# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Timothy Warren' _publ_contact_author_email THW@GEORGETOWN.EDU _publ_section_title ; Reversible RS-NO Bond Cleavage and Formation at Copper(I) Thiolates ; _publ_contact_author 'Timothy H. Warren' loop_ _publ_author_name 'Tim Warren' 'Ercheng Li' 'Marie M. Melzer' # Attachment 'cmpd_3-rev-resub.CIF' data_c:IPrCuSCH2ArtBu _database_code_depnum_ccdc_archive 'CCDC 736333' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IPrCuSCH2ArtBu _chemical_melting_point ? _chemical_formula_moiety 'C38 H51 Cu1 N2 S1' _chemical_formula_sum 'C38 H51 Cu N2 S' _chemical_formula_weight 631.39 _journal_name_requested 'Chemical Communications' 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 C2/c _symmetry_space_group_name_Hall -C2yc 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 29.689(3) _cell_length_b 15.6315(13) _cell_length_c 17.0794(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.8040(10) _cell_angle_gamma 90.00 _cell_volume 7898.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 4.787 _cell_measurement_theta_max 56.581 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.58 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7037 _exptl_absorpt_correction_T_max 0.7114 _exptl_absorpt_process_details "SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38" _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'APEX II platform CCDm Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32710 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8618 _reflns_number_gt 6873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565' _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^)+(0.0433P)^2^+11.5173P] 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 8618 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.330561(8) 0.562767(17) 0.994791(14) 0.02574(8) Uani 1 1 d . . . N2 N 0.32579(5) 0.48701(11) 0.83691(10) 0.0251(4) Uani 1 1 d . . . N1 N 0.26045(6) 0.50891(12) 0.87634(10) 0.0284(4) Uani 1 1 d . . . S1 S 0.353634(18) 0.60078(4) 1.11107(3) 0.03274(13) Uani 1 1 d . . . C1 C 0.30502(7) 0.52038(14) 0.89777(12) 0.0255(4) Uani 1 1 d . . . C2 C 0.25375(7) 0.47023(16) 0.80377(13) 0.0335(5) Uani 1 1 d . . . C3 C 0.29488(7) 0.45622(15) 0.77846(13) 0.0316(5) Uani 1 1 d . . . C4 C 0.22486(7) 0.54342(16) 0.92003(13) 0.0328(5) Uani 1 1 d . . . C5 C 0.20821(8) 0.49400(17) 0.97944(14) 0.0377(5) Uani 1 1 d . . . C6 C 0.17315(8) 0.5300(2) 1.01876(16) 0.0472(6) Uani 1 1 d . . . C7 C 0.15623(8) 0.6102(2) 0.99891(16) 0.0494(7) Uani 1 1 d . . . C8 C 0.17389(8) 0.65815(18) 0.94067(15) 0.0427(6) Uani 1 1 d . . . C9 C 0.20915(7) 0.62562(16) 0.89982(14) 0.0350(5) Uani 1 1 d . . . C10 C 0.37421(7) 0.49093(14) 0.83170(11) 0.0265(4) Uani 1 1 d . . . C11 C 0.40049(7) 0.42140(15) 0.85822(12) 0.0289(5) Uani 1 1 d . . . C12 C 0.44735(7) 0.42893(16) 0.85509(12) 0.0335(5) Uani 1 1 d . . . C13 C 0.46583(7) 0.50129(17) 0.82524(12) 0.0362(6) Uani 1 1 d . . . C14 C 0.43863(7) 0.56817(17) 0.79698(13) 0.0357(5) Uani 1 1 d . . . C15 C 0.39179(7) 0.56480(15) 0.80019(12) 0.0302(5) Uani 1 1 d . . . C16 C 0.22671(9) 0.40608(18) 1.00187(16) 0.0456(6) Uani 1 1 d . . . C17 C 0.22950(8) 0.68007(17) 0.83846(14) 0.0404(6) Uani 1 1 d . . . C18 C 0.38094(8) 0.34215(15) 0.89285(13) 0.0337(5) Uani 1 1 d . . . C19 C 0.36255(8) 0.63985(16) 0.77060(14) 0.0377(5) Uani 1 1 d . . . C20 C 0.24298(16) 0.4011(3) 1.0885(2) 0.0873(12) Uani 1 1 d . . . C21 C 0.19267(13) 0.3371(2) 0.9801(3) 0.1019(16) Uani 1 1 d . . . C22 C 0.25372(9) 0.75772(19) 0.87631(17) 0.0503(7) Uani 1 1 d . . . C23 C 0.19367(10) 0.7070(2) 0.77332(16) 0.0510(7) Uani 1 1 d . . . C24 C 0.38814(9) 0.34594(17) 0.98291(14) 0.0420(6) Uani 1 1 d . . . C25 C 0.40097(9) 0.26035(17) 0.86127(15) 0.0447(6) Uani 1 1 d . . . C26 C 0.37589(11) 0.7218(2) 0.8144(2) 0.0632(8) Uani 1 1 d . . . C27 C 0.36429(11) 0.6501(2) 0.68191(16) 0.0576(8) Uani 1 1 d . . . C28 C 0.41512(7) 0.58328(16) 1.11965(13) 0.0349(5) Uani 1 1 d . . . C29 C 0.43921(7) 0.64686(15) 1.07232(12) 0.0313(5) Uani 1 1 d . . . C30 C 0.45836(8) 0.62387(15) 1.00439(12) 0.0335(5) Uani 1 1 d . . . C31 C 0.47962(8) 0.68378(15) 0.96032(13) 0.0361(5) Uani 1 1 d . . . C32 C 0.48202(8) 0.76978(15) 0.98064(14) 0.0354(5) Uani 1 1 d . . . C33 C 0.46292(8) 0.79258(17) 1.05022(16) 0.0435(6) Uani 1 1 d . . . C34 C 0.44229(8) 0.73234(17) 1.09454(15) 0.0412(6) Uani 1 1 d . . . C35 C 0.50235(9) 0.83834(17) 0.93058(16) 0.0437(6) Uani 1 1 d . . . C36 C 0.52319(11) 0.8005(2) 0.85939(17) 0.0574(8) Uani 1 1 d . . . C37 C 0.46479(11) 0.9009(2) 0.8999(2) 0.0650(9) Uani 1 1 d . . . C38 C 0.53951(10) 0.8884(2) 0.97920(18) 0.0563(7) Uani 1 1 d . . . H12 H 0.4666 0.3835 0.8738 0.04 Uiso 1 1 calc R . . H13 H 0.4977 0.5054 0.824 0.043 Uiso 1 1 calc R . . H14 H 0.452 0.617 0.7751 0.043 Uiso 1 1 calc R . . H16 H 0.2534 0.3957 0.9712 0.055 Uiso 1 1 calc R . . H17 H 0.2525 0.6446 0.8139 0.048 Uiso 1 1 calc R . . H18 H 0.3477 0.3417 0.8778 0.04 Uiso 1 1 calc R . . H19 H 0.3306 0.6264 0.7807 0.045 Uiso 1 1 calc R . . H2 H 0.2255 0.4561 0.7767 0.04 Uiso 1 1 calc R . . H20A H 0.2643 0.4478 1.1017 0.131 Uiso 1 1 calc R . . H20B H 0.258 0.3461 1.0995 0.131 Uiso 1 1 calc R . . H20C H 0.2171 0.4064 1.1202 0.131 Uiso 1 1 calc R . . H21A H 0.2055 0.2813 0.9956 0.153 Uiso 1 1 calc R . . H21B H 0.1849 0.3379 0.9232 0.153 Uiso 1 1 calc R . . H21C H 0.1654 0.3471 1.0073 0.153 Uiso 1 1 calc R . . H22A H 0.2319 0.7935 0.9013 0.075 Uiso 1 1 calc R . . H22B H 0.2675 0.7909 0.8359 0.075 Uiso 1 1 calc R . . H22C H 0.2773 0.7385 0.916 0.075 Uiso 1 1 calc R . . H23A H 0.1791 0.656 0.7494 0.076 Uiso 1 1 calc R . . H23B H 0.2081 