# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'M. Hosseini' _publ_contact_author_address ; Laboratoire de Chimie de Coordination Organique Universite Louis Pasteur 4 rue Blaise Pascal 67000 Strasbourg FRANCE ; _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Octanuclear Cu(I) cubic complex decorated with six peripheral chelates ; loop_ _publ_author_name 'M. Hosseini' 'Stephane A. Baudron' 'Nathalie Kyritsakas' ###Material relevant to compound (Et4N)4[Cu8(2)6](THF)6 at 173K ######## data_e461 _database_code_depnum_ccdc_archive 'CCDC 294746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H48 Cu8 S12, 4(C8 H20 N), 6(C4 H8 O)' _chemical_formula_sum 'C138 H176 Cu8 N4 O6 S12' _chemical_formula_weight 2879.87 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0263(5) _cell_length_b 22.3943(7) _cell_length_c 19.7820(8) _cell_angle_alpha 90.00 _cell_angle_beta 112.7590(10) _cell_angle_gamma 90.00 _cell_volume 6546.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5739 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 24.12 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8385 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details sadabs _exptl_special_details ; One of the THF molecules is highly disordered, a disorder model has been designed accordingly. The hydrogen atoms of this molecule have not been introduced but are included in the formula of the compound. The high disorder of the THF molecules is reflected in the high Ueq max/min for the O atoms. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58035 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14973 _reflns_number_gt 8212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1068P)^2^+3.0921P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14973 _refine_ls_number_parameters 721 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1370 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.2115 _refine_ls_wR_factor_gt 0.1757 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7194(4) 0.9683(2) 0.6882(3) 0.0278(12) Uani 1 1 d . . . C2 C 0.7916(4) 0.9599(3) 0.7530(3) 0.0329(13) Uani 1 1 d . . . C3 C 0.8210(4) 0.9033(3) 0.7943(3) 0.0346(14) Uani 1 1 d . . . C4 C 0.7888(4) 0.8453(3) 0.7819(4) 0.0428(16) Uani 1 1 d . . . H4 H 0.7364 0.8363 0.7395 0.051 Uiso 1 1 calc R . . C5 C 0.8325(5) 0.8002(3) 0.8309(4) 0.055(2) Uani 1 1 d . . . H5 H 0.8097 0.7605 0.8219 0.066 Uiso 1 1 calc R . . C6 C 0.9089(5) 0.8124(4) 0.8926(4) 0.063(2) Uani 1 1 d . . . H6 H 0.9374 0.7813 0.9264 0.075 Uiso 1 1 calc R . . C7 C 0.9440(5) 0.8696(3) 0.9056(4) 0.056(2) Uani 1 1 d . . . H7 H 0.9971 0.8782 0.9476 0.067 Uiso 1 1 calc R . . C8 C 0.9010(4) 0.9134(3) 0.8568(3) 0.0416(16) Uani 1 1 d . . . C9 C 0.9239(4) 0.9769(3) 0.8576(4) 0.0479(17) Uani 1 1 d . . . C10 C 0.9951(5) 1.0082(4) 0.9099(4) 0.070(2) Uani 1 1 d . . . H10 H 1.0374 0.9884 0.9515 0.084 Uiso 1 1 calc R . . C11 C 1.0025(6) 1.0691(4) 0.8998(5) 0.085(3) Uani 1 1 d . . . H11 H 1.0509 1.0914 0.9341 0.102 Uiso 1 1 calc R . . C12 C 0.9400(6) 1.0965(3) 0.8404(4) 0.069(2) Uani 1 1 d . . . H12 H 0.9456 1.1382 0.8345 0.082 Uiso 1 1 calc R . . C13 C 0.8684(5) 1.0662(3) 0.7879(4) 0.0508(18) Uani 1 1 d . . . H13 H 0.8263 1.0869 0.7470 0.061 Uiso 1 1 calc R . . C14 C 0.8594(4) 1.0055(3) 0.7964(3) 0.0415(15) Uani 1 1 d . . . C15 C 0.3666(4) 1.0609(2) 0.6249(3) 0.0314(13) Uani 1 1 d . . . C16 C 0.3209(4) 1.0776(3) 0.6678(3) 0.0348(14) Uani 1 1 d . . . C17 C 0.3524(4) 1.0739(3) 0.7489(3) 0.0379(14) Uani 1 1 d . . . C18 C 0.4306(5) 1.0525(3) 0.8032(4) 0.0511(18) Uani 1 1 d . . . H18 H 0.4775 1.0363 0.7906 0.061 Uiso 1 1 calc R . . C19 C 0.4406(5) 1.0546(4) 0.8770(4) 0.061(2) Uani 1 1 d . . . H19 H 0.4949 1.0401 0.9139 0.073 Uiso 1 1 calc R . . C20 C 0.3732(6) 1.0773(4) 0.8974(4) 0.060(2) Uani 1 1 d . . . H20 H 0.3814 1.0790 0.9476 0.072 Uiso 1 1 calc R . . C21 C 0.2929(5) 1.0976(3) 0.8427(4) 0.0500(18) Uani 1 1 d . . . H21 H 0.2450 1.1120 0.8553 0.060 Uiso 1 1 calc R . . C22 C 0.2834(4) 1.0967(3) 0.7703(4) 0.0415(15) Uani 1 1 d . . . C23 C 0.2085(4) 1.1155(3) 0.7052(4) 0.0409(16) Uani 1 1 d . . . C24 C 0.1256(5) 1.1414(3) 0.6987(4) 0.0509(18) Uani 1 1 d . . . H24 H 0.1121 1.1487 0.7407 0.061 Uiso 1 1 calc R . . C25 C 0.0645(5) 1.1560(3) 0.6290(5) 0.058(2) Uani 1 1 d . . . H25 H 0.0082 1.1736 0.6234 0.069 Uiso 1 1 calc R . . C26 C 0.0833(5) 1.1458(3) 0.5680(5) 0.057(2) Uani 1 1 d . . . H26 H 0.0407 1.1570 0.5210 0.068 Uiso 1 1 calc R . . C27 C 0.1651(4) 1.1190(3) 0.5749(4) 0.0465(17) Uani 1 1 d . . . H27 H 0.1767 1.1111 0.5322 0.056 Uiso 1 1 calc R . . C28 C 0.2285(4) 1.1041(3) 0.6423(4) 0.0390(15) Uani 1 1 d . . . C29 C 0.3949(4) 0.8348(2) 0.5047(3) 0.0280(12) Uani 1 1 d . . . C30 C 0.3520(4) 0.7812(3) 0.5013(3) 0.0337(14) Uani 1 1 d . . . C31 C 0.2718(4) 0.7702(3) 0.5195(3) 0.0360(14) Uani 1 1 d . . . C32 C 0.2170(4) 0.8066(3) 0.5423(4) 0.0452(17) Uani 1 1 d . . . H32 H 0.2277 0.8484 0.5481 0.054 Uiso 1 1 calc R . . C33 C 0.1457(5) 0.7806(4) 0.5566(4) 0.057(2) Uani 1 1 d . . . H33 H 0.1091 0.8056 0.5728 0.069 Uiso 1 1 calc R . . C34 C 0.1268(5) 0.7205(4) 0.5482(4) 0.064(2) Uani 1 1 d . . . H34 H 0.0792 0.7042 0.5598 0.077 Uiso 1 1 calc R . . C35 C 0.1778(5) 0.6839(4) 0.5227(4) 0.061(2) Uani 1 1 d . . . H35 H 0.1639 0.6426 0.5150 0.073 Uiso 1 1 calc R . . C36 C 0.2499(5) 0.7077(3) 0.5082(4) 0.0455(17) Uani 1 1 d . . . C37 C 0.3125(5) 0.6793(3) 0.4831(4) 0.0500(18) Uani 1 1 d . . . C38 C 0.3196(6) 0.6199(3) 0.4649(5) 0.065(2) Uani 1 1 d . . . H38 H 0.2769 0.5914 0.4673 0.078 Uiso 1 1 calc R . . C39 C 0.3878(7) 0.6024(3) 0.4435(5) 0.072(3) Uani 1 1 d . . . H39 H 0.3916 0.5620 0.4304 0.086 Uiso 1 1 calc R . . C40 C 0.4497(6) 0.6427(3) 0.4410(4) 0.056(2) Uani 1 1 d . . . H40 H 0.4971 0.6297 0.4270 0.067 Uiso 1 1 calc R . . C41 C 0.4455(5) 0.7030(3) 0.4585(4) 0.0478(17) Uani 1 1 d . . . H41 H 0.4900 0.7304 0.4571 0.057 Uiso 1 1 calc R . . C42 C 0.3757(5) 0.7221(3) 0.4780(3) 0.0425(16) Uani 1 1 d . . . C43 C 0.4799(8) 0.2179(4) 0.2963(6) 0.097(3) Uani 1 1 d . . . H43A H 0.5281 0.1942 0.3336 0.116 Uiso 1 1 calc R . . H43B H 0.4375 0.1897 0.2612 0.116 Uiso 1 1 calc R . . C44 C 0.4260(8) 0.2559(5) 0.3364(5) 0.104(3) Uani 1 1 d . . . H44A H 0.4010 0.2286 0.3624 0.156 Uiso 1 1 calc R . . H44B H 0.3767 0.2782 0.2995 0.156 Uiso 1 1 calc R . . H44C H 0.4678 0.2839 0.3714 0.156 Uiso 1 1 calc R . . C45 C 0.5992(7) 0.2918(5) 0.3111(5) 0.096(3) Uani 1 1 d . . . H45A H 0.5751 0.3160 0.3413 0.115 Uiso 1 1 calc R . . H45B H 0.6428 0.2630 0.3444 0.115 Uiso 1 1 calc R . . C46 C 0.6497(6) 0.3317(4) 0.2824(5) 0.091(2) Uani 1 1 d . . . H46A H 0.6973 0.3518 0.3232 0.137 Uiso 1 1 calc R . . H46B H 0.6085 0.3615 0.2503 0.137 Uiso 1 1 calc R . . H46C H 0.6771 0.3085 0.2543 0.137 Uiso 1 1 calc R . . C47 C 0.5596(7) 0.2136(5) 0.2160(5) 0.098(3) Uani 1 1 d . . . H47A H 0.5085 0.1936 0.1769 0.117 Uiso 1 1 calc R . . H47B H 0.5919 0.2377 0.1919 0.117 Uiso 1 1 calc R . . C48 C 0.6222(8) 0.1669(5) 0.2608(5) 0.104(3) Uani 1 1 d . . . H48A H 0.6433 0.1426 0.2294 0.156 Uiso 1 1 calc R . . H48B H 0.5905 0.1414 0.2834 0.156 Uiso 1 1 calc R . . H48C H 0.6741 0.1859 0.2991 0.156 Uiso 1 1 calc R . . C49 C 0.4598(6) 0.2979(4) 0.2004(5) 0.079(3) Uani 1 1 d . . . H49A H 0.4947 0.3168 0.1743 0.095 Uiso 1 1 calc R . . H49B H 0.4403 0.3300 0.2254 0.095 Uiso 1 1 calc R . . C50 C 0.3761(6) 0.2683(4) 0.1442(5) 0.091(2) Uani 1 1 d . . . H50A H 0.3401 0.2982 0.1088 0.137 Uiso 1 1 calc R . . H50B H 0.3397 0.2510 0.1693 0.137 Uiso 1 1 calc R . . H50C H 0.3945 0.2368 0.1186 0.137 Uiso 1 1 calc R . . C51 C 1.0503(8) -0.0200(5) 0.3520(6) 0.107(3) Uani 1 1 d D . . H51A H 1.0182 -0.0559 0.3255 0.128 Uiso 1 1 calc R . . H51B H 1.0967 -0.0097 0.3325 0.128 Uiso 1 1 calc R . . C52 C 1.0962(7) -0.0353(5) 0.4289(7) 0.131(5) Uani 1 1 d D . . H52A H 1.1387 -0.0681 0.4338 0.196 Uiso 1 1 calc R . . H52B H 1.0515 -0.0477 0.4487 0.196 Uiso 1 1 calc R . . H52C H 1.1294 -0.0004 0.4560 0.196 Uiso 1 1 calc R . . C53 C 1.0281(7) 0.0894(5) 0.3755(7) 0.107(3) Uani 1 1 d . . . H53A H 0.9860 0.1237 0.3641 0.128 Uiso 1 1 calc R . . H53B H 1.0455 0.0802 0.4281 0.128 Uiso 1 1 calc R . . C54 C 1.1091(7) 0.1093(5) 0.3659(7) 0.108(3) Uani 1 1 d . . . H54A H 1.1347 0.1439 0.3976 0.163 Uiso 1 1 calc R . . H54B H 1.0937 0.1205 0.3146 0.163 Uiso 1 1 calc R . . H54C H 1.1536 0.0769 0.3792 0.163 Uiso 1 1 calc R . . C55 C 0.9454(9) 0.0517(6) 0.2566(8) 0.122(3) Uani 1 1 d . . . H55A H 0.9151 0.0911 0.2485 0.147 Uiso 1 1 calc R . . H55B H 0.9985 0.0550 0.2430 0.147 Uiso 1 1 calc R . . C56 C 0.8848(7) 0.0089(5) 0.2111(7) 0.108(3) Uani 1 1 d . . . H56A H 