.58656(13) 0.9418(3) 0.56230(16) 0.0626(16) Uani 0.532(6) 1 d PDU A 1 H13E H 0.5714 0.9017 0.5504 0.075 Uiso 0.532(6) 1 calc PR A 1 C14E C 0.59279(16) 0.9963(4) 0.52827(18) 0.0664(18) Uani 0.532(6) 1 d PDU A 1 H14E H 0.5819 0.9929 0.4931 0.080 Uiso 0.532(6) 1 calc PR A 1 C15E C 0.61453(14) 1.0558(3) 0.5443(2) 0.0621(16) Uani 0.532(6) 1 d PDU A 1 H15E H 0.6185 1.0934 0.5208 0.075 Uiso 0.532(6) 1 calc PR A 1 C16E C 0.63028(12) 1.0590(3) 0.5957(2) 0.0514(14) Uani 0.532(6) 1 d PDU A 1 H16E H 0.6454 1.0990 0.6077 0.062 Uiso 0.532(6) 1 calc PR A 1 C17E C 0.62403(12) 1.0043(3) 0.62940(19) 0.0397(13) Uani 0.532(6) 1 d PDU A 1 H17E H 0.6350 1.0073 0.6645 0.048 Uiso 0.532(6) 1 calc PR A 1 C12' C 0.59799(9) 0.9335(2) 0.60777(18) 0.0399(15) Uani 0.468(6) 1 d PDU A 2 C13' C 0.57934(14) 0.9101(4) 0.56085(17) 0.0642(18) Uani 0.468(6) 1 d PDU A 2 H13' H 0.5662 0.8653 0.5585 0.077 Uiso 0.468(6) 1 calc PR A 2 C14' C 0.58002(16) 0.9523(4) 0.51744(18) 0.0715(19) Uani 0.468(6) 1 d PDU A 2 H14' H 0.5674 0.9368 0.4849 0.086 Uiso 0.468(6) 1 calc PR A 2 C15' C 0.59922(16) 1.0173(4) 0.5218(2) 0.0545(17) Uani 0.468(6) 1 d PDU A 2 H15' H 0.5995 1.0465 0.4919 0.065 Uiso 0.468(6) 1 calc PR A 2 C16' C 0.61805(16) 1.0408(3) 0.5685(2) 0.0601(16) Uani 0.468(6) 1 d PDU A 2 H16' H 0.6313 1.0855 0.5707 0.072 Uiso 0.468(6) 1 calc PR A 2 C17' C 0.61736(14) 0.9985(3) 0.6120(2) 0.0447(15) Uani 0.468(6) 1 d PDU A 2 H17' H 0.6301 1.0139 0.6445 0.054 Uiso 0.468(6) 1 calc PR A 2 N1F N 0.52608(6) 1.10978(16) 0.64307(11) 0.0528(7) Uani 1 1 d . . . C2F C 0.55580(9) 1.1272(2) 0.63670(16) 0.0661(10) Uani 1 1 d . . . H2F H 0.5730 1.0914 0.6474 0.079 Uiso 1 1 calc R . . C3F C 0.56216(10) 1.1963(3) 0.61483(18) 0.0800(13) Uani 1 1 d . . . H3F H 0.5835 1.2085 0.6117 0.096 Uiso 1 1 calc R . . C4F C 0.53671(11) 1.2469(3) 0.59776(19) 0.0820(13) Uani 1 1 d . . . H4F H 0.5404 1.2937 0.5816 0.098 Uiso 1 1 calc R . . C5F C 0.50622(10) 1.2295(2) 0.60411(16) 0.0721(11) Uani 1 1 d . . . H5F H 0.4886 1.2641 0.5929 0.087 Uiso 1 1 calc R . . C6F C 0.50167(8) 1.1606(2) 0.62709(14) 0.0584(9) Uani 1 1 d . . . C7F C 0.46887(8) 1.1368(2) 0.63429(15) 0.0621(10) Uani 1 1 d . . . H7FA H 0.4574 1.1818 0.6444 0.075 Uiso 1 1 calc R . . H7FB H 0.4556 1.1159 0.6018 0.075 Uiso 1 1 calc R . . N8F N 0.47354(6) 1.07776(15) 0.67463(10) 0.0443(6) Uani 1 1 d . . . C9F C 0.45359(6) 1.07254(15) 0.70490(11) 0.0373(6) Uani 1 1 d . . . O10F O 0.45803(4) 1.02552(10) 0.74205(7) 0.0364(4) Uani 1 1 d . . . C11F C 0.42229(7) 1.11985(17) 0.69819(14) 0.0477(7) Uani 1 1 d . . . H11M H 0.4220 1.1474 0.7304 0.057 Uiso 1 1 calc R . . H11N H 0.4213 1.1585 0.6708 0.057 Uiso 1 1 calc R . . C12F C 0.39329(6) 1.06668(16) 0.68430(12) 0.0421(6) Uani 1 1 d . . . C13F C 0.37896(7) 1.03769(17) 0.72227(12) 0.0431(6) Uani 1 1 d . . . H13F H 0.3874 1.0524 0.7569 0.052 Uiso 1 1 calc R . . C14F C 0.35267(7) 0.98769(18) 0.71056(14) 0.0501(7) Uani 1 1 d . . . H14F H 0.3429 0.9692 0.7369 0.060 Uiso 1 1 calc R . . C15F C 0.34085(8) 0.9652(2) 0.66075(15) 0.0573(9) Uani 1 1 d . . . H15F H 0.3231 0.9304 0.6525 0.069 Uiso 1 1 calc R . . C16F C 0.35473(9) 0.9931(3) 0.62269(15) 0.0677(10) Uani 1 1 d . . . H16F H 0.3465 0.9773 0.5882 0.081 Uiso 1 1 calc R . . C17F C 0.38083(8) 1.0445(2) 0.63423(13) 0.0567(8) Uani 1 1 d . . . H17F H 0.3900 1.0641 0.6076 0.068 Uiso 1 1 calc R . . Cl1G Cl 0.306275(14) 0.65780(3) 0.68716(2) 0.03159(13) Uani 1 1 d . . . O1G O 0.30721(5) 0.57817(11) 0.70286(8) 0.0474(5) Uani 1 1 d . . . O2G O 0.31766(5) 0.66064(10) 0.64022(7) 0.0369(4) Uani 1 1 d . . . O3G O 0.27350(5) 0.68671(11) 0.67764(8) 0.0433(4) Uani 1 1 d . . . O4G O 0.32712(5) 0.70432(12) 0.72504(7) 0.0453(5) Uani 1 1 d . . . Cl1H Cl 0.34878(2) 0.72323(5) 0.45408(3) 0.0550(2) Uani 1 1 d . . . O1H O 0.34249(5) 0.69634(11) 0.50157(8) 0.0436(4) Uani 1 1 d . . . O2H O 0.32898(8) 0.78894(16) 0.43732(12) 0.0821(10) Uani 1 1 d . . . O3H O 0.38232(7) 0.74309(16) 0.46183(14) 0.0839(9) Uani 1 1 d . . . O4H O 0.34039(7) 0.66202(16) 0.41652(9) 0.0683(7) Uani 1 1 d . . . Cl1I Cl 0.50860(10) 0.71728(19) 0.62808(13) 0.0396(7) Uani 0.499(5) 1 d PDU B 1 O1I O 0.49044(12) 0.7796(3) 0.6415(3) 0.093(2) Uani 0.499(5) 1 d PDU B 1 O2I O 0.54176(11) 0.7389(5) 0.6347(3) 0.058(2) Uani 0.499(5) 1 d PDU B 1 O3I O 0.49503(16) 0.6970(4) 0.57609(15) 0.0698(19) Uani 0.499(5) 1 d PDU B 1 O4I O 0.50568(13) 0.6531(3) 0.6597(2) 0.085(2) Uani 0.499(5) 1 d PDU B 1 Cl1' Cl 0.50992(10) 0.73447(19) 0.63556(15) 0.0443(8) Uani 0.501(5) 1 d PDU B 2 O1I' O 0.50619(12) 0.8129(2) 0.61968(16) 0.0549(13) Uani 0.501(5) 1 d PDU B 2 O2I' O 0.54341(12) 0.7147(4) 0.6441(3) 0.058(2) Uani 0.501(5) 1 d PDU B 2 O3I' O 0.49096(17) 0.6864(4) 0.5973(3) 0.090(2) Uani 0.501(5) 1 d PDU B 2 O4I' O 0.49963(14) 0.7292(4) 0.68239(18) 0.0823(18) Uani 0.501(5) 1 d PDU B 2 N1S N 0.48284(9) 0.9830(3) 0.57190(16) 0.0884(12) Uani 1 1 d . . . C2S C 0.48449(10) 0.9366(3) 0.54446(14) 0.0687(10) Uani 1 1 d . . . C3S C 0.48518(15) 0.8766(3) 0.50671(18) 0.1041(18) Uani 1 1 d . . . H3S1 H 0.4632 0.8686 0.4857 0.156 Uiso 1 1 calc R . . H3S2 H 0.4932 0.8286 0.5244 0.156 Uiso 1 1 calc R . . H3S3 H 0.4997 0.8922 0.4847 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1A 0.02712(14) 0.02126(14) 0.02126(13) 0.00207(10) 0.00646(11) 0.00320(10) Cu2A 0.02774(15) 0.02592(15) 0.02220(14) -0.00186(10) 0.00369(11) 0.00106(11) Cu3A 0.03282(16) 0.02047(14) 0.02980(15) 0.00373(11) 0.01073(12) 0.00611(11) Cu4A 0.02513(14) 0.03167(15) 0.02179(14) -0.00407(11) 0.00586(11) -0.00239(11) O1A 0.0318(8) 0.0216(7) 0.0221(7) -0.0003(6) 0.0065(6) 0.0041(6) O2A 0.0282(8) 0.0243(8) 0.0242(8) 0.0019(6) 0.0063(6) 0.0009(6) N1A 0.0310(10) 0.0224(9) 0.0225(9) 0.0005(7) 0.0041(8) 0.0017(7) C2A 0.0347(12) 0.0279(12) 0.0258(11) 0.0002(9) 0.0049(9) 0.0006(10) C3A 0.0421(14) 0.0340(13) 0.0226(11) 0.0039(10) 0.0028(10) -0.0003(11) C4A 0.0432(14) 0.0317(13) 0.0282(12) 0.0068(10) 0.0009(10) 0.0062(11) C5A 0.0373(13) 0.0312(13) 0.0309(12) 0.0046(10) 0.0061(10) 0.0092(10) C6A 0.0325(12) 0.0215(10) 0.0262(11) -0.0014(9) 0.0059(9) 0.0007(9) C7A 0.0350(12) 0.0228(11) 0.0280(11) 0.0044(9) 0.0100(9) 0.0073(9) N8A 0.0305(10) 0.0218(9) 0.0247(9) 0.0026(7) 0.0077(8) 0.0059(8) C9A 0.0337(12) 0.0238(11) 0.0263(11) 0.0020(9) 0.0094(9) 0.0026(9) O10A 0.0376(9) 0.0239(8) 0.0315(9) 0.0069(7) 0.0142(7) 0.0081(7) C11A 0.0424(14) 0.0326(13) 0.0395(14) 0.0111(11) 0.0201(11) 0.0122(11) C12A 0.0370(13) 0.0286(12) 0.0357(13) 0.0061(10) 0.0194(11) 0.0087(10) C13A 0.0445(15) 0.0293(12) 0.0383(14) -0.0004(10) 0.0175(11) -0.0021(11) C14A 0.0467(15) 0.0424(15) 0.0315(13) 0.0026(11) 0.0103(11) -0.0028(12) C15A 0.0471(15) 0.0361(14) 0.0333(13) 0.0070(11) 0.0154(11) 0.0002(11) C16A 0.0416(14) 0.0324(13) 0.0394(14) 0.0017(11) 0.0164(11) -0.0018(11) C17A 0.0364(13) 0.0398(14) 0.0321(13) 0.0020(11) 0.0105(10) 0.0038(11) N1B 0.0329(11) 0.0341(11) 0.0268(10) -0.0027(8) 0.0006(8) 0.0073(9) C2B 0.0379(14) 0.0514(16) 0.0279(12) -0.0015(11) 0.0040(10) 0.0103(12) C3B 0.0489(17) 0.0619(19) 0.0304(14) -0.0069(13) 0.0006(12) 0.0142(15) C4B 0.0552(18) 0.0559(19) 0.0349(15) -0.0146(13) -0.0086(13) 0.0082(15) C5B 0.0463(16) 0.0535(18) 0.0406(16) -0.0125(13) -0.0037(13) -0.0032(14) C6B 0.0353(13) 0.0374(14) 0.0358(14) -0.0064(11) -0.0011(11) 0.0026(11) C7B 0.0359(14) 0.0449(15) 0.0380(14) -0.0078(12) 0.0033(11) -0.0096(11) N8B 0.0286(10) 0.0331(11) 0.0294(10) -0.0036(8) 0.0034(8) -0.0032(8) C9B 0.0299(12) 0.0326(13) 0.0342(13) 0.0003(10) 0.0053(10) -0.0025(10) O10B 0.0301(9) 0.0399(10) 0.0304(9) -0.0044(7) 0.0071(7) -0.0076(7) C11B 0.0457(16) 0.0581(18) 0.0378(15) -0.0010(13) 0.0088(12) -0.0221(14) C12B 0.0343(14) 0.0479(16) 0.0490(16) -0.0078(13) 0.0150(12) -0.0146(12) C13B 0.0528(19) 0.085(3) 0.0404(17) -0.0096(16) 0.0121(14) 0.0032(17) C14B 0.057(2) 0.152(5) 0.0449(19) -0.028(2) 0.0132(17) -0.018(3) C15B 0.053(2) 0.137(4) 0.091(3) -0.080(3) 0.043(2) -0.044(3) C16B 0.061(2) 0.083(3) 0.119(4) -0.023(3) 0.053(3) -0.006(2) C17B 0.056(2) 0.079(3) 0.090(3) 0.014(2) 0.039(2) 0.0023(19) N1C 0.0324(10) 0.0235(10) 0.0330(10) 0.0016(8) 0.0045(8) 0.0016(8) C2C 0.0312(13) 0.0275(12) 0.0534(16) 0.0043(11) 0.0078(11) 0.0004(10) C3C 0.0335(14) 0.0338(14) 0.0687(19) 0.0120(13) 0.0148(13) -0.0032(11) C4C 0.0395(15) 0.0298(13) 0.0610(18) 0.0120(12) 0.0075(13) -0.0028(11) C5C 0.0367(13) 0.0253(12) 0.0485(15) 0.0061(11) 0.0047(11) 0.0032(10) C6C 0.0326(12) 0.0263(12) 0.0321(12) 0.0010(10) 0.0013(10) 0.0025(9) C7C 0.0465(15) 0.0272(12) 0.0473(15) 0.0112(11) 0.0170(12) 0.0129(11) N8C 0.0374(11) 0.0245(10) 0.0308(10) 0.0042(8) 0.0095(8) 0.0088(8) C9C 0.0343(12) 0.0255(11) 0.0283(11) -0.0019(9) 0.0044(9) 0.0055(9) O10C 0.0341(9) 0.0254(8) 0.0251(8) -0.0001(6) 0.0068(7) 0.0046(7) C11C 0.0432(15) 0.0310(13) 0.0481(15) 0.0063(11) 0.0169(12) 0.0117(11) C12C 0.0388(14) 0.0372(14) 0.0562(17) 0.0098(13) 0.0154(13) 0.0136(12) C13C 0.0425(16) 0.068(2) 0.0466(17) 0.0101(15) 0.0112(13) 0.0155(15) C14C 0.054(2) 0.086(3) 0.058(2) 0.0223(19) 0.0244(16) 0.0236(19) C15C 0.054(2) 0.074(3) 0.105(3) 0.041(2) 0.035(2) 0.019(2) C16C 0.055(2) 0.057(2) 0.130(4) 0.013(2) 0.037(2) 0.0010(18) C17C 0.0502(18) 0.0449(18) 0.086(3) -0.0021(17) 0.0222(17) 0.0044(14) N1D 0.0294(10) 0.0371(11) 0.0251(10) -0.0037(8) 0.0073(8) -0.0002(8) C2D 0.0307(12) 0.0421(14) 0.0279(12) -0.0023(10) 0.0045(10) 0.0017(10) C3D 0.0327(13) 0.0513(16) 0.0307(13) -0.0047(11) 0.0095(10) 0.0056(11) C4D 0.0402(14) 0.0553(17) 0.0296(13) -0.0123(12) 0.0103(11) 0.0029(12) C5D 0.0355(14) 0.0643(19) 0.0318(13) -0.0178(13) 0.0073(11) -0.0047(13) C6D 0.0304(12) 0.0497(15) 0.0275(12) -0.0091(11) 0.0076(10) -0.0013(11) C7D 0.0315(13) 0.071(2) 0.0297(13) -0.0187(13) 0.0104(10) -0.0063(13) N8D 0.0275(10) 0.0443(12) 0.0263(10) -0.0114(9) 0.0073(8) -0.0044(9) C9D 0.0269(11) 0.0266(11) 0.0286(12) -0.0052(9) 0.0055(9) -0.0011(9) O10D 0.0283(8) 0.0231(8) 0.0269(8) -0.0025(6) 0.0077(6) 0.0011(6) C11D 0.0298(12) 0.0434(14) 0.0341(13) -0.0122(11) 0.0082(10) -0.0060(11) C12D 0.0269(12) 0.0393(14) 0.0334(13) -0.0082(11) 0.0056(10) -0.0055(10) C13D 0.0372(15) 0.0430(16) 0.0624(19) 0.0028(14) 0.0131(13) -0.0058(12) C14D 0.0430(17) 0.074(2) 0.062(2) 0.0126(18) 0.0168(15) -0.0119(16) C15D 0.0385(16) 0.117(3) 0.0474(18) -0.022(2) 0.0208(14) -0.0238(19) C16D 0.0359(16) 0.077(2) 0.080(2) -0.045(2) 0.0209(16) -0.0070(16) C17D 0.0342(14) 0.0414(15) 0.0642(19) -0.0173(14) 0.0147(13) -0.0070(12) Cu1B 0.02124(14) 0.02770(15) 0.04854(19) -0.00117(13) 0.00827(13) 0.00050(11) Cu2B 0.02861(16) 0.04109(19) 0.04818(19) 0.00640(14) 0.01444(14) 0.00481(13) O1B 0.0246(8) 0.0346(9) 0.0464(10) -0.0060(8) 0.0096(7) -0.0005(7) N1E 0.0263(10) 0.0314(11) 0.0577(14) -0.0032(10) 0.0044(10) -0.0011(9) C2E 