0.7395 0.7332 0.076 Uiso 1 1 calc R . . H23C H 0.1709 0.7429 0.7957 0.076 Uiso 1 1 calc R . . H24A H 0.4206 0.3493 0.999 0.063 Uiso 1 1 calc R . . H24B H 0.3755 0.2944 1.0053 0.063 Uiso 1 1 calc R . . H24C H 0.3729 0.3966 1.0019 0.063 Uiso 1 1 calc R . . H25A H 0.398 0.2616 0.8037 0.067 Uiso 1 1 calc R . . H25B H 0.3847 0.2107 0.8797 0.067 Uiso 1 1 calc R . . H25C H 0.433 0.2563 0.8801 0.067 Uiso 1 1 calc R . . H26A H 0.3752 0.7123 0.871 0.095 Uiso 1 1 calc R . . H26B H 0.3546 0.7674 0.7975 0.095 Uiso 1 1 calc R . . H26C H 0.4065 0.7384 0.803 0.095 Uiso 1 1 calc R . . H27A H 0.3952 0.6638 0.6703 0.086 Uiso 1 1 calc R . . H27B H 0.344 0.6964 0.663 0.086 Uiso 1 1 calc R . . H27C H 0.3548 0.5966 0.6556 0.086 Uiso 1 1 calc R . . H28A H 0.4267 0.5878 1.1755 0.042 Uiso 1 1 calc R . . H28B H 0.4216 0.5248 1.1014 0.042 Uiso 1 1 calc R . . H3 H 0.3014 0.4305 0.7303 0.038 Uiso 1 1 calc R . . H30 H 0.4569 0.5659 0.9876 0.04 Uiso 1 1 calc R . . H31 H 0.493 0.6654 0.9146 0.043 Uiso 1 1 calc R . . H33 H 0.4642 0.8505 1.0671 0.052 Uiso 1 1 calc R . . H34 H 0.4299 0.7499 1.1415 0.049 Uiso 1 1 calc R . . H36A H 0.5467 0.7592 0.8772 0.086 Uiso 1 1 calc R . . H36B H 0.5366 0.8465 0.83 0.086 Uiso 1 1 calc R . . H36C H 0.4997 0.7717 0.8254 0.086 Uiso 1 1 calc R . . H37A H 0.4411 0.8694 0.8685 0.098 Uiso 1 1 calc R . . H37B H 0.4776 0.9448 0.8673 0.098 Uiso 1 1 calc R . . H37C H 0.4518 0.9282 0.9445 0.098 Uiso 1 1 calc R . . H38A H 0.5268 0.9146 1.0246 0.084 Uiso 1 1 calc R . . H38B H 0.5514 0.9332 0.9465 0.084 Uiso 1 1 calc R . . H38C H 0.564 0.8493 0.9974 0.084 Uiso 1 1 calc R . . H6 H 0.1609 0.4988 1.0597 0.057 Uiso 1 1 calc R . . H7 H 0.1321 0.6327 1.0257 0.059 Uiso 1 1 calc R . . H8 H 0.1621 0.7134 0.9283 0.051 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 0.02230(13) 0.03451(15) 0.02089(13) -0.00130(11) 0.00472(9) 0.00176(11) N2 0.0203(8) 0.0323(10) 0.0231(8) -0.0025(7) 0.0038(6) 0.0016(7) N1 0.0207(8) 0.0354(10) 0.0297(9) -0.0040(8) 0.0051(7) 0.0006(7) S1 0.0288(3) 0.0478(3) 0.0222(3) -0.0045(2) 0.0053(2) 0.0049(2) C1 0.0215(10) 0.0310(11) 0.0245(10) 0.0006(8) 0.0050(8) 0.0010(8) C2 0.0238(10) 0.0444(13) 0.0320(12) -0.0087(10) 0.0007(9) -0.0021(9) C3 0.0276(11) 0.0398(13) 0.0274(11) -0.0080(9) 0.0017(8) -0.0017(9) C4 0.0201(10) 0.0470(14) 0.0318(11) -0.0104(10) 0.0056(8) -0.0023(9) C5 0.0277(11) 0.0492(14) 0.0373(13) -0.0085(11) 0.0085(9) -0.0051(10) C6 0.0350(13) 0.0668(18) 0.0422(14) -0.0058(13) 0.0166(11) -0.0053(13) C7 0.0273(12) 0.071(2) 0.0520(16) -0.0184(14) 0.0149(11) 0.0011(12) C8 0.0247(11) 0.0563(16) 0.0476(15) -0.0105(12) 0.0069(10) 0.0059(11) C9 0.0226(11) 0.0463(14) 0.0363(12) -0.0074(10) 0.0031(9) 0.0027(10) C10 0.0192(9) 0.0413(12) 0.0194(9) -0.0041(9) 0.0044(7) 0.0005(9) C11 0.0259(10) 0.0413(13) 0.0196(10) -0.0071(9) 0.0026(8) 0.0037(9) C12 0.0240(10) 0.0511(14) 0.0252(11) -0.0078(10) 0.0023(8) 0.0079(10) C13 0.0190(10) 0.0656(16) 0.0245(11) -0.0141(11) 0.0049(8) -0.0010(10) C14 0.0284(11) 0.0551(15) 0.0245(11) -0.0061(10) 0.0077(8) -0.0094(11) C15 0.0257(10) 0.0436(13) 0.0217(10) -0.0020(9) 0.0040(8) -0.0014(9) C16 0.0371(13) 0.0524(16) 0.0498(15) -0.0013(12) 0.0184(11) -0.0058(12) C17 0.0353(13) 0.0476(15) 0.0393(13) 0.0030(11) 0.0099(10) 0.0124(11) C18 0.0291(11) 0.0385(13) 0.0336(12) -0.0022(10) 0.0030(9) 0.0052(10) C19 0.0292(12) 0.0456(14) 0.0382(13) 0.0074(11) 0.0031(9) -0.0032(10) C20 0.126(4) 0.081(3) 0.057(2) 0.0208(19) 0.023(2) 0.027(2) C21 0.062(2) 0.055(2) 0.188(5) -0.025(3) 0.006(3) -0.0111(18) C22 0.0397(14) 0.0564(17) 0.0549(17) 0.0071(13) 0.0045(12) -0.0024(12) C23 0.0546(16) 0.0601(18) 0.0381(14) -0.0046(13) 0.0027(12) 0.0149(14) C24 0.0500(15) 0.0436(14) 0.0338(13) 0.0007(11) 0.0113(11) -0.0004(12) C25 0.0518(15) 0.0428(14) 0.0390(14) -0.0053(11) 0.0014(11) 0.0095(12) C26 0.0589(19) 0.0511(18) 0.077(2) -0.0131(16) -0.0079(16) 0.0096(15) C27 0.0618(19) 0.068(2) 0.0422(15) 0.0211(14) 0.0007(13) -0.0043(15) C28 0.0306(11) 0.0493(14) 0.0240(11) -0.0006(10) -0.0015(9) 0.0058(10) C29 0.0233(10) 0.0448(13) 0.0246(10) -0.0057(9) -0.0046(8) 0.0062(9) C30 0.0416(13) 0.0346(12) 0.0238(11) -0.0036(9) -0.0002(9) 0.0054(10) C31 0.0427(13) 0.0400(13) 0.0252(11) -0.0055(10) 0.0017(9) 0.0032(10) C32 0.0305(11) 0.0385(13) 0.0360(12) -0.0063(10) -0.0042(9) 0.0035(10) C33 0.0349(13) 0.0401(14) 0.0557(16) -0.0201(12) 0.0058(11) -0.0017(11) C34 0.0318(12) 0.0506(15) 0.0420(14) -0.0187(12) 0.0080(10) -0.0016(11) C35 0.0462(15) 0.0391(14) 0.0446(14) -0.0020(11) -0.0038(11) 0.0002(11) C36 0.078(2) 0.0526(17) 0.0429(15) 0.0049(13) 0.0123(14) -0.0058(15) C37 0.0611(19) 0.0451(17) 0.085(2) 0.0094(16) -0.0132(17) 0.0006(15) C38 0.0559(17) 0.0559(18) 0.0563(18) -0.0038(14) 0.0000(14) -0.0188(14) _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 C1 1.884(2) . ? Cu1 S1 2.1304(6) . ? N2 C1 1.356(3) . ? N2 C3 1.385(3) . ? N2 C10 1.449(2) . ? N1 C2 1.378(3) . ? N1 C4 1.448(3) . ? S1 C28 1.840(2) . ? C1 N1 1.355(3) . ? C2 C3 1.347(3) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C5 1.398(3) . ? C4 C9 1.400(3) . ? C5 C6 1.403(3) . ? C5 C16 1.517(4) . ? C6 C7 1.382(4) . ? C6 H6 0.95 . ? C7 H7 0.95 . ? C8 C7 1.383(4) . ? C8 H8 0.95 . ? C9 C8 1.401(3) . ? C9 C17 1.515(3) . ? C11 C10 1.391(3) . ? C11 C12 1.402(3) . ? C11 C18 1.510(3) . ? C12 H12 0.95 . ? C13 C12 1.374(4) . ? C13 H13 0.95 . ? C14 C13 1.383(4) . ? C14 H14 0.95 . ? C15 C10 1.394(3) . ? C15 C14 1.397(3) . ? C15 C19 1.520(3) . ? C16 C21 1.503(4) . ? C16 C20 1.520(5) . ? C16 H16 1 . ? C17 C22 1.527(4) . ? C17 C23 1.533(4) . ? C17 H17 1 . ? C18 C25 1.527(3) . ? C18 C24 1.536(3) . ? C18 H18 1 . ? C19 C26 1.519(4) . ? C19 C27 1.528(3) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.382(3) . ? C29 C34 1.390(3) . ? C29 C28 1.500(3) . ? C30 H30 0.95 . ? C31 C30 1.386(3) . ? C31 C32 1.389(3) . ? C31 H31 0.95 . ? C32 C33 1.405(3) . ? C32 C35 1.527(4) . ? C33 C34 1.383(4) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? C35 C36 1.528(4) . ? C35 C38 1.538(4) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C35 1.541(4) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? 