0.8667 0.0207 0.1597 0.163 Uiso 1 1 calc R . . H56B H 0.8311 0.0065 0.2233 0.163 Uiso 1 1 calc R . . H56C H 0.9145 -0.0302 0.2189 0.163 Uiso 1 1 calc R . . C57 C 0.9099(8) 0.0167(6) 0.3603(8) 0.122(3) Uani 1 1 d . . . H57A H 0.9401 0.0128 0.4143 0.147 Uiso 1 1 calc R . . H57B H 0.8886 -0.0235 0.3403 0.147 Uiso 1 1 calc R . . C58 C 0.8244(7) 0.0588(4) 0.3422(7) 0.097(3) Uani 1 1 d . . . H58A H 0.7836 0.0418 0.3634 0.145 Uiso 1 1 calc R . . H58B H 0.7925 0.0621 0.2889 0.145 Uiso 1 1 calc R . . H58C H 0.8442 0.0985 0.3630 0.145 Uiso 1 1 calc R . . C59 C 0.7915(9) 0.7582(5) 0.1354(7) 0.105(4) Uani 1 1 d . . . H59A H 0.8175 0.7189 0.1555 0.126 Uiso 1 1 calc R . . H59B H 0.7607 0.7752 0.1657 0.126 Uiso 1 1 calc R . . C60 C 0.7309(8) 0.7535(5) 0.0600(6) 0.104(4) Uani 1 1 d . . . H60A H 0.6875 0.7871 0.0447 0.125 Uiso 1 1 calc R . . H60B H 0.6975 0.7152 0.0496 0.125 Uiso 1 1 calc R . . C61 C 0.8009(9) 0.7566(6) 0.0244(7) 0.118(4) Uani 1 1 d . . . H61A H 0.8123 0.7165 0.0087 0.142 Uiso 1 1 calc R . . H61B H 0.7801 0.7836 -0.0186 0.142 Uiso 1 1 calc R . . C62 C 0.8762(9) 0.7785(5) 0.0787(7) 0.119(5) Uani 1 1 d . . . H62A H 0.9214 0.7460 0.0965 0.143 Uiso 1 1 calc R . . H62B H 0.9025 0.8101 0.0579 0.143 Uiso 1 1 calc R . . C63 C 0.2736(10) 0.4083(7) 0.5593(10) 0.162(7) Uani 1 1 d . . . H63A H 0.2387 0.3886 0.5847 0.194 Uiso 1 1 calc R . . H63B H 0.2518 0.3925 0.5086 0.194 Uiso 1 1 calc R . . C64 C 0.2575(8) 0.4729(5) 0.5567(8) 0.121(3) Uani 1 1 d . . . H64A H 0.2640 0.4915 0.5136 0.145 Uiso 1 1 calc R . . H64B H 0.1969 0.4823 0.5563 0.145 Uiso 1 1 calc R . . C65 C 0.3270(9) 0.4910(6) 0.6228(8) 0.131(5) Uani 1 1 d . . . H65A H 0.3014 0.5074 0.6572 0.158 Uiso 1 1 calc R . . H65B H 0.3655 0.5219 0.6135 0.158 Uiso 1 1 calc R . . C66 C 0.3802(8) 0.4359(5) 0.6532(8) 0.121(3) Uani 1 1 d . . . H66A H 0.4457 0.4449 0.6745 0.145 Uiso 1 1 calc R . . H66B H 0.3628 0.4186 0.6919 0.145 Uiso 1 1 calc R . . N1 N 0.5208(4) 0.2560(3) 0.2571(3) 0.0519(15) Uani 1 1 d . . . N2 N 0.9755(5) 0.0365(3) 0.3325(4) 0.069(2) Uani 1 1 d . . . O1 O 0.8623(6) 0.7994(6) 0.1315(6) 0.157(4) Uani 1 1 d . . . O2 O 0.3597(7) 0.3952(4) 0.5933(6) 0.141(3) Uani 1 1 d . . . S5 S 0.70440(9) 1.03754(6) 0.64007(8) 0.0316(3) Uani 1 1 d . . . S6 S 0.48027(10) 1.03519(6) 0.66499(8) 0.0312(3) Uani 1 1 d . . . S7 S 0.63830(10) 0.91146(6) 0.64834(8) 0.0319(3) Uani 1 1 d . . . S8 S 0.47430(10) 0.84452(6) 0.46294(8) 0.0317(3) Uani 1 1 d . . . S9 S 0.37293(10) 0.89680(6) 0.55145(8) 0.0308(3) Uani 1 1 d . . . S10 S 0.68431(10) 0.93564(7) 0.47204(8) 0.0327(3) Uani 1 1 d . . . Cu1 Cu 0.58813(5) 0.90763(3) 0.52487(4) 0.03173(19) Uani 1 1 d . . . Cu2 Cu 0.49827(5) 0.95160(3) 0.60804(4) 0.03134(19) Uani 1 1 d . . . Cu3 Cu 0.55998(5) 1.06901(3) 0.60103(4) 0.03150(19) Uani 1 1 d . . . Cu4 Cu 0.65420(5) 1.02080(3) 0.51887(4) 0.03209(19) Uani 1 1 d . . . C67 C 0.8095(9) 0.2839(7) 0.7326(10) 0.086(2) Uiso 0.50 1 d PD . . O3 O 0.9029(8) 0.2919(5) 0.7734(6) 0.086(2) Uiso 0.50 1 d PD . . C69 C 0.8857(11) 0.2195(7) 0.6860(9) 0.086(2) Uiso 0.50 1 d PD . . C68 C 0.8041(10) 0.2233(7) 0.6971(10) 0.086(2) Uiso 0.50 1 d PD . . C70 C 0.9420(9) 0.2685(8) 0.7185(11) 0.086(2) Uiso 0.50 1 d PD . . O3A O 0.8711(17) 0.2971(9) 0.7202(13) 0.086(5) Uiso 0.25 1 d PD . . C68A C 0.897(2) 0.2345(13) 0.6380(18) 0.086(5) Uiso 0.25 1 d PD . . C67A C 0.9255(19) 0.2888(13) 0.675(2) 0.086(5) Uiso 0.25 1 d PD . . C69A C 0.832(2) 0.2071(10) 0.6638(19) 0.086(5) Uiso 0.25 1 d PD . . C70A C 0.7944(17) 0.2604(14) 0.6868(19) 0.086(5) Uiso 0.25 1 d PD . . O4 O 0.9177(9) 0.2478(6) 0.7400(7) 0.021(3) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.028(3) 0.027(3) -0.002(2) 0.007(2) 0.001(2) C2 0.026(3) 0.039(3) 0.028(3) -0.004(3) 0.004(2) 0.002(3) C3 0.031(3) 0.036(3) 0.033(3) 0.004(3) 0.008(3) 0.008(3) C4 0.035(3) 0.037(4) 0.043(4) -0.001(3) 0.000(3) 0.004(3) C5 0.056(4) 0.038(4) 0.051(4) 0.009(3) 0.000(4) 0.013(4) C6 0.059(5) 0.056(5) 0.048(5) 0.015(4) -0.007(4) 0.015(4) C7 0.040(4) 0.055(5) 0.051(4) 0.008(4) -0.005(3) 0.007(4) C8 0.036(3) 0.043(4) 0.034(3) 0.004(3) 0.001(3) -0.001(3) C9 0.031(3) 0.066(5) 0.036(4) -0.003(3) 0.001(3) -0.004(3) C10 0.064(5) 0.071(6) 0.043(4) 0.000(4) -0.015(4) -0.005(5) C11 0.084(6) 0.075(6) 0.050(5) -0.007(4) -0.024(5) -0.021(5) C12 0.080(6) 0.046(4) 0.056(5) -0.008(4) 0.000(4) -0.012(4) C13 0.050(4) 0.041(4) 0.042(4) -0.008(3) -0.003(3) -0.005(3) C14 0.040(3) 0.041(4) 0.035(4) 0.002(3) 0.007(3) 0.006(3) C15 0.035(3) 0.027(3) 0.029(3) 0.001(2) 0.009(3) -0.003(3) C16 0.034(3) 0.027(3) 0.047(4) -0.002(3) 0.019(3) -0.001(3) C17 0.042(4) 0.036(3) 0.039(4) -0.004(3) 0.018(3) -0.006(3) C18 0.052(4) 0.067(5) 0.038(4) 0.003(3) 0.021(3) 0.004(4) C19 0.059(5) 0.083(6) 0.042(4) 0.002(4) 0.021(4) 0.007(4) C20 0.076(5) 0.066(5) 0.047(5) -0.006(4) 0.035(4) -0.004(4) C21 0.062(5) 0.042(4) 0.056(5) -0.012(3) 0.035(4) -0.006(4) C22 0.048(4) 0.033(3) 0.046(4) -0.011(3) 0.021(3) -0.010(3) C23 0.045(4) 0.023(3) 0.064(5) -0.006(3) 0.031(3) -0.002(3) C24 0.053(4) 0.037(4) 0.075(5) -0.013(4) 0.039(4) -0.008(3) C25 0.040(4) 0.051(5) 0.086(6) -0.016(4) 0.028(4) 0.003(4) C26 0.043(4) 0.057(5) 0.065(5) 0.000(4) 0.014(4) 0.009(4) C27 0.041(4) 0.046(4) 0.057(5) -0.003(3) 0.024(3) 0.009(3) C28 0.038(3) 0.025(3) 0.055(4) 0.002(3) 0.020(3) 0.001(3) C29 0.024(3) 0.028(3) 0.025(3) 0.002(2) 0.002(2) 0.001(2) C30 0.033(3) 0.027(3) 0.034(3) -0.001(2) 0.005(3) -0.004(3) C31 0.035(3) 0.037(3) 0.027(3) 0.005(3) 0.002(3) -0.007(3) C32 0.032(3) 0.056(4) 0.042(4) -0.002(3) 0.008(3) -0.012(3) C33 0.037(4) 0.079(6) 0.051(5) -0.003(4) 0.013(3) -0.011(4) C34 0.044(4) 0.079(6) 0.062(5) 0.015(4) 0.012(4) -0.023(4) C35 0.048(4) 0.055(5) 0.065(5) 0.004(4) 0.006(4) -0.018(4) C36 0.044(4) 0.036(4) 0.045(4) 0.003(3) 0.005(3) -0.016(3) C37 0.055(4) 0.032(4) 0.046(4) 0.002(3) 0.000(3) -0.011(3) C38 0.077(6) 0.032(4) 0.073(6) 0.005(4) 0.015(5) -0.015(4) C39 0.101(7) 0.030(4) 0.075(6) 0.001(4) 0.023(5) 0.001(5) C40 0.085(6) 0.025(3) 0.063(5) 0.006(3) 0.033(4) 0.007(4) C41 0.064(5) 0.033(4) 0.046(4) 0.002(3) 0.021(4) 0.006(3) C42 0.055(4) 0.025(3) 0.036(4) 0.003(3) 0.006(3) -0.004(3) C43 0.144(10) 0.060(6) 0.084(7) 0.023(5) 0.041(7) -0.011(6) C44 0.141(7) 0.111(6) 0.064(4) 0.014(4) 0.043(5) 0.063(5) C45 0.095(7) 0.097(7) 0.063(6) 0.021(6) -0.005(5) -0.014(6) C46 0.081(5) 0.085(5) 0.078(5) 0.014(4) -0.002(4) -0.011(4) C47 0.105(8) 0.111(8) 0.069(7) 0.010(6) 0.024(6) 0.043(7) C48 0.141(7) 0.111(6) 0.064(4) 0.014(4) 0.043(5) 0.063(5) C49 0.095(7) 0.061(5) 0.066(6) 0.023(4) 0.015(5) 0.009(5) C50 0.081(5) 0.085(5) 0.078(5) 0.014(4) -0.002(4) -0.011(4) C51 0.103(6) 0.087(6) 0.123(7) -0.003(5) 0.035(5) -0.027(5) C52 0.072(7) 0.113(10) 0.208(17) 0.017(10) 0.054(9) -0.007(7) C53 0.103(6) 0.087(6) 0.123(7) -0.003(5) 0.035(5) -0.027(5) C54 0.105(6) 0.092(5) 0.136(7) -0.029(5) 0.054(5) -0.057(5) C55 0.122(7) 0.122(7) 0.137(8) -0.027(6) 0.066(6) -0.009(6) C56 0.105(6) 0.092(5) 0.136(7) -0.029(5) 0.054(5) -0.057(5) C57 0.122(7) 0.122(7) 0.137(8) -0.027(6) 0.066(6) -0.009(6) C58 0.088(7) 0.061(6) 0.142(10) -0.002(6) 0.045(7) 0.023(6) C59 0.130(10) 0.089(8) 0.109(10) -0.007(7) 0.061(8) 0.022(7) C60 0.126(9) 0.117(9) 0.090(8) -0.043(7) 0.065(8) -0.043(8) C61 0.133(11) 0.108(9) 0.107(10) -0.019(8) 0.039(9) -0.007(8) C62 0.141(11) 0.098(8) 0.081(8) -0.042(7) 0.003(8) -0.008(8) C63 0.118(12) 0.162(15) 0.26(2) 0.015(14) 0.136(14) -0.010(11) C64 0.092(6) 0.075(6) 0.185(11) 0.002(6) 0.040(6) -0.013(5) C65 0.103(9) 0.151(13) 0.146(13) 0.025(10) 0.054(9) -0.009(9) C66 0.092(6) 0.075(6) 0.185(11) 0.002(6) 0.040(6) -0.013(5) N1 0.063(4) 0.045(3) 0.036(3) 0.007(3) 0.007(3) 0.015(3) N2 0.082(5) 0.064(4) 0.083(5) -0.035(4) 0.057(4) -0.037(4) O1 0.083(5) 0.278(13) 0.130(8) -0.050(9) 0.063(6) -0.016(7) O2 0.136(8) 0.119(7) 0.183(10) -0.051(7) 0.077(7) -0.031(6) S5 0.0279(7) 0.0299(8) 0.0292(7) 0.0013(6) 0.0024(6) -0.0016(6) S6 0.0306(7) 0.0301(8) 0.0301(8) -0.0024(6) 0.0086(6) 0.0007(6) S7 0.0304(7) 0.0284(8) 0.0291(7) 0.0022(6) 0.0028(6) 0.0013(6) S8 0.0327(8) 0.0250(7) 0.0333(8) -0.0016(6) 0.0082(6) -0.0007(6) S9 0.0315(8) 0.0272(7) 0.0308(8) 0.0004(6) 0.0087(6) -0.0014(6) S10 0.0288(7) 0.0335(8) 0.0331(8) 0.0008(6) 0.0091(6) 0.0049(7) Cu1 0.0310(4) 0.0297(4) 0.0298(4) 0.0001(3) 0.0066(3) -0.0006(3) Cu2 0.0296(4) 0.0275(4) 0.0314(4) -0.0011(3) 0.0058(3) 0.0008(3) Cu3 0.0295(4) 0.0298(4) 0.0314(4) 0.0015(3) 0.0075(3) 0.0011(3) Cu4 0.0326(4) 0.0277(4) 0.0310(4) 0.0017(3) 0.0069(3) 0.0016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.367(7) . ? C1 S7 1.771(6) . ? C1 S5 1.787(6) . ? C2 C3 1.483(8) . ? C2 C14 1.496(9) . ? C3 