0.0374(15) 0.0462(16) 0.0535(18) -0.0075(14) 0.0006(13) 0.0007(12) C3E 0.0488(18) 0.056(2) 0.0573(19) -0.0030(16) -0.0039(15) 0.0000(15) C4E 0.0467(18) 0.0491(19) 0.078(3) 0.0032(17) -0.0126(17) 0.0075(14) C5E 0.0332(14) 0.0425(16) 0.076(2) -0.0015(15) 0.0006(14) 0.0086(12) C6E 0.0281(13) 0.0305(13) 0.0658(19) -0.0050(13) 0.0047(12) 0.0001(10) C7E 0.0281(13) 0.0358(14) 0.0664(19) -0.0021(13) 0.0122(12) 0.0046(11) N8E 0.0218(10) 0.0325(11) 0.0597(15) -0.0056(10) 0.0109(9) 0.0007(8) C9E 0.0287(13) 0.0360(14) 0.0625(18) -0.0059(13) 0.0179(12) -0.0031(11) O10E 0.0326(10) 0.0476(12) 0.0569(12) 0.0023(9) 0.0193(9) 0.0030(8) C11E 0.0450(17) 0.0463(17) 0.092(3) -0.0011(17) 0.0393(18) 0.0004(14) C12E 0.029(2) 0.057(3) 0.042(3) -0.017(2) 0.009(2) 0.004(2) C13E 0.044(3) 0.077(3) 0.061(3) -0.036(3) 0.000(2) 0.004(3) C14E 0.063(3) 0.086(4) 0.051(3) 0.004(3) 0.016(3) 0.015(3) C15E 0.063(3) 0.081(4) 0.047(3) 0.016(3) 0.021(3) 0.032(3) C16E 0.043(3) 0.063(3) 0.056(3) 0.004(3) 0.026(2) 0.009(2) C17E 0.029(2) 0.057(3) 0.036(3) -0.006(2) 0.011(2) -0.001(2) C12' 0.025(2) 0.055(3) 0.039(3) -0.020(2) 0.008(2) -0.002(2) C13' 0.050(3) 0.078(4) 0.058(3) -0.033(3) -0.001(3) -0.002(3) C14' 0.066(4) 0.087(4) 0.057(3) -0.011(3) 0.007(3) 0.015(3) C15' 0.057(3) 0.071(4) 0.043(3) 0.024(3) 0.025(3) 0.019(3) C16' 0.057(3) 0.079(3) 0.049(3) 0.013(3) 0.021(3) 0.016(3) C17' 0.035(3) 0.059(3) 0.042(3) -0.002(3) 0.014(3) -0.002(3) N1F 0.0412(14) 0.0541(16) 0.0676(17) 0.0201(13) 0.0221(12) 0.0071(12) C2F 0.0489(19) 0.065(2) 0.091(3) 0.024(2) 0.0300(18) 0.0027(17) C3F 0.062(2) 0.086(3) 0.100(3) 0.030(3) 0.036(2) -0.007(2) C4F 0.078(3) 0.072(3) 0.102(3) 0.038(2) 0.031(2) 0.003(2) C5F 0.068(2) 0.072(3) 0.080(3) 0.032(2) 0.026(2) 0.014(2) C6F 0.0512(18) 0.064(2) 0.064(2) 0.0246(17) 0.0209(16) 0.0105(16) C7F 0.0467(18) 0.073(2) 0.071(2) 0.0353(19) 0.0219(16) 0.0202(16) N8F 0.0342(12) 0.0459(14) 0.0543(14) 0.0157(11) 0.0131(10) 0.0101(10) C9F 0.0284(12) 0.0301(13) 0.0544(16) -0.0019(12) 0.0116(11) 0.0005(10) O10F 0.0321(9) 0.0292(9) 0.0496(11) 0.0023(8) 0.0125(8) 0.0019(7) C11F 0.0373(15) 0.0328(14) 0.077(2) 0.0102(14) 0.0214(14) 0.0086(12) C12F 0.0306(13) 0.0344(14) 0.0609(18) 0.0065(13) 0.0100(12) 0.0125(11) C13F 0.0352(14) 0.0422(15) 0.0518(17) 0.0074(13) 0.0100(12) 0.0092(11) C14F 0.0355(15) 0.0443(16) 0.069(2) 0.0105(15) 0.0096(14) 0.0051(12) C15F 0.0386(16) 0.0492(18) 0.081(2) -0.0017(17) 0.0071(16) 0.0051(13) C16F 0.051(2) 0.084(3) 0.061(2) -0.016(2) -0.0022(17) 0.0102(19) C17F 0.0451(17) 0.076(2) 0.0506(18) 0.0084(16) 0.0136(14) 0.0159(16) Cl1G 0.0342(3) 0.0245(3) 0.0343(3) 0.0014(2) 0.0042(2) 0.0051(2) O1G 0.0583(13) 0.0332(10) 0.0536(12) 0.0142(9) 0.0187(10) 0.0080(9) O2G 0.0433(10) 0.0336(9) 0.0330(9) -0.0030(7) 0.0074(8) 0.0010(8) O3G 0.0369(10) 0.0388(10) 0.0525(12) -0.0063(9) 0.0067(9) 0.0084(8) O4G 0.0496(11) 0.0494(12) 0.0319(9) -0.0103(8) -0.0010(8) 0.0030(9) Cl1H 0.0664(5) 0.0463(4) 0.0649(5) 0.0195(4) 0.0409(4) 0.0168(4) O1H 0.0581(12) 0.0324(10) 0.0421(11) 0.0045(8) 0.0149(9) 0.0009(9) O2H 0.109(2) 0.0642(16) 0.095(2) 0.0448(15) 0.0698(18) 0.0412(16) O3H 0.0736(18) 0.0544(15) 0.144(3) 0.0099(16) 0.0677(19) 0.0045(13) O4H 0.0909(19) 0.0747(17) 0.0475(13) 0.0031(12) 0.0329(13) 0.0229(14) Cl1I 0.0273(10) 0.0475(14) 0.0419(10) -0.0152(10) 0.0036(7) 0.0085(10) O1I 0.050(3) 0.084(4) 0.139(5) -0.058(4) 0.006(3) 0.025(3) O2I 0.031(3) 0.066(4) 0.074(5) -0.019(4) 0.010(3) -0.001(2) O3I 0.063(4) 0.107(5) 0.038(3) -0.009(3) 0.007(2) -0.023(3) O4I 0.058(3) 0.101(4) 0.088(4) 0.032(3) -0.003(3) -0.007(3) Cl1' 0.0341(11) 0.0450(14) 0.0574(16) 0.0006(12) 0.0179(11) 0.0059(10) O1I' 0.068(3) 0.048(3) 0.043(2) -0.0001(19) 0.002(2) 0.021(2) O2I' 0.043(3) 0.079(5) 0.051(3) 0.009(3) 0.010(2) 0.031(3) O3I' 0.062(4) 0.098(5) 0.110(6) -0.039(5) 0.021(4) -0.033(3) O4I' 0.075(3) 0.097(4) 0.094(4) 0.003(3) 0.057(3) -0.001(3) N1S 0.068(2) 0.125(3) 0.075(2) -0.016(2) 0.0218(19) -0.005(2) C2S 0.059(2) 0.103(3) 0.0438(19) 0.005(2) 0.0105(16) 0.012(2) C3S 0.139(5) 0.114(4) 0.065(3) 0.005(3) 0.033(3) 0.043(4) _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 Cu1A N8A 1.9282(19) . ? Cu1A O2A 1.9384(16) . ? Cu1A N1A 1.9884(19) . ? Cu1A O1A 2.0390(16) . ? Cu1A O10D 2.1955(16) . ? Cu1A Cu2A 2.9838(7) . ? Cu1A Cu3A 3.0792(6) . ? Cu2A N8B 1.937(2) . ? Cu2A O1A 1.9664(16) . ? Cu2A N1B 1.986(2) . ? Cu2A O2A 2.0375(16) . ? Cu2A O10C 2.1881(16) . ? Cu2A Cu4A 3.0587(6) . ? Cu3A O10A 1.9412(16) . ? Cu3A N8C 1.967(2) . ? Cu3A O1A 1.9861(16) . ? Cu3A N1C 2.010(2) . ? Cu4A O10B 1.9391(17) . ? Cu4A N8D 1.970(2) . ? Cu4A O2A 1.9850(16) . ? Cu4A N1D 1.989(2) . ? Cu4A O10C 2.2781(16) . ? O1A H1AO 0.9001 . ? O2A H2AO 0.9001 . ? N1A C6A 1.344(3) . ? N1A C2A 1.348(3) . ? C2A C3A 1.383(3) . ? C2A H2A 0.9500 . ? C3A C4A 1.385(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.378(4) . ? C4A H4A 0.9500 . ? C5A C6A 1.391(3) . ? C5A H5A 0.9500 . ? C6A C7A 1.510(3) . ? C7A N8A 1.457(3) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? N8A C9A 1.307(3) . ? C9A O10A 1.272(3) . ? C9A C11A 1.526(3) . ? C11A C12A 1.510(3) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A C17A 1.387(4) . ? C12A C13A 1.388(4) . ? C13A C14A 1.389(4) . ? C13A H13A 0.9500 . ? C14A C15A 1.381(4) . ? C14A H14A 0.9500 . ? C15A C16A 1.375(4) . ? C15A H15A 0.9500 . ? C16A C17A 1.391(4) . ? C16A H16A 0.9500 . ? C17A H17A 0.9500 . ? N1B C6B 1.341(4) . ? N1B C2B 1.350(3) . ? C2B C3B 1.369(4) . ? C2B H2B 0.9500 . ? C3B C4B 1.378(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.380(5) . ? C4B H4B 0.9500 . ? C5B C6B 1.397(4) . ? C5B H5B 0.9500 . ? C6B C7B 1.495(4) . ? C7B N8B 1.458(3) . ? C7B H7BA 0.9900 . ? C7B H7BB 0.9900 . ? N8B C9B 1.315(3) . ? C9B O10B 1.269(3) . ? C9B C11B 1.521(4) . ? C11B C12B 1.501(4) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B C13B 1.357(5) . ? C12B C17B 1.371(5) . ? C13B C14B 1.391(5) . ? C13B H13B 0.9500 . ? C14B C15B 1.380(7) . ? C14B H14B 0.9500 . ? C15B C16B 1.317(7) . ? C15B H15B 0.9500 . ? C16B C17B 1.377(6) . ? C16B H16B 0.9500 . ? C17B H17B 0.9500 . ? N1C C6C 1.337(3) . ? N1C C2C 1.343(3) . ? C2C C3C 1.373(4) . ? C2C H2C 0.9500 . ? C3C C4C 1.387(4) . ? C3C H3C 0.9500 . ? C4C C5C 1.369(4) . ? C4C H4C 0.9500 . ? C5C C6C 1.389(4) . ? C5C H5C 0.9500 . ? C6C C7C 1.488(4) . ? C7C N8C 1.464(3) . ? C7C H7CA 0.9900 . ? C7C H7CB 0.9900 . ? N8C C9C 1.317(3) . ? C9C O10C 1.266(3) . ? C9C C11C 1.532(3) . ? C11C C12C 1.496(4) . ? C11C H11E 0.9900 . ? C11C H11F 0.9900 . ? C12C C17C 1.383(5) . ? C12C C13C 1.395(4) . ? C13C C14C 1.389(5) . ? C13C H13C 0.9500 . ? C14C C15C 1.365(6) . ? C14C H14C 0.9500 . ? C15C C16C 1.362(6) . ? C15C H15C 0.9500 . ? C16C C17C 1.392(5) . ? C16C H16C 0.9500 . ? C17C H17C 0.9500 . ? N1D C6D 1.334(3) . ? N1D C2D 1.344(3) . ? C2D C3D 1.381(4) . ? C2D H2D 0.9500 . ? C3D C4D 1.379(4) . ? C3D H3D 0.9500 . ? C4D C5D 1.379(4) . ? C4D H4D 0.9500 . ? C5D C6D 1.388(4) . ? C5D H5D 0.9500 . ? C6D C7D 1.506(3) . ? C7D N8D 1.465(3) . ? C7D H7DA 0.9900 . ? C7D H7DB 0.9900 . ? N8D C9D 1.317(3) . ? C9D O10D 1.262(3) . ? C9D C11D 1.540(3) . ? C11D C12D 1.504(3) . ? C11D H11G 0.9900 . ? C11D H11H 0.9900 . ? C12D C17D 1.381(4) . ? C12D C13D 1.386(4) . ? C13D C14D 1.386(4) . ? C13D H13D 0.9500 . ? C14D C15D 1.377(6) . ? C14D H14D 0.9500 . ? C15D C16D 1.392(6) . ? C15D H15D 0.9500 . ? C16D C17D 1.381(4) . ? C16D H16D 0.9500 . ? C17D H17D 0.9500 . ? Cu1B N8E 1.942(2) . ? Cu1B O1B 1.9589(18) 2_656 ? Cu1B N1E 1.992(2) . ? Cu1B O1B 2.0369(18) . ? Cu1B O10F 2.1506(18) 2_656 ? Cu1B Cu1B 2.9856(8) 2_656 ? Cu1B Cu2B 3.0413(6) . ? Cu2B O10E 1.9623(19) . ? Cu2B O1B 1.9841(19) . ? Cu2B N8F 1.994(2) . ? Cu2B N1F 1.999(3) . ? Cu2B O10F 2.284(2) 2_656 ? O1B Cu1B 1.9590(18) 2_656 ? O1B H1BO 0.8999 . ? N1E C2E 1.339(4) . ? N1E C6E 1.341(4) . ? C2E C3E 1.380(4) . ? C2E H2E 0.9500 . ? C3E C4E 1.385(5) . ? C3E H3E 0.9500 . ? C4E C5E 1.371(5) . ? C4E H4E 0.9500 . ? C5E C6E 1.393(4) . ? C5E H5E 0.9500 . ? C6E C7E 1.492(4) . ? C7E N8E 1.456(3) . ? C7E H7EA 0.9900 . ? C7E H7EB 0.9900 . ? N8E C9E 1.304(4) . ? C9E O10E 1.269(4) . ? C9E C11E 1.531(4) . ? C11E C12' 1.480(6) . ? C11E C12E 1.532(6) . ? C11E H11I 0.9900 . ? C11E H11J 0.9900 . ? C11E H11K 0.9600 . ? C11E H11L 0.9599 . ? C12E C13E 1.378(3) . ? C12E C17E 1.381(3) . ? C13E C14E 1.381(3) . ? C13E H13E 0.9500 . ? C14E C15E 1.384(3) . ? C14E H14E 0.9500 . ? C15E C16E 1.385(3) . ? C15E H15E 0.9500 . ? C16E C17E 1.378(3) . ? C16E H16E 0.9500 . ? C17E H17E 0.9500 . ? C12' C13' 1.383(3) . ? C12' C17' 1.383(3) . ? C13' C14' 1.381(3) . ? C13' H13' 0.9500 . ? C14' C15' 1.379(4) . ? C14' H14' 0.9500 . ? C15' C16' 1.383(3) . ? C15' H15' 0.9500 . ? C16' C17' 1.384(3) . ? C16' H16' 0.9500 . ? C17' H17' 0.9500 . ? N1F C2F 1.339(4) . ? N1F C6F 1.350(4) . ? C2F C3F 1.388(5) . ? C2F H2F 0.9500 . ? C3F C4F 1.383(6) . ? C3F H3F 0.9500 . ? C4F C5F 1.370(6) . ? C4F H4F 0.9500 . ? C5F C6F 1.380(5) . ? C5F H5F 0.9500 . ? C6F C7F 1.499(5) . ? C7F N8F 1.471(4) . ? C7F H7FA 0.9900 . ? C7F H7FB 0.9900 . ? N8F C9F 1.299(4) . ? C9F O10F 1.268(3) . ? C9F C11F 1.532(4) . ? O10F Cu1B 2.1506(18) 2_656 ? O10F Cu2B 2.284(2) 2_656 ? C11F C12F 1.511(4) . ? C11F H11M 0.9900 . ? C11F H11N 0.9900 . ? C12F C17F 1.379(5) . ? C12F C13F 1.391(4) . ? C13F C14F 1.388(4) . ? C13F H13F 0.9500 . ? C14F C15F 1.370(5) . ? C14F H14F 0.9500 . ? C15F C16F 1.375(6) . ? C15F H15F 0.9500 . ? C16F C17F 1.397(5) . ? C16F H16F 0.9500 . ? C17F H17F 0.9500 . ? Cl1G O4G 1.432(2) . ? Cl1G O3G 1.4389(19) . ? Cl1G O1G 1.444(2) . ? Cl1G O2G 1.4461(19) . ? Cl1H O3H 1.426(3) . ? Cl1H O2H 1.426(3) . ? Cl1H O1H 1.436(2) . ? Cl1H O4H 1.451(3) . ? Cl1I O1I 1.421(3) . ? Cl1I O2I 1.421(3) . ? Cl1I O4I 1.424(3) . ? Cl1I O3I 1.424(3) . ? Cl1' O3I' 1.420(3) . ? Cl1' O4I' 1.421(3) . ? Cl1' O2I' 1.422(3) . ? Cl1' O1I' 1.427(3) . ? N1S C2S 1.105(6) . ? C2S C3S 1.457(7) . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? 