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 N2 C1 Cu1 129.34(15) . . ? N2 C3 H3 127 . . ? N1 C1 N2 103.80(17) . . ? N1 C1 Cu1 126.59(15) . . ? N1 C2 H2 126.5 . . ? S1 C28 H28A 109.2 . . ? S1 C28 H28B 109.2 . . ? C1 Cu1 S1 172.90(6) . . ? C1 N2 C3 111.70(17) . . ? C1 N2 C10 123.22(17) . . ? C1 N1 C2 111.40(17) . . ? C1 N1 C4 123.35(18) . . ? C10 C11 C12 116.9(2) . . ? C10 C11 C18 123.02(19) . . ? C10 C15 C14 116.9(2) . . ? C10 C15 C19 123.09(19) . . ? C11 C18 C25 112.00(19) . . ? C11 C18 C24 109.56(19) . . ? C11 C18 H18 108 . . ? C11 C10 C15 123.72(19) . . ? C11 C10 N2 118.62(19) . . ? C11 C12 H12 119.6 . . ? C12 C11 C18 120.0(2) . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14 119.6 . . ? C13 C12 C11 120.8(2) . . ? C13 C12 H12 119.6 . . ? C14 C15 C19 120.0(2) . . ? C14 C13 H13 119.6 . . ? C15 C14 H14 119.6 . . ? C15 C10 N2 117.66(19) . . ? C15 C19 C27 110.1(2) . . ? C15 C19 H19 107.7 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? C2 N1 C4 124.78(18) . . ? C2 C3 N2 106.02(19) . . ? C2 C3 H3 127 . . ? C20 C16 H16 107.5 . . ? C21 C16 C5 111.5(3) . . ? C21 C16 C20 110.9(3) . . ? C21 C16 H16 107.5 . . ? C22 C17 C23 111.3(2) . . ? C22 C17 H17 107.8 . . ? C23 C17 H17 107.8 . . ? C24 C18 H18 108 . . ? C25 C18 C24 111.1(2) . . ? C25 C18 H18 108 . . ? C26 C19 C15 111.6(2) . . ? C26 C19 C27 111.8(2) . . ? C26 C19 H19 107.7 . . ? C27 C19 H19 107.7 . . ? C28 S1 Cu1 105.80(7) . . ? C29 C28 S1 111.92(15) . . ? C29 C28 H28A 109.2 . . ? C29 C28 H28B 109.2 . . ? C29 C30 C31 121.2(2) . . ? C29 C30 H30 119.4 . . ? C29 C34 H34 119.1 . . ? C3 N2 C10 124.85(17) . . ? C3 C2 N1 107.07(19) . . ? C3 C2 H2 126.5 . . ? C30 C31 C32 122.3(2) . . ? C30 C31 H31 118.8 . . ? C30 C29 C34 117.2(2) . . ? C30 C29 C28 121.9(2) . . ? C31 C32 C33 116.2(2) . . ? C31 C32 C35 123.6(2) . . ? C31 C30 H30 119.4 . . ? C32 C31 H31 118.8 . . ? C32 C33 H33 119.4 . . ? C32 C35 C36 112.3(2) . . ? C32 C35 C38 110.7(2) . . ? C32 C35 C37 109.1(2) . . ? C33 C32 C35 120.1(2) . . ? C33 C34 C29 121.8(2) . . ? C33 C34 H34 119.1 . . ? C34 C29 C28 120.9(2) . . ? C34 C33 C32 121.3(2) . . ? C34 C33 H33 119.4 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? C36 C35 C38 107.8(2) . . ? C36 C35 C37 107.7(2) . . ? C38 C35 C37 109.1(2) . . ? C4 C9 C8 117.2(2) . . ? C4 C9 C17 122.8(2) . . ? C4 C5 C6 116.6(2) . . ? C4 C5 C16 122.8(2) . . ? C5 C4 C9 123.7(2) . . ? C5 C4 N1 119.1(2) . . ? C5 C6 H6 119.5 . . ? C5 C16 C20 111.8(2) . . ? C5 C16 H16 107.5 . . ? C6 C5 C16 120.7(2) . . ? C6 C7 C8 121.1(2) . . ? C6 C7 H7 119.5 . . ? C7 C6 C5 121.0(3) . . ? C7 C6 H6 119.5 . . ? C7 C8 C9 120.4(3) . . ? C7 C8 H8 119.8 . . ? C8 C9 C17 119.9(2) . . ? C8 C7 H7 119.5 . . ? C9 C4 N1 117.2(2) . . ? C9 C17 C22 110.8(2) . . ? C9 C17 C23 111.3(2) . . ? C9 C17 H17 107.8 . . ? C9 C8 H8 119.8 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H28A C28 H28B 107.9 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.366 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.055 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 -0.039 0.250 256.2 26.0 2 0.500 0.039 0.750 256.2 26.3 3 0.000 0.461 0.250 256.2 26.0 4 0.281 0.208 0.185 8.5 0.0 5 0.719 0.208 0.315 8.5 0.2 6 0.219 0.292 0.815 8.5 0.2 7 0.781 0.292 0.685 8.5 -0.1 8 0.000 0.539 0.750 256.2 26.3 9 0.219 0.708 0.315 8.5 0.2 10 0.781 0.708 0.185 8.5 0.0 11 0.281 0.792 0.685 8.5 -0.1 12 0.719 0.792 0.815 8.5 0.2 _platon_squeeze_details ; Because disordered pentanes of solvation were found in the initial refinement that could not be satisfactorily modeled, the SQUEEZE subroutine of PLATON was used. 105 solvent electrons were identified corresponding to 1/3 molecule of pentane per IPrCuSCH2ArtBu and the reflection data were refined excluding the solvent to give the results below. PLATON: Spek, A. L. Acta Crystallogr. 1990, A46, C-34. ; # Attachment 'cmpd_4-rev-resub.CIF' data_c:IPrCu2SBnBF4 _database_code_depnum_ccdc_archive 'CCDC 736334' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IPrCu2SBnBF4 _chemical_melting_point ? _chemical_formula_moiety 'C61 H79 Cu2 N4 S, B F4' _chemical_formula_sum 'C61 H79 B Cu2 F4 N4 S' _chemical_formula_weight 1114.23 _journal_name_requested 'Chemical Communications' 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc 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 32.857(3) _cell_length_b 12.3716(12) _cell_length_c 31.680(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.4190(10) _cell_angle_gamma 90.00 _cell_volume 12820(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 4.787 _cell_measurement_theta_max 56.581 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8653 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details "SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38" _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'APEX II platform CCDm Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46584 _diffrn_reflns_av_R_equivalents 0.1259 _diffrn_reflns_av_sigmaI/netI 0.1415 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11276 _reflns_number_gt 5518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565' _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^)+(0.0783P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11276 _refine_ls_number_parameters 674 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1697 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 0.002 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.13346(2) 0.65521(5) 0.12245(2) 0.0356(2) Uani 1 1 d . . . Cu2 Cu 0.23956(2) 0.62858(5) 0.10787(2) 0.0325(2) Uani 1 1 d . . . N1 N 0.05424(13) 0.6838(4) 0.15142(14) 0.0390(12) Uani 1 1 d . . . N2 N 0.04995(14) 0.5657(4) 0.10210(15) 0.0418(12) Uani 1 1 d . . . N3 N 0.31139(14) 0.4969(4) 0.13238(14) 0.0362(11) Uani 1 1 d . . . N4 N 0.28296(14) 0.4513(4) 0.07160(14) 0.0383(12) Uani 1 1 d . . . S1 S 0.19008(4) 0.73825(11) 0.11506(4) 0.0332(4) Uani 1 1 d . . . F1 F 0.41799(11) 1.0793(3) 0.10816(13) 0.0715(12) Uani 1 1 d . . . F2 F 0.38195(13) 1.2112(4) 0.07086(13) 0.0932(15) Uani 1 1 d . . . F3 F 0.36675(14) 1.1672(4) 0.13632(16) 0.1036(16) Uani 1 1 d . . . F4 F 0.42363(12) 1.2555(3) 0.12865(14) 0.0850(13) Uani 1 1 d . . . B1 B 0.3980(3) 1.1763(8) 0.1103(3) 0.064(3) Uani 1 1 d . . . C1 C 0.07779(17) 0.6260(5) 0.12672(17) 0.0371(14) Uani 1 1 d . . . C2 C 0.01301(18) 0.6616(5) 0.14189(19) 0.0459(16) Uani 1 1 d . . . C3 C 0.01058(18) 0.5887(5) 0.11168(19) 0.0451(16) Uani 1 1 d . . . C4 C 0.07169(17) 0.7578(6) 0.1836(2) 0.0464(16) Uani 1 1 d . . . C5 C 0.08345(18) 0.7151(6) 0.2236(2) 0.0523(18) Uani 1 1 d . . . C6 C 0.1015(2) 0.7884(8) 0.2539(2) 0.067(2) Uani 1 1 d . . . C7 C 0.1063(2) 0.8952(7) 0.2435(3) 0.074(2) Uani 1 1 d . . . C8 C 0.0937(2) 0.9321(6) 0.2047(3) 0.068(2) Uani 1 1 d . . . C9 C 0.0756(2) 0.8648(6) 0.1730(2) 0.0610(19) Uani 1 1 d . . . C10 C 0.06022(17) 0.4794(5) 0.07438(19) 0.0406(15) Uani 1 1 d . . . C11 C 0.06100(18) 0.3746(5) 0.0915(2) 0.0499(17) Uani 1 1 d . . . C12 C 0.06986(19) 0.2917(6) 0.0636(3) 0.061(2) Uani 1 1 d . . . C13 C 0.0772(2) 0.3108(6) 0.0223(2) 0.0597(19) Uani 1 1 d . . . C14 C 0.07671(18) 0.4156(5) 0.0070(2) 0.0484(17) Uani 1 1 d . . . C15 C 0.06801(16) 0.5030(5) 0.03265(18) 0.0385(15) Uani 1 1 d . . . C16 C 0.0785(2) 0.5959(6) 0.2348(2) 0.061(2) Uani 1 1 d . . . C17 C 0.0604(2) 0.9100(6) 0.1305(2) 0.065(2) Uani 1 1 d . . . C18 C 0.05273(19) 0.3523(6) 0.1374(2) 0.0592(19) Uani 1 1 d . . . C19 C 0.06674(19) 0.6162(5) 0.01544(18) 0.0443(16) Uani 1 1 d . . . C20 C 0.1192(2) 0.5392(7) 0.2382(2) 0.087(3) Uani 1 1 d . . . C21 C 0.0569(3) 0.5825(8) 0.2749(2) 0.106(3) Uani 1 1 d . . . C22 C 0.0935(2) 0.9696(6) 0.1093(2) 0.076(2) Uani 1 1 d . . . C23 C 0.0231(2) 0.9804(7) 0.1340(3) 0.101(3) Uani 1 1 d . . . C24 C 0.0113(2) 0.2946(7) 0.1390(2) 0.090(3) Uani 1 1 d . . . C25 C 0.0875(2) 0.2887(6) 0.1607(2) 0.079(2) Uani 1 1 d . . . C26 C 0.1083(3) 0.6518(8) 0.0066(3) 0.128(4) Uani 1 1 d . . . C27 C 0.0381(3) 0.6287(7) -0.0229(3) 0.140(5) Uani 1 1 d . . . C28 C 0.28044(17) 0.5250(4) 0.10275(17) 0.0348(14) Uani 1 1 d . . . C29 C 0.33218(18) 0.4069(5) 0.11904(19) 0.0427(15) Uani 1 1 d . . . C30 C 0.31465(17) 0.3793(5) 0.08107(18) 0.0419(15) Uani 1 1 d . . . C31 C 0.31844(17) 0.5549(5) 0.17189(18) 0.0385(15) Uani 1 1 d . . . C32 C 0.29267(19) 0.5309(5) 0.20319(18) 0.0454(16) Uani 1 1 d . . . C33 C 0.2989(2) 0.5892(6) 0.2404(2) 0.061(2) Uani 1 1 d . . . C34 C 0.3294(3) 0.6634(7) 0.2469(2) 0.072(2) Uani 1 1 d . . . C35 C 0.3549(2) 0.6823(5) 0.2167(3) 0.068(2) Uani 1 1 d . . . C36 C 0.35061(19) 0.6289(5) 0.1764(2) 0.0519(17) Uani 1 1 d . . . C37 C 0.25706(19) 0.4569(5) 0.03192(16) 0.0387(15) Uani 1 1 d . . . C38 C 0.22165(19) 0.3996(5) 0.02757(17) 0.0392(15) Uani 1 1 d . . . C39 C 0.1966(2) 0.4107(5) -0.01033(19) 0.0548(18) Uani 1 1 d . . . C40 C 0.2085(3) 0.4755(6) -0.0420(2) 0.063(2) Uani 1 1 d . . . C41 C 0.2448(3) 0.5302(6) -0.0373(2) 0.065(2) Uani 1 1 d . . . C42 C 0.2707(2) 0.5239(5) 0.00073(18) 0.0458(17) Uani 1 1 d . . . C43 C 0.26035(19) 0.4430(5) 0.19778(18) 0.0473(16) Uani 1 1 d . . . C44 C 0.3780(2) 0.6503(6) 0.1421(3) 0.077(2) Uani 1 1 d . . . C45 C 0.20758(18) 0.3292(5) 0.06297(18) 0.0463(16) Uani 1 1 d . . . C46 C 0.3104(2) 0.5859(6) 0.0074(2) 0.067(2) Uani 1 1 d . . . C47 C 0.2762(2) 0.3404(5) 0.21931(19) 0.0591(19) Uani 1 1 d . . . C48 C 0.2196(2) 0.4754(6) 0.2128(2) 0.080(2) Uani 1 1 d . . . C49 C 0.4221(2) 0.6110(8) 0.1545(4) 0.133(4) Uani 1 1 d . . . C50 C 0.3788(3) 0.7681(7) 0.1299(3) 0.119(3) Uani 1 1 d . . . C51 C 0.17722(18) 0.3900(5) 0.08781(19) 0.0506(17) Uani 1 1 d . . . C52 C 0.1904(2) 0.2213(5) 0.0467(2) 0.0563(18) Uani 1 1 d . . . C53 C 0.3384(2) 0.5623(6) -0.0270(2) 0.070(2) Uani 1 1 d . . . C54 C 0.3021(3) 0.7075(6) 0.0109(3) 0.096(3) Uani 1 1 d . . . C55 C 0.20246(17) 0.8058(5) 0.16706(16) 0.0383(15) Uani 1 1 d . . . C56 C 0.22950(19) 0.9001(5) 0.16259(16) 0.0363(14) Uani 1 1 d . . . C57 C 0.2125(2) 1.0010(5) 0.15299(17) 0.0493(17) Uani 1 1 d . . . C58 C 0.2365(3) 1.0893(6) 0.14862(18) 0.0581(19) Uani 1 1 d . . . C59 C 0.2780(3) 1.0790(6) 0.15240(19) 0.067(2) Uani 1 1 d . . . C60 C 0.2967(2) 0.9791(7) 0.16145(19) 0.063(2) Uani 1 1 d . . . C61 C 0.27193(19) 0.8886(5) 0.16690(18) 0.0469(16) Uani 1 1 d . . . H12 H 0.0708 0.2193 0.0737 0.074 Uiso 1 1 calc R . . H13 H 0.0826 0.2522 0.0043 0.072 Uiso 1 1 calc R . . H14 H 0.0824 0.4283 -0.0214 0.058 Uiso 1 1 calc R . . H16 H 0.0609 0.5615 0.211 0.074 Uiso 1 1 calc R . . H17 H 0.0516 0.8474 0.1119 0.078 Uiso 1 1 calc R . . H18 H 0.051 0.4235 0.152 0.071 Uiso 1 1 calc R . . H19 H 0.0573 0.6649 0.0378 0.053 Uiso 1 1 calc R . . H2 H -0.0091 0.6931 0.1547 0.055 Uiso 1 1 calc R . . H20A H 0.1374 0.5728 0.2608 0.13 Uiso 1 1 calc R . . H20B H 0.1313 0.5451 0.2112 0.13 Uiso 1 1 calc R . . H20C H 0.1153 0.4628 0.2449 0.13 Uiso 1 1 calc R . . H21A H 0.0479 