C4 1.384(8) . ? C3 C8 1.414(8) . ? C4 C5 1.388(9) . ? C4 H4 0.9500 . ? C5 C6 1.382(10) . ? C5 H5 0.9500 . ? C6 C7 1.383(11) . ? C6 H6 0.9500 . ? C7 C8 1.361(9) . ? C7 H7 0.9500 . ? C8 C9 1.466(10) . ? C9 C10 1.397(10) . ? C9 C14 1.406(9) . ? C10 C11 1.390(12) . ? C10 H10 0.9500 . ? C11 C12 1.361(11) . ? C11 H11 0.9500 . ? C12 C13 1.390(9) . ? C12 H12 0.9500 . ? C13 C14 1.385(9) . ? C13 H13 0.9500 . ? C15 C16 1.371(8) . ? C15 S10 1.772(6) 3_676 ? C15 S6 1.778(6) . ? C16 C17 1.486(9) . ? C16 C28 1.491(8) . ? C17 C18 1.383(9) . ? C17 C22 1.421(9) . ? C18 C19 1.407(9) . ? C18 H18 0.9500 . ? C19 C20 1.388(10) . ? C19 H19 0.9500 . ? C20 C21 1.399(10) . ? C20 H20 0.9500 . ? C21 C22 1.381(9) . ? C21 H21 0.9500 . ? C22 C23 1.443(9) . ? C23 C24 1.409(9) . ? C23 C28 1.422(9) . ? C24 C25 1.387(11) . ? C24 H24 0.9500 . ? C25 C26 1.370(11) . ? C25 H25 0.9500 . ? C26 C27 1.400(9) . ? C26 H26 0.9500 . ? C27 C28 1.369(9) . ? C27 H27 0.9500 . ? C29 C30 1.371(8) . ? C29 S9 1.777(6) . ? C29 S8 1.778(6) . ? C30 C31 1.484(9) . ? C30 C42 1.498(9) . ? C31 C32 1.394(9) . ? C31 C36 1.439(9) . ? C32 C33 1.405(9) . ? C32 H32 0.9500 . ? C33 C34 1.377(11) . ? C33 H33 0.9500 . ? C34 C35 1.383(11) . ? C34 H34 0.9500 . ? C35 C36 1.399(10) . ? C35 H35 0.9500 . ? C36 C37 1.430(11) . ? C37 C38 1.394(10) . ? C37 C42 1.426(9) . ? C38 C39 1.373(12) . ? C38 H38 0.9500 . ? C39 C40 1.355(11) . ? C39 H39 0.9500 . ? C40 C41 1.402(9) . ? C40 H40 0.9500 . ? C41 C42 1.383(10) . ? C41 H41 0.9500 . ? C43 N1 1.467(11) . ? C43 C44 1.621(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.459(13) . ? C45 N1 1.524(10) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.481(12) . ? C47 N1 1.529(11) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N1 1.500(9) . ? C49 C50 1.523(12) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.450(9) . ? C51 N2 1.681(13) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.452(13) . ? C53 N2 1.512(12) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.413(14) . ? C55 N2 1.428(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N2 1.433(12) . ? C57 C58 1.586(14) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.434(14) . ? C59 O1 1.487(14) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.539(15) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.359(14) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O1 1.242(13) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 O2 1.312(16) . ? C63 C64 1.467(17) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.410(17) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.488(16) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O2 1.429(15) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? S5 Cu4 2.2458(16) . ? S5 Cu3 2.2511(16) . ? S6 Cu3 2.2488(17) . ? S6 Cu2 2.2599(16) . ? S7 Cu2 2.2573(16) . ? S7 Cu1 2.2584(16) . ? S8 Cu1 2.2577(16) . ? S8 Cu3 2.2618(16) 3_676 ? S9 Cu2 2.2482(16) . ? S9 Cu4 2.2498(16) 3_676 ? S10 C15 1.772(6) 3_676 ? S10 Cu4 2.2525(16) . ? S10 Cu1 2.2600(17) . ? Cu1 Cu3 2.7452(10) 3_676 ? Cu1 Cu2 2.7541(10) . ? Cu1 Cu4 2.7668(10) . ? Cu2 Cu4 2.8124(9) 3_676 ? Cu2 Cu3 2.8313(10) . ? Cu3 S8 2.2618(16) 3_676 ? Cu3 Cu1 2.7452(10) 3_676 ? Cu3 Cu4 2.8260(10) . ? Cu4 S9 2.2498(16) 3_676 ? Cu4 Cu2 2.8124(9) 3_676 ? C67 O3 1.411(14) . ? C67 C68 1.514(14) . ? O3 C70 1.541(14) . ? C69 C70 1.409(14) . ? C69 C68 1.410(13) . ? O3A C70A 1.413(17) . ? O3A C67A 1.478(16) . ? C68A C67A 1.406(15) . ? C68A C69A 1.468(16) . ? C69A C70A 1.484(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 C2 C1 S7 121.9(4) . . ? C2 C1 S5 120.6(4) . . ? S7 C1 S5 117.5(3) . . ? C1 C2 C3 127.3(5) . . ? C1 C2 C14 127.5(6) . . ? C3 C2 C14 105.2(5) . . ? C4 C3 C8 117.1(5) . . ? C4 C3 C2 133.4(5) . . ? C8 C3 C2 109.4(5) . . ? C3 C4 C5 120.5(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.5(7) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.4(7) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 118.5(6) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C3 123.0(6) . . ? C7 C8 C9 129.4(6) . . ? C3 C8 C9 107.6(5) . . ? C10 C9 C14 121.7(7) . . ? C10 C9 C8 128.6(7) . . ? C14 C9 C8 109.6(5) . . ? C11 C10 C9 118.6(7) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C12 C11 C10 119.4(7) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 123.0(8) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 118.9(7) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C9 118.4(6) . . ? C13 C14 C2 133.4(6) . . ? C9 C14 C2 108.2(6) . . ? C16 C15 S10 121.7(5) . 3_676 ? C16 C15 S6 120.9(5) . . ? S10 C15 S6 117.4(3) 3_676 . ? C15 C16 C17 127.9(6) . . ? C15 C16 C28 126.7(6) . . ? C17 C16 C28 105.4(5) . . ? C18 C17 C22 118.0(6) . . ? C18 C17 C16 133.2(6) . . ? C22 C17 C16 108.8(5) . . ? C17 C18 C19 120.0(7) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 121.6(7) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 118.8(7) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 119.8(7) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C17 121.9(6) . . ? C21 C22 C23 129.8(6) . . ? C17 C22 C23 108.3(6) . . ? C24 C23 C28 121.2(7) . . ? C24 C23 C22 129.1(7) . . ? C28 C23 C22 109.7(6) . . ? C25 C24 C23 117.8(7) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C26 C25 C24 121.7(7) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C27 120.1(7) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.9(7) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C23 118.3(6) . . ? C27 C28 C16 133.9(6) . . ? C23 C28 C16 107.8(6) . . ? C30 C29 S9 120.8(5) . . ? C30 C29 S8 121.3(5) . . ? S9 C29 S8 117.9(3) . . ? C29 C30 C31 126.8(6) . . ? C29 C30 C42 127.3(6) . . ? C31 C30 C42 105.9(5) . . ? C32 C31 C36 118.2(6) . . ? C32 C31 C30 134.0(6) . . ? C36 C31 C30 107.8(6) . . ? C31 C32 C33 119.1(7) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 122.6(8) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C33 C34 C35 119.3(7) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 120.1(7) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 130.3(7) . . ? C35 C36 C31 120.6(7) . . ? C37 C36 C31 109.0(6) . . ? C38 C37 C42 119.5(8) . . ? C38 C37 C36 130.7(7) . . ? C42 C37 C36 109.7(6) . . ? C39 C38 C37 120.3(7) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 120.2(7) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 121.7(8) . . ? C39 C40 H40 119.1 . . ? C41 C40 H40 119.1 . . ? C42 C41 C40 119.2(7) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C41 C42 C37 118.9(6) . . ? C41 C42 C30 133.4(6) . . ? C37 C42 C30 107.5(6) . . ? N1 C43 C44 112.7(7) . . ? N1 C43 H43A 109.1 . . ? C44 C43 H43A 109.1 . . ? N1 C43 H43B 109.1 . . ? C44 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N1 118.7(8) . . ? C46 C45 H45A 107.6 . . ? N1 C45 H45A 107.6 . . ? C46 C45 H45B 107.6 . . ? N1 C45 H45B 107.6 . . ? H45A C45 H45B 107.1 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N1 116.2(8) . . ? C48 C47 H47A 108.2 . . ? N1 C47 H47A 108.2 . . ? C48 C47 H47B 108.2 . . ? N1 C47 H47B 108.2 . . ? H47A C47 H47B 107.4 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N1 C49 C50 114.1(7) . . ? N1 C49 H49A 108.7 . . ? C50 C49 H49A 108.7 . . ? N1 C49 H49B 108.7 . . ? C50 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N2 116.5(10) . . ? C52 C51 H51A 108.2 . . ? N2 C51 H51A 108.2 . . ? C52 C51 H51B 108.2 . . ? N2 C51 H51B 108.2 . . ? H51A C51 H51B 107.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N2 119.9(10) . . ? C54 C53 H53A 107.3 . . ? N2 C53 H53A 107.3 . . ? C54 C53 H53B 107.3 . . ? N2 C53 H53B 107.3 . . ? H53A C53 H53B 106.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N2 112.2(11) . . ? C56 C55 H55A 109.2 . . ? N2 C55 H55A 109.2 . . ? C56 C55 H55B 109.2 . . ? N2 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N2 C57 C58 115.3(10) . . ? N2 C57 H57A 108.4 . . ? C58 C57 H57A 108.4 . . ? N2 C57 H57B 108.4 . . ? C58 C57 H57B 108.4 . . ? H57A C57 H57B 107.