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 N8A Cu1A O2A 171.57(8) . . ? N8A Cu1A N1A 83.42(8) . . ? O2A Cu1A N1A 96.20(7) . . ? N8A Cu1A O1A 96.01(7) . . ? O2A Cu1A O1A 82.32(6) . . ? N1A Cu1A O1A 166.09(7) . . ? N8A Cu1A O10D 94.19(7) . . ? O2A Cu1A O10D 93.97(6) . . ? N1A Cu1A O10D 106.87(7) . . ? O1A Cu1A O10D 87.04(6) . . ? N8A Cu1A Cu2A 133.58(6) . . ? O2A Cu1A Cu2A 42.64(5) . . ? N1A Cu1A Cu2A 133.35(6) . . ? O1A Cu1A Cu2A 40.93(5) . . ? O10D Cu1A Cu2A 98.49(4) . . ? N8A Cu1A Cu3A 81.04(6) . . ? O2A Cu1A Cu3A 102.40(5) . . ? N1A Cu1A Cu3A 152.59(6) . . ? O1A Cu1A Cu3A 39.46(5) . . ? O10D Cu1A Cu3A 52.34(4) . . ? Cu2A Cu1A Cu3A 72.409(10) . . ? N8B Cu2A O1A 173.56(8) . . ? N8B Cu2A N1B 83.14(9) . . ? O1A Cu2A N1B 98.31(8) . . ? N8B Cu2A O2A 94.26(8) . . ? O1A Cu2A O2A 81.68(6) . . ? N1B Cu2A O2A 154.17(8) . . ? N8B Cu2A O10C 96.86(8) . . ? O1A Cu2A O10C 87.63(6) . . ? N1B Cu2A O10C 122.90(7) . . ? O2A Cu2A O10C 82.92(6) . . ? N8B Cu2A Cu1A 132.11(6) . . ? O1A Cu2A Cu1A 42.79(5) . . ? N1B Cu2A Cu1A 129.64(6) . . ? O2A Cu2A Cu1A 40.13(4) . . ? O10C Cu2A Cu1A 91.50(4) . . ? N8B Cu2A Cu4A 81.27(6) . . ? O1A Cu2A Cu4A 98.50(5) . . ? N1B Cu2A Cu4A 160.37(6) . . ? O2A Cu2A Cu4A 39.87(4) . . ? O10C Cu2A Cu4A 48.02(4) . . ? Cu1A Cu2A Cu4A 69.988(10) . . ? O10A Cu3A N8C 170.22(8) . . ? O10A Cu3A O1A 88.79(7) . . ? N8C Cu3A O1A 99.82(8) . . ? O10A Cu3A N1C 87.68(8) . . ? N8C Cu3A N1C 82.62(8) . . ? O1A Cu3A N1C 158.87(7) . . ? O10A Cu3A Cu1A 74.72(5) . . ? N8C Cu3A Cu1A 114.89(6) . . ? O1A Cu3A Cu1A 40.73(4) . . ? N1C Cu3A Cu1A 155.02(6) . . ? O10B Cu4A N8D 162.58(8) . . ? O10B Cu4A O2A 88.34(7) . . ? N8D Cu4A O2A 99.26(8) . . ? O10B Cu4A N1D 86.73(8) . . ? N8D Cu4A N1D 82.00(8) . . ? O2A Cu4A N1D 165.25(8) . . ? O10B Cu4A O10C 93.40(7) . . ? N8D Cu4A O10C 103.15(8) . . ? O2A Cu4A O10C 81.80(6) . . ? N1D Cu4A O10C 112.35(7) . . ? O10B Cu4A Cu2A 75.22(5) . . ? N8D Cu4A Cu2A 120.52(6) . . ? O2A Cu4A Cu2A 41.15(4) . . ? N1D Cu4A Cu2A 148.87(6) . . ? O10C Cu4A Cu2A 45.56(4) . . ? Cu2A O1A Cu3A 129.98(8) . . ? Cu2A O1A Cu1A 96.29(7) . . ? Cu3A O1A Cu1A 99.80(7) . . ? Cu2A O1A H1AO 103.8 . . ? Cu3A O1A H1AO 123.1 . . ? Cu1A O1A H1AO 90.2 . . ? Cu1A O2A Cu4A 124.10(8) . . ? Cu1A O2A Cu2A 97.23(7) . . ? Cu4A O2A Cu2A 98.99(7) . . ? Cu1A O2A H2AO 109.1 . . ? Cu4A O2A H2AO 117.9 . . ? Cu2A O2A H2AO 104.0 . . ? C6A N1A C2A 119.5(2) . . ? C6A N1A Cu1A 113.54(15) . . ? C2A N1A Cu1A 126.94(16) . . ? N1A C2A C3A 121.7(2) . . ? N1A C2A H2A 119.1 . . ? C3A C2A H2A 119.1 . . ? C2A C3A C4A 118.8(2) . . ? C2A C3A H3A 120.6 . . ? C4A C3A H3A 120.6 . . ? C5A C4A C3A 119.5(2) . . ? C5A C4A H4A 120.2 . . ? C3A C4A H4A 120.2 . . ? C4A C5A C6A 119.1(2) . . ? C4A C5A H5A 120.5 . . ? C6A C5A H5A 120.5 . . ? N1A C6A C5A 121.3(2) . . ? N1A C6A C7A 116.4(2) . . ? C5A C6A C7A 122.3(2) . . ? N8A C7A C6A 109.07(18) . . ? N8A C7A H7AA 109.9 . . ? C6A C7A H7AA 109.9 . . ? N8A C7A H7AB 109.9 . . ? C6A C7A H7AB 109.9 . . ? H7AA C7A H7AB 108.3 . . ? C9A N8A C7A 120.49(19) . . ? C9A N8A Cu1A 125.70(16) . . ? C7A N8A Cu1A 113.80(14) . . ? O10A C9A N8A 123.5(2) . . ? O10A C9A C11A 116.9(2) . . ? N8A C9A C11A 119.6(2) . . ? C9A O10A Cu3A 134.58(15) . . ? C12A C11A C9A 113.8(2) . . ? C12A C11A H11A 108.8 . . ? C9A C11A H11A 108.8 . . ? C12A C11A H11B 108.8 . . ? C9A C11A H11B 108.8 . . ? H11A C11A H11B 107.7 . . ? C17A C12A C13A 118.6(2) . . ? C17A C12A C11A 120.9(2) . . ? C13A C12A C11A 120.4(2) . . ? C12A C13A C14A 120.5(3) . . ? C12A C13A H13A 119.7 . . ? C14A C13A H13A 119.7 . . ? C15A C14A C13A 120.2(3) . . ? C15A C14A H14A 119.9 . . ? C13A C14A H14A 119.9 . . ? C16A C15A C14A 119.8(2) . . ? C16A C15A H15A 120.1 . . ? C14A C15A H15A 120.1 . . ? C15A C16A C17A 120.1(3) . . ? C15A C16A H16A 119.9 . . ? C17A C16A H16A 119.9 . . ? C12A C17A C16A 120.7(2) . . ? C12A C17A H17A 119.6 . . ? C16A C17A H17A 119.6 . . ? C6B N1B C2B 119.1(2) . . ? C6B N1B Cu2A 113.81(17) . . ? C2B N1B Cu2A 126.62(19) . . ? N1B C2B C3B 122.4(3) . . ? N1B C2B H2B 118.8 . . ? C3B C2B H2B 118.8 . . ? C2B C3B C4B 118.9(3) . . ? C2B C3B H3B 120.6 . . ? C4B C3B H3B 120.6 . . ? C3B C4B C5B 119.5(3) . . ? C3B C4B H4B 120.2 . . ? C5B C4B H4B 120.2 . . ? C4B C5B C6B 119.0(3) . . ? C4B C5B H5B 120.5 . . ? C6B C5B H5B 120.5 . . ? N1B C6B C5B 121.1(3) . . ? N1B C6B C7B 116.9(2) . . ? C5B C6B C7B 122.0(3) . . ? N8B C7B C6B 109.8(2) . . ? N8B C7B H7BA 109.7 . . ? C6B C7B H7BA 109.7 . . ? N8B C7B H7BB 109.7 . . ? C6B C7B H7BB 109.7 . . ? H7BA C7B H7BB 108.2 . . ? C9B N8B C7B 119.6(2) . . ? C9B N8B Cu2A 125.46(17) . . ? C7B N8B Cu2A 114.81(16) . . ? O10B C9B N8B 123.1(2) . . ? O10B C9B C11B 116.0(2) . . ? N8B C9B C11B 120.9(2) . . ? C9B O10B Cu4A 134.70(16) . . ? C12B C11B C9B 114.6(2) . . ? C12B C11B H11C 108.6 . . ? C9B C11B H11C 108.6 . . ? C12B C11B H11D 108.6 . . ? C9B C11B H11D 108.6 . . ? H11C C11B H11D 107.6 . . ? C13B C12B C17B 117.9(3) . . ? C13B C12B C11B 122.4(3) . . ? C17B C12B C11B 119.7(3) . . ? C12B C13B C14B 119.7(4) . . ? C12B C13B H13B 120.1 . . ? C14B C13B H13B 120.1 . . ? C15B C14B C13B 120.3(4) . . ? C15B C14B H14B 119.8 . . ? C13B C14B H14B 119.8 . . ? C16B C15B C14B 120.1(4) . . ? C16B C15B H15B 119.9 . . ? C14B C15B H15B 119.9 . . ? C15B C16B C17B 119.5(4) . . ? C15B C16B H16B 120.2 . . ? C17B C16B H16B 120.2 . . ? C12B C17B C16B 122.3(4) . . ? C12B C17B H17B 118.8 . . ? C16B C17B H17B 118.8 . . ? C6C N1C C2C 118.9(2) . . ? C6C N1C Cu3A 114.44(17) . . ? C2C N1C Cu3A 126.23(17) . . ? N1C C2C C3C 122.0(2) . . ? N1C C2C H2C 119.0 . . ? C3C C2C H2C 119.0 . . ? C2C C3C C4C 119.0(3) . . ? C2C C3C H3C 120.5 . . ? C4C C3C H3C 120.5 . . ? C5C C4C C3C 119.2(3) . . ? C5C C4C H4C 120.4 . . ? C3C C4C H4C 120.4 . . ? C4C C5C C6C 118.9(2) . . ? C4C C5C H5C 120.5 . . ? C6C C5C H5C 120.5 . . ? N1C C6C C5C 121.9(2) . . ? N1C C6C C7C 117.2(2) . . ? C5C C6C C7C 120.9(2) . . ? N8C C7C C6C 110.8(2) . . ? N8C C7C H7CA 109.5 . . ? C6C C7C H7CA 109.5 . . ? N8C C7C H7CB 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 108.1 . . ? C9C N8C C7C 117.5(2) . . ? C9C N8C Cu3A 128.06(16) . . ? C7C N8C Cu3A 114.46(16) . . ? O10C C9C N8C 122.8(2) . . ? O10C C9C C11C 118.0(2) . . ? N8C C9C C11C 119.3(2) . . ? C9C O10C Cu2A 129.47(15) . . ? C9C O10C Cu4A 138.32(15) . . ? Cu2A O10C Cu4A 86.42(6) . . ? C12C C11C C9C 116.3(2) . . ? C12C C11C H11E 108.2 . . ? C9C C11C H11E 108.2 . . ? C12C C11C H11F 108.2 . . ? C9C C11C H11F 108.2 . . ? H11E C11C H11F 107.4 . . ? C17C C12C C13C 118.2(3) . . ? C17C C12C C11C 122.0(3) . . ? C13C C12C C11C 119.8(3) . . ? C14C C13C C12C 120.6(4) . . ? C14C C13C H13C 119.7 . . ? C12C C13C H13C 119.7 . . ? C15C C14C C13C 120.0(4) . . ? C15C C14C H14C 120.0 . . ? C13C C14C H14C 120.0 . . ? C16C C15C C14C 120.3(4) . . ? C16C C15C H15C 119.9 . . ? C14C C15C H15C 119.9 . . ? C15C C16C C17C 120.4(4) . . ? C15C C16C H16C 119.8 . . ? C17C C16C H16C 119.8 . . ? C12C C17C C16C 120.4(4) . . ? C12C C17C H17C 119.8 . . ? C16C C17C H17C 119.8 . . ? C6D N1D C2D 119.2(2) . . ? C6D N1D Cu4A 114.94(16) . . ? C2D N1D Cu4A 125.71(17) . . ? N1D C2D C3D 122.1(2) . . ? N1D C2D H2D 119.0 . . ? C3D C2D H2D 119.0 . . ? C4D C3D C2D 118.6(2) . . ? C4D C3D H3D 120.7 . . ? C2D C3D H3D 120.7 . . ? C3D C4D C5D 119.6(2) . . ? C3D C4D H4D 120.2 . . ? C5D C4D H4D 120.2 . . ? C4D C5D C6D 118.7(2) . . ? C4D C5D H5D 120.6 . . ? C6D C5D H5D 120.6 . . ? N1D C6D C5D 121.8(2) . . ? N1D C6D C7D 115.8(2) . . ? C5D C6D C7D 122.4(2) . . ? N8D C7D C6D 109.4(2) . . ? N8D C7D H7DA 109.8 . . ? C6D C7D H7DA 109.8 . . ? N8D C7D H7DB 109.8 . . ? C6D C7D H7DB 109.8 . . ? H7DA C7D H7DB 108.2 . . ? C9D N8D C7D 119.4(2) . . ? C9D N8D Cu4A 128.39(16) . . ? C7D N8D Cu4A 112.23(16) . . ? O10D C9D N8D 122.6(2) . . ? O10D C9D C11D 118.3(2) . . ? N8D C9D C11D 119.1(2) . . ? C9D O10D Cu1A 119.34(15) . . ? C12D C11D C9D 114.7(2) . . ? C12D C11D H11G 108.6 . . ? C9D C11D H11G 108.6 . . ? C12D C11D H11H 108.6 . . ? C9D C11D H11H 108.6 . . ? H11G C11D H11H 107.6 . . ? C17D C12D C13D 119.5(3) . . ? C17D C12D C11D 120.4(3) . . ? C13D C12D C11D 120.0(2) . . ? C12D C13D C14D 120.3(3) . . ? C12D C13D H13D 119.9 . . ? C14D C13D H13D 119.9 . . ? C15D C14D C13D 119.8(3) . . ? C15D C14D H14D 120.1 . . ? C13D C14D H14D 120.1 . . ? C14D C15D C16D 120.4(3) . . ? C14D C15D H15D 119.8 . . ? C16D C15D H15D 119.8 . . ? C17D C16D C15D 119.3(3) . . ? C17D C16D H16D 120.3 . . ? C15D C16D H16D 120.3 . . ? C12D C17D C16D 120.7(3) . . ? C12D C17D H17D 119.6 . . ? C16D C17D H17D 119.6 . . ? N8E Cu1B O1B 172.97(8) . 2_656 ? N8E Cu1B N1E 83.08(10) . . ? O1B Cu1B N1E 98.36(9) 2_656 . ? N8E Cu1B O1B 94.91(9) . . ? O1B Cu1B O1B 81.79(8) 2_656 . ? N1E Cu1B O1B 163.91(8) . . ? N8E Cu1B O10F 94.47(8) . 2_656 ? O1B Cu1B O10F 91.43(7) 2_656 2_656 ? N1E Cu1B O10F 111.21(8) . 2_656 ? O1B Cu1B O10F 84.84(7) . 2_656 ? N8E Cu1B Cu1B 132.53(7) . 2_656 ? O1B Cu1B Cu1B 42.66(5) 2_656 2_656 ? N1E Cu1B Cu1B 133.78(7) . 2_656 ? O1B Cu1B Cu1B 40.67(5) . 2_656 ? O10F Cu1B Cu1B 96.17(5) 2_656 2_656 ? N8E Cu1B Cu2B 81.94(7) . . ? O1B Cu1B Cu2B 99.20(5) 2_656 . ? N1E Cu1B Cu2B 153.35(7) . . ? O1B Cu1B Cu2B 40.21(5) . . ? O10F Cu1B Cu2B 48.56(5) 2_656 . ? Cu1B Cu1B Cu2B 71.462(12) 2_656 . ? O10E Cu2B O1B 89.49(8) . . ? O10E Cu2B N8F 165.86(10) . . ? O1B Cu2B N8F 99.13(9) . . ? O10E Cu2B N1F 88.89(10) . . ? O1B Cu2B N1F 175.03(11) . . ? N8F Cu2B N1F 81.57(10) . . ? O10E Cu2B O10F 89.38(8) . 2_656 ? O1B Cu2B O10F 82.61(7) . 2_656 ? N8F Cu2B O10F 102.75(9) . 2_656 ? N1F Cu2B O10F 102.07(10) . 2_656 ? O10E Cu2B Cu1B 75.27(6) . . ? O1B Cu2B Cu1B 41.51(5) . . ? N8F Cu2B Cu1B 118.50(7) . . ? N1F Cu2B Cu1B 142.13(8) . . ? O10F Cu2B Cu1B 44.90(5) 2_656 . ? Cu1B O1B Cu2B 126.42(9) 2_656 . ? Cu1B O1B Cu1B 96.67(8) 2_656 . ? Cu2B O1B Cu1B 98.28(8) . . ? Cu1B O1B H1BO 110.7 2_656 . ? Cu2B O1B H1BO 111.2 . . ? Cu1B O1B H1BO 110.7 . . ? C2E N1E C6E 119.5(3) . . ? C2E N1E Cu1B 127.45(19) . . ? C6E N1E Cu1B 112.9(2) . . ? N1E C2E C3E 122.0(3) . . ? N1E C2E H2E 119.0 . . ? C3E C2E H2E 119.0 . . ? C2E C3E C4E 118.8(3) . . ? C2E C3E H3E 120.6 . . ? C4E C3E H3E 120.6 . . ? C5E C4E C3E 119.2(3) . . ? C5E C4E H4E 120.4 . . ? C3E C4E H4E 120.4 . . ? C4E C5E C6E 119.4(3) . . ? C4E C5E H5E 120.3 . . ? C6E C5E H5E 120.3 . . ? N1E C6E C5E 121.0(3) . . ? N1E C6E C7E 117.2(2) . . ? C5E C6E C7E 121.8(3) . . ? N8E C7E C6E 109.7(2) . . ? N8E C7E H7EA 109.7 . . ? C6E C7E H7EA 109.7 . . ? N8E C7E H7EB 109.7 . . ? C6E C7E H7EB 109.7 . . ? H7EA C7E H7EB 108.2 . . ? C9E N8E C7E 121.6(2) . . ? C9E N8E Cu1B 125.09(18) . . ? C7E N8E Cu1B 113.19(19) . . ? O10E C9E N8E 123.8(2) . . ? O10E C9E C11E 115.9(3) . . ? N8E C9E C11E 120.3(3) . . ? C9E O10E Cu2B 133.81(19) . . ? C12' C11E C9E 114.7(2) . . ? C9E C11E C12E 113.8(2) . . ? C9E C11E H11I 108.8 . . ? C12E C11E H11I 108.8 . . ? C9E C11E H11J 108.8 . . ? C12E C11E H11J 108.8 . . ? H11I C11E H11J 107.7 . . ? C12' C11E H11K 108.2 . . ? C9E C11E H11K 108.4 . . ? C12' C11E H11L 109.5 . . ? C9E C11E H11L 108.4 . . ? H11K C11E H11L 107.5 . . ? C13E C12E C17E 118.3(3) . . ? C13E C12E C11E 123.7(3) . . ? C17E C12E C11E 118.0(3) . . ? C12E C13E C14E 120.4(3) . . ? C12E C13E H13E 119.8 . . ? C14E C13E H13E 119.8 . . ? C13E C14E C15E 121.3(3) . . ? C13E C14E H14E 119.3 . . ? C15E C14E H14E 119.3 . . ? C14E C15E C16E 118.2(3) . . ? C14E C15E H15E 120.9 . . ? C16E C15E H15E 120.9 . . ? C17E C16E C15E 120.2(3) . . ? C17E C16E H16E 119.9 . . ? C15E C16E H16E 119.9 . . ? C16E C17E C12E 121.6(3) . . ? C16E C17E H17E 119.2 . . ? C12E C17E H17E 119.2 . . ? C13' C12' C17' 121.2(3) . . ? C13' C12' C11E 118.2(3) . . ? C17' C12' C11E 120.7(3) . . ? C14' C13' C12' 119.5(3) . . ? C14' C13' H13' 120.3 . . ? C12' C13' H13' 120.3 . . ? C15' C14' C13' 119.3(3) . . ? C15' C14' H14' 120.4 . . ? C13' C14' H14' 120.4 . . ? C14' C15' C16' 121.6(3) . . ? C14' C15' H15' 119.2 . . ? C16' C15' H15' 119.2 . . ? C15' C16' C17' 119.1(3) . . ? C15' C16' H16' 120.4 . . ? C17' C16' H16' 120.4 . . ? C12' C17' C16' 119.4(3) . . ? C12' C17' H17' 120.3 . . ? C16' C17' H17' 120.3 . . ? C2F N1F C6F 118.7(3) . . ? C2F N1F Cu2B 126.9(2) . . ? C6F N1F Cu2B 114.3(2) . . ? N1F C2F C3F 121.8(4) . . ? N1F C2F H2F 119.1 . . ? C3F C2F H2F 119.1 . . ? C4F C3F C2F 118.6(4) . . ? C4F C3F H3F 120.7 . . ? C2F C3F H3F 120.7 . . ? C5F C4F C3F 120.0(4) . . ? C5F C4F H4F 120.0 . . ? C3F C4F H4F 120.0 . . ? C4F C5F C6F 118.5(4) . . ? C4F C5F H5F 120.7 . . ? C6F C5F H5F 120.7 . . ? N1F C6F C5F 122.3(3) . . ? N1F C6F C7F 116.1(3) . . ? C5F C6F C7F 121.6(3) . . ? N8F C7F C6F 108.3(3) . . ? N8F C7F H7FA 110.0 . . ? C6F C7F H7FA 110.0 . . ? N8F C7F H7FB 110.0 . . ? C6F C7F H7FB 110.0 . . ? H7FA C7F H7FB 108.4 . . ? C9F N8F C7F 120.7(2) . . ? C9F N8F Cu2B 128.17(19) . . ? C7F N8F Cu2B 111.12(19) . . ? O10F C9F N8F 122.3(2) . . ? O10F C9F C11F 114.0(2) . . ? N8F C9F C11F 123.7(3) . . ? C9F O10F Cu1B 125.72(17) . 