0.5073 0.2773 0.159 Uiso 1 1 calc R . . H21B H 0.033 0.6304 0.2736 0.159 Uiso 1 1 calc R . . H21C H 0.0757 0.6011 0.2997 0.159 Uiso 1 1 calc R . . H22A H 0.1007 1.0364 0.1249 0.114 Uiso 1 1 calc R . . H22B H 0.0833 0.9874 0.08 0.114 Uiso 1 1 calc R . . H22C H 0.1177 0.9236 0.1092 0.114 Uiso 1 1 calc R . . H23A H 0.0009 0.9364 0.1434 0.151 Uiso 1 1 calc R . . H23B H 0.0144 1.012 0.1062 0.151 Uiso 1 1 calc R . . H23C H 0.0299 1.0384 0.1545 0.151 Uiso 1 1 calc R . . H24A H -0.0104 0.3387 0.1243 0.135 Uiso 1 1 calc R . . H24B H 0.0059 0.2845 0.1686 0.135 Uiso 1 1 calc R . . H24C H 0.0122 0.224 0.1251 0.135 Uiso 1 1 calc R . . H25A H 0.0901 0.2187 0.1468 0.118 Uiso 1 1 calc R . . H25B H 0.0817 0.2772 0.1901 0.118 Uiso 1 1 calc R . . H25C H 0.113 0.3293 0.1602 0.118 Uiso 1 1 calc R . . H26A H 0.1266 0.6497 0.0329 0.193 Uiso 1 1 calc R . . H26B H 0.1069 0.7258 -0.0045 0.193 Uiso 1 1 calc R . . H26C H 0.1188 0.6034 -0.0143 0.193 Uiso 1 1 calc R . . H27A H 0.0485 0.5887 -0.0464 0.21 Uiso 1 1 calc R . . H27B H 0.0356 0.7054 -0.0304 0.21 Uiso 1 1 calc R . . H27C H 0.0113 0.6001 -0.0175 0.21 Uiso 1 1 calc R . . H29 H 0.3547 0.3718 0.1343 0.051 Uiso 1 1 calc R . . H3 H -0.0138 0.5572 0.0987 0.054 Uiso 1 1 calc R . . H30 H 0.3224 0.3214 0.0638 0.05 Uiso 1 1 calc R . . H33 H 0.2813 0.5772 0.2621 0.073 Uiso 1 1 calc R . . H34 H 0.3328 0.7022 0.2729 0.086 Uiso 1 1 calc R . . H35 H 0.3765 0.7329 0.2223 0.082 Uiso 1 1 calc R . . H39 H 0.1713 0.3734 -0.0141 0.066 Uiso 1 1 calc R . . H40 H 0.1913 0.4825 -0.0677 0.076 Uiso 1 1 calc R . . H41 H 0.2526 0.5732 -0.06 0.079 Uiso 1 1 calc R . . H43 H 0.2555 0.4272 0.1668 0.057 Uiso 1 1 calc R . . H44 H 0.367 0.6088 0.1164 0.093 Uiso 1 1 calc R . . H45 H 0.2322 0.3134 0.0831 0.056 Uiso 1 1 calc R . . H46 H 0.3248 0.5618 0.035 0.08 Uiso 1 1 calc R . . H47A H 0.2803 0.352 0.25 0.089 Uiso 1 1 calc R . . H47B H 0.3023 0.3205 0.2088 0.089 Uiso 1 1 calc R . . H47C H 0.2564 0.282 0.2131 0.089 Uiso 1 1 calc R . . H48A H 0.1998 0.4167 0.2069 0.12 Uiso 1 1 calc R . . H48B H 0.2095 0.5408 0.1977 0.12 Uiso 1 1 calc R . . H48C H 0.223 0.4897 0.2433 0.12 Uiso 1 1 calc R . . H49A H 0.4344 0.6537 0.1785 0.199 Uiso 1 1 calc R . . H49B H 0.4384 0.6197 0.1303 0.199 Uiso 1 1 calc R . . H49C H 0.4217 0.5346 0.1626 0.199 Uiso 1 1 calc R . . H50A H 0.3515 0.7904 0.118 0.179 Uiso 1 1 calc R . . H50B H 0.3984 0.7787 0.1087 0.179 Uiso 1 1 calc R . . H50C H 0.3871 0.8117 0.1551 0.179 Uiso 1 1 calc R . . H51A H 0.1532 0.4099 0.0687 0.076 Uiso 1 1 calc R . . H51B H 0.1902 0.4555 0.1002 0.076 Uiso 1 1 calc R . . H51C H 0.1688 0.3436 0.1105 0.076 Uiso 1 1 calc R . . H52A H 0.1657 0.2336 0.0275 0.084 Uiso 1 1 calc R . . H52B H 0.1837 0.1769 0.0707 0.084 Uiso 1 1 calc R . . H52C H 0.2108 0.1838 0.0314 0.084 Uiso 1 1 calc R . . H53A H 0.3453 0.4853 -0.0266 0.105 Uiso 1 1 calc R . . H53B H 0.3634 0.6052 -0.022 0.105 Uiso 1 1 calc R . . H53C H 0.3244 0.5812 -0.0547 0.105 Uiso 1 1 calc R . . H54A H 0.2901 0.7348 -0.0165 0.144 Uiso 1 1 calc R . . H54B H 0.3278 0.7454 0.019 0.144 Uiso 1 1 calc R . . H54C H 0.2831 0.7198 0.0324 0.144 Uiso 1 1 calc R . . H55A H 0.1769 0.83 0.1784 0.046 Uiso 1 1 calc R . . H55B H 0.2162 0.7538 0.1874 0.046 Uiso 1 1 calc R . . H57 H 0.1836 1.0085 0.1494 0.059 Uiso 1 1 calc R . . H58 H 0.2243 1.1581 0.1429 0.07 Uiso 1 1 calc R . . H59 H 0.2945 1.1408 0.1488 0.08 Uiso 1 1 calc R . . H6 H 0.1103 0.7639 0.2817 0.081 Uiso 1 1 calc R . . H60 H 0.3256 0.9726 0.1639 0.075 Uiso 1 1 calc R . . H61 H 0.284 0.8201 0.1735 0.056 Uiso 1 1 calc R . . H7 H 0.1188 0.9436 0.2641 0.089 Uiso 1 1 calc R . . H8 H 0.0972 1.0065 0.1986 0.082 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 0.0313(4) 0.0445(4) 0.0310(4) -0.0048(3) 0.0028(3) -0.0007(3) Cu2 0.0370(4) 0.0370(4) 0.0241(4) -0.0014(3) 0.0056(3) 0.0010(3) N1 0.028(3) 0.051(3) 0.039(3) -0.006(2) 0.004(2) 0.001(2) N2 0.031(3) 0.052(3) 0.041(3) -0.002(3) 0.000(2) 0.001(2) N3 0.033(3) 0.041(3) 0.035(3) 0.001(2) 0.006(2) 0.004(2) N4 0.045(3) 0.041(3) 0.030(3) 0.005(2) 0.010(2) 0.011(2) S1 0.0356(8) 0.0380(9) 0.0263(8) -0.0051(6) 0.0055(6) -0.0010(7) B1 0.043(5) 0.099(8) 0.048(6) -0.024(5) -0.009(4) 0.022(5) F1 0.052(2) 0.071(3) 0.091(3) -0.015(2) 0.002(2) 0.025(2) F2 0.091(3) 0.119(4) 0.063(3) -0.031(3) -0.024(2) 0.057(3) F3 0.079(3) 0.112(4) 0.127(4) 0.010(3) 0.051(3) 0.033(3) F4 0.066(3) 0.090(3) 0.093(3) -0.014(3) -0.021(2) 0.013(2) C1 0.035(3) 0.048(4) 0.028(3) -0.005(3) 0.001(3) -0.001(3) C2 0.031(4) 0.060(4) 0.046(4) -0.007(3) 0.001(3) -0.001(3) C3 0.030(4) 0.057(4) 0.047(4) 0.004(3) -0.003(3) -0.004(3) C4 0.032(4) 0.059(5) 0.049(4) -0.017(4) 0.005(3) 0.009(3) C5 0.033(4) 0.085(5) 0.040(4) -0.015(4) 0.008(3) 0.010(4) C6 0.058(5) 0.112(7) 0.032(4) -0.016(4) 0.004(3) 0.013(5) C7 0.079(6) 0.082(6) 0.060(6) -0.029(5) -0.001(4) 0.003(5) C8 0.066(5) 0.064(5) 0.073(6) -0.012(4) 0.004(4) 0.019(4) C9 0.057(5) 0.061(5) 0.064(5) -0.016(4) 0.000(4) 0.023(4) C10 0.031(4) 0.039(4) 0.049(4) -0.002(3) -0.008(3) -0.004(3) C11 0.041(4) 0.050(4) 0.055(4) 0.000(4) -0.013(3) -0.010(3) C12 0.048(4) 0.047(4) 0.085(6) 0.004(4) -0.011(4) 0.002(3) C13 0.056(5) 0.049(5) 0.072(6) -0.019(4) -0.007(4) 0.002(4) C14 0.045(4) 0.053(4) 0.046(4) -0.015(3) -0.004(3) -0.004(3) C15 0.033(3) 0.049(4) 0.031(3) -0.005(3) -0.009(3) -0.003(3) C16 0.060(5) 0.087(6) 0.037(4) 0.004(4) 0.005(3) -0.002(4) C17 0.063(5) 0.063(5) 0.068(5) -0.003(4) -0.004(4) 0.016(4) C18 0.055(4) 0.063(5) 0.059(5) 0.029(4) 0.000(4) -0.012(4) C19 0.052(4) 0.050(4) 0.030(3) 0.002(3) -0.002(3) -0.012(3) C20 0.078(6) 0.099(6) 0.082(6) 0.027(5) -0.003(5) 0.003(5) C21 0.102(7) 0.168(9) 0.051(5) -0.011(5) 