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 O1 102.5(10) . . ? C60 C59 H59A 111.3 . . ? O1 C59 H59A 111.3 . . ? C60 C59 H59B 111.3 . . ? O1 C59 H59B 111.3 . . ? H59A C59 H59B 109.2 . . ? C59 C60 C61 98.7(10) . . ? C59 C60 H60A 112.0 . . ? C61 C60 H60A 112.0 . . ? C59 C60 H60B 112.0 . . ? C61 C60 H60B 112.0 . . ? H60A C60 H60B 109.7 . . ? C62 C61 C60 103.7(11) . . ? C62 C61 H61A 111.0 . . ? C60 C61 H61A 111.0 . . ? C62 C61 H61B 111.0 . . ? C60 C61 H61B 111.0 . . ? H61A C61 H61B 109.0 . . ? O1 C62 C61 114.0(14) . . ? O1 C62 H62A 108.7 . . ? C61 C62 H62A 108.7 . . ? O1 C62 H62B 108.7 . . ? C61 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? O2 C63 C64 112.0(13) . . ? O2 C63 H63A 109.2 . . ? C64 C63 H63A 109.2 . . ? O2 C63 H63B 109.2 . . ? C64 C63 H63B 109.2 . . ? H63A C63 H63B 107.9 . . ? C65 C64 C63 100.7(13) . . ? C65 C64 H64A 111.6 . . ? C63 C64 H64A 111.6 . . ? C65 C64 H64B 111.6 . . ? C63 C64 H64B 111.6 . . ? H64A C64 H64B 109.4 . . ? C64 C65 C66 105.1(13) . . ? C64 C65 H65A 110.7 . . ? C66 C65 H65A 110.7 . . ? C64 C65 H65B 110.7 . . ? C66 C65 H65B 110.7 . . ? H65A C65 H65B 108.8 . . ? O2 C66 C65 106.4(12) . . ? O2 C66 H66A 110.5 . . ? C65 C66 H66A 110.5 . . ? O2 C66 H66B 110.5 . . ? C65 C66 H66B 110.5 . . ? H66A C66 H66B 108.6 . . ? C43 N1 C49 117.7(7) . . ? C43 N1 C45 110.6(7) . . ? C49 N1 C45 108.5(6) . . ? C43 N1 C47 106.1(7) . . ? C49 N1 C47 105.8(6) . . ? C45 N1 C47 107.7(7) . . ? C55 N2 C57 118.5(9) . . ? C55 N2 C53 107.0(8) . . ? C57 N2 C53 111.0(8) . . ? C55 N2 C51 110.0(8) . . ? C57 N2 C51 104.1(8) . . ? C53 N2 C51 105.5(7) . . ? C62 O1 C59 101.4(12) . . ? C63 O2 C66 98.1(11) . . ? C1 S5 Cu4 110.07(19) . . ? C1 S5 Cu3 111.25(19) . . ? Cu4 S5 Cu3 77.87(5) . . ? C15 S6 Cu3 110.3(2) . . ? C15 S6 Cu2 110.61(19) . . ? Cu3 S6 Cu2 77.80(5) . . ? C1 S7 Cu2 109.19(19) . . ? C1 S7 Cu1 113.72(19) . . ? Cu2 S7 Cu1 75.16(5) . . ? C29 S8 Cu1 113.42(19) . . ? C29 S8 Cu3 107.59(18) . 3_676 ? Cu1 S8 Cu3 74.81(5) . 3_676 ? C29 S9 Cu2 111.50(19) . . ? C29 S9 Cu4 110.42(19) . 3_676 ? Cu2 S9 Cu4 77.40(5) . 3_676 ? C15 S10 Cu4 109.0(2) 3_676 . ? C15 S10 Cu1 113.7(2) 3_676 . ? Cu4 S10 Cu1 75.63(5) . . ? S8 Cu1 S7 119.04(6) . . ? S8 Cu1 S10 118.38(6) . . ? S7 Cu1 S10 117.93(6) . . ? S8 Cu1 Cu3 52.66(4) . 3_676 ? S7 Cu1 Cu3 142.66(5) . 3_676 ? S10 Cu1 Cu3 91.87(5) . 3_676 ? S8 Cu1 Cu2 92.78(5) . . ? S7 Cu1 Cu2 52.40(4) . . ? S10 Cu1 Cu2 141.71(5) . . ? Cu3 Cu1 Cu2 90.31(3) 3_676 . ? S8 Cu1 Cu4 142.42(5) . . ? S7 Cu1 Cu4 91.69(5) . . ? S10 Cu1 Cu4 52.06(4) . . ? Cu3 Cu1 Cu4 89.86(3) 3_676 . ? Cu2 Cu1 Cu4 89.73(3) . . ? S9 Cu2 S7 122.22(6) . . ? S9 Cu2 S6 116.02(6) . . ? S7 Cu2 S6 117.06(6) . . ? S9 Cu2 Cu1 94.61(5) . . ? S7 Cu2 Cu1 52.44(4) . . ? S6 Cu2 Cu1 142.28(5) . . ? S9 Cu2 Cu4 51.32(4) . 3_676 ? S7 Cu2 Cu4 143.56(5) . 3_676 ? S6 Cu2 Cu4 91.64(4) . 3_676 ? Cu1 Cu2 Cu4 91.13(3) . 3_676 ? S9 Cu2 Cu3 138.09(5) . . ? S7 Cu2 Cu3 93.94(5) . . ? S6 Cu2 Cu3 50.92(4) . . ? Cu1 Cu2 Cu3 91.69(3) . . ? Cu4 Cu2 Cu3 87.22(3) 3_676 . ? S6 Cu3 S5 115.72(6) . . ? S6 Cu3 S8 122.37(6) . 3_676 ? S5 Cu3 S8 117.06(6) . 3_676 ? S6 Cu3 Cu1 95.43(5) . 3_676 ? S5 Cu3 Cu1 141.66(5) . 3_676 ? S8 Cu3 Cu1 52.53(4) 3_676 3_676 ? S6 Cu3 Cu4 137.83(5) . . ? S5 Cu3 Cu4 50.98(4) . . ? S8 Cu3 Cu4 94.22(5) 3_676 . ? Cu1 Cu3 Cu4 91.03(3) 3_676 . ? S6 Cu3 Cu2 51.28(4) . . ? S5 Cu3 Cu2 91.42(5) . . ? S8 Cu3 Cu2 143.97(5) 3_676 . ? Cu1 Cu3 Cu2 91.47(3) 3_676 . ? Cu4 Cu3 Cu2 87.02(3) . . ? S5 Cu4 S9 115.27(6) . 3_676 ? S5 Cu4 S10 122.35(6) . . ? S9 Cu4 S10 117.46(6) 3_676 . ? S5 Cu4 Cu1 95.29(5) . . ? S9 Cu4 Cu1 142.39(5) 3_676 . ? S10 Cu4 Cu1 52.31(4) . . ? S5 Cu4 Cu2 138.16(5) . 3_676 ? S9 Cu4 Cu2 51.27(4) 3_676 3_676 ? S10 Cu4 Cu2 93.97(5) . 3_676 ? Cu1 Cu4 Cu2 91.42(3) . 3_676 ? S5 Cu4 Cu3 51.15(4) . . ? S9 Cu4 Cu3 91.36(5) 3_676 . ? S10 Cu4 Cu3 143.81(5) . . ? Cu1 Cu4 Cu3 91.53(3) . . ? Cu2 Cu4 Cu3 87.50(3) 3_676 . ? O3 C67 C68 103.8(8) . . ? C67 O3 C70 100.6(8) . . ? C70 C69 C68 110.5(7) . . ? C69 C68 C67 103.6(7) . . ? C69 C70 O3 102.9(8) . . ? C70A O3A C67A 104.8(10) . . ? C67A C68A C69A 107.9(9) . . ? C68A C67A O3A 106.2(7) . . ? C68A C69A C70A 101.4(11) . . ? O3A C70A C69A 103.3(12) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.610 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.126 ###Material relevant to compound (Et4N)4[Cu8(1)6](DMSO)6 at 173K ######## data_e419b _database_code_depnum_ccdc_archive 'CCDC 294747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H36 Cu8 N12 S12, 4(C8 H20 N), 6(C2 H6 O S)' _chemical_formula_sum 'C116 H152 Cu8 N16 O6 S18' _chemical_formula_weight 2951.94 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' 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 Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' 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 39.0401(13) _cell_length_b 17.3267(6) _cell_length_c 24.2754(8) _cell_angle_alpha 90.00 _cell_angle_beta 124.138(2) _cell_angle_gamma 90.00 _cell_volume 13591.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5518 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 24.26 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6112 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7561 _exptl_absorpt_correction_T_max 0.8855 _exptl_absorpt_process_details sadabs _exptl_special_details ; Two of the three independent DMSO molecules show severe positional disorder. This disorder has been modeled accordingly over two positions. The corresponding atoms have been thus refined using isotropic thermal parameters and hydrogen atoms were not introduced on these atoms. Note however that the hydrogen atoms have been introduced in the formula and the moiety of the compound. A void is detected in the checkcif, however no relevant electron density can be assigned to any additional molecule ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77661 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 30.02 _reflns_number_total 19820 _reflns_number_gt 11777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1411P)^2^+13.1410P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19820 _refine_ls_number_parameters 724 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2466 _refine_ls_wR_factor_gt 0.2064 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.184279(17) 0.81176(3) 0.45692(3) 0.02753(14) Uani 1 1 d . . . Cu2 Cu 0.240483(17) 0.85215(3) 0.42783(3) 0.02873(15) Uani 1 1 d . . . Cu3 Cu 0.193578(18) 0.65818(3) 0.43891(3) 0.02853(15) Uani 1 1 d . . . Cu4 Cu 0.248634(17) 0.80378(3) 0.59099(3) 0.02863(15) Uani 1 1 d . . . S1 S 0.26980(4) 0.94700(6) 0.50369(6) 0.0280(2) Uani 1 1 d . . . S2 S 0.20720(3) 0.90469(6) 0.53578(6) 0.0272(2) Uani 1 1 d . . . S3 S 0.15066(3) 0.70869(7) 0.46307(6) 0.0276(2) Uani 1 1 d . . . S4 S 0.17110(4) 0.84602(6) 0.35645(6) 0.0280(2) Uani 1 1 d . . . S5 S 0.18275(3) 0.67622(6) 0.33918(5) 0.0273(2) Uani 1 1 d . . . S6 S 0.27720(4) 0.80101(7) 0.39086(6) 0.0282(2) Uani 1 1 d . . . N1 N 0.27601(17) 1.2494(3) 0.5921(2) 0.0481(12) Uani 1 1 d . . . N2 N 0.21021(17) 1.2120(3) 0.6140(3) 0.0544(13) Uani 1 1 d . . . N3 N 0.11333(16) 0.6158(3) 0.6779(2) 0.0502(12) Uani 1 1 d . . . N4 N 0.04835(14) 0.5771(3) 0.5341(2) 0.0408(10) Uani 1 1 d . . . N5 N 0.06545(14) 0.8736(3) 0.0774(2) 0.0414(10) Uani 1 1 d . . . N6 N 0.06814(15) 0.7006(3) 0.0643(2) 0.0443(11) Uani 1 1 d . . . C1 C 0.23804(13) 0.9756(2) 0.5305(2) 0.0255(9) Uani 1 1 d . . . C2 C 0.23770(14) 1.0515(3) 0.5479(2) 0.0295(10) Uani 1 1 d . . . C3 C 0.26441(15) 1.1151(3) 0.5529(2) 0.0306(10) Uani 1 1 d . . . C4 C 0.29413(18) 1.1230(3) 0.5388(3) 0.0442(13) Uani 1 1 d . . . H4 H 0.3008 1.0817 0.5219 0.053 Uiso 1 1 calc R . . C5 C 0.3138(2) 1.1943(4) 0.5504(3) 0.0567(16) Uani 1 1 d . . . H5 H 0.3328 1.2021 0.5393 0.068 Uiso 1 1 calc R . . C6 C 0.3045(2) 1.2538(3) 0.5787(3) 0.0567(17) Uani 1 1 d . . . H6 H 0.3193 1.2996 0.5888 0.068 Uiso 1 1 calc R . . C7 C 0.25698(17) 1.1810(3) 0.5791(2) 0.0370(11) Uani 1 1 d . . . C8 C 0.21302(15) 1.0858(3) 0.5709(2) 0.0325(10) Uani 1 1 d . . . C9 C 0.18138(17) 1.0575(3) 0.5765(3) 0.0461(14) Uani 1 1 d . . . H9 H 0.1716 1.0072 0.5642 0.055 Uiso 1 1 calc R . . C10 C 0.1653(2) 1.1076(4) 0.6013(4) 0.0623(18) Uani 1 1 d . . . H10 H 0.1442 1.0913 0.6056 0.075 Uiso 1 1 calc R . . C11 C 0.1808(2) 1.1823(4) 0.6196(4) 0.072(2) Uani 1 1 d . . . H11 H 0.1699 1.2139 0.6370 0.086 Uiso 1 1 calc R . . C12 C 0.22485(17) 1.1628(3) 0.5893(3) 0.0360(11) Uani 1 1 d . . . C13 C 0.16952(14) 0.6881(2) 0.5469(2) 0.0263(9) Uani 1 1 d . . . C14 C 0.14303(15) 0.6619(2) 0.5638(2) 0.0273(9) Uani 1 1 d . . . C15 C 0.15158(15) 0.6570(3) 0.6303(2) 0.0316(10) Uani 1 1 d . . . C16 C 0.18491(18) 0.6795(3) 0.6942(3) 0.0426(12) Uani 1 1 d . . . H16 H 0.2090 0.6995 0.7006 0.051 Uiso 1 1 calc R . . C17 C 0.1811(2) 0.6712(4) 0.7473(3) 0.0573(17) Uani 1 1 d . . . H17 H 0.2021 0.6881 0.7896 0.069 Uiso 1 1 calc R . . C18 C 0.1458(2) 0.6375(4) 0.7367(3) 0.0619(18) Uani 1 1 d . . . H18 H 0.1447 0.6295 0.7736 0.074 Uiso 1 1 calc R . . C19 C 0.11674(16) 0.6255(3) 0.6268(3) 0.0362(11) Uani 1 1 d . . . C20 C 0.10022(15) 0.6319(3) 0.5187(2) 0.0319(10) Uani 1 1 d . . . C21 C 0.07409(17) 0.6195(3) 0.4504(3) 0.0430(13) Uani 1 1 d . . . H21 H 0.0822 0.6333 0.4223 0.052 Uiso 1 1 calc R . . C22 C 0.03561(17) 0.5858(4) 