2_656 ? C9F O10F Cu2B 140.07(17) . 2_656 ? Cu1B O10F Cu2B 86.54(6) 2_656 2_656 ? C12F C11F C9F 109.2(2) . . ? C12F C11F H11M 109.8 . . ? C9F C11F H11M 109.8 . . ? C12F C11F H11N 109.8 . . ? C9F C11F H11N 109.8 . . ? H11M C11F H11N 108.3 . . ? C17F C12F C13F 118.5(3) . . ? C17F C12F C11F 121.2(3) . . ? C13F C12F C11F 120.3(3) . . ? C14F C13F C12F 121.3(3) . . ? C14F C13F H13F 119.3 . . ? C12F C13F H13F 119.3 . . ? C15F C14F C13F 119.5(3) . . ? C15F C14F H14F 120.2 . . ? C13F C14F H14F 120.2 . . ? C14F C15F C16F 120.0(3) . . ? C14F C15F H15F 120.0 . . ? C16F C15F H15F 120.0 . . ? C15F C16F C17F 120.6(4) . . ? C15F C16F H16F 119.7 . . ? C17F C16F H16F 119.7 . . ? C12F C17F C16F 120.0(3) . . ? C12F C17F H17F 120.0 . . ? C16F C17F H17F 120.0 . . ? O4G Cl1G O3G 109.79(12) . . ? O4G Cl1G O1G 111.29(13) . . ? O3G Cl1G O1G 110.33(13) . . ? O4G Cl1G O2G 108.94(12) . . ? O3G Cl1G O2G 109.36(12) . . ? O1G Cl1G O2G 107.08(12) . . ? O3H Cl1H O2H 110.08(18) . . ? O3H Cl1H O1H 109.18(18) . . ? O2H Cl1H O1H 109.01(14) . . ? O3H Cl1H O4H 110.81(17) . . ? O2H Cl1H O4H 109.64(19) . . ? O1H Cl1H O4H 108.09(14) . . ? O1I Cl1I O2I 109.9(3) . . ? O1I Cl1I O4I 108.7(3) . . ? O2I Cl1I O4I 110.5(5) . . ? O1I Cl1I O3I 108.5(3) . . ? O2I Cl1I O3I 110.6(3) . . ? O4I Cl1I O3I 108.5(3) . . ? O3I' Cl1' O4I' 111.3(3) . . ? O3I' Cl1' O2I' 110.4(3) . . ? O4I' Cl1' O2I' 109.7(5) . . ? O3I' Cl1' O1I' 110.0(3) . . ? O4I' Cl1' O1I' 106.8(3) . . ? O2I' Cl1' O1I' 108.5(3) . . ? N1S C2S C3S 177.2(5) . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8A Cu1A Cu2A N8B -145.75(11) . . . . ? O2A Cu1A Cu2A N8B 23.49(11) . . . . ? N1A Cu1A Cu2A N8B -12.85(11) . . . . ? O1A Cu1A Cu2A N8B -174.46(11) . . . . ? O10D Cu1A Cu2A N8B 110.13(9) . . . . ? Cu3A Cu1A Cu2A N8B 156.07(8) . . . . ? N8A Cu1A Cu2A O1A 28.71(10) . . . . ? O2A Cu1A Cu2A O1A -162.05(10) . . . . ? N1A Cu1A Cu2A O1A 161.61(10) . . . . ? O10D Cu1A Cu2A O1A -75.41(8) . . . . ? Cu3A Cu1A Cu2A O1A -29.47(7) . . . . ? N8A Cu1A Cu2A N1B -23.06(12) . . . . ? O2A Cu1A Cu2A N1B 146.18(11) . . . . ? N1A Cu1A Cu2A N1B 109.84(11) . . . . ? O1A Cu1A Cu2A N1B -51.77(11) . . . . ? O10D Cu1A Cu2A N1B -127.18(9) . . . . ? Cu3A Cu1A Cu2A N1B -81.24(9) . . . . ? N8A Cu1A Cu2A O2A -169.24(11) . . . . ? N1A Cu1A Cu2A O2A -36.34(10) . . . . ? O1A Cu1A Cu2A O2A 162.05(10) . . . . ? O10D Cu1A Cu2A O2A 86.64(8) . . . . ? Cu3A Cu1A Cu2A O2A 132.58(7) . . . . ? N8A Cu1A Cu2A O10C 113.60(9) . . . . ? O2A Cu1A Cu2A O10C -77.16(8) . . . . ? N1A Cu1A Cu2A O10C -113.50(9) . . . . ? O1A Cu1A Cu2A O10C 84.89(8) . . . . ? O10D Cu1A Cu2A O10C 9.48(6) . . . . ? Cu3A Cu1A Cu2A O10C 55.43(4) . . . . ? N8A Cu1A Cu2A Cu4A 157.41(8) . . . . ? O2A Cu1A Cu2A Cu4A -33.35(7) . . . . ? N1A Cu1A Cu2A Cu4A -69.69(8) . . . . ? O1A Cu1A Cu2A Cu4A 128.70(7) . . . . ? O10D Cu1A Cu2A Cu4A 53.29(4) . . . . ? Cu3A Cu1A Cu2A Cu4A 99.234(15) . . . . ? N8A Cu1A Cu3A O10A -4.51(8) . . . . ? O2A Cu1A Cu3A O10A 167.66(7) . . . . ? N1A Cu1A Cu3A O10A -60.72(13) . . . . ? O1A Cu1A Cu3A O10A 106.49(9) . . . . ? O10D Cu1A Cu3A O10A -106.93(8) . . . . ? Cu2A Cu1A Cu3A O10A 136.95(6) . . . . ? N8A Cu1A Cu3A N8C 173.53(9) . . . . ? O2A Cu1A Cu3A N8C -14.30(8) . . . . ? N1A Cu1A Cu3A N8C 117.32(14) . . . . ? O1A Cu1A Cu3A N8C -75.47(10) . . . . ? O10D Cu1A Cu3A N8C 71.11(9) . . . . ? Cu2A Cu1A Cu3A N8C -45.01(7) . . . . ? N8A Cu1A Cu3A O1A -110.99(9) . . . . ? O2A Cu1A Cu3A O1A 61.17(8) . . . . ? N1A Cu1A Cu3A O1A -167.21(14) . . . . ? O10D Cu1A Cu3A O1A 146.59(9) . . . . ? Cu2A Cu1A Cu3A O1A 30.46(7) . . . . ? N8A Cu1A Cu3A N1C 42.18(15) . . . . ? O2A Cu1A Cu3A N1C -145.65(15) . . . . ? N1A Cu1A Cu3A N1C -14.04(19) . . . . ? O1A Cu1A Cu3A N1C 153.17(16) . . . . ? O10D Cu1A Cu3A N1C -60.24(15) . . . . ? Cu2A Cu1A Cu3A N1C -176.37(14) . . . . ? N8B Cu2A Cu4A O10B -2.66(9) . . . . ? O1A Cu2A Cu4A O10B 170.83(7) . . . . ? N1B Cu2A Cu4A O10B -40.5(2) . . . . ? O2A Cu2A Cu4A O10B 104.86(9) . . . . ? O10C Cu2A Cu4A O10B -110.16(8) . . . . ? Cu1A Cu2A Cu4A O10B 138.42(6) . . . . ? N8B Cu2A Cu4A N8D -174.52(10) . . . . ? O1A Cu2A Cu4A N8D -1.03(9) . . . . ? N1B Cu2A Cu4A N8D 147.6(2) . . . . ? O2A Cu2A Cu4A N8D -67.00(10) . . . . ? O10C Cu2A Cu4A N8D 77.98(10) . . . . ? Cu1A Cu2A Cu4A N8D -33.44(8) . . . . ? N8B Cu2A Cu4A O2A -107.52(10) . . . . ? O1A Cu2A Cu4A O2A 65.97(8) . . . . ? N1B Cu2A Cu4A O2A -145.4(2) . . . . ? O10C Cu2A Cu4A O2A 144.97(9) . . . . ? Cu1A Cu2A Cu4A O2A 33.55(7) . . . . ? N8B Cu2A Cu4A N1D 53.91(14) . . . . ? O1A Cu2A Cu4A N1D -132.60(13) . . . . ? N1B Cu2A Cu4A N1D 16.1(2) . . . . ? O2A Cu2A Cu4A N1D 161.43(14) . . . . ? O10C Cu2A Cu4A N1D -53.59(13) . . . . ? Cu1A Cu2A Cu4A N1D -165.01(12) . . . . ? N8B Cu2A Cu4A O10C 107.50(9) . . . . ? O1A Cu2A Cu4A O10C -79.01(8) . . . . ? N1B Cu2A Cu4A O10C 69.7(2) . . . . ? O2A Cu2A Cu4A O10C -144.97(9) . . . . ? Cu1A Cu2A Cu4A O10C -111.42(6) . . . . ? N1B Cu2A O1A Cu3A -109.27(11) . . . . ? O2A Cu2A O1A Cu3A 96.84(11) . . . . ? O10C Cu2A O1A Cu3A 13.65(10) . . . . ? Cu1A Cu2A O1A Cu3A 108.42(12) . . . . ? Cu4A Cu2A O1A Cu3A 60.56(10) . . . . ? N1B Cu2A O1A Cu1A 142.31(8) . . . . ? O2A Cu2A O1A Cu1A -11.58(6) . . . . ? O10C Cu2A O1A Cu1A -94.77(7) . . . . ? Cu4A Cu2A O1A Cu1A -47.86(6) . . . . ? O10A Cu3A O1A Cu2A -174.56(11) . . . . ? N8C Cu3A O1A Cu2A 10.12(12) . . . . ? N1C Cu3A O1A Cu2A 105.1(2) . . . . ? Cu1A Cu3A O1A Cu2A -106.86(12) . . . . ? O10A Cu3A O1A Cu1A -67.70(7) . . . . ? N8C Cu3A O1A Cu1A 116.98(8) . . . . ? N1C Cu3A O1A Cu1A -148.09(18) . . . . ? N8A Cu1A O1A Cu2A -159.52(7) . . . . ? O2A Cu1A O1A Cu2A 12.16(6) . . . . ? N1A Cu1A O1A Cu2A -72.6(3) . . . . ? O10D Cu1A O1A Cu2A 106.58(7) . . . . ? Cu3A Cu1A O1A Cu2A 132.46(9) . . . . ? N8A Cu1A O1A Cu3A 68.02(8) . . . . ? O2A Cu1A O1A Cu3A -120.30(7) . . . . ? N1A Cu1A O1A Cu3A 154.9(3) . . . . ? O10D Cu1A O1A Cu3A -25.88(6) . . . . ? Cu2A Cu1A O1A Cu3A -132.46(9) . . . . ? N1A Cu1A O2A Cu4A -99.66(10) . . . . ? O1A Cu1A O2A Cu4A 94.27(10) . . . . ? O10D Cu1A O2A Cu4A 7.80(10) . . . . ? Cu2A Cu1A O2A Cu4A 106.02(11) . . . . ? Cu3A Cu1A O2A Cu4A 60.08(9) . . . . ? N1A Cu1A O2A Cu2A 154.31(7) . . . . ? O1A Cu1A O2A Cu2A -11.76(6) . . . . ? O10D Cu1A O2A Cu2A -98.22(7) . . . . ? Cu3A Cu1A O2A Cu2A -45.94(6) . . . . ? O10B Cu4A O2A Cu1A -174.34(10) . . . . ? N8D Cu4A O2A Cu1A 21.42(11) . . . . ? N1D Cu4A O2A Cu1A 115.2(3) . . . . ? O10C Cu4A O2A Cu1A -80.67(9) . . . . ? Cu2A Cu4A O2A Cu1A -105.12(11) . . . . ? O10B Cu4A O2A Cu2A -69.22(7) . . . . ? N8D Cu4A O2A Cu2A 126.54(8) . . . . ? N1D Cu4A O2A Cu2A -139.7(3) . . . . ? O10C Cu4A O2A Cu2A 24.46(6) . . . . ? N8B Cu2A O2A Cu1A -162.75(8) . . . . ? O1A Cu2A O2A Cu1A 12.22(6) . . . . ? N1B Cu2A O2A Cu1A -79.69(19) . . . . ? O10C Cu2A O2A Cu1A 100.85(7) . . . . ? Cu4A Cu2A O2A Cu1A 126.31(9) . . . . ? N8B Cu2A O2A Cu4A 70.94(8) . . . . ? O1A Cu2A O2A Cu4A -114.10(7) . . . . ? N1B Cu2A O2A Cu4A 154.00(16) . . . . ? O10C Cu2A O2A Cu4A -25.46(7) . . . . ? Cu1A Cu2A O2A Cu4A -126.31(9) . . . . ? N8A Cu1A N1A C6A 9.61(16) . . . . ? O2A Cu1A N1A C6A -161.92(16) . . . . ? O1A Cu1A N1A C6A -78.8(4) . . . . ? O10D Cu1A N1A C6A 102.01(16) . . . . ? Cu2A Cu1A N1A C6A -138.10(13) . . . . ? Cu3A Cu1A N1A C6A 65.3(2) . . . . ? N8A Cu1A N1A C2A -170.8(2) . . . . ? O2A Cu1A N1A C2A 17.7(2) . . . . ? O1A Cu1A N1A C2A 100.8(3) . . . . ? O10D Cu1A N1A C2A -78.4(2) . . . . ? Cu2A Cu1A N1A C2A 41.5(2) . . . . ? Cu3A Cu1A N1A C2A -115.07(19) . . . . ? C6A N1A C2A C3A 0.1(3) . . . . ? Cu1A N1A C2A C3A -179.47(18) . . . . ? N1A C2A C3A C4A -0.4(4) . . . . ? C2A C3A C4A C5A 0.3(4) . . . . ? C3A C4A C5A C6A 0.0(4) . . . . ? C2A N1A C6A C5A 0.3(3) . . . . ? Cu1A N1A C6A C5A 179.88(19) . . . . ? C2A N1A C6A C7A -179.6(2) . . . . ? Cu1A N1A C6A C7A 0.0(3) . . . . ? C4A C5A C6A N1A -0.3(4) . . . . ? C4A C5A C6A C7A 179.5(2) . . . . ? N1A C6A C7A N8A -13.4(3) . . . . ? C5A C6A C7A N8A 166.7(2) . . . . ? C6A C7A N8A C9A -160.3(2) . . . . ? C6A C7A N8A Cu1A 21.0(2) . . . . ? O2A Cu1A N8A C9A -108.1(5) . . . . ? O1A Cu1A N8A C9A -30.0(2) . . . . ? O10D Cu1A N8A C9A 57.5(2) . . . . ? Cu2A Cu1A N8A C9A -48.4(2) . . . . ? Cu3A Cu1A N8A C9A 6.68(19) . . . . ? N1A Cu1A N8A C7A -17.41(16) . . . . ? O1A Cu1A N8A C7A 148.62(16) . . . . ? O10D Cu1A N8A C7A -123.93(16) . . . . ? Cu2A Cu1A N8A C7A 130.17(14) . . . . ? Cu3A Cu1A N8A C7A -174.75(16) . . . . ? C7A N8A C9A O10A 175.3(2) . . . . ? Cu1A N8A C9A O10A -6.2(3) . . . . ? C7A N8A C9A C11A -5.4(3) . . . . ? Cu1A N8A C9A C11A 173.04(18) . . . . ? N8A C9A O10A Cu3A -1.4(4) . . . . ? C11A C9A O10A Cu3A 179.34(18) . . . . ? O1A Cu3A O10A C9A 43.4(2) . . . . ? N1C Cu3A O10A C9A -157.5(2) . . . . ? Cu1A Cu3A O10A C9A 4.6(2) . . . . ? O10A C9A C11A C12A 2.8(3) . . . . ? N8A C9A C11A C12A -176.5(2) . . . . ? C9A C11A C12A C17A -101.8(3) . . . . ? C9A C11A C12A C13A 77.3(3) . . . . ? C17A C12A C13A C14A -0.3(4) . . . . ? C11A C12A C13A C14A -179.4(2) . . . . ? C12A C13A C14A C15A 0.7(4) . . . . ? C13A C14A C15A C16A -0.8(4) . . . . ? C14A C15A C16A C17A 0.5(4) . . . . ? C13A C12A C17A C16A 0.0(4) . . . . ? C11A C12A C17A C16A 179.1(2) . . . . ? C15A C16A C17A C12A -0.1(4) . . . . ? N8B Cu2A N1B C6B 10.82(18) . . . . ? O1A Cu2A N1B C6B -162.85(18) . . . . ? O2A Cu2A N1B C6B -74.8(3) . . . . ? O10C Cu2A N1B C6B 104.58(18) . . . . ? Cu1A Cu2A N1B C6B -130.22(16) . . . . ? Cu4A Cu2A N1B C6B 48.5(3) . . . . ? N8B Cu2A N1B C2B -176.9(2) . . . . ? O1A Cu2A N1B C2B 9.5(2) . . . . ? O2A Cu2A N1B C2B 97.5(3) . . . . ? O10C Cu2A N1B C2B -83.1(2) . . . . ? Cu1A Cu2A N1B C2B 42.1(2) . . . . ? Cu4A Cu2A N1B C2B -139.23(19) . . . . ? C6B N1B C2B C3B 1.0(4) . . . . ? Cu2A N1B C2B C3B -171.0(2) . . . . ? N1B C2B C3B C4B -0.2(4) . . . . ? C2B C3B C4B C5B -0.2(5) . . . . ? C3B C4B C5B C6B -0.2(5) . . . . ? C2B N1B C6B C5B -1.3(4) . . . . ? Cu2A N1B C6B C5B 171.6(2) . . . . ? C2B N1B C6B C7B 178.1(2) . . . . ? Cu2A N1B C6B C7B -9.0(3) . . . . ? C4B C5B C6B N1B 1.0(4) . . . . ? C4B C5B C6B C7B -178.4(3) . . . . ? N1B C6B C7B N8B 0.6(3) . . . . ? C5B C6B C7B N8B 180.0(3) . . . . ? C6B C7B N8B C9B -174.9(2) . . . . ? C6B C7B N8B Cu2A 8.4(3) . . . . ? N1B Cu2A N8B C9B 173.0(2) . . . . ? O2A Cu2A N8B C9B -32.9(2) . . . . ? O10C Cu2A N8B C9B 50.5(2) . . . . ? Cu1A Cu2A N8B C9B -47.8(2) . . . . ? Cu4A Cu2A N8B C9B 5.0(2) . . . . ? N1B Cu2A N8B C7B -10.52(19) . . . . ? O2A Cu2A N8B C7B 143.66(18) . . . . ? O10C Cu2A N8B C7B -132.97(18) . . . . ? Cu1A Cu2A N8B C7B 128.73(16) . . . . ? Cu4A Cu2A N8B C7B -178.54(19) . . . . ? C7B N8B C9B O10B 177.8(2) . . . . ? Cu2A N8B C9B O10B -5.8(4) . . . . ? C7B N8B C9B C11B -3.2(4) . . . . ? Cu2A N8B C9B C11B 173.1(2) . . . . ? N8B C9B O10B Cu4A 1.6(4) . . . . ? C11B C9B O10B Cu4A -177.4(2) . . . . ? N8D Cu4A O10B C9B 157.5(3) . . . . ? O2A Cu4A O10B C9B 41.0(2) . . . . ? N1D Cu4A O10B C9B -152.9(2) . . . . ? O10C Cu4A O10B C9B -40.7(2) . . . . ? Cu2A Cu4A O10B C9B 1.5(2) . . . . ? O10B C9B C11B C12B -11.3(4) . . . . ? N8B C9B C11B C12B 169.7(3) . . . . ? C9B C11B C12B C13B 72.2(4) . . . . ? C9B C11B C12B C17B -106.4(3) . . . . ? C17B C12B C13B C14B -2.4(6) . . . . ? C11B C12B C13B C14B 179.0(4) . . . . ? C12B C13B C14B C15B 0.6(7) . . . . ? C13B C14B C15B C16B 1.1(7) . . . . ? C14B C15B C16B C17B -0.8(7) . . . . ? C13B C12B C17B C16B 2.8(6) . . . . ? C11B C12B C17B C16B -178.6(4) . . . . ? C15B C16B C17B C12B -1.2(7) . . . . ? O10A Cu3A N1C C6C -172.82(18) . . . . ? N8C Cu3A N1C C6C 5.92(17) . . . . ? O1A Cu3A N1C C6C -92.2(3) . . . . ? Cu1A Cu3A N1C C6C 142.56(14) . . . . ? O10A Cu3A N1C C2C -0.7(2) . . . . ? N8C Cu3A N1C C2C 178.1(2) . . . . ? O1A Cu3A N1C C2C 79.9(3) . . . . ? Cu1A Cu3A N1C C2C -45.3(3) . . . . ? C6C N1C C2C C3C 0.0(4) . . . . ? Cu3A N1C C2C C3C -171.8(2) . . . . ? N1C C2C C3C C4C -1.4(5) . . . . ? C2C C3C C4C C5C 1.2(5) . . . . ? C3C C4C C5C C6C 0.3(4) . . . . ? C2C N1C C6C C5C 1.6(4) . . . . ? Cu3A N1C C6C C5C 174.4(2) . . . . ? C2C N1C C6C C7C -177.5(2) . . . . ? Cu3A N1C C6C C7C -4.7(3) . . . . ? C4C C5C C6C N1C -1.8(4) . . . . ? C4C C5C C6C C7C 177.3(3) . . . . ? N1C C6C C7C N8C -0.1(3) . . . . ? C5C C6C C7C N8C -179.2(2) . . . . ? C6C C7C N8C C9C -175.8(2) . . . . ? C6C C7C N8C Cu3A 5.0(3) . . . . ? O1A Cu3A N8C C9C -26.2(2) . . . . ? N1C Cu3A N8C C9C 175.0(2) . . . . ? Cu1A Cu3A N8C C9C 13.7(2) . . . . ? O1A Cu3A N8C C7C 152.84(18) . . . . ? N1C Cu3A N8C C7C -5.93(18) . . . . ? Cu1A Cu3A N8C C7C -167.29(16) . . . . ? C7C N8C C9C O10C -179.9(2) . . . . ? Cu3A N8C C9C O10C -0.9(4) . . . . ? C7C N8C C9C C11C -1.6(4) . . . . ? Cu3A N8C C9C C11C 177.40(18) . . . . ? N8C C9C O10C Cu2A 52.0(3) . . . . ? C11C C9C O10C Cu2A -126.3(2) . . . . ? N8C C9C O10C Cu4A -91.5(3) . . . . ? C11C C9C O10C Cu4A 90.2(3) . . . . ? N8B Cu2A O10C C9C 131.7(2) . . . . ? O1A Cu2A O10C C9C -53.0(2) . . . . ? N1B Cu2A O10C C9C 45.4(2) . . . . ? O2A Cu2A O10C C9C -134.9(2) . . . . ? Cu1A Cu2A O10C C9C -95.6(2) . . . . ? Cu4A Cu2A O10C C9C -156.6(2) . . . . ? N8B Cu2A O10C Cu4A -71.71(7) . . . . ? O1A Cu2A O10C Cu4A 103.67(6) . . . . ? N1B Cu2A O10C Cu4A -157.96(8) . . . . ? O2A Cu2A O10C Cu4A 21.76(6) . . . . ? Cu1A Cu2A O10C Cu4A 61.05(4) . . . . ? O10B Cu4A O10C C9C -142.0(2) . . . . ? N8D Cu4A O10C C9C 32.5(2) . . . . ? O2A Cu4A O10C C9C 130.2(2) . . . . ? N1D Cu4A O10C C9C -54.1(2) . . . . ? Cu2A Cu4A O10C C9C 152.6(3) . . . . ? O10B Cu4A O10C Cu2A 65.40(7) . . . . ? N8D Cu4A O10C Cu2A -120.09(7) . . . . ? O2A Cu4A O10C Cu2A -22.43(6) . . . . ? N1D Cu4A O10C Cu2A 153.26(7) . . . . ? O10C C9C C11C C12C 3.2(4) . . . . ? N8C C9C C11C C12C -175.1(2) . . . . ? C9C C11C C12C C17C 57.7(4) . . . . ? C9C C11C C12C C13C -123.7(3) . . . . ? C17C C12C C13C C14C 0.9(5) . . . . ? C11C C12C C13C C14C -177.7(3) . . . . ? C12C C13C C14C C15C -0.3(5) . . . . ? C13C C14C C15C C16C -0.5(6) . . . . ? C14C C15C C16C C17C 0.6(6) . . . . ? C13C C12C C17C C16C -0.8(5) . . . . ? C11C C12C C17C C16C 177.8(3) . . . . ? C15C C16C C17C C12C 0.0(6) . . . . ? O10B Cu4A N1D C6D -152.3(2) . . . . ? N8D Cu4A N1D C6D 14.4(2) . . . . ? O2A Cu4A N1D C6D -81.6(4) . . . . ? O10C Cu4A N1D C6D 115.35(19) . . . . ? Cu2A Cu4A N1D C6D 153.77(15) . . . . ? O10B Cu4A N1D C2D 23.4(2) . . . . ? N8D Cu4A N1D C2D -169.9(2) . . . . ? O2A Cu4A N1D C2D 94.1(3) . . . . ? O10C Cu4A N1D C2D -69.0(2) . . . . ? Cu2A Cu4A N1D C2D -30.5(3) . . . . ? C6D N1D C2D C3D 0.2(4) . . . . ? Cu4A N1D C2D C3D -175.4(2) . . . . ? N1D C2D C3D C4D 1.0(4) . . . . ? C2D C3D C4D C5D -0.8(5) . . . . ? C3D C4D C5D C6D -0.4(5) . . . . ? C2D N1D C6D C5D -1.5(4) . . . . ? Cu4A N1D C6D C5D 174.5(2) . . . . ? C2D N1D C6D C7D 179.9(3) . . . . ? Cu4A N1D C6D C7D -4.1(3) . . . . ? C4D C5D C6D N1D 1.6(5) . . . . ? C4D C5D C6D C7D -179.9(3) . . . . ? N1D C6D C7D N8D -13.1(4) . . . . ? C5D C6D C7D N8D 168.2(3) . . . . ? C6D C7D N8D C9D -157.4(2) . . . . ? C6D C7D N8D Cu4A 24.2(3) . . . . ? O10B Cu4A N8D C9D -149.4(2) . . . . ? O2A Cu4A N8D C9D -34.5(2) . . . . ? N1D Cu4A N8D C9D 160.4(2) . . . . ? O10C Cu4A N8D C9D 49.2(2) . . . . ? Cu2A Cu4A N8D C9D 3.4(3) . . . . ? O10B Cu4A N8D C7D 28.8(4) . . . . ? O2A Cu4A N8D C7D 143.73(19) . . . . ? N1D Cu4A N8D C7D -21.4(2) . . . . ? O10C Cu4A N8D C7D -132.60(19) . . . . ? Cu2A Cu4A N8D C7D -178.42(17) . . . . ? C7D N8D C9D O10D 175.7(2) . . . . ? Cu4A N8D C9D O10D -6.2(4) . . . . ? C7D N8D C9D C11D -5.6(4) . . . . ? Cu4A N8D C9D C11D 172.48(18) . . . . ? N8D C9D O10D Cu1A 59.5(3) . . . . ? C11D C9D O10D Cu1A -119.2(2) . . . . ? N8A Cu1A O10D C9D 126.67(17) . . . . ? O2A Cu1A O10D C9D -55.43(17) . . . . ? N1A Cu1A O10D C9D 42.28(18) . . . . ? O1A Cu1A O10D C9D -137.52(17) . . . . ? Cu2A Cu1A O10D C9D -98.11(16) . . . . ? Cu3A Cu1A O10D C9D -158.04(18) . . . . ? O10D C9D C11D C12D 4.3(3) . . . . ? N8D C9D C11D C12D -174.5(2) . . . . ? C9D C11D C12D C17D 69.8(3) . . . . ? C9D C11D C12D C13D -114.0(3) . . . . ? C17D C12D C13D C14D -1.6(4) . . . . ? C11D C12D C13D C14D -177.8(3) . . . . ? C12D C13D C14D C15D 0.1(5) . . . . ? C13D C14D C15D C16D 1.7(5) . . . . ? C14D C15D C16D C17D -1.9(5) . . . . ? C13D C12D C17D C16D 1.4(5) . . . . ? C11D C12D C17D C16D 177.6(3) . . . . ? C15D C16D C17D C12D 0.4(5) . . . . ? N8E Cu1B Cu2B O10E 1.08(9) . . . . ? O1B Cu1B Cu2B O10E -171.91(8) 2_656 . . . ? N1E Cu1B Cu2B O10E 57.48(17) . . . . ? O1B Cu1B Cu2B O10E -106.46(10) . . . . ? O10F Cu1B Cu2B O10E 104.37(9) 2_656 . . . ? Cu1B Cu1B Cu2B O10E -139.06(7) 2_656 . . . ? N8E Cu1B Cu2B O1B 107.54(10) . . . . ? O1B Cu1B Cu2B O1B -65.45(8) 2_656 . . . ? N1E Cu1B Cu2B O1B 163.94(17) . . . . ? O10F Cu1B Cu2B O1B -149.17(10) 2_656 . . . ? Cu1B Cu1B Cu2B O1B -32.60(8) 2_656 . . . ? N8E Cu1B Cu2B N8F 177.60(11) . . . . ? O1B Cu1B Cu2B N8F 4.62(11) 2_656 . . . ? N1E Cu1B Cu2B N8F -125.99(18) . . . . ? O1B Cu1B Cu2B N8F 70.07(12) . . . . ? O10F Cu1B Cu2B N8F -79.10(11) 2_656 . . . ? Cu1B Cu1B Cu2B N8F 37.47(9) 2_656 . . . ? N8E Cu1B Cu2B N1F -67.16(15) . . . . ? O1B Cu1B Cu2B N1F 119.86(15) 2_656 . . . ? N1E Cu1B Cu2B N1F -10.8(2) . . . . ? O1B Cu1B Cu2B N1F -174.70(16) . . . . ? O10F Cu1B Cu2B N1F 36.13(15) 2_656 . . . ? Cu1B Cu1B Cu2B N1F 152.71(14) 2_656 . . . ? N8E Cu1B Cu2B O10F -103.29(9) . . . 2_656 ? O1B Cu1B Cu2B O10F 83.72(9) 2_656 . . 2_656 ? N1E Cu1B Cu2B O10F -46.89(17) . . . 2_656 ? O1B Cu1B Cu2B O10F 149.17(10) . . . 2_656 ? Cu1B Cu1B Cu2B O10F 116.58(7) 2_656 . . 2_656 ? O10E Cu2B O1B Cu1B 172.73(12) . . . 2_656 ? N8F Cu2B O1B Cu1B -18.52(14) . . . 2_656 ? O10F Cu2B O1B Cu1B 83.28(11) 2_656 . . 2_656 ? Cu1B Cu2B O1B Cu1B 104.67(14) . . . 2_656 ? O10E Cu2B O1B Cu1B 68.05(9) . . . . ? N8F Cu2B O1B Cu1B -123.20(10) . . . . ? O10F Cu2B O1B Cu1B -21.39(7) 2_656 . . . ? N8E Cu1B O1B Cu1B 160.24(9) . . . 2_656 ? O1B Cu1B O1B Cu1B -13.51(11) 2_656 . . 2_656 ? N1E Cu1B O1B Cu1B 78.2(3) . . . 2_656 ? O10F Cu1B O1B Cu1B -105.71(8) 2_656 . . 2_656 ? Cu2B Cu1B O1B Cu1B -128.40(11) . . . 2_656 ? N8E Cu1B O1B Cu2B -71.37(9) . . . . ? O1B Cu1B O1B Cu2B 114.88(5) 2_656 . . . ? N1E Cu1B O1B Cu2B -153.4(3) . . . . ? O10F Cu1B O1B Cu2B 22.69(7) 2_656 . . . ? Cu1B Cu1B O1B Cu2B 128.40(11) 2_656 . . . ? N8E Cu1B N1E C2E 170.7(3) . . . . ? O1B Cu1B N1E C2E -16.2(2) 2_656 . . . ? O1B Cu1B N1E C2E -105.6(4) . . . . ? O10F Cu1B N1E C2E 78.6(2) 2_656 . . . ? Cu1B Cu1B N1E C2E -43.5(3) 2_656 . . . ? Cu2B Cu1B N1E C2E 114.5(2) . . . . ? N8E Cu1B N1E C6E -13.26(19) . . . . ? O1B Cu1B N1E C6E 159.79(18) 2_656 . . . ? O1B Cu1B N1E C6E 70.4(4) . . . . ? O10F Cu1B N1E C6E -105.39(19) 2_656 . . . ? Cu1B Cu1B N1E C6E 132.50(16) 2_656 . . . ? Cu2B Cu1B N1E C6E -69.4(3) . . . . ? C6E N1E C2E C3E -1.3(4) . . . . ? Cu1B N1E C2E C3E 174.6(2) . . . . ? N1E C2E C3E C4E 0.0(5) . . . . ? C2E C3E C4E C5E 1.1(5) . . . . ? C3E C4E C5E C6E -1.0(5) . . . . ? C2E N1E C6E C5E 1.3(4) . . . . ? Cu1B N1E C6E C5E -175.0(2) . . . . ? C2E N1E C6E C7E -178.1(3) . . . . ? Cu1B N1E C6E C7E 5.5(3) . . . . ? C4E C5E C6E N1E -0.2(5) . . . . ? C4E C5E C6E C7E 179.2(3) . . . . ? N1E C6E C7E N8E 9.0(3) . . . . ? C5E C6E C7E N8E -170.4(3) . . . . ? C6E C7E N8E C9E 157.1(2) . . . . ? C6E C7E N8E Cu1B -19.7(3) . . . . ? N1E Cu1B N8E C9E -158.2(2) . . . . ? O1B Cu1B N8E C9E 37.8(2) . . . . ? O10F Cu1B N8E C9E -47.4(2) 2_656 . . . ? Cu1B Cu1B N8E C9E 55.2(3) 2_656 . . . ? Cu2B Cu1B N8E C9E -0.3(2) . . . . ? N1E Cu1B N8E C7E 18.38(18) . . . . ? O1B Cu1B N8E C7E -145.57(18) . . . . ? O10F Cu1B N8E C7E 129.24(18) 2_656 . . . ? Cu1B Cu1B N8E C7E -128.17(16) 2_656 . . . ? Cu2B Cu1B N8E C7E 176.27(18) . . . . ? C7E N8E C9E O10E -177.6(3) . . . . ? Cu1B N8E C9E O10E -1.2(4) . . . . ? C7E N8E C9E C11E 2.8(4) . . . . ? Cu1B N8E C9E C11E 179.2(2) . . . . ? N8E C9E O10E Cu2B 3.3(4) . . . . ? C11E C9E O10E Cu2B -177.1(2) . . . . ? O1B Cu2B O10E C9E -42.0(3) . . . . ? N8F Cu2B O10E C9E -170.0(4) . . . . ? N1F Cu2B O10E C9E 142.7(3) . . . . ? O10F Cu2B O10E C9E 40.6(3) 2_656 . . . ? Cu1B Cu2B O10E C9E -2.6(2) . . . . ? O10E C9E C11E C12' 7.0(4) . . . . ? N8E C9E