0.025(5) -0.038(6) C22 0.094(6) 0.082(6) 0.053(5) -0.002(4) 0.009(4) 0.016(5) C23 0.074(6) 0.111(7) 0.117(8) 0.021(6) 0.006(5) 0.048(5) C24 0.070(6) 0.115(7) 0.082(6) 0.048(5) -0.006(5) -0.017(5) C25 0.078(6) 0.089(6) 0.065(5) 0.025(4) -0.008(4) 0.004(5) C26 0.112(8) 0.113(8) 0.164(10) 0.054(7) 0.031(7) -0.018(7) C27 0.111(8) 0.096(7) 0.196(12) 0.071(7) -0.075(8) -0.026(6) C28 0.043(4) 0.039(4) 0.024(3) 0.003(3) 0.011(3) -0.003(3) C29 0.034(4) 0.051(4) 0.044(4) 0.012(3) 0.006(3) 0.005(3) C30 0.043(4) 0.051(4) 0.032(4) -0.003(3) 0.007(3) 0.009(3) C31 0.039(4) 0.042(4) 0.032(4) -0.003(3) -0.007(3) 0.005(3) C32 0.053(4) 0.059(4) 0.022(3) 0.004(3) -0.009(3) 0.001(3) C33 0.076(5) 0.069(5) 0.036(4) 0.001(4) -0.008(4) 0.013(4) C34 0.083(6) 0.079(6) 0.049(5) -0.024(4) -0.017(5) 0.019(5) C35 0.064(5) 0.042(4) 0.088(6) -0.016(4) -0.046(5) 0.000(4) C36 0.041(4) 0.045(4) 0.066(5) -0.003(4) -0.015(3) -0.002(3) C37 0.056(4) 0.042(4) 0.018(3) 0.000(3) 0.003(3) 0.014(3) C38 0.045(4) 0.047(4) 0.025(3) -0.006(3) 0.002(3) 0.016(3) C39 0.062(5) 0.069(5) 0.032(4) -0.010(3) 0.000(3) 0.025(4) C40 0.087(6) 0.068(5) 0.032(4) -0.004(4) -0.002(4) 0.034(5) C41 0.122(7) 0.054(5) 0.024(4) 0.011(3) 0.024(4) 0.044(5) C42 0.076(5) 0.037(4) 0.028(4) 0.000(3) 0.018(3) 0.019(3) C43 0.052(4) 0.068(5) 0.022(3) 0.006(3) 0.004(3) 0.001(4) C44 0.051(5) 0.062(5) 0.121(7) -0.004(5) 0.021(5) -0.013(4) C45 0.043(4) 0.060(4) 0.036(4) 0.003(3) 0.006(3) 0.009(3) C46 0.100(6) 0.058(5) 0.048(5) 0.008(4) 0.035(4) -0.005(4) C47 0.073(5) 0.063(5) 0.041(4) -0.008(3) 0.001(3) -0.001(4) C48 0.071(6) 0.079(6) 0.094(6) 0.036(5) 0.029(5) 0.009(4) C49 0.052(6) 0.153(10) 0.196(12) 0.025(8) 0.031(6) 0.013(6) C50 0.140(9) 0.080(7) 0.143(9) 0.017(6) 0.042(7) -0.012(6) C51 0.046(4) 0.059(4) 0.048(4) -0.019(3) 0.009(3) -0.004(3) C52 0.075(5) 0.044(4) 0.048(4) -0.008(3) -0.004(4) 0.011(4) C53 0.102(6) 0.059(5) 0.053(5) 0.009(4) 0.030(4) 0.000(4) C54 0.143(8) 0.068(6) 0.087(6) -0.013(5) 0.061(6) -0.010(5) C55 0.042(4) 0.047(4) 0.027(3) -0.004(3) 0.007(3) -0.003(3) C56 0.052(4) 0.040(4) 0.016(3) -0.008(3) 0.001(3) -0.004(3) C57 0.067(5) 0.047(4) 0.033(4) -0.008(3) 0.000(3) -0.011(4) C58 0.089(6) 0.059(5) 0.026(4) -0.005(3) 0.004(4) -0.013(4) C59 0.112(7) 0.059(5) 0.032(4) -0.014(4) 0.022(4) -0.039(5) C60 0.059(5) 0.095(6) 0.034(4) -0.028(4) 0.009(3) -0.024(5) C61 0.047(4) 0.058(4) 0.036(4) -0.011(3) 0.006(3) -0.010(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 Cu1 C1 1.882(6) . ? Cu1 S1 2.1570(16) . ? Cu2 C28 1.874(6) . ? Cu2 S1 2.1462(16) . ? N1 C1 1.355(7) . ? N1 C2 1.387(7) . ? N1 C4 1.447(7) . ? N2 C1 1.367(7) . ? N2 C3 1.386(7) . ? N2 C10 1.442(7) . ? N3 C29 1.392(7) . ? N3 C31 1.442(7) . ? N4 C30 1.381(7) . ? N4 C37 1.452(7) . ? S1 C55 1.858(5) . ? F1 B1 1.372(9) . ? F2 B1 1.380(9) . ? F3 B1 1.381(9) . ? F4 B1 1.383(9) . ? C2 C3 1.313(8) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C4 C9 1.375(9) . ? C5 C4 1.394(8) . ? C5 C6 1.409(9) . ? C5 C16 1.529(9) . ? C6 C7 1.375(10) . ? C6 H6 0.95 . ? C7 H7 0.95 . ? C8 C7 1.340(9) . ? C8 H8 0.95 . ? C9 C8 1.393(9) . ? C9 C17 1.499(9) . ? C11 C12 1.403(9) . ? C11 C10 1.405(8) . ? C11 C18 1.528(9) . ? C12 H12 0.95 . ? C13 C12 1.372(9) . ? C13 H13 0.95 . ? C14 C13 1.383(9) . ? C14 H14 0.95 . ? C15 C14 1.398(8) . ? C15 C10 1.400(8) . ? C15 C19 1.502(8) . ? C16 C20 1.505(9) . ? C16 C21 1.523(9) . ? C16 H16 1 . ? C17 C23 1.517(9) . ? C17 C22 1.521(9) . ? C17 H17 1 . ? C18 C24 1.541(9) . ? C18 H18 1 . ? C19 C27 1.473(9) . ? C19 C26 1.486(10) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C18 1.519(8) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 N4 1.352(6) . ? C28 N3 1.363(7) . ? C29 H29 0.95 . ? C30 C29 1.329(7) . ? C30 H30 0.95 . ? C31 C32 1.395(8) . ? C31 C36 1.396(8) . ? C32 C33 1.380(8) . ? C32 C43 1.518(8) . ? C33 C34 1.360(10) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? C35 C34 1.353(10) . ? C35 H35 0.95 . ? C36 C35 1.432(9) . ? C36 C44 1.498(10) . ? C37 C38 1.358(8) . ? C37 C42 1.396(8) . ? C38 C39 1.397(8) . ? C39 C40 1.371(9) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? C41 C40 1.365(10) . ? C41 H41 0.95 . ? C42 C41 1.412(9) . ? C42 C46 1.510(9) . ? C43 C48 1.516(8) . ? C43 H43 1 . ? C44 C50 1.508(10) . ? C44 C49 1.544(10) . ? C44 H44 1 . ? C45 C52 1.520(8) . ? C45 C38 1.526(8) . ? C45 C51 1.526(8) . ? C45 H45 1 . ? C46 C53 1.519(8) . ? C46 C54 1.534(9) . ? C46 H46 1 . ? C47 C43 1.511(8) . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 C57 1.390(8) . ? C56 C61 1.395(8) . ? C56 C55 1.481(7) . ? C57 C58 1.362(8) . ? C57 H57 0.95 . ? C58 H58 0.95 . ? C59 C58 1.363(9) . ? C59 C60 1.397(10) . ? C59 H59 0.95 . ? C60 H60 0.95 . ? C61 C60 1.405(9) . ? C61 H61 0.95 . ? 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 Cu2 S1 Cu1 112.34(7) . . ? N1 C1 N2 103.3(5) . . ? N1 C1 Cu1 123.5(4) . . ? N1 C2 H2 126.7 . . ? N2 C1 Cu1 131.8(4) . . ? N2 C3 H3 126.1 . . ? N3 C28 Cu2 127.5(4) . . ? N3 C29 H29 126.4 . . ? N4 C28 N3 103.7(5) . . ? N4 C28 Cu2 128.2(4) . . ? N4 C30 H30 126.8 . . ? S1 C55 H55A 109.5 . . ? S1 C55 H55B 109.5 . . ? F1 B1 F2 111.8(6) . . ? F1 B1 F3 110.2(8) . . ? F1 B1 F4 111.5(6) . . ? F2 B1 F3 108.8(6) . . ? F2 B1 F4 108.9(8) . . ? F3 B1 F4 105.3(6) . . ? C1 Cu1 S1 162.41(18) . . ? C1 N1 C2 111.7(5) . . ? C1 N1 C4 122.0(5) . . ? C1 N2 C3 110.6(5) . . ? C1 N2 C10 124.7(5) . . ? C2 N1 C4 126.3(5) . . ? C2 C3 N2 107.9(5) . . ? C2 C3 H3 126.1 . . ? C3 N2 C10 124.2(5) . . ? C3 C2 N1 106.6(5) . . ? C3 C2 H2 126.7 . . ? C4 C5 C6 116.0(7) . . ? C4 C5 C16 123.3(6) . . ? C4 C9 C8 116.3(7) . . ? C4 C9 C17 123.2(6) . . ? C5 C4 N1 117.3(6) . . ? C5 C16 H16 107.6 . . ? C5 C6 H6 119.8 . . ? C6 C5 C16 120.7(7) . . ? C6 C7 H7 119.5 . . ? C7 C6 C5 120.4(7) . . ? C7 C6 H6 119.8 . . ? C7 C8 C9 122.1(8) . . ? C7 C8 H8 118.9 . . ? C8 C9 C17 120.5(7) . . ? C8 C7 C6 121.0(7) . . ? C8 C7 H7 119.5 . . ? C9 C4 C5 124.2(6) . . ? C9 C4 N1 118.5(6) . . ? C9 C17 C23 110.7(6) . . ? C9 C17 C22 112.8(6) . . ? C9 C17 H17 107.1 . . ? C9 C8 H8 118.9 . . ? C10 C11 C18 122.4(6) . . ? C10 C15 C19 122.3(5) . . ? C11 C10 N2 116.4(6) . . ? C11 C18 C24 110.6(5) . . ? C11 C18 H18 107.7 . . ? C11 C12 H12 118.7 . . ? C12 C11 C10 115.4(6) . . ? C12 C11 C18 122.2(6) . . ? C12 C13 C14 119.9(6) . . ? C12 C13 H13 120 . . ? C13 C14 C15 121.1(6) . . ? C13 C14 H14 119.4 . . ? C13 C12 C11 122.7(7) . . ? C13 C12 H12 118.7 . . ? C14 C15 C10 116.9(6) . . ? C14 C15 C19 120.7(6) . . ? C14 C13 H13 120 . . ? C15 C19 H19 107.7 . . ? C15 C14 H14 119.4 . . ? C15 C10 C11 123.9(6) . . ? C15 C10 N2 119.7(5) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? C20 C16 C21 111.7(6) . . ? C20 C16 C5 110.7(6) . . ? C20 C16 H16 107.6 . . ? C21 C16 C5 111.5(6) . . ? C21 C16 H16 107.6 . . ? C22 C17 H17 107.1 . . ? C23 C17 C22 111.6(6) . . ? C23 C17 H17 107.1 . . ? C24 C18 H18 107.7 . . ? C25 C18 C11 111.3(6) . . ? C25 C18 C24 111.7(6) . . ? C25 C18 H18 107.7 . . ? C26 C19 C15 110.5(6) . . ? C26 C19 H19 107.7 . . ? C27 C19 C26 109.9(7) . . ? C27 C19 C15 113.0(5) . . ? C27 C19 H19 107.7 . . ? C28 Cu2 S1 176.01(17) . . ? C28 N4 C30 111.9(5) . . ? C28 N4 C37 121.9(5) . . ? C28 N3 C29 110.5(5) . . ? C28 N3 C31 121.3(5) . . ? C29 N3 C31 128.2(5) . . ? C29 C30 N4 106.5(5) . . ? C29 C30 H30 126.8 . . ? C30 N4 C37 125.9(5) . . ? C30 C29 N3 107.3(5) . . ? C30 C29 H29 126.4 . . ? C31 C32 C43 122.5(5) . . ? C31 C36 C35 113.8(6) . . ? C31 C36 C44 122.9(6) . . ? C32 C31 C36 124.9(6) . . ? C32 C31 N3 116.9(5) . . ? C32 C33 H33 119 . . ? C32 C43 H43 107.2 . . ? C33 C32 C31 116.4(6) . . ? C33 C32 C43 121.1(6) . . ? C33 C34 H34 119.8 . . ? C34 C33 C32 122.1(7) . . ? C34 C33 H33 119 . . ? C34 C35 C36 122.5(7) . . ? C34 C35 H35 118.8 . . ? C35 C36 C44 123.3(6) . . ? C35 C34 C33 120.3(7) . . ? C35 C34 H34 119.8 . . ? C36 C31 N3 118.2(5) . . ? C36 C35 H35 118.8 . . ? C36 C44 C50 112.5(7) . . ? C36 C44 C49 111.9(7) . . ? C36 C44 H44 107.6 . . ? C37 C42 C41 115.3(7) . . ? C37 C42 C46 122.3(6) . . ? C37 C38 C39 117.7(6) . . ? C37 C38 C45 122.7(5) . . ? C38 C37 C42 124.6(6) . . ? C38 C37 N4 119.3(5) . . ? C38 C45 C51 110.8(5) . . ? C38 C45 H45 107.2 . . ? C38 C39 H39 119.9 . . ? C39 C38 C45 119.5(6) . . ? C39 C40 H40 119.5 . . ? C40 C39 C38 120.1(7) . . ? C40 C39 H39 119.9 . . ? C40 C41 C42 121.1(6) . . ? C40 C41 H41 119.4 . . ? C41 C42 C46 122.4(6) . . ? C41 C40 C39 121.1(7) . . ? C41 C40 H40 119.5 . . ? C42 C37 N4 116.1(6) . . ? C42 C46 C53 112.0(6) . . ? C42 C46 C54 110.5(6) . . ? C42 C46 H46 107.6 . . ? C42 C41 H41 119.4 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? C45 C52 H52A 109.5 . . ? C45 C52 H52B 109.5 . . ? C45 C52 H52C 109.5 . . ? C46 C53 H53A 109.5 . . ? C46 C53 H53B 109.5 . . ? C46 C53 H53C 109.5 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? C47 C43 C48 111.0(5) . . ? C47 C43 C32 110.0(5) . . ? C47 C43 H43 107.2 . . ? C48 C43 C32 113.9(6) . . ? C48 C43 H43 107.2 . . ? C49 C44 H44 107.6 . . ? C50 C44 C49 109.3(7) . . ? C50 C44 H44 107.6 . . ? C51 C45 H45 107.2 . . ? C52 C45 C38 112.4(5) . . ? C52 C45 C51 111.6(5) . . ? C52 C45 H45 107.2 . . ? C53 C46 C54 111.4(6) . . ? C53 C46 H46 107.6 . . ? C54 C46 H46 107.6 . . ? C55 S1 Cu2 105.89(19) . . ? C55 S1 Cu1 103.70(18) . . ? C56 C61 C60 119.4(6) . . ? C56 C61 H61 120.3 . . ? C56 C55 S1 110.7(4) . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? C56 C57 H57 119.4 . . ? C57 C56 C61 119.4(6) . . ? C57 C56 C55 119.7(6) . . ? C57 C58 C59 120.0(7) . . ? C57 C58 H58 120 . . ? C58 C59 C60 121.2(7) . . ? C58 C59 H59 119.4 . . ? C58 C57 C56 121.2(7) . . ? C58 C57 H57 119.4 . . ? C59 C60 C61 118.9(7) . . ? C59 C60 H60 120.6 . . ? C59 C58 H58 120 . . ? C60 C61 H61 120.3 . . ? C60 C59 H59 119.4 . . ? C61 C56 C55 120.9(6) . . ? C61 C60 H60 120.6 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? H55A C55 H55B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.866 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.104 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 224.4 59.6 2 0.500 0.500 0.000 224.4 59.6 3 0.500 0.589 0.250 135.1 20.2 4 1.000 1.089 0.250 135.1 20.2 5 0.000 1.000 0.500 224.5 59.8 6 0.500 0.500 0.500 224.5 59.8 7 0.500 0.411 0.750 135.2 20.0 8 1.000 -0.089 0.750 135.2 20.0 _platon_squeeze_details ; Because disordered pentanes of solvation were found in the initial refinement that could not be satisfactorily modeled, the SQUEEZE subroutine of PLATON was used. 319 solvent electrons were identified corresponding to 1 molecule of pentane per IPrCu2SBnBF4 and the reflection data were refined excluding the solvent to give the results below. PLATON: Spek, A. L. Acta Crystallogr. 1990, A46, C-34. ; # Attachment 'cmpd_5-rev-resub.CIF' data_c:IPrCu2StBuBF4 _database_code_depnum_ccdc_archive 'CCDC 736335' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IPrCu2StBuBF4 _chemical_melting_point ? _chemical_formula_moiety 'C58 H81 Cu2 N4 S, 2(C4 H8 O), B F4' _chemical_formula_sum 'C66 H97 B Cu2 F4 N4 O2 S' _chemical_formula_weight 1224.43 _journal_name_requested 'Chemical Communications' 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.348(3) _cell_length_b 17.138(4) _cell_length_c 17.187(4) _cell_angle_alpha 75.961(3) _cell_angle_beta 75.033(3) _cell_angle_gamma 72.937(3) _cell_volume 3303.