0.4251(3) 0.0477(14) Uani 1 1 d . . . H22 H 0.0176 0.5770 0.3797 0.057 Uiso 1 1 calc R . . C23 C 0.02429(17) 0.5655(3) 0.4681(3) 0.0438(13) Uani 1 1 d . . . H23 H -0.0014 0.5426 0.4502 0.053 Uiso 1 1 calc R . . C24 C 0.08536(15) 0.6087(3) 0.5578(3) 0.0320(10) Uani 1 1 d . . . C25 C 0.15864(14) 0.7662(2) 0.3037(2) 0.0264(9) Uani 1 1 d . . . C26 C 0.13108(14) 0.7725(3) 0.2360(2) 0.0300(10) Uani 1 1 d . . . C27 C 0.11174(14) 0.8430(3) 0.1961(2) 0.0312(10) Uani 1 1 d . . . C28 C 0.11431(16) 0.9223(3) 0.2118(3) 0.0365(11) Uani 1 1 d . . . H28 H 0.1305 0.9395 0.2556 0.044 Uiso 1 1 calc R . . C29 C 0.09166(17) 0.9733(3) 0.1592(3) 0.0436(13) Uani 1 1 d . . . H29 H 0.0923 1.0257 0.1680 0.052 Uiso 1 1 calc R . . C30 C 0.06802(17) 0.9474(3) 0.0936(3) 0.0435(13) Uani 1 1 d . . . H30 H 0.0534 0.9834 0.0597 0.052 Uiso 1 1 calc R . . C31 C 0.08709(15) 0.8246(3) 0.1278(2) 0.0321(10) Uani 1 1 d . . . C32 C 0.11464(14) 0.7088(3) 0.1864(2) 0.0305(10) Uani 1 1 d . . . C33 C 0.11705(17) 0.6282(3) 0.1896(3) 0.0405(12) Uani 1 1 d . . . H33 H 0.1329 0.6033 0.2305 0.049 Uiso 1 1 calc R . . C34 C 0.09599(18) 0.5864(3) 0.1321(3) 0.0468(14) Uani 1 1 d . . . H34 H 0.0970 0.5327 0.1337 0.056 Uiso 1 1 calc R . . C35 C 0.07297(18) 0.6241(4) 0.0710(3) 0.0484(14) Uani 1 1 d . . . H35 H 0.0602 0.5943 0.0325 0.058 Uiso 1 1 calc R . . C36 C 0.08866(15) 0.7405(3) 0.1214(2) 0.0340(10) Uani 1 1 d . . . N7 N 0.99978(16) 0.2288(3) 0.3683(2) 0.0523(13) Uani 1 1 d . . . C37 C 1.0015(2) 0.1626(5) 0.4084(3) 0.0616(19) Uani 1 1 d . . . H37A H 0.9760 0.1614 0.4067 0.074 Uiso 1 1 calc R . . H37B H 1.0241 0.1706 0.4545 0.074 Uiso 1 1 calc R . . C38 C 1.0071(3) 0.0854(5) 0.3858(5) 0.090(3) Uani 1 1 d . . . H38A H 1.0074 0.0454 0.4133 0.135 Uiso 1 1 calc R . . H38B H 1.0329 0.0852 0.3893 0.135 Uiso 1 1 calc R . . H38C H 0.9848 0.0767 0.3403 0.135 Uiso 1 1 calc R . . C39 C 0.9641(3) 0.2237(4) 0.2943(3) 0.070(2) Uani 1 1 d . . . H39A H 0.9631 0.2713 0.2724 0.084 Uiso 1 1 calc R . . H39B H 0.9699 0.1821 0.2739 0.084 Uiso 1 1 calc R . . C40 C 0.9224(3) 0.2102(6) 0.2818(4) 0.096(3) Uani 1 1 d . . . H40A H 0.9019 0.2073 0.2348 0.144 Uiso 1 1 calc R . . H40B H 0.9158 0.2520 0.3003 0.144 Uiso 1 1 calc R . . H40C H 0.9227 0.1627 0.3025 0.144 Uiso 1 1 calc R . . C41 C 0.9934(2) 0.3006(5) 0.3991(3) 0.068(2) Uani 1 1 d . . . H41A H 0.9675 0.2945 0.3954 0.082 Uiso 1 1 calc R . . H41B H 1.0154 0.3019 0.4461 0.082 Uiso 1 1 calc R . . C42 C 0.9926(3) 0.3782(5) 0.3689(4) 0.080(2) Uani 1 1 d . . . H42A H 0.9883 0.4186 0.3915 0.120 Uiso 1 1 calc R . . H42B H 0.9705 0.3787 0.3226 0.120 Uiso 1 1 calc R . . H42C H 1.0185 0.3863 0.3738 0.120 Uiso 1 1 calc R . . C43 C 1.0398(2) 0.2371(6) 0.3691(4) 0.094(2) Uani 1 1 d . . . H43A H 1.0416 0.1938 0.3455 0.112 Uiso 1 1 calc R . . H43B H 1.0380 0.2839 0.3456 0.112 Uiso 1 1 calc R . . C44 C 1.0788(2) 0.2401(6) 0.4390(4) 0.094(2) Uani 1 1 d . . . H44A H 1.1025 0.2447 0.4367 0.141 Uiso 1 1 calc R . . H44B H 1.0811 0.1936 0.4623 0.141 Uiso 1 1 calc R . . H44C H 1.0776 0.2838 0.4621 0.141 Uiso 1 1 calc R . . N8 N 0.25178(16) 0.4390(3) 0.7025(3) 0.0525(13) Uani 1 1 d . . . C45 C 0.2769(2) 0.4815(4) 0.6818(4) 0.0578(16) Uani 1 1 d . . . H45A H 0.2598 0.5220 0.6507 0.069 Uiso 1 1 calc R . . H45B H 0.3003 0.5061 0.7208 0.069 Uiso 1 1 calc R . . C46 C 0.2931(3) 0.4320(5) 0.6499(4) 0.083(2) Uani 1 1 d . . . H46A H 0.3085 0.4634 0.6386 0.124 Uiso 1 1 calc R . . H46B H 0.2703 0.4085 0.6104 0.124 Uiso 1 1 calc R . . H46C H 0.3108 0.3925 0.6806 0.124 Uiso 1 1 calc R . . C47 C 0.2122(2) 0.4074(4) 0.6429(4) 0.071(2) Uani 1 1 d . . . H47A H 0.1981 0.3783 0.6586 0.086 Uiso 1 1 calc R . . H47B H 0.2193 0.3716 0.6201 0.086 Uiso 1 1 calc R . . C48 C 0.1822(2) 0.4669(4) 0.5928(3) 0.0605(17) Uani 1 1 d . . . H48A H 0.1582 0.4412 0.5568 0.091 Uiso 1 1 calc R . . H48B H 0.1954 0.4954 0.5757 0.091 Uiso 1 1 calc R . . H48C H 0.1740 0.5018 0.6142 0.091 Uiso 1 1 calc R . . C49 C 0.2751(2) 0.3703(4) 0.7465(4) 0.084(3) Uani 1 1 d . . . H49A H 0.2814 0.3354 0.7221 0.101 Uiso 1 1 calc R . . H49B H 0.2571 0.3430 0.7556 0.101 Uiso 1 1 calc R . . C50 C 0.3156(2) 0.3906(5) 0.8131(4) 0.089(3) Uani 1 1 d . . . H50A H 0.3289 0.3440 0.8371 0.134 Uiso 1 1 calc R . . H50B H 0.3095 0.4224 0.8390 0.134 Uiso 1 1 calc R . . H50C H 0.3336 0.4180 0.8048 0.134 Uiso 1 1 calc R . . C51 C 0.2437(2) 0.4996(4) 0.7408(4) 0.0615(17) Uani 1 1 d . . . H51A H 0.2702 0.5190 0.7776 0.074 Uiso 1 1 calc R . . H51B H 0.2288 0.5427 0.7113 0.074 Uiso 1 1 calc R . . C52 C 0.2196(3) 0.4709(7) 0.7679(4) 0.104(3) Uani 1 1 d . . . H52A H 0.2161 0.5121 0.7907 0.157 Uiso 1 1 calc R . . H52B H 0.2344 0.4293 0.7984 0.157 Uiso 1 1 calc R . . H52C H 0.1930 0.4529 0.7319 0.157 Uiso 1 1 calc R . . S7A S 0.42191(14) 0.6825(3) 0.4628(2) 0.0805(17) Uiso 0.539(8) 1 d P A 1 C53A C 0.4026(4) 0.6327(8) 0.4998(7) 0.068(4) Uiso 0.539(8) 1 d P A 1 S7B S 0.4457(3) 0.6286(7) 0.5017(6) 0.168(4) Uiso 0.461(8) 1 d P A 2 C53B C 0.4318(7) 0.5888(14) 0.5439(12) 0.104(7) Uiso 0.461(8) 1 d P A 2 O1 O 0.4268(3) 0.6301(6) 0.4272(5) 0.148(3) Uani 1 1 d . . . C54 C 0.4708(3) 0.7017(6) 0.5302(5) 0.098(3) Uani 1 1 d . . . C55 C 0.3888(7) 0.0222(15) 0.5984(12) 0.263(10) Uiso 1 1 d . . . S8A S 0.4281(3) 0.0356(6) 0.6721(5) 0.1191(14) Uiso 0.336(5) 1 d P B 3 O2A O 0.4480(5) 0.0992(10) 0.7022(8) 0.063(4) Uiso 0.336(5) 1 d P B 3 C56A C 0.4227(9) -0.0110(17) 0.7344(15) 0.092(8) Uiso 0.336(5) 1 d P B 3 S8B S 0.40144(16) 0.0726(3) 0.6700(3) 0.1191(14) Uiso 0.664(5) 1 d P B 4 O2B O 0.4316(4) 0.1288(8) 0.6933(7) 0.125(4) Uiso 0.664(5) 1 d P B 4 C56B C 0.3903(6) -0.0011(11) 0.6861(10) 0.122(6) Uiso 0.664(5) 1 d P B 4 S9 S 0.09009(10) 0.03017(19) 0.31873(15) 0.1106(9) Uani 1 1 d . . . O3 O 0.0593(2) 0.0840(4) 0.3061(4) 0.125(3) Uani 1 1 d . . . C57 C 0.0694(4) -0.0608(8) 0.3171(8) 0.168(6) Uani 1 1 d . . . H57A H 0.0479 -0.0739 0.2721 0.253 Uiso 1 1 calc R . . H57B H 0.0582 -0.0591 0.3435 0.253 Uiso 1 1 calc R . . H57C H 0.0909 -0.0990 0.3349 0.253 Uiso 1 1 calc R . . C58 C 0.1237(3) 0.0265(8) 0.4004(5) 0.133(4) Uani 1 1 d . . . H58A H 0.1400 0.0728 0.4154 0.200 Uiso 1 1 calc R . . H58B H 0.1414 -0.0174 0.4118 0.200 Uiso 1 1 calc R . . H58C H 0.1090 0.0221 0.4215 0.200 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0308(3) 0.0242(3) 0.0264(3) -0.0020(2) 0.0153(2) -0.0020(2) Cu2 0.0299(3) 0.0269(3) 0.0274(3) -0.0036(2) 0.0149(2) -0.0008(2) Cu3 0.0308(3) 0.0278(3) 0.0259(3) -0.0007(2) 0.0152(2) 0.0005(2) Cu4 0.0289(3) 0.0251(3) 0.0281(3) -0.0008(2) 0.0138(2) -0.0013(2) S1 0.0327(6) 0.0224(5) 0.0287(6) -0.0022(4) 0.0170(5) -0.0017(4) S2 0.0297(6) 0.0220(5) 0.0297(6) -0.0026(4) 0.0165(5) -0.0006(4) S3 0.0278(5) 0.0294(6) 0.0258(5) -0.0002(4) 0.0152(5) -0.0029(4) S4 0.0295(6) 0.0254(5) 0.0233(5) -0.0017(4) 0.0113(5) 0.0007(4) S5 0.0288(6) 0.0249(5) 0.0218(5) -0.0024(4) 0.0103(5) -0.0001(4) S6 0.0289(6) 0.0296(6) 0.0266(6) -0.0005(5) 0.0159(5) -0.0022(4) N1 0.067(3) 0.023(2) 0.046(3) -0.003(2) 0.027(3) -0.009(2) N2 0.064(3) 0.034(2) 0.071(4) -0.010(2) 0.042(3) 0.001(2) N3 0.055(3) 0.062(3) 0.045(3) 0.005(2) 0.035(3) -0.008(2) N4 0.039(2) 0.038(2) 0.046(3) 0.007(2) 0.025(2) -0.0019(19) N5 0.038(2) 0.045(3) 0.027(2) 0.008(2) 0.0103(19) 0.001(2) N6 0.048(3) 0.043(3) 0.026(2) -0.0061(19) 0.010(2) -0.007(2) C1 0.028(2) 0.023(2) 0.023(2) 0.0007(17) 0.0128(18) 0.0007(17) C2 0.033(2) 0.022(2) 0.029(2) -0.0005(18) 0.014(2) -0.0018(18) C3 0.033(2) 0.023(2) 0.027(2) 0.0018(18) 0.011(2) -0.0015(18) C4 0.051(3) 0.030(3) 0.056(3) -0.003(2) 0.032(3) -0.007(2) C5 0.062(4) 0.044(3) 0.069(4) -0.005(3) 0.040(4) -0.018(3) C6 0.077(4) 0.023(3) 0.054(4) -0.006(3) 0.027(3) -0.017(3) C7 0.049(3) 0.021(2) 0.029(2) -0.0007(19) 0.015(2) 0.001(2) C8 0.033(2) 0.024(2) 0.032(2) -0.0039(19) 0.014(2) 0.0043(19) C9 0.045(3) 0.039(3) 0.063(4) -0.009(3) 0.035(3) 0.003(2) C10 0.062(4) 0.048(4) 0.095(5) -0.016(4) 0.055(4) 0.003(3) C11 0.082(5) 0.045(4) 0.101(6) -0.017(4) 0.060(5) 0.015(4) C12 0.046(3) 0.021(2) 0.037(3) -0.005(2) 0.020(2) 0.003(2) C13 0.030(2) 0.023(2) 0.025(2) 0.0003(17) 0.0147(19) 0.0007(17) C14 0.036(2) 0.021(2) 0.027(2) -0.0037(18) 0.019(2) -0.0042(18) C15 0.037(3) 0.028(2) 0.034(3) 0.000(2) 0.023(2) -0.002(2) C16 0.043(3) 0.051(3) 0.036(3) 0.000(3) 0.023(3) -0.006(3) C17 0.057(4) 0.080(5) 0.034(3) 0.000(3) 0.025(3) -0.009(3) C18 0.064(4) 0.087(5) 0.047(4) 0.008(4) 0.038(4) -0.008(4) C19 0.039(3) 0.034(3) 0.039(3) 0.005(2) 0.024(2) -0.003(2) C20 0.034(3) 0.028(2) 0.036(3) 0.000(2) 0.021(2) -0.0016(19) C21 0.043(3) 0.054(3) 0.036(3) -0.007(3) 0.025(3) -0.018(3) C22 0.042(3) 0.055(3) 0.043(3) -0.011(3) 0.022(3) -0.017(3) C23 0.037(3) 