C11E C12' -173.4(3) . . . . ? O10E C9E C11E C12E 18.8(4) . . . . ? N8E C9E C11E C12E -161.6(3) . . . . ? C9E C11E C12E C13E -91.5(3) . . . . ? C9E C11E C12E C17E 88.6(3) . . . . ? C17E C12E C13E C14E 0.1(3) . . . . ? C11E C12E C13E C14E -179.8(2) . . . . ? C12E C13E C14E C15E -0.5(5) . . . . ? C13E C14E C15E C16E 0.6(6) . . . . ? C14E C15E C16E C17E -0.4(6) . . . . ? C15E C16E C17E C12E 0.1(6) . . . . ? C13E C12E C17E C16E 0.1(4) . . . . ? C11E C12E C17E C16E -180.0(3) . . . . ? C9E C11E C12' C13' -88.7(3) . . . . ? C9E C11E C12' C17' 91.4(4) . . . . ? C17' C12' C13' C14' -0.1(3) . . . . ? C11E C12' C13' C14' -180.0(2) . . . . ? C12' C13' C14' C15' -0.2(5) . . . . ? C13' C14' C15' C16' 0.6(6) . . . . ? C14' C15' C16' C17' -0.6(6) . . . . ? C13' C12' C17' C16' 0.0(5) . . . . ? C11E C12' C17' C16' 180.0(3) . . . . ? C15' C16' C17' C12' 0.3(6) . . . . ? O10E Cu2B N1F C2F -24.0(3) . . . . ? N8F Cu2B N1F C2F 166.4(4) . . . . ? O10F Cu2B N1F C2F 65.1(3) 2_656 . . . ? Cu1B Cu2B N1F C2F 39.9(4) . . . . ? O10E Cu2B N1F C6F 156.5(3) . . . . ? N8F Cu2B N1F C6F -13.0(3) . . . . ? O10F Cu2B N1F C6F -114.4(3) 2_656 . . . ? Cu1B Cu2B N1F C6F -139.5(2) . . . . ? C6F N1F C2F C3F 0.9(6) . . . . ? Cu2B N1F C2F C3F -178.5(3) . . . . ? N1F C2F C3F C4F -2.2(7) . . . . ? C2F C3F C4F C5F 2.1(8) . . . . ? C3F C4F C5F C6F -0.8(8) . . . . ? C2F N1F C6F C5F 0.5(6) . . . . ? Cu2B N1F C6F C5F 180.0(3) . . . . ? C2F N1F C6F C7F 178.7(4) . . . . ? Cu2B N1F C6F C7F -1.8(4) . . . . ? C4F C5F C6F N1F -0.5(7) . . . . ? C4F C5F C6F C7F -178.6(4) . . . . ? N1F C6F C7F N8F 21.8(5) . . . . ? C5F C6F C7F N8F -160.0(4) . . . . ? C6F C7F N8F C9F 147.6(3) . . . . ? C6F C7F N8F Cu2B -31.3(4) . . . . ? O10E Cu2B N8F C9F 158.1(3) . . . . ? O1B Cu2B N8F C9F 31.1(3) . . . . ? N1F Cu2B N8F C9F -153.9(3) . . . . ? O10F Cu2B N8F C9F -53.3(3) 2_656 . . . ? Cu1B Cu2B N8F C9F -8.0(3) . . . . ? O10E Cu2B N8F C7F -23.1(5) . . . . ? O1B Cu2B N8F C7F -150.1(2) . . . . ? N1F Cu2B N8F C7F 24.9(3) . . . . ? O10F Cu2B N8F C7F 125.5(2) 2_656 . . . ? Cu1B Cu2B N8F C7F 170.8(2) . . . . ? C7F N8F C9F O10F -175.5(3) . . . . ? Cu2B N8F C9F O10F 3.2(4) . . . . ? C7F N8F C9F C11F 6.7(5) . . . . ? Cu2B N8F C9F C11F -174.6(2) . . . . ? N8F C9F O10F Cu1B -56.1(3) . . . 2_656 ? C11F C9F O10F Cu1B 121.9(2) . . . 2_656 ? N8F C9F O10F Cu2B 81.9(4) . . . 2_656 ? C11F C9F O10F Cu2B -100.1(3) . . . 2_656 ? O10F C9F C11F C12F -64.7(3) . . . . ? N8F C9F C11F C12F 113.3(3) . . . . ? C9F C11F C12F C17F -84.3(3) . . . . ? C9F C11F C12F C13F 94.3(3) . . . . ? C17F C12F C13F C14F -0.2(4) . . . . ? C11F C12F C13F C14F -178.8(3) . . . . ? C12F C13F C14F C15F 1.1(4) . . . . ? C13F C14F C15F C16F -1.0(5) . . . . ? C14F C15F C16F C17F -0.1(5) . . . . ? C13F C12F C17F C16F -0.9(5) . . . . ? C11F C12F C17F C16F 177.7(3) . . . . ? C15F C16F C17F C12F 1.1(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1A H1AO O1G 0.90 2.22 3.023(3) 148.4 . O1A H1AO O2G 0.90 2.22 3.025(2) 148.4 . O2A H2AO O1H 0.90 1.93 2.832(3) 180.0 . O1B H1BO O1I 0.90 1.96 2.833(5) 162.9 . O1B H1BO O1I' 0.90 2.01 2.889(5) 163.9 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.429 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.078 #===END data_bh4175m _database_code_depnum_ccdc_archive 'CCDC 285147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H58 Cu2 N4 O6, 2(C F3 O3 S)' _chemical_formula_sum 'C58 H58 Cu2 F6 N4 O12 S2' _chemical_formula_weight 1308.32 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3265(8) _cell_length_b 12.2802(8) _cell_length_c 12.5623(9) _cell_angle_alpha 83.3530(10) _cell_angle_beta 63.4270(10) _cell_angle_gamma 70.6400(10) _cell_volume 1473.27(18) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8394 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.25 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7433 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_process_details Bruker(2001)SADABS,BrukerAXSInc.,Madison,WI _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17882 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6932 _reflns_number_gt 6774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.7451P] 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 SHELXL _refine_ls_extinction_coef 0.0059(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6932 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.026 _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 Cu1 Cu 1.073809(13) 0.407787(10) 0.405299(11) 0.01654(3) Uani 1 1 d . . . O1 O 0.99853(8) 0.34763(6) 0.31609(7) 0.01855(15) Uani 1 1 d . . . O2 O 1.09284(8) 0.46122(7) 0.53286(7) 0.02043(16) Uani 1 1 d . . . O3 O 1.19000(10) 0.50219(8) 0.25188(8) 0.02899(19) Uani 1 1 d . . . H3 H 1.1845 0.5732 0.2688 0.043 Uiso 1 1 d R . . N1 N 1.24443(9) 0.26975(8) 0.35559(8) 0.01870(18) Uani 1 1 d . . . N2 N 1.01560(9) 0.16163(8) 0.36821(8) 0.01617(17) Uani 1 1 d . . . H2 H 1.0101 0.0938 0.3544 0.026(4) Uiso 1 1 d R . . C1 C 1.37253(12) 0.28102(11) 0.29802(12) 0.0267(3) Uani 1 1 d . . . H1A H 1.3815 0.3561 0.2902 0.032 Uiso 1 1 calc R . . C2 C 1.49119(12) 0.18700(12) 0.25008(12) 0.0303(3) Uani 1 1 d . . . H2A H 1.5804 0.1972 0.2109 0.036 Uiso 1 1 calc R . . C3 C 1.47788(12) 0.07804(11) 0.26015(12) 0.0275(3) Uani 1 1 d . . . H3A H 1.5577 0.0124 0.2257 0.033 Uiso 1 1 calc R . . C4 C 1.34672(11) 0.06552(10) 0.32113(10) 0.0218(2) Uani 1 1 d . . . H4A H 1.3355 -0.0088 0.3297 0.026 Uiso 1 1 calc R . . C5 C 1.23225(10) 0.16331(9) 0.36939(9) 0.01656(19) Uani 1 1 d . . . C6 C 1.08737(10) 0.15608(9) 0.44146(9) 0.0175(2) Uani 1 1 d . . . H6A H 1.0925 0.0827 0.4839 0.021 Uiso 1 1 calc R . . H6B H 1.0328 0.2204 0.5021 0.021 Uiso 1 1 calc R . . C7 C 0.97967(10) 0.25448(9) 0.31019(9) 0.01522(19) Uani 1 1 d . . . C8 C 0.92235(10) 0.24236(9) 0.22256(9) 0.01480(19) Uani 1 1 d . . . C9 C 0.87715(10) 0.13278(9) 0.24514(9) 0.0168(2) Uani 1 1 d . . . C10 C 0.77180(11) 0.12343(10) 0.35728(10) 0.0207(2) Uani 1 1 d . . . H10A H 0.7322 0.1830 0.4167 0.025 Uiso 1 1 calc R . . C11 C 0.72493(12) 0.02826(11) 0.38223(11) 0.0267(2) Uani 1 1 d . . . H11A H 0.6539 0.0229 0.4587 0.032 Uiso 1 1 calc R . . C12 C 0.78119(13) -0.05929(11) 0.29609(12) 0.0290(3) Uani 1 1 d . . . H12A H 0.7498 -0.1249 0.3137 0.035 Uiso 1 1 calc R . . C13 C 0.88305(13) -0.05024(11) 0.18471(12) 0.0281(2) Uani 1 1 d . . . H13A H 0.9209 -0.1093 0.1251 0.034 Uiso 1 1 calc R . . C14 C 0.93089(12) 0.04553(10) 0.15918(11) 0.0228(2) Uani 1 1 d . . . H14A H 1.0009 0.0510 0.0822 0.027 Uiso 1 1 calc R . . C15 C 0.79154(10) 0.34412(9) 0.23808(9) 0.0175(2) Uani 1 1 d . . . C16 C 0.73667(11) 0.34953(10) 0.15671(10) 0.0213(2) Uani 1 1 d . . . H16A H 0.7841 0.2944 0.0921 0.026 Uiso 1 1 calc R . . C17 C 0.61386(12) 0.43443(11) 0.16928(12) 0.0276(3) Uani 1 1 d . . . H17A H 0.5780 0.4370 0.1133 0.033 Uiso 1 1 calc R . . C18 C 0.54321(12) 0.51565(11) 0.26335(13) 0.0314(3) Uani 1 1 d . . . H18A H 0.4594 0.5741 0.2718 0.038 Uiso 1 1 calc R . . C19 C 0.59588(13) 0.51053(11) 0.34416(12) 0.0305(3) Uani 1 1 d . . . H19A H 0.5479 0.5661 0.4085 0.037 Uiso 1 1 calc R . . C20 C 0.71875(12) 0.42500(10) 0.33317(11) 0.0236(2) Uani 1 1 d . . . H20A H 0.7528 0.4220 0.3906 0.028 Uiso 1 1 calc R . . C21 C 1.04879(10) 0.23993(9) 0.10168(9) 0.01613(19) Uani 1 1 d . . . C22 C 1.04886(11) 0.32973(10) 0.02274(10) 0.0193(2) Uani 1 1 d . . . H22A H 0.9655 0.3918 0.0385 0.023 Uiso 1 1 calc R . . C23 C 1.17007(12) 0.32942(11) -0.07907(10) 0.0238(2) Uani 1 1 d . . . H23A H 1.1680 0.3905 -0.1327 0.029 Uiso 1 1 calc R . . C24 C 1.29334(12) 0.24088(11) -0.10259(11) 0.0266(3) Uani 1 1 d . . . H24A H 1.3759 0.2412 -0.1716 0.032 Uiso 1 1 calc R . . C25 C 1.29480(12) 0.15154(11) -0.02396(11) 0.0247(2) Uani 1 1 d . . . H25A H 1.3790 0.0906 -0.0392 0.030 Uiso 1 1 calc R . . C26 C 1.17382(11) 0.15072(10) 0.07692(10) 0.0205(2) Uani 1 1 d . . . H26A H 1.1761 0.0888 0.1296 0.025 Uiso 1 1 calc R . . C27 C 1.2144(2) 0.49228(17) 0.13252(13) 0.0510(4) Uani 1 1 d . . . H27A H 1.3067 0.4982 0.0792 0.076 Uiso 1 1 calc R . . H27B H 1.1435 0.5544 0.1172 0.076 Uiso 1 1 calc R . . H27C H 1.2098 0.4173 0.1182 0.076 Uiso 1 1 calc R . . C28 C 1.14216(14) 0.38461(11) 0.60829(12) 0.0298(3) Uani 1 1 d . . . H28A H 1.1202 0.4276 0.6793 0.045 Uiso 1 1 calc R . . H28B H 1.2431 0.3490 0.5655 0.045 Uiso 1 1 calc R . . H28C H 1.0972 0.3243 0.6322 0.045 Uiso 1 1 calc R . . S1 S 1.23370(3) 0.80843(2) 0.28141(3) 0.02368(6) Uani 1 1 d . . . F1 F 1.22794(10) 0.81393(10) 0.07434(9) 0.0526(3) Uani 1 1 d . . . F2 F 1.41554(9) 0.69738(8) 0.07782(8) 0.0430(2) Uani 1 1 d . . . F3 F 1.37970(9) 0.88102(8) 0.07547(8) 0.0428(2) Uani 1 1 d . . . O4 O 1.17744(11) 0.71372(8) 0.31193(10) 0.0428(3) Uani 1 1 d . . . O5 O 1.13088(9) 0.92176(7) 0.30921(9) 0.0281(2) Uani 1 1 d . . . O6 O 1.34590(10) 0.79432(9) 0.31213(9) 0.0356(2) Uani 1 1 d . . . C29 C 1.31831(13) 0.79985(12) 0.11873(12) 0.0295(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02201(6) 0.01099(6) 0.01767(6) -0.00218(4) -0.00993(5) -0.00375(5) O1 0.0265(3) 0.0123(3) 0.0201(3) -0.0012(3) -0.0123(3) -0.0064(3) O2 0.0284(3) 0.0125(3) 0.0233(3) -0.0027(3) -0.0168(3) -0.0012(3) O3 0.0476(5) 0.0208(4) 0.0229(4) 0.0034(3) -0.0141(3) -0.0189(4) N1 0.0197(4) 0.0157(4) 0.0205(4) -0.0018(3) -0.0077(3) -0.0061(3) N2 0.0186(3) 0.0137(4) 0.0189(4) 0.0005(3) -0.0095(3) -0.0064(3) C1 0.0240(5) 0.0234(5) 0.0334(6) 0.0010(4) -0.0100(4) -0.0117(4) C2 0.0192(5) 0.0352(6) 0.0338(6) -0.0022(5) -0.0078(4) -0.0095(5) C3 0.0192(5) 0.0273(6) 0.0322(6) -0.0099(5) -0.0108(4) 0.0003(4) C4 0.0231(4) 0.0169(5) 0.0281(5) -0.0038(4) -0.0149(4) -0.0025(4) C5 0.0198(4) 0.0160(4) 0.0165(4) -0.0005(3) -0.0097(3) -0.0057(4) C6 0.0200(4) 0.0176(5) 0.0170(4) 0.0025(3) -0.0093(4) -0.0072(4) C7 0.0150(4) 0.0142(4) 0.0142(4) -0.0022(3) -0.0043(3) -0.0038(3) C8 0.0164(4) 0.0124(4) 0.0152(4) -0.0011(3) -0.0066(3) -0.0039(3) C9 0.0189(4) 0.0146(4) 0.0213(4) 0.0019(3) -0.0119(4) -0.0064(3) C10 0.0211(4) 0.0216(5) 0.0222(5) 0.0031(4) -0.0109(4) -0.0086(4) C11 0.0277(5) 0.0299(6) 0.0308(5) 0.0123(4) -0.0172(4) -0.0163(4) C12 0.0360(5) 0.0211(5) 0.0449(6) 0.0119(4) -0.0274(5) -0.0168(4) C13 0.0368(5) 0.0181(5) 0.0380(6) -0.0004(4) -0.0220(5) -0.0105(4) C14 0.0279(5) 0.0185(5) 0.0253(5) -0.0012(4) -0.0131(4) -0.0086(4) C15 0.0158(4) 0.0145(4) 0.0195(5) 0.0029(4) -0.0060(4) -0.0045(3) C16 0.0191(4) 0.0224(5) 0.0223(5) 0.0044(4) -0.0086(4) -0.0082(4) C17 0.0208(5) 0.0312(6) 0.0326(6) 0.0144(5) -0.0143(4) -0.0109(4) C18 0.0188(5) 0.0235(6) 0.0412(7) 0.0110(5) -0.0092(5) -0.0026(4) C19 0.0236(5) 0.0196(5) 0.0330(6) -0.0013(5) -0.0033(5) -0.0002(4) C20 0.0224(5) 0.0188(5) 0.0227(5) -0.0009(4) -0.0062(4) -0.0028(4) C21 0.0176(4) 0.0164(4) 0.0157(4) -0.0026(3) -0.0068(3) -0.0066(3) C22 0.0201(4) 0.0182(5) 0.0192(5) 0.0000(4) -0.0075(4) -0.0068(4) C23 0.0267(5) 0.0257(5) 0.0189(5) 0.0021(4) -0.0068(4) -0.0130(4) C24 0.0219(5) 0.0327(6) 0.0205(5) -0.0047(4) -0.0014(4) -0.0123(4) C25 0.0181(4) 0.0256(6) 0.0245(5) -0.0067(4) -0.0053(4) -0.0031(4) C26 0.0200(4) 0.0188(5) 0.0200(5) -0.0028(4) -0.0075(4) -0.0036(4) C27 0.0801(10) 0.0624(10) 0.0236(6) 0.0095(6) -0.0192(7) -0.0457(8) C28 0.0446(6) 0.0178(5) 0.0352(6) -0.0006(4) -0.0293(5) -0.0023(5) S1 0.02394(12) 0.01213(11) 0.02764(13) -0.00290(10) -0.00443(10) -0.00535(10) F1 0.0421(4) 0.0713(7) 0.0434(5) -0.0159(5) -0.0231(4) -0.0042(5) F2 0.0401(4) 0.0299(4) 0.0346(4) -0.0102(3) -0.0038(4) 0.0046(4) F3 0.0366(4) 0.0352(4) 0.0404(5) 0.0099(4) -0.0041(4) -0.0126(3) O4 0.0428(5) 0.0208(4) 0.0457(6) -0.0095(4) 0.0045(5) -0.0175(4) O5 0.0240(4) 0.0155(4) 0.0367(5) -0.0050(3) -0.0069(3) -0.0032(3) O6 0.0371(5) 0.0266(5) 0.0401(5) -0.0026(4) -0.0195(4) -0.0014(4) C29 0.0258(5) 0.0250(6) 0.0305(6) -0.0033(5) -0.0085(5) -0.0032(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.9213(8) . ? Cu1 O2 1.9283(8) 2_766 ? Cu1 N1 1.9978(9) . ? Cu1 O1 1.9982(8) . ? Cu1 O3 2.2395(9) . ? Cu1 Cu1 2.9604(3) 2_766 ? O1 C7 1.2471(13) . ? O2 C28 1.4191(14) . ? O2 Cu1 1.9283(8) 2_766 ? O3 C27 1.4105(18) . ? O3 H3 0.8970 . ? N1 C5 1.3429(14) . ? N1 C1 1.3486(15) . ? N2 C7 1.3276(14) . ? N2 C6 1.4596(14) . ? N2 H2 0.8973 . ? C1 C2 1.3820(17) . ? C1 H1A 0.9500 . ? C2 C3 1.381(2) . ? C2 H2A 0.9500 . ? C3 C4 1.3869(17) . ? C3 H3A 0.9500 . ? C4 C5 1.3870(14) . ? C4 H4A 0.9500 . ? C5 C6 1.5063(14) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5482(15) . ? C8 C15 1.5379(14) . ? C8 C9 1.5466(15) . ? C8 C21 1.5474(13) . ? C9 C14 1.3899(15) . ? C9 C10 1.4039(15) . ? C10 C11 1.3870(17) . ? C10 H10A 0.9500 . ? C11 C12 1.3896(19) . ? C11 H11A 0.9500 . ? C12 C13 1.3805(19) . ? C12 H12A 0.9500 . ? C13 C14 1.3998(17) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.3942(16) . ? C15 C16 1.4004(17) . ? C16 C17 1.3882(16) . ? C16 H16A 0.9500 . ? C17 C18 1.389(2) . ? C17 H17A 0.9500 . ? C18 C19 1.376(2) . ? C18 H18A 0.9500 . ? C19 C20 1.3969(17) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.3951(15) . ? C21 C26 1.3995(14) . ? C22 C23 1.3954(15) . ? C22 H22A 0.9500 . ? C23 C24 1.3848(17) . ? C23 H23A 0.9500 . ? C24 C25 1.3898(19) . ? C24 H24A 0.9500 . ? C25 C26 1.3915(15) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? S1 O6 1.4391(11) . ? S1 O4 1.4407(10) . ? S1 O5 1.4453(9) . ? S1 C29 1.8267(14) . ? F1 C29 1.3265(18) . ? F2 C29 1.3360(15) . ? F3 C29 1.3298(17) . ? 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 O2 Cu1 O2 79.47(4) . 2_766 ? O2 Cu1 N1 96.49(4) . . ? O2 Cu1 N1 175.08(4) 2_766 . ? O2 Cu1 O1 161.66(3) . . ? O2 Cu1 O1 91.00(3) 2_766 . ? N1 Cu1 O1 92.11(4) . . ? O2 Cu1 O3 101.37(4) . . ? O2 Cu1 O3 94.12(3) 2_766 . ? N1 Cu1 O3 89.42(4) . . ? O1 Cu1 O3 94.86(3) . . ? O2 Cu1 Cu1 39.82(2) . 2_766 ? O2 Cu1 Cu1 39.65(2) 2_766 2_766 ? N1 Cu1 Cu1 136.25(3) . 2_766 ? O1 Cu1 Cu1 128.86(2) . 2_766 ? O3 Cu1 Cu1 100.06(2) . 2_766 ? C7 O1 Cu1 135.45(7) . . ? C28 O2 Cu1 122.50(7) . . ? C28 O2 Cu1 122.23(7) . 2_766 ? Cu1 O2 Cu1 100.53(4) . 2_766 ? C27 O3 Cu1 126.30(9) . . ? C27 O3 H3 110.7 . . ? Cu1 O3 H3 116.2 . . ? C5 N1 C1 118.79(9) . . ? C5 N1 Cu1 119.71(7) . . ? C1 N1 Cu1 121.20(8) . . ? C7 N2 C6 123.45(9) . . ? C7 N2 H2 120.8 . . ? C6 N2 H2 114.9 . . ? N1 C1 C2 122.21(12) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 118.85(11) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.28(11) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 118.88(11) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.91(10) . . ? N1 C5 C6 116.18(9) . . ? C4 C5 C6 121.90(10) . . ? N2 C6 C5 112.59(8) . . ? N2 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O1 C7 N2 123.76(10) . . ? O1 C7 C8 118.49(9) . . ? N2 C7 C8 117.55(9) . . ? C15 C8 C9 105.64(8) . . ? C15 C8 C21 113.17(8) . . ? C9 C8 C21 114.50(8) . . ? C15 C8 C7 111.58(8) . . ? C9 C8 C7 111.35(8) . . ? C21 C8 C7 100.77(8) . . ? C14 C9 C10 118.27(10) . . ? C14 C9 C8 123.67(9) . . ? C10 C9 C8 118.00(9) . . ? C11 C10 C9 120.73(11) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 120.39(11) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 119.51(11) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 120.30(12) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C9 C14 C13 120.77(11) . . ? C9 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C20 C15 C16 118.41(10) . . ? C20 C15 C8 123.97(10) . . ? C16 C15 C8 117.40(9) . . ? C17 C16 C15 120.85(11) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 120.28(13) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C19 C18 C17 119.26(11) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 121.08(12) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C15 C20 C19 120.10(12) . . ? C15 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C26 118.23(9) . . ? C22 C21 C8 122.86(9) . . ? C26 C21 C8 118.44(9) . . ? C21 C22 C23 120.73(10) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C22 120.58(11) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 119.18(10) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C24 C25 C26 120.46(11) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C21 120.82(11) . . ? C25 C26 H26A 119.6 . . ? C21 C26 H26A 119.6 . . ? O3 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O6 S1 O4 114.67(7) . . ? O6 S1 O5 115.05(6) . . ? O4 S1 O5 114.76(6) . . ? O6 S1 C29 103.46(6) . . ? O4 S1 C29 103.21(7) . . ? O5 S1 C29 103.42(6) . . ? F1 C29 F3 107.65(12) . . ? F1 C29 F2 107.62(12) . . ? F3 C29 F2 107.80(10) . . ? F1 C29 S1 111.64(9) . . ? F3 C29 S1 110.89(10) . . ? F2 C29 S1 111.06(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cu1 O1 C7 -67.88(15) . . . . ? O2 Cu1 O1 C7 -125.98(10) 2_766 . . . ? N1 Cu1 O1 C7 50.20(10) . . . . ? O3 Cu1 O1 C7 139.80(9) . . . . ? Cu1 Cu1 O1 C7 -113.12(9) 2_766 . . . ? O2 Cu1 O2 C28 139.60(11) 2_766 . . . ? N1 Cu1 O2 C28 -37.56(9) . . . . ? O1 Cu1 O2 C28 79.90(13) . . . . ? O3 Cu1 O2 C28 -128.27(9) . . . . ? Cu1 Cu1 O2 C28 139.60(11) 2_766 . . . ? O2 Cu1 O2 Cu1 0.0 2_766 . . 2_766 ? N1 Cu1 O2 Cu1 -177.16(4) . . . 2_766 ? O1 Cu1 O2 Cu1 -59.70(11) . . . 2_766 ? O3 Cu1 O2 Cu1 92.13(4) . . . 2_766 ? O2 Cu1 O3 C27 177.50(12) . . . . ? O2 Cu1 O3 C27 -102.43(13) 2_766 . . . ? N1 Cu1 O3 C27 81.00(13) . . . . ? O1 Cu1 O3 C27 -11.08(13) . . . . ? Cu1 Cu1 O3 C27 -141.96(12) 2_766 . . . ? O2 Cu1 N1 C5 113.84(9) . . . . ? O1 Cu1 N1 C5 -49.93(9) . . . . ? O3 Cu1 N1 C5 -144.77(9) . . . . ? Cu1 Cu1 N1 C5 111.21(8) 2_766 . . . ? O2 Cu1 N1 C1 -72.48(10) . . . . ? O1 Cu1 N1 C1 123.75(10) . . . . ? O3 Cu1 N1 C1 28.91(10) . . . . ? Cu1 Cu1 N1 C1 -75.11(11) 2_766 . . . ? C5 N1 C1 C2 1.77(19) . . . . ? Cu1 N1 C1 C2 -171.97(10) . . . . ? N1 C1 C2 C3 0.9(2) . . . . ? C1 C2 C3 C4 -2.0(2) . . . . ? C2 C3 C4 C5 0.61(19) . . . . ? C1 N1 C5 C4 -3.26(17) . . . . ? Cu1 N1 C5 C4 170.57(9) . . . . ? C1 N1 C5 C6 176.07(11) . . . . ? Cu1 N1 C5 C6 -10.10(13) . . . . ? C3 C4 C5 N1 2.09(18) . . . . ? C3 C4 C5 C6 -177.20(11) . . . . ? C7 N2 C6 C5 -65.95(12) . . . . ? N1 C5 C6 N2 90.53(12) . . . . ? C4 C5 C6 N2 -90.15(12) . . . . ? Cu1 O1 C7 N2 -2.61(16) . . . . ? Cu1 O1 C7 C8 -177.37(6) . . . . ? C6 N2 C7 O1 -2.96(15) . . . . ? C6 N2 C7 C8 171.84(8) . . . . ? O1 C7 C8 C15 -50.51(12) . . . . ? N2 C7 C8 C15 134.40(9) . . . . ? O1 C7 C8 C9 -168.28(8) . . . . ? N2 C7 C8 C9 16.63(12) . . . . ? O1 C7 C8 C21 69.88(10) . . . . ? N2 C7 C8 C21 -105.21(10) . . . . ? C15 C8 C9 C14 116.53(11) . . . . ? C21 C8 C9 C14 -8.68(15) . . . . ? C7 C8 C9 C14 -122.17(11) . . . . ? C15 C8 C9 C10 -60.72(12) . . . . ? C21 C8 C9 C10 174.07(9) . . . . ? C7 C8 C9 C10 60.58(12) . . . . ? C14 C9 C10 C11 1.40(17) . . . . ? C8 C9 C10 C11 178.80(10) . . . . ? C9 C10 C11 C12 -0.36(18) . . . . ? C10 C11 C12 C13 -0.83(19) . . . . ? C11 C12 C13 C14 0.95(19) . . . . ? C10 C9 C14 C13 -1.27(17) . . . . ? C8 C9 C14 C13 -178.51(11) . . . . ? C12 C13 C14 C9 0.11(19) . . . . ? C9 C8 C15 C20 109.80(12) . . . . ? C21 C8 C15 C20 -124.17(11) . . . . ? C7 C8 C15 C20 -11.35(14) . . . . ? C9 C8 C15 C16 -64.74(11) . . . . ? C21 C8 C15 C16 61.30(13) . . . . ? C7 C8 C15 C16 174.11(9) . . . . ? C20 C15 C16 C17 0.97(17) . . . . ? C8 C15 C16 C17 175.82(10) . . . . ? C15 C16 C17 C18 -0.04(18) . . . . ? C16 C17 C18 C19 -0.39(19) . . . . ? C17 C18 C19 C20 -0.1(2) . . . . ? C16 C15 C20 C19 -1.49(17) . . . . ? C8 C15 C20 C19 -175.97(11) . . . . ? C18 C19 C20 C15 1.10(19) . . . . ? C15 C8 C21 C22 8.39(15) . . . . ? C9 C8 C21 C22 129.54(11) . . . . ? C7 C8 C21 C22 -110.86(11) . . . . ? C15 C8 C21 C26 -179.60(10) . . . . ? C9 C8 C21 C26 -58.45(13) . . . . ? C7 C8 C21 C26 61.15(12) . . . . ? C26 C21 C22 C23 0.98(17) . . . . ? C8 C21 C22 C23 173.01(11) . . . . ? C21 C22 C23 C24 -1.17(19) . . . . ? C22 C23 C24 C25 0.5(2) . . . . ? C23 C24 C25 C26 0.3(2) . . . . ? C24 C25 C26 C21 -0.44(19) . . . . ? C22 C21 C26 C25 -0.18(17) . . . . ? C8 C21 C26 C25 -172.57(11) . . . . ? O6 S1 C29 F1 -178.61(10) . . . . ? O4 S1 C29 F1 61.58(12) . . . . ? O5 S1 C29 F1 -58.30(11) . . . . ? O6 S1 C29 F3 -58.57(10) . . . . ? O4 S1 C29 F3 -178.38(9) . . . . ? O5 S1 C29 F3 61.73(10) . . . . ? O6 S1 C29 F2 61.27(11) . . . . ? O4 S1 C29 F2 -58.53(12) . . . . ? O5 S1 C29 F2 -178.42(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O4 0.90 1.83 2.7293(14) 175.8 . N2 H2 O5 0.90 2.08 2.8321(12) 140.8 1_545 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.520 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.057 #===END #===END data_bh4177m _database_code_depnum_ccdc_archive 'CCDC 285410' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H49 Cu2 F6 N4 O13.50 S2' _chemical_formula_weight 962.91 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.080(2) _cell_length_b 10.766(3) _cell_length_c 11.438(3) _cell_angle_alpha 76.204(3) _cell_angle_beta 80.283(3) _cell_angle_gamma 77.456(3) _cell_volume 1051.8(4) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6985 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.26 _exptl_crystal_description rod _exptl_crystal_colour blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 497 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6330 _exptl_absorpt_correction_T_max 0.7004 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8881 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4790 _reflns_number_gt 4099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+5.0372P] 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_number_reflns 4790 