0.039(3) 0.057(4) 0.001(3) 0.027(3) -0.011(2) C24 0.034(2) 0.026(2) 0.042(3) 0.002(2) 0.024(2) -0.0028(19) C25 0.028(2) 0.023(2) 0.024(2) -0.0024(17) 0.0127(19) -0.0015(17) C26 0.031(2) 0.028(2) 0.026(2) -0.0023(19) 0.013(2) -0.0058(19) C27 0.027(2) 0.034(3) 0.026(2) 0.0014(19) 0.0104(19) -0.0039(19) C28 0.040(3) 0.031(2) 0.030(2) 0.003(2) 0.014(2) 0.005(2) C29 0.047(3) 0.030(3) 0.045(3) 0.004(2) 0.021(3) 0.005(2) C30 0.040(3) 0.039(3) 0.038(3) 0.013(2) 0.014(2) 0.003(2) C31 0.030(2) 0.034(2) 0.028(2) 0.003(2) 0.014(2) 0.000(2) C32 0.025(2) 0.033(2) 0.025(2) -0.0009(19) 0.0089(19) 0.0001(19) C33 0.048(3) 0.029(3) 0.028(3) -0.002(2) 0.012(2) 0.002(2) C34 0.052(3) 0.034(3) 0.032(3) -0.011(2) 0.010(3) -0.004(2) C35 0.053(3) 0.049(3) 0.027(3) -0.011(2) 0.013(3) -0.006(3) C36 0.031(2) 0.039(3) 0.022(2) 0.002(2) 0.009(2) -0.001(2) N7 0.054(3) 0.075(4) 0.028(2) -0.011(2) 0.023(2) -0.013(3) C37 0.045(3) 0.090(5) 0.048(4) 0.023(4) 0.025(3) 0.004(3) C38 0.077(6) 0.079(6) 0.121(8) 0.036(6) 0.058(6) 0.013(5) C39 0.104(6) 0.053(4) 0.023(3) -0.006(3) 0.018(3) 0.000(4) C40 0.071(6) 0.106(7) 0.059(5) -0.018(5) 0.004(4) 0.022(5) C41 0.060(4) 0.106(6) 0.039(3) -0.032(4) 0.029(3) -0.011(4) C42 0.104(6) 0.066(5) 0.083(6) -0.027(4) 0.061(5) -0.025(4) C43 0.070(4) 0.143(6) 0.094(4) -0.039(4) 0.062(3) -0.032(4) C44 0.070(4) 0.143(6) 0.094(4) -0.039(4) 0.062(3) -0.032(4) N8 0.058(3) 0.024(2) 0.062(3) 0.007(2) 0.025(3) 0.000(2) C45 0.068(4) 0.040(3) 0.069(4) -0.001(3) 0.040(4) 0.002(3) C46 0.087(6) 0.078(5) 0.071(5) -0.010(4) 0.037(5) 0.029(4) C47 0.059(4) 0.038(3) 0.076(5) 0.001(3) 0.013(4) -0.008(3) C48 0.065(4) 0.052(4) 0.061(4) 0.007(3) 0.032(4) 0.006(3) C49 0.071(5) 0.033(3) 0.095(6) 0.023(4) 0.014(4) 0.000(3) C50 0.071(5) 0.061(5) 0.082(6) 0.018(4) 0.010(4) 0.001(4) C51 0.073(5) 0.056(4) 0.063(4) 0.009(3) 0.043(4) 0.000(3) C52 0.078(6) 0.161(10) 0.069(5) 0.030(6) 0.038(5) -0.025(6) O1 0.167(8) 0.159(8) 0.165(8) -0.050(7) 0.123(7) -0.020(6) C54 0.076(6) 0.112(8) 0.111(8) -0.016(6) 0.055(6) -0.005(5) S9 0.122(2) 0.125(2) 0.1011(19) 0.0285(17) 0.0727(18) 0.0370(19) O3 0.136(6) 0.125(6) 0.125(6) 0.064(5) 0.081(5) 0.084(5) C57 0.114(9) 0.184(15) 0.239(17) -0.007(13) 0.119(11) -0.046(9) C58 0.112(9) 0.155(11) 0.090(8) 0.003(8) 0.030(7) 0.020(8) _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 S2 2.2663(12) . ? Cu1 S3 2.2704(12) . ? Cu1 S4 2.2709(13) . ? Cu1 Cu2 2.7462(8) . ? Cu1 Cu3 2.7536(8) . ? Cu1 Cu4 2.7833(8) . ? Cu2 S1 2.2441(13) . ? Cu2 S4 2.2547(13) . ? Cu2 S6 2.2560(13) . ? Cu2 Cu3 2.7886(8) 7_566 ? Cu2 Cu4 2.8119(8) 7_566 ? Cu3 S5 2.2337(12) . ? Cu3 S3 2.2406(13) . ? Cu3 S1 2.2518(13) 7_566 ? Cu3 Cu2 2.7886(8) 7_566 ? Cu3 Cu4 2.8088(8) 7_566 ? Cu4 S6 2.2375(13) 7_566 ? Cu4 S2 2.2443(12) . ? Cu4 S5 2.2523(13) 7_566 ? Cu4 Cu3 2.8088(8) 7_566 ? Cu4 Cu2 2.8119(8) 7_566 ? S1 C1 1.765(4) . ? S1 Cu3 2.2518(13) 7_566 ? S2 C1 1.775(4) . ? S3 C13 1.768(5) . ? S4 C25 1.757(4) . ? S5 C25 1.774(5) . ? S5 Cu4 2.2523(13) 7_566 ? S6 C13 1.766(5) 7_566 ? S6 Cu4 2.2375(13) 7_566 ? N1 C6 1.325(9) . ? N1 C7 1.340(6) . ? N2 C11 1.331(9) . ? N2 C12 1.341(7) . ? N3 C18 1.325(8) . ? N3 C19 1.332(7) . ? N4 C24 1.336(6) . ? N4 C23 1.341(7) . ? N5 C30 1.324(7) . ? N5 C31 1.332(6) . ? N6 C35 1.336(8) . ? N6 C36 1.338(6) . ? C1 C2 1.383(6) . ? C2 C3 1.475(6) . ? C2 C8 1.482(7) . ? C3 C4 1.389(7) . ? C3 C7 1.415(7) . ? C4 C5 1.398(8) . ? C4 H4 0.9300 . ? C5 C6 1.394(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.442(8) . ? C8 C12 1.400(7) . ? C8 C9 1.406(7) . ? C9 C10 1.391(8) . ? C9 H9 0.9300 . ? C10 C11 1.393(9) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C13 C14 1.386(6) . ? C13 S6 1.766(5) 7_566 ? C14 C15 1.457(6) . ? C14 C20 1.486(7) . ? C15 C16 1.409(7) . ? C15 C19 1.422(7) . ? C16 C17 1.385(8) . ? C16 H16 0.9300 . ? C17 C18 1.384(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.445(7) . ? C20 C21 1.393(7) . ? C20 C24 1.419(7) . ? C21 C22 1.392(7) . ? C21 H21 0.9300 . ? C22 C23 1.387(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C26 1.374(6) . ? C26 C27 1.476(7) . ? C26 C32 1.486(6) . ? C27 C31 1.408(7) . ? C27 C28 1.415(7) . ? C28 C29 1.387(7) . ? C28 H28 0.9300 . ? C29 C30 1.394(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.470(7) . ? C32 C33 1.400(7) . ? C32 C36 1.423(6) . ? C33 C34 1.364(7) . ? C33 H33 0.9300 . ? C34 C35 1.392(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? N7 C37 1.484(8) . ? N7 C39 1.539(8) . ? N7 C41 1.541(9) . ? N7 C43 1.559(8) . ? C37 C38 1.509(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.497(12) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.522(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.517(12) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? N8 C47 1.507(8) . ? N8 C49 1.514(8) . ? N8 C45 1.522(8) . ? N8 C51 1.548(9) . ? C45 C46 1.510(9) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.523(9) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.539(10) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.502(10) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? S7A O1 1.340(9) . ? S7A C53A 1.696(15) . ? S7A C54 1.709(11) . ? S7B C54 1.509(14) . ? S7B O1 1.525(13) . ? S7B C53B 1.56(3) . ? C55 S8A 1.59(2) . ? C55 S8B 1.75(2) . ? S8A O2A 1.310(17) . ? S8A C56A 1.83(3) . ? S8B O2B 1.382(13) . ? S8B C56B 1.472(19) . ? S9 O3 1.412(6) . ? S9 C58 1.654(11) . ? S9 C57 1.761(13) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? 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 S2 Cu1 S3 118.17(5) . . ? S2 Cu1 S4 117.75(5) . . ? S3 Cu1 S4 119.04(5) . . ? S2 Cu1 Cu2 92.43(4) . . ? S3 Cu1 Cu2 142.39(4) . . ? S4 Cu1 Cu2 52.37(3) . . ? S2 Cu1 Cu3 142.75(4) . . ? S3 Cu1 Cu3 51.89(3) . . ? S4 Cu1 Cu3 93.03(4) . . ? Cu2 Cu1 Cu3 90.57(2) . . ? S2 Cu1 Cu4 51.54(3) . . ? S3 Cu1 Cu4 93.43(4) . . ? S4 Cu1 Cu4 141.32(4) . . ? Cu2 Cu1 Cu4 89.21(2) . . ? Cu3 Cu1 Cu4 91.42(2) . . ? S1 Cu2 S4 120.31(5) . . ? S1 Cu2 S6 117.95(5) . . ? S4 Cu2 S6 115.67(5) . . ? S1 Cu2 Cu1 95.10(4) . . ? S4 Cu2 Cu1 52.91(3) . . ? S6 Cu2 Cu1 141.25(4) . . ? S1 Cu2 Cu3 51.79(3) . 7_566 ? S4 Cu2 Cu3 144.82(4) . 7_566 ? S6 Cu2 Cu3 93.29(4) . 7_566 ? Cu1 Cu2 Cu3 92.07(2) . 7_566 ? S1 Cu2 Cu4 141.53(4) . 7_566 ? S4 Cu2 Cu4 93.20(4) . 7_566 ? S6 Cu2 Cu4 50.97(3) . 7_566 ? Cu1 Cu2 Cu4 90.70(2) . 7_566 ? Cu3 Cu2 Cu4 90.09(2) 7_566 7_566 ? S5 Cu3 S3 120.97(5) . . ? S5 Cu3 S1 116.89(5) . 7_566 ? S3 Cu3 S1 117.55(5) . 7_566 ? S5 Cu3 Cu1 94.31(4) . . ? S3 Cu3 Cu1 52.87(3) . . ? S1 Cu3 Cu1 141.11(4) 7_566 . ? S5 Cu3 Cu2 139.14(4) . 7_566 ? S3 Cu3 Cu2 93.47(4) . 7_566 ? S1 Cu3 Cu2 51.54(3) 7_566 7_566 ? Cu1 Cu3 Cu2 89.77(2) . 7_566 ? S5 Cu3 Cu4 51.53(3) . 7_566 ? S3 Cu3 Cu4 143.42(4) . 7_566 ? S1 Cu3 Cu4 91.54(4) 7_566 7_566 ? Cu1 Cu3 Cu4 90.62(2) . 7_566 ? Cu2 Cu3 Cu4 87.84(2) 7_566 7_566 ? S6 Cu4 S2 119.76(5) 7_566 . ? S6 Cu4 S5 116.98(5) 7_566 7_566 ? S2 Cu4 S5 118.93(5) . 7_566 ? S6 Cu4 Cu1 93.43(4) 7_566 . ? S2 Cu4 Cu1 52.26(3) . . ? S5 Cu4 Cu1 141.66(4) 7_566 . ? S6 Cu4 Cu3 139.24(4) 7_566 7_566 ? S2 Cu4 Cu3 94.42(4) . 7_566 ? S5 Cu4 Cu3 50.94(3) 7_566 7_566 ? Cu1 Cu4 Cu3 90.86(2) . 7_566 ? S6 Cu4 Cu2 51.56(3) 7_566 7_566 ? S2 Cu4 Cu2 140.85(4) . 7_566 ? S5 Cu4 Cu2 92.62(4) 7_566 7_566 ? Cu1 Cu4 Cu2 88.70(2) . 7_566 ? Cu3 Cu4 Cu2 88.11(2) 7_566 7_566 ? C1 S1 Cu2 111.59(15) . . ? C1 S1 Cu3 109.43(15) . 7_566 ? Cu2 S1 Cu3 76.67(4) . 7_566 ? C1 S2 Cu4 106.97(15) . . ? C1 S2 Cu1 113.16(15) . . ? Cu4 S2 Cu1 76.20(4) . . ? C13 S3 Cu3 109.44(15) . . ? C13 S3 Cu1 110.57(15) . . ? Cu3 S3 Cu1 75.24(4) . . ? C25 S4 Cu2 108.60(15) . . ? C25 S4 Cu1 112.31(15) . . ? Cu2 S4 Cu1 74.72(4) . . ? C25 S5 Cu3 112.01(15) . . ? C25 S5 Cu4 108.24(15) . 7_566 ? Cu3 S5 Cu4 77.53(4) . 7_566 ? C13 S6 Cu4 111.26(15) 7_566 7_566 ? C13 S6 Cu2 108.90(15) 7_566 . ? Cu4 S6 Cu2 77.48(4) 7_566 . ? C6 N1 C7 115.1(5) . . ? C11 N2 C12 114.1(5) . . ? C18 N3 C19 115.7(5) . . ? C24 N4 C23 116.0(4) . . ? C30 N5 C31 116.1(5) . . ? C35 N6 C36 115.1(5) . . ? C2 C1 S1 120.6(3) . . ? C2 C1 S2 120.9(3) . . ? S1 C1 S2 118.5(2) . . ? C1 C2 C3 127.5(4) . . ? C1 C2 C8 128.0(4) . . ? C3 C2 C8 104.4(4) . . ? C4 C3 C7 116.3(5) . . ? C4 C3 C2 134.7(5) . . ? C7 C3 C2 109.0(4) . . ? C3 C4 C5 118.5(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 119.2(6) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 124.5(5) . . ? N1 C6 H6 117.8 . . ? C5 C6 H6 117.8 . . ? N1 C7 C3 126.4(5) . . ? N1 C7 C12 125.1(5) . . ? C3 C7 C12 108.5(4) . . ? C12 C8 C9 116.8(5) . . ? C12 C8 C2 109.5(4) . . ? C9 C8 C2 133.6(4) . . ? C10 C9 C8 117.4(5) . . ? C10 C9 H9 121.3 . . ? C8 C9 H9 121.3 . . ? C9 C10 C11 119.7(6) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N2 C11 C10 125.0(6) . . ? N2 C11 H11 117.5 . . ? C10 C11 H11 117.5 . . ? N2 C12 C8 127.0(5) . . ? N2 C12 C7 124.5(5) . . ? C8 C12 C7 108.5(4) . . ? C14 C13 S6 119.9(3) . 7_566 ? C14 C13 S3 120.6(3) . . ? S6 C13 S3 119.5(3) 7_566 . ? C13 C14 C15 127.1(4) . . ? C13 C14 C20 127.9(4) . . ? C15 C14 C20 105.0(4) . . ? C16 C15 C19 115.7(5) . . ? C16 C15 C14 134.4(4) . . ? C19 C15 C14 109.8(4) . . ? C17 C16 C15 118.7(5) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C18 C17 C16 119.2(6) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N3 C18 C17 124.8(6) . . ? N3 C18 H18 117.6 . . ? C17 C18 H18 117.6 . . ? N3 C19 C15 125.7(5) . . ? N3 C19 C24 126.3(5) . . ? C15 C19 C24 107.9(4) . . ? C21 C20 C24 116.8(4) . . ? C21 C20 C14 134.4(4) . . ? C24 C20 C14 108.7(4) . . ? C22 C21 C20 118.5(5) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C23 C22 C21 119.7(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? N4 C23 C22 123.7(5) . . ? N4 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? N4 C24 C20 125.2(5) . . ? N4 C24 C19 126.2(4) . . ? C20 C24 C19 108.6(4) . . ? C26 C25 S4 121.3(3) . . ? C26 C25 S5 119.7(3) . . ? S4 C25 S5 118.9(2) . . ? C25 C26 C27 128.3(4) . . ? C25 C26 C32 127.1(4) . . ? C27 C26 C32 104.6(4) . . ? C31 C27 C28 115.8(4) . . ? C31 C27 C26 110.2(4) . . ? C28 C27 C26 134.0(4) . . ? C29 C28 C27 117.4(5) . . ? C29 C28 H28 121.3 . . ? C27 C28 H28 121.3 . . ? C28 C29 C30 121.1(5) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? N5 C30 C29 122.8(5) . . ? N5 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N5 C31 C27 126.8(5) . . ? N5 C31 C36 125.2(4) . . ? C27 C31 C36 107.9(4) . . ? C33 C32 C36 115.4(4) . . ? C33 C32 C26 135.3(4) . . ? C36 C32 C26 109.1(4) . . ? C34 C33 C32 119.4(5) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? N6 C35 C34 123.9(5) . . ? N6 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? N6 C36 C32 126.1(5) . . ? N6 C36 C31 125.8(4) . . ? C32 C36 C31 108.0(4) . . ? C37 N7 C39 113.5(5) . . ? C37 N7 C41 105.4(5) . . ? C39 N7 C41 109.0(5) . . ? C37 N7 C43 112.9(6) . . ? C39 N7 C43 105.4(5) . . ? C41 N7 C43 110.7(6) . . ? N7 C37 C38 114.0(6) . . ? N7 C37 H37A 108.7 . . ? C38 C37 H37A 108.7 . . ? N7 C37 H37B 108.7 . . ? C38 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N7 114.5(6) . . ? C40 C39 H39A 108.6 . . ? N7 C39 H39A 108.6 . . ? C40 C39 H39B 108.6 . . ? N7 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N7 116.5(5) . . ? C42 C41 H41A 108.2 . . ? N7 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? N7 C41 H41B 108.2 . . ? H41A C41 H41B 107.3 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N7 112.8(6) . . ? C44 C43 H43A 109.0 . . ? N7 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? N7 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 N8 C49 106.1(5) . . ? C47 N8 C45 111.3(6) . . ? C49 N8 C45 111.7(5) . . ? C47 N8 C51 112.3(6) . . ? C49 N8 C51 110.7(6) . . ? C45 N8 C51 104.9(4) . . ? C46 C45 N8 115.3(6) . . ? C46 C45 H45A 108.5 . . ? N8 C45 H45A 108.5 . . ? C46 C45 H45B 108.5 . . ? N8 C45 H45B 108.5 . . ? H45A C45 H45B 107.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N8 C47 C48 115.8(5) . . ? N8 C47 H47A 108.3 . . ? C48 C47 H47A 108.3 . . ? N8 C47 H47B 108.3 . . ? C48 C47 H47B 108.3 . . ? H47A C47 H47B 107.4 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N8 C49 C50 114.7(6) . . ? N8 C49 H49A 108.6 . . ? C50 C49 H49A 108.6 . . ? N8 C49 H49B 108.6 . . ? C50 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N8 115.2(7) . . ? C52 C51 H51A 108.5 . . ? N8 C51 H51A 108.5 . . ? C52 C51 H51B 108.5 . . ? N8 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O1 S7A C53A 105.3(7) . . ? O1 S7A C54 105.2(6) . . ? C53A S7A C54 100.4(6) . . ? C54 S7B O1 106.7(9) . . ? C54 S7B C53B 116.4(12) . . ? O1 S7B C53B 132.1(12) . . ? S7A O1 S7B 52.6(5) . . ? S7B C54 S7A 46.4(5) . . ? S8A C55 S8B 41.7(7) . . ? O2A S8A C55 130.3(14) . . ? O2A S8A C56A 102.5(13) . . ? C55 S8A C56A 112.3(14) . . ? O2B S8B C56B 144.5(11) . . ? O2B S8B C55 117.3(10) . . ? C56B S8B C55 82.6(11) . . ? O3 S9 C58 106.9(6) . . ? O3 S9 C57 105.3(6) . . ? C58 S9 C57 92.1(7) . . ? S9 C57 H57A 109.5 . . ? S9 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? S9 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? S9 C58 H58A 109.5 . . ? S9 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? S9 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.702 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.310 ###Material relevant to compound (n-Bu4N)2[Cu(1)2] at 173K ######### data_e411a _database_code_depnum_ccdc_archive 'CCDC 294748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H36 N), C24 H12 Cu N4 S4, 2(C2 H3 N)' _chemical_formula_sum 'C60 H90 Cu N8 S4' _chemical_formula_weight 1115.18 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' 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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6672(7) _cell_length_b 8.7381(3) _cell_length_c 18.9133(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.396(2) _cell_angle_gamma 90.00 _cell_volume 3024.24(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4957 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.72 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1198 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8899 _exptl_absorpt_correction_T_max 0.9681 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 29283 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6879 _reflns_number_gt 4429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0875P)^2^+1.9170P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6879 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _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 0.0000 0.0000 0.0000 0.02812(17) Uani 1 2 d S . . S1 S 0.12282(5) -0.05495(11) 0.01771(4) 0.0322(2) Uani 1 1 d . . . S2 S 0.02548(5) -0.10960(10) 0.11330(4) 0.0320(2) Uani 1 1 d . . . N1 N 0.36353(16) -0.2882(4) 0.22271(17) 0.0425(8) Uani 1 1 d . . . N2 N 0.25928(18) -0.3654(4) 0.32260(15) 0.0409(8) Uani 1 1 d . . . C1 C 0.11611(17) -0.1256(3) 0.10276(16) 0.0245(6) Uani 1 1 d . . . C2 C 0.17310(17) -0.1864(4) 0.15234(16) 0.0240(7) Uani 1 1 d . . . C3 C 0.24993(17) -0.1956(4) 0.14584(16) 0.0268(7) Uani 1 1 d . . . C4 C 0.28790(18) -0.1543(4) 0.09208(18) 0.0322(7) Uani 1 1 d . . . H4 H 0.2640 -0.1096 0.0493 0.039 Uiso 1 1 calc R . . C5 C 0.3629(2) -0.1823(4) 0.1049(2) 0.0405(9) Uani 1 1 d . . . H5 H 0.3899 -0.1574 0.0701 0.049 Uiso 1 1 calc R . . C6 C 0.3971(2) -0.2471(5) 0.1694(2) 0.0457(10) Uani 1 1 d . . . H6 H 0.4472 -0.2635 0.1762 0.055 Uiso 1 1 calc R . . C7 C 0.29141(18) -0.2619(4) 0.20960(18) 0.0305(7) Uani 1 1 d . . . C8 C 0.16978(18) -0.2541(4) 0.22300(16) 0.0258(7) Uani 1 1 d . . . C9 C 0.1131(2) -0.2845(4) 0.25923(17) 0.0321(8) Uani 1 1 d . . . H9 H 0.0651 -0.2592 0.2390 0.039 Uiso 1 1 calc R . . C10 C 0.1309(2) -0.3539(4) 0.32641(18) 0.0404(9) Uani 1 1 d . . . H10 H 0.0945 -0.3758 0.3521 0.049 Uiso 1 1 calc R . . C11 C 0.2036(2) -0.3907(4) 0.35530(19) 0.0437(10) Uani 1 1 d . . . H11 H 0.2137 -0.4362 0.4006 0.052 Uiso 1 1 calc R . . C12 C 0.24149(19) -0.2991(4) 0.25765(17) 0.0315(8) Uani 1 1 d . . . N3 N 0.22796(15) 0.4059(3) 0.97935(14) 0.0273(6) Uani 1 1 d . . . C13 C 0.2790(2) 0.5292(4) 0.9606(2) 0.0363(8) Uani 1 1 d . . . H13A H 0.2497 0.6053 0.9306 0.044 Uiso 1 1 calc R . . H13B H 0.3023 0.5795 1.0049 0.044 Uiso 1 1 calc R . . C14 C 0.3382(2) 0.4743(5) 0.9220(3) 0.0511(11) Uani 1 1 d . . . H14A H 0.3598 0.3812 0.9447 0.061 Uiso 1 1 calc R . . H14B H 0.3166 0.4508 0.8722 0.061 Uiso 1 1 calc R . . C15 C 0.3969(2) 0.5935(5) 0.9240(3) 0.0544(11) Uani 1 1 d . . . H15A H 0.4177 0.6178 0.9739 0.065 Uiso 1 1 calc R . . H15B H 0.3750 0.6862 0.9011 0.065 Uiso 1 1 calc R . . C16 C 0.4576(3) 0.5424(6) 0.8866(3) 0.0706(15) Uani 1 1 d . . . H16A H 0.4934 0.6223 0.8895 0.106 Uiso 1 1 calc R . . H16B H 0.4376 0.5204 0.8369 0.106 Uiso 1 1 calc R . . H16C H 0.4804 0.4520 0.9098 0.106 Uiso 1 1 calc R . . C17 C 0.27067(18) 0.2917(4) 1.03241(17) 0.0298(7) Uani 1 1 d . . . H17A H 0.2373 0.2118 1.0410 0.036 Uiso 1 1 calc R . . H17B H 0.3074 0.2442 1.0097 0.036 Uiso 1 1 calc R . . C18 C 0.3085(2) 0.3554(4) 1.1048(2) 0.0406(9) Uani 1 1 d . . . H18A H 0.2727 0.4028 1.1286 0.049 Uiso 1 1 calc R . . H18B H 0.3434 0.4331 1.0975 0.049 Uiso 1 1 calc R . . C19 C 0.3476(2) 0.2285(5) 1.1519(2) 0.0444(9) Uani 1 1 d . . . H19A H 0.3817 0.1787 1.1267 0.053 Uiso 1 1 calc R . . H19B H 0.3121 0.1527 1.1599 0.053 Uiso 1 1 calc R . . C20 C 