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1781 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.50831(6) 0.87641(4) 0.59422(5) 0.02479(13) Uani 1 1 d . . . O3 O 0.2914(4) 0.9387(3) 0.7153(3) 0.0346(7) Uani 1 1 d . . . H3 H 0.2583 1.0234 0.6996 0.042 Uiso 1 1 d R . . O1 O 0.6181(3) 0.8109(3) 0.7415(3) 0.0289(6) Uani 1 1 d . . . O2 O 0.4332(3) 0.9564(3) 0.4409(3) 0.0282(6) Uani 1 1 d . . . N1 N 0.4571(4) 0.7019(3) 0.6099(3) 0.0276(7) Uani 1 1 d . . . N2 N 0.7756(4) 0.6216(3) 0.7194(3) 0.0285(8) Uani 1 1 d . . . H2 H 0.8444 0.5567 0.7481 0.043 Uiso 1 1 d R . . C1 C 0.4085(6) 0.8957(4) 0.3515(4) 0.0354(10) Uani 1 1 d . . . H1A H 0.3587 0.9613 0.2879 0.053 Uiso 1 1 calc R . . H1B H 0.3434 0.8314 0.3884 0.053 Uiso 1 1 calc R . . H1C H 0.5062 0.8521 0.3161 0.053 Uiso 1 1 calc R . . C2 C 0.2723(6) 0.8930(5) 0.8423(5) 0.0439(12) Uani 1 1 d . . . H2A H 0.1636 0.9028 0.8721 0.066 Uiso 1 1 calc R . . H2B H 0.3201 0.9436 0.8808 0.066 Uiso 1 1 calc R . . H2C H 0.3201 0.8010 0.8620 0.066 Uiso 1 1 calc R . . C3 C 0.3120(5) 0.6877(4) 0.6227(4) 0.0320(9) Uani 1 1 d . . . H3A H 0.2346 0.7632 0.6127 0.038 Uiso 1 1 calc R . . C4 C 0.2713(5) 0.5666(4) 0.6501(4) 0.0340(10) Uani 1 1 d . . . H4A H 0.1676 0.5588 0.6586 0.041 Uiso 1 1 calc R . . C5 C 0.3846(6) 0.4568(4) 0.6650(4) 0.0339(10) Uani 1 1 d . . . H5A H 0.3596 0.3724 0.6854 0.041 Uiso 1 1 calc R . . C6 C 0.5350(5) 0.4717(4) 0.6497(4) 0.0305(9) Uani 1 1 d . . . H6A H 0.6143 0.3976 0.6590 0.037 Uiso 1 1 calc R . . C7 C 0.5685(5) 0.5959(4) 0.6209(4) 0.0267(8) Uani 1 1 d . . . C8 C 0.7300(5) 0.6192(4) 0.6043(4) 0.0279(9) Uani 1 1 d . . . H8A H 0.7996 0.5494 0.5690 0.033 Uiso 1 1 calc R . . H8B H 0.7376 0.7032 0.5471 0.033 Uiso 1 1 calc R . . C9 C 0.7144(5) 0.7145(4) 0.7814(4) 0.0269(8) Uani 1 1 d . . . C10 C 0.7650(5) 0.6975(4) 0.9060(4) 0.0308(9) Uani 1 1 d . . . C11 C 0.9386(6) 0.6785(6) 0.8935(5) 0.0458(12) Uani 1 1 d . . . H11A H 0.9728 0.7523 0.8348 0.069 Uiso 1 1 calc R . . H11B H 0.9835 0.5978 0.8652 0.069 Uiso 1 1 calc R . . H11C H 0.9707 0.6732 0.9724 0.069 Uiso 1 1 calc R . . C12 C 0.7113(8) 0.5769(5) 0.9885(5) 0.0501(14) Uani 1 1 d . . . H12A H 0.7427 0.5638 1.0691 0.075 Uiso 1 1 calc R . . H12B H 0.7567 0.5004 0.9537 0.075 Uiso 1 1 calc R . . H12C H 0.6002 0.5893 0.9954 0.075 Uiso 1 1 calc R . . C13 C 0.6942(6) 0.8171(5) 0.9596(5) 0.0405(11) Uani 1 1 d . . . H13A H 0.7278 0.8942 0.9062 0.061 Uiso 1 1 calc R . . H13B H 0.7263 0.8049 1.0399 0.061 Uiso 1 1 calc R . . H13C H 0.5832 0.8291 0.9673 0.061 Uiso 1 1 calc R . . S1 S 1.01678(12) 0.28293(9) 0.70623(10) 0.0295(2) Uani 1 1 d . . . F1 F 0.7738(3) 0.2272(3) 0.8506(3) 0.0541(9) Uani 1 1 d . . . F2 F 0.9162(4) 0.0642(3) 0.7854(3) 0.0469(7) Uani 1 1 d . . . F3 F 0.9854(3) 0.1368(3) 0.9224(3) 0.0430(7) Uani 1 1 d . . . O6 O 1.0070(4) 0.3910(3) 0.7641(3) 0.0390(8) Uani 1 1 d . . . O5 O 1.1685(4) 0.2086(3) 0.6883(3) 0.0365(7) Uani 1 1 d . . . O4 O 0.9309(4) 0.3115(3) 0.6050(3) 0.0413(8) Uani 1 1 d . . . C14 C 0.9172(5) 0.1717(4) 0.8224(4) 0.0342(10) Uani 1 1 d . . . O7 O 0.0000 1.0000 0.5000 0.078(4) Uani 0.50 2 d SP A 1 H7B' H 0.0346 0.9912 0.4252 0.118 Uiso 0.25 1 d PR A 1 H7A' H 0.0594 0.9945 0.5551 0.118 Uiso 0.25 1 d PR A 1 O8 O 0.0292(9) 1.1547(9) 0.4228(8) 0.056(2) Uani 0.50 1 d P B 2 H8B' H -0.0259 1.2075 0.4683 0.085 Uiso 0.50 1 d PR B 2 H8A' H 0.0528 1.0699 0.4487 0.085 Uiso 0.50 1 d PR B 2 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 0.0282(3) 0.0150(2) 0.0314(3) -0.00025(18) -0.00902(19) -0.00547(17) O3 0.0385(17) 0.0213(13) 0.0399(17) -0.0031(12) -0.0037(13) -0.0012(12) O1 0.0338(15) 0.0218(13) 0.0324(15) -0.0041(11) -0.0123(12) -0.0034(11) O2 0.0381(15) 0.0182(12) 0.0305(15) -0.0008(11) -0.0127(12) -0.0078(11) N1 0.0326(17) 0.0185(14) 0.0318(18) -0.0020(13) -0.0083(14) -0.0050(13) N2 0.0291(17) 0.0210(15) 0.0345(19) -0.0015(13) -0.0111(14) -0.0021(13) C1 0.048(3) 0.0229(19) 0.038(2) -0.0030(17) -0.014(2) -0.0099(18) C2 0.041(3) 0.039(3) 0.042(3) -0.002(2) -0.001(2) 0.000(2) C3 0.031(2) 0.0253(19) 0.040(2) -0.0041(17) -0.0069(18) -0.0067(16) C4 0.036(2) 0.032(2) 0.036(2) -0.0054(18) -0.0035(18) -0.0151(18) C5 0.049(3) 0.0222(18) 0.033(2) -0.0034(16) -0.0076(19) -0.0129(18) C6 0.042(2) 0.0177(17) 0.032(2) -0.0024(15) -0.0103(18) -0.0055(16) C7 0.033(2) 0.0211(17) 0.0269(19) -0.0039(15) -0.0064(16) -0.0053(15) C8 0.033(2) 0.0204(17) 0.029(2) -0.0018(15) -0.0071(16) -0.0032(15) C9 0.0278(19) 0.0196(16) 0.034(2) -0.0012(15) -0.0067(16) -0.0077(15) C10 0.037(2) 0.0243(18) 0.031(2) -0.0015(16) -0.0098(17) -0.0041(16) C11 0.037(3) 0.053(3) 0.052(3) -0.019(2) -0.017(2) -0.001(2) C12 0.081(4) 0.036(3) 0.033(3) 0.006(2) -0.012(3) -0.021(3) C13 0.047(3) 0.036(2) 0.040(3) -0.012(2) -0.015(2) 0.000(2) S1 0.0303(5) 0.0189(4) 0.0369(6) -0.0007(4) -0.0040(4) -0.0053(4) F1 0.0349(15) 0.0500(18) 0.067(2) 0.0004(16) 0.0043(14) -0.0085(13) F2 0.0541(17) 0.0299(13) 0.0625(19) -0.0028(13) -0.0144(14) -0.0221(12) F3 0.0503(16) 0.0408(15) 0.0351(15) 0.0026(12) -0.0066(12) -0.0132(13) O6 0.0375(17) 0.0222(14) 0.059(2) -0.0095(14) -0.0114(15) -0.0046(12) O5 0.0358(16) 0.0230(14) 0.0453(19) 0.0000(13) 0.0018(14) -0.0072(12) O4 0.050(2) 0.0303(16) 0.0409(18) -0.0011(14) -0.0103(15) -0.0052(14) C14 0.032(2) 0.029(2) 0.041(2) -0.0018(18) -0.0073(18) -0.0099(17) O7 0.061(7) 0.104(9) 0.081(8) -0.069(7) -0.045(6) 0.045(7) O8 0.052(5) 0.060(5) 0.054(5) -0.010(4) -0.010(4) -0.002(4) _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 O2 1.919(3) 2_676 ? Cu1 O2 1.927(3) . ? Cu1 N1 1.992(3) . ? Cu1 O1 2.006(3) . ? Cu1 O3 2.279(3) . ? Cu1 Cu1 2.9916(10) 2_676 ? O3 C2 1.411(6) . ? O3 H3 0.8808 . ? O1 C9 1.251(5) . ? O2 C1 1.407(5) . ? O2 Cu1 1.919(3) 2_676 ? N1 C3 1.339(6) . ? N1 C7 1.347(5) . ? N2 C9 1.332(5) . ? N2 C8 1.453(6) . ? N2 H2 0.8697 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.382(6) . ? C3 H3A 0.9500 . ? C4 C5 1.386(6) . ? C4 H4A 0.9500 . ? C5 C6 1.387(7) . ? C5 H5A 0.9500 . ? C6 C7 1.386(6) . ? C6 H6A 0.9500 . ? C7 C8 1.514(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.529(6) . ? C10 C13 1.527(6) . ? C10 C11 1.532(7) . ? C10 C12 1.533(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? S1 O4 1.440(4) . ? S1 O5 1.443(3) . ? S1 O6 1.449(3) . ? S1 C14 1.823(5) . ? F1 C14 1.330(5) . ? F2 C14 1.327(5) . ? F3 C14 1.328(5) . ? O7 H7B' 0.8803 . ? O7 H7A' 0.8804 . ? O7 H8A' 0.9956 . ? O8 H8B' 0.8801 . ? O8 H8A' 0.8805 . ? 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 O2 Cu1 O2 77.85(14) 2_676 . ? O2 Cu1 N1 173.09(14) 2_676 . ? O2 Cu1 N1 97.25(13) . . ? O2 Cu1 O1 93.48(12) 2_676 . ? O2 Cu1 O1 169.45(13) . . ? N1 Cu1 O1 90.85(13) . . ? O2 Cu1 O3 93.94(12) 2_676 . ? O2 Cu1 O3 97.18(12) . . ? N1 Cu1 O3 91.50(13) . . ? O1 Cu1 O3 89.33(12) . . ? O2 Cu1 Cu1 39.02(9) 2_676 2_676 ? O2 Cu1 Cu1 38.83(8) . 2_676 ? N1 Cu1 Cu1 135.89(11) . 2_676 ? O1 Cu1 Cu1 132.23(9) . 2_676 ? O3 Cu1 Cu1 97.15(8) . 2_676 ? C2 O3 Cu1 123.0(3) . . ? C2 O3 H3 108.3 . . ? Cu1 O3 H3 112.9 . . ? C9 O1 Cu1 137.3(3) . . ? C1 O2 Cu1 123.8(3) . 2_676 ? C1 O2 Cu1 128.4(2) . . ? Cu1 O2 Cu1 102.15(14) 2_676 . ? C3 N1 C7 119.7(4) . . ? C3 N1 Cu1 120.6(3) . . ? C7 N1 Cu1 119.3(3) . . ? C9 N2 C8 123.2(3) . . ? C9 N2 H2 120.5 . . ? C8 N2 H2 116.2 . . ? O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 H2A 109.5 . . ? O3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 122.1(4) . . ? N1 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? N1 C7 C6 121.0(4) . . ? N1 C7 C8 116.9(3) . . ? C6 C7 C8 122.1(4) . . ? N2 C8 C7 110.9(3) . . ? N2 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? O1 C9 N2 122.3(4) . . ? O1 C9 C10 120.7(4) . . ? N2 C9 C10 117.0(3) . . ? C13 C10 C9 110.1(3) . . ? C13 C10 C11 109.7(4) . . ? C9 C10 C11 109.4(4) . . ? C13 C10 C12 109.7(4) . . ? C9 C10 C12 107.9(4) . . ? C11 C10 C12 109.9(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 S1 O5 115.4(2) . . ? O4 S1 O6 115.0(2) . . ? O5 S1 O6 114.0(2) . . ? O4 S1 C14 103.9(2) . . ? O5 S1 C14 103.54(19) . . ? O6 S1 C14 102.7(2) . . ? F2 C14 F3 107.6(4) . . ? F2 C14 F1 108.1(4) . . ? F3 C14 F1 108.5(4) . . ? F2 C14 S1 111.3(3) . . ? F3 C14 S1 110.3(3) . . ? F1 C14 S1 111.0(3) . . ? H7B' O7 H7A' 123.3 . . ? H7B' O7 H8A' 64.1 . . ? H7A' O7 H8A' 87.0 . . ? H8B' O8 H8A' 123.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cu1 O3 C2 -109.9(4) 2_676 . . . ? O2 Cu1 O3 C2 171.9(4) . . . . ? N1 Cu1 O3 C2 74.4(4) . . . . ? O1 Cu1 O3 C2 -16.4(4) . . . . ? Cu1 Cu1 O3 C2 -148.9(4) 2_676 . . . ? O2 Cu1 O1 C9 -127.2(4) 2_676 . . . ? O2 Cu1 O1 C9 -92.8(7) . . . . ? N1 Cu1 O1 C9 47.4(4) . . . . ? O3 Cu1 O1 C9 138.9(4) . . . . ? Cu1 Cu1 O1 C9 -122.0(4) 2_676 . . . ? O2 Cu1 O2 C1 153.7(4) 2_676 . . . ? N1 Cu1 O2 C1 -21.4(4) . . . . ? O1 Cu1 O2 C1 118.4(7) . . . . ? O3 Cu1 O2 C1 -113.8(4) . . . . ? Cu1 Cu1 O2 C1 153.7(4) 2_676 . . . ? O2 Cu1 O2 Cu1 0.0 2_676 . . 2_676 ? N1 Cu1 O2 Cu1 -175.05(15) . . . 2_676 ? O1 Cu1 O2 Cu1 -35.2(7) . . . 2_676 ? O3 Cu1 O2 Cu1 92.50(14) . . . 2_676 ? O2 Cu1 N1 C3 -109.8(11) 2_676 . . . ? O2 Cu1 N1 C3 -65.4(4) . . . . ? O1 Cu1 N1 C3 121.4(3) . . . . ? O3 Cu1 N1 C3 32.1(3) . . . . ? Cu1 Cu1 N1 C3 -69.8(4) 2_676 . . . ? O2 Cu1 N1 C7 77.4(12) 2_676 . . . ? O2 Cu1 N1 C7 121.9(3) . . . . ? O1 Cu1 N1 C7 -51.4(3) . . . . ? O3 Cu1 N1 C7 -140.7(3) . . . . ? Cu1 Cu1 N1 C7 117.4(3) 2_676 . . . ? C7 N1 C3 C4 1.7(7) . . . . ? Cu1 N1 C3 C4 -171.1(4) . . . . ? N1 C3 C4 C5 0.2(7) . . . . ? C3 C4 C5 C6 -1.2(7) . . . . ? C4 C5 C6 C7 0.4(7) . . . . ? C3 N1 C7 C6 -2.4(6) . . . . ? Cu1 N1 C7 C6 170.4(3) . . . . ? C3 N1 C7 C8 179.5(4) . . . . ? Cu1 N1 C7 C8 -7.6(5) . . . . ? C5 C6 C7 N1 1.4(7) . . . . ? C5 C6 C7 C8 179.3(4) . . . . ? C9 N2 C8 C7 -67.1(5) . . . . ? N1 C7 C8 N2 90.6(4) . . . . ? C6 C7 C8 N2 -87.4(5) . . . . ? Cu1 O1 C9 N2 2.0(7) . . . . ? Cu1 O1 C9 C10 -177.0(3) . . . . ? C8 N2 C9 O1 -3.9(6) . . . . ? C8 N2 C9 C10 175.1(4) . . . . ? O1 C9 C10 C13 -5.6(6) . . . . ? N2 C9 C10 C13 175.4(4) . . . . ? O1 C9 C10 C11 -126.3(4) . . . . ? N2 C9 C10 C11 54.7(5) . . . . ? O1 C9 C10 C12 114.1(5) . . . . ? N2 C9 C10 C12 -64.9(5) . . . . ? O4 S1 C14 F2 60.6(4) . . . . ? O5 S1 C14 F2 -60.3(4) . . . . ? O6 S1 C14 F2 -179.3(3) . . . . ? O4 S1 C14 F3 179.9(3) . . . . ? O5 S1 C14 F3 59.0(4) . . . . ? O6 S1 C14 F3 -59.9(3) . . . . ? O4 S1 C14 F1 -59.8(4) . . . . ? O5 S1 C14 F1 179.2(3) . . . . ? O6 S1 C14 F1 60.3(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O5 0.88 1.97 2.840(4) 171.7 1_465 O7 H7B' F2 0.88 2.56 3.424(3) 166.4 2_666 O8 H8B' O4 0.88 2.07 2.896(10) 155.7 1_465 N2 H2 O6 0.87 2.05 2.886(5) 162.1 . _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.762 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.155