0.3889(3) 0.2859(6) 1.2243(2) 0.0623(13) Uani 1 1 d . . . H20A H 0.4126 0.2014 1.2518 0.093 Uiso 1 1 calc R . . H20B H 0.3553 0.3331 1.2500 0.093 Uiso 1 1 calc R . . H20C H 0.4249 0.3594 1.2168 0.093 Uiso 1 1 calc R . . C21 C 0.17062(18) 0.4885(4) 1.01253(18) 0.0292(7) Uani 1 1 d . . . H21A H 0.1460 0.5631 0.9781 0.035 Uiso 1 1 calc R . . H21B H 0.1952 0.5439 1.0549 0.035 Uiso 1 1 calc R . . C22 C 0.11324(18) 0.3838(4) 1.03430(18) 0.0303(7) Uani 1 1 d . . . H22A H 0.0777 0.3550 0.9917 0.036 Uiso 1 1 calc R . . H22B H 0.1366 0.2913 1.0559 0.036 Uiso 1 1 calc R . . C23 C 0.07445(19) 0.4627(4) 1.08759(19) 0.0333(8) Uani 1 1 d . . . H23A H 0.0502 0.5539 1.0655 0.040 Uiso 1 1 calc R . . H23B H 0.1101 0.4938 1.1296 0.040 Uiso 1 1 calc R . . C24 C 0.01808(19) 0.3572(4) 1.1111(2) 0.0388(8) Uani 1 1 d . . . H24A H -0.0056 0.4103 1.1446 0.058 Uiso 1 1 calc R . . H24B H 0.0422 0.2677 1.1339 0.058 Uiso 1 1 calc R . . H24C H -0.0177 0.3273 1.0697 0.058 Uiso 1 1 calc R . . C25 C 0.19295(19) 0.3153(4) 0.91317(17) 0.0326(8) Uani 1 1 d . . . H25A H 0.1628 0.2357 0.9279 0.039 Uiso 1 1 calc R . . H25B H 0.2313 0.2655 0.8937 0.039 Uiso 1 1 calc R . . C26 C 0.1460(2) 0.4090(5) 0.8534(2) 0.0489(11) Uani 1 1 d . . . H26A H 0.1731 0.4990 0.8438 0.059 Uiso 1 1 calc R . . H26B H 0.1024 0.4432 0.8693 0.059 Uiso 1 1 calc R . . C27 C 0.1240(2) 0.3169(5) 0.7839(2) 0.0483(10) Uani 1 1 d . . . H27A H 0.1032 0.2202 0.7950 0.058 Uiso 1 1 calc R . . H27B H 0.0865 0.3725 0.7511 0.058 Uiso 1 1 calc R . . C28 C 0.1877(2) 0.2853(6) 0.7466(2) 0.0579(12) Uani 1 1 d . . . H28A H 0.1707 0.2269 0.7035 0.087 Uiso 1 1 calc R . . H28B H 0.2247 0.2285 0.7784 0.087 Uiso 1 1 calc R . . H28C H 0.2077 0.3805 0.7342 0.087 Uiso 1 1 calc R . . C29 C 0.4561(4) 0.5356(7) 0.3713(3) 0.0923(11) Uani 1 1 d . . . H29A H 0.4906 0.6124 0.3923 0.138 Uiso 1 1 calc R . . H29B H 0.4154 0.5834 0.3402 0.138 Uiso 1 1 calc R . . H29C H 0.4793 0.4654 0.3438 0.138 Uiso 1 1 calc R . . C30 C 0.4311(4) 0.4550(8) 0.4268(3) 0.0923(11) Uani 1 1 d . . . N4 N 0.4121(3) 0.3916(6) 0.4716(3) 0.0923(11) 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 0.0304(3) 0.0242(3) 0.0262(3) -0.0017(2) -0.0030(2) 0.0038(2) S1 0.0325(5) 0.0358(5) 0.0267(4) 0.0044(3) 0.0026(3) 0.0014(4) S2 0.0262(4) 0.0367(5) 0.0321(4) 0.0021(4) 0.0028(3) 0.0061(4) N1 0.0286(17) 0.0453(19) 0.0484(18) -0.0058(15) -0.0054(14) 0.0059(14) N2 0.0472(19) 0.0427(19) 0.0277(15) 0.0024(13) -0.0049(13) 0.0046(15) C1 0.0247(16) 0.0210(16) 0.0271(15) -0.0031(13) 0.0035(12) -0.0011(13) C2 0.0235(16) 0.0244(17) 0.0240(15) -0.0045(13) 0.0043(12) -0.0013(13) C3 0.0270(17) 0.0226(17) 0.0285(16) -0.0069(13) -0.0005(13) -0.0012(13) C4 0.0294(18) 0.0312(19) 0.0363(18) -0.0051(15) 0.0073(14) -0.0043(14) C5 0.030(2) 0.043(2) 0.050(2) -0.0097(18) 0.0115(17) -0.0048(16) C6 0.0229(19) 0.050(2) 0.063(3) -0.012(2) 0.0055(18) -0.0006(17) C7 0.0275(18) 0.0251(18) 0.0354(18) -0.0055(14) -0.0022(14) 0.0000(14) C8 0.0315(18) 0.0220(17) 0.0222(15) -0.0045(12) 0.0014(13) 0.0011(13) C9 0.0359(19) 0.0320(19) 0.0288(16) -0.0001(14) 0.0072(14) 0.0009(15) C10 0.057(3) 0.037(2) 0.0306(18) 0.0009(15) 0.0150(17) -0.0032(18) C11 0.068(3) 0.034(2) 0.0261(17) 0.0064(15) 0.0023(18) 0.0026(19) C12 0.037(2) 0.0258(18) 0.0278(16) -0.0035(14) -0.0027(14) -0.0008(14) N3 0.0282(15) 0.0208(14) 0.0329(14) -0.0018(11) 0.0058(11) 0.0024(11) C13 0.039(2) 0.0249(19) 0.047(2) -0.0011(15) 0.0144(17) -0.0035(15) C14 0.053(3) 0.043(2) 0.066(3) -0.005(2) 0.034(2) -0.0060(19) C15 0.046(3) 0.049(3) 0.073(3) 0.000(2) 0.024(2) -0.001(2) C16 0.058(3) 0.067(3) 0.098(4) -0.001(3) 0.042(3) -0.003(3) C17 0.0246(17) 0.0277(18) 0.0355(17) -0.0003(14) 0.0024(14) 0.0046(13) C18 0.041(2) 0.034(2) 0.043(2) -0.0040(16) -0.0010(17) -0.0033(16) C19 0.038(2) 0.044(2) 0.047(2) 0.0052(18) -0.0006(18) 0.0018(17) C20 0.054(3) 0.077(3) 0.047(2) 0.009(2) -0.012(2) -0.009(2) C21 0.0300(18) 0.0235(17) 0.0343(17) -0.0044(14) 0.0072(14) 0.0052(14) C22 0.0279(18) 0.0273(18) 0.0341(17) -0.0087(14) 0.0019(14) -0.0006(14) C23 0.0329(19) 0.0269(19) 0.0405(19) -0.0070(15) 0.0084(15) 0.0021(14) C24 0.033(2) 0.038(2) 0.046(2) 0.0000(17) 0.0088(16) 0.0039(16) C25 0.0349(19) 0.0289(19) 0.0334(17) -0.0061(14) 0.0046(15) 0.0049(15) C26 0.059(3) 0.050(3) 0.0343(19) -0.0019(18) 0.0011(18) 0.021(2) C27 0.045(2) 0.062(3) 0.0346(19) -0.0028(19) -0.0012(17) 0.006(2) C28 0.054(3) 0.086(4) 0.034(2) -0.012(2) 0.0075(19) 0.005(2) C29 0.107(3) 0.104(3) 0.066(2) -0.0036(17) 0.0151(18) -0.046(2) C30 0.107(3) 0.104(3) 0.066(2) -0.0036(17) 0.0151(18) -0.046(2) N4 0.107(3) 0.104(3) 0.066(2) -0.0036(17) 0.0151(18) -0.046(2) _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 S1 2.3012(9) 3 ? Cu1 S1 2.3012(9) . ? Cu1 S2 2.3092(8) . ? Cu1 S2 2.3092(8) 3 ? S1 C1 1.750(3) . ? S2 C1 1.748(3) . ? N1 C6 1.338(5) . ? N1 C7 1.340(4) . ? N2 C11 1.329(5) . ? N2 C12 1.339(4) . ? C1 C2 1.378(4) . ? C2 C3 1.466(4) . ? C2 C8 1.474(4) . ? C3 C4 1.397(5) . ? C3 C7 1.421(4) . ? C4 C5 1.395(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.461(5) . ? C8 C9 1.394(5) . ? C8 C12 1.424(5) . ? C9 C10 1.387(5) . ? C9 H9 0.9300 . ? C10 C11 1.396(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? N3 C25 1.516(4) . ? N3 C17 1.524(4) . ? N3 C21 1.525(4) . ? N3 C13 1.525(4) . ? C13 C14 1.517(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.507(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.518(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.516(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.516(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.518(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.526(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.518(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.530(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.525(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.526(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.523(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.418(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N4 1.126(7) . ? 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 S1 Cu1 S1 180.00(5) 3 . ? S1 Cu1 S2 103.78(3) 3 . ? S1 Cu1 S2 76.22(3) . . ? S1 Cu1 S2 76.22(3) 3 3 ? S1 Cu1 S2 103.78(3) . 3 ? S2 Cu1 S2 180.00(4) . 3 ? C1 S1 Cu1 87.55(11) . . ? C1 S2 Cu1 87.35(11) . . ? C6 N1 C7 114.7(3) . . ? C11 N2 C12 115.1(3) . . ? C2 C1 S2 126.0(2) . . ? C2 C1 S1 125.1(2) . . ? S2 C1 S1 108.86(17) . . ? C1 C2 C3 126.9(3) . . ? C1 C2 C8 127.4(3) . . ? C3 C2 C8 105.7(3) . . ? C4 C3 C7 117.0(3) . . ? C4 C3 C2 133.8(3) . . ? C7 C3 C2 109.2(3) . . ? C5 C4 C3 117.7(3) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N1 C6 C5 124.9(3) . . ? N1 C6 H6 117.5 . . ? C5 C6 H6 117.5 . . ? N1 C7 C3 125.9(3) . . ? N1 C7 C12 126.0(3) . . ? C3 C7 C12 108.1(3) . . ? C9 C8 C12 117.1(3) . . ? C9 C8 C2 133.9(3) . . ? C12 C8 C2 108.9(3) . . ? C10 C9 C8 117.8(3) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N2 C11 C10 124.6(3) . . ? N2 C11 H11 117.7 . . ? C10 C11 H11 117.7 . . ? N2 C12 C8 125.6(3) . . ? N2 C12 C7 126.4(3) . . ? C8 C12 C7 108.0(3) . . ? C25 N3 C17 106.6(2) . . ? C25 N3 C21 111.3(3) . . ? C17 N3 C21 110.9(2) . . ? C25 N3 C13 111.4(3) . . ? C17 N3 C13 110.2(3) . . ? C21 N3 C13 106.5(2) . . ? C14 C13 N3 115.9(3) . . ? C14 C13 H13A 108.3 . . ? N3 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? N3 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C13 111.4(3) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 113.0(4) . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N3 116.3(3) . . ? C18 C17 H17A 108.2 . . ? N3 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? N3 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C19 110.3(3) . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 112.8(3) . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 114.5(3) . . ? N3 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? N3 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 111.1(3) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 111.5(3) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 115.0(3) . . ? N3 C25 H25A 108.5 . . ? C26 C25 H25A 108.5 . . ? N3 C25 H25B 108.5 . . ? C26 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C25 C26 C27 111.9(3) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 113.1(4) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 C29 179.0(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.498 _refine_diff_density_min -1.318 _refine_diff_density_rms 0.084 ######################################################################### #===END