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7011 _cell_measurement_theta_min 4.709 _cell_measurement_theta_max 50.020 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8677 _exptl_absorpt_correction_T_max 0.8797 _exptl_absorpt_process_details "SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38" _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'APEX II platform CCDm Bruker' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32174 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11602 _reflns_number_gt 8024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows; Ferrugia L J (1997), J. Appl. Cryst. 30, 565' _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. The tert-butyl group was modeled over two sets of positions in which S1A, C55A, C56A, C57A, C58A and S1B, C55B, C56B, C57B, C58B are assigned occupancies of 0.530 and 0.470. Both positions were refined aniosotropically. The fluorine atoms in the BF4 anion exibit disorder. They were modeled over two sets of positions in which F1A, F2A, F3A, F4A; F1B, F2B, F3B, F4B are assigned occupancies of 0.640 and 0.360. DFIX restraints were employed setting each B-F distance similar to give a tetrahedron of F1A-F4A and F1B-F4B about B1. Each set of F positions were refined anisotropically. One THF (C59-C62;O63) was modeled with the O atom over two sets of positions (O63A and O63B) with equal occupancies. The other THF was modeled as two separate THF rings (C63-C66;O67) and (O76;C69-C72) sharing a common O atom (O67) with occupancies of 0.74 and 0.26. The lower occupancy THF C atoms were refined isotropically. ; _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^)+(0.0648P)^2^+2.0772P] 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 11602 _refine_ls_number_parameters 853 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.088 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.75509(4) 0.02332(2) 0.28486(3) 0.02888(14) Uani 1 1 d . . . Cu2 Cu 0.69919(4) 0.25034(3) 0.28030(3) 0.02968(14) Uani 1 1 d . . . S1A S 0.7716(3) 0.1240(3) 0.3349(2) 0.0281(7) Uani 0.53 1 d PD E 1 S1B S 0.8016(4) 0.1240(4) 0.3101(3) 0.0396(13) Uani 0.47 1 d PDU D 2 N1 N 0.8043(2) -0.15183(16) 0.27993(17) 0.0239(6) Uani 1 1 d . . . N2 N 0.6414(2) -0.08872(17) 0.24647(18) 0.0263(7) Uani 1 1 d . D . N3 N 0.6110(2) 0.42189(16) 0.30248(16) 0.0210(6) Uani 1 1 d . . . N4 N 0.5609(2) 0.40629(16) 0.19834(16) 0.0207(6) Uani 1 1 d . . . C1 C 0.7322(3) -0.0752(2) 0.2675(2) 0.0244(8) Uani 1 1 d . D . C2 C 0.7590(3) -0.2116(2) 0.2671(2) 0.0298(8) Uani 1 1 d . . . C3 C 0.6571(3) -0.1721(2) 0.2460(2) 0.0325(9) Uani 1 1 d . . . C4 C 0.9177(3) -0.1675(2) 0.2976(2) 0.0272(8) Uani 1 1 d . . . C5 C 1.0122(3) -0.1699(2) 0.2315(3) 0.0378(10) Uani 1 1 d . . . C6 C 1.1213(3) -0.1835(2) 0.2491(3) 0.0502(12) Uani 1 1 d . . . C7 C 1.1329(4) -0.1949(2) 0.3294(3) 0.0487(12) Uani 1 1 d . . . C8 C 1.0394(4) -0.1940(2) 0.3925(3) 0.0435(11) Uani 1 1 d . . . C9 C 0.9290(3) -0.1815(2) 0.3785(2) 0.0324(9) Uani 1 1 d . . . C10 C 0.5416(3) -0.0254(2) 0.2235(2) 0.0280(8) Uani 1 1 d . . . C11 C 0.5559(3) 0.0226(2) 0.1455(2) 0.0310(9) Uani 1 1 d . . . C12 C 0.4564(3) 0.0791(2) 0.1229(3) 0.0364(10) Uani 1 1 d . . . C13 C 0.3503(3) 0.0861(2) 0.1758(3) 0.0390(10) Uani 1 1 d . . . C14 C 0.3407(3) 0.0381(2) 0.2529(3) 0.0365(10) Uani 1 1 d . . . C15 C 0.4363(3) -0.0191(2) 0.2791(2) 0.0313(9) Uani 1 1 d . . . C16 C 0.9980(4) -0.1573(3) 0.1441(3) 0.0534(13) Uani 1 1 d . . . C17 C 0.8274(4) -0.1867(3) 0.4497(2) 0.0455(11) Uani 1 1 d . . . C18 C 0.6710(3) 0.0178(2) 0.0855(2) 0.0359(9) Uani 1 1 d . . . C19 C 0.4260(3) -0.0716(2) 0.3648(2) 0.0344(9) Uani 1 1 d . . . C20 C 1.0009(5) -0.0688(3) 0.1009(3) 0.085(2) Uani 1 1 d . . . C21 C 1.0903(4) -0.2192(3) 0.0963(3) 0.0681(16) Uani 1 1 d . . . C22 C 0.8061(5) -0.1219(3) 0.5027(3) 0.0817(19) Uani 1 1 d . . . C23 C 0.8431(4) -0.2736(3) 0.5000(3) 0.0571(13) Uani 1 1 d . . . C24 C 0.6648(4) 0.0071(4) 0.0011(3) 0.0649(14) Uani 1 1 d . . . C25 C 0.7145(4) 0.0947(3) 0.0781(3) 0.0435(10) Uani 1 1 d . . . C26 C 0.4730(3) -0.0376(3) 0.4207(3) 0.0408(10) Uani 1 1 d . . . C27 C 0.3024(3) -0.0796(3) 0.4048(3) 0.0439(10) Uani 1 1 d . . . C28 C 0.6219(3) 0.3637(2) 0.2575(2) 0.0210(7) Uani 1 1 d . . . C29 C 0.5453(3) 0.4981(2) 0.2722(2) 0.0225(8) Uani 1 1 d . D . C30 C 0.5135(3) 0.4884(2) 0.2073(2) 0.0230(8) Uani 1 1 d . D . C31 C 0.6664(3) 0.4041(2) 0.3713(2) 0.0236(8) Uani 1 1 d . . . C32 C 0.6100(3) 0.3708(2) 0.4477(2) 0.0265(8) Uani 1 1 d . . . C33 C 0.6684(4) 0.3511(2) 0.5127(2) 0.0346(9) Uani 1 1 d . . . C34 C 0.7746(4) 0.3671(2) 0.5003(2) 0.0375(10) Uani 1 1 d . . . C35 C 0.8273(3) 0.4029(2) 0.4243(3) 0.0358(10) Uani 1 1 d . . . C36 C 0.7751(3) 0.4220(2) 0.3570(2) 0.0272(8) Uani 1 1 d . . . C37 C 0.5453(3) 0.3708(2) 0.1350(2) 0.0227(8) Uani 1 1 d . . . C38 C 0.6097(3) 0.3874(2) 0.0563(2) 0.0259(8) Uani 1 1 d . . . C39 C 0.5901(3) 0.3547(2) -0.0041(2) 0.0323(9) Uani 1 1 d . . . C40 C 0.5086(3) 0.3083(2) 0.0140(2) 0.0340(9) Uani 1 1 d . . . C41 C 0.4468(3) 0.2925(2) 0.0928(2) 0.0339(9) Uani 1 1 d . . . C42 C 0.4635(3) 0.3229(2) 0.1561(2) 0.0262(8) Uani 1 1 d . . . C43 C 0.4909(3) 0.3553(2) 0.4623(2) 0.0310(9) Uani 1 1 d . . . C44 C 0.8299(3) 0.4646(2) 0.2741(2) 0.0335(9) Uani 1 1 d . . . C45 C 0.7005(3) 0.4369(2) 0.0372(2) 0.0307(8) Uani 1 1 d . . . C46 C 0.3955(3) 0.3036(2) 0.2427(2) 0.0304(8) Uani 1 1 d . . . C47 C 0.4960(4) 0.2628(3) 0.4857(3) 0.0528(12) Uani 1 1 d . . . C48 C 0.4051(4) 0.4010(3) 0.5273(3) 0.0453(11) Uani 1 1 d . . . C49 C 0.9575(4) 0.4237(3) 0.2484(3) 0.0575(13) Uani 1 1 d . . . C50 C 0.8133(4) 0.5560(3) 0.2746(3) 0.0463(11) Uani 1 1 d . . . C51 C 0.8131(3) 0.3820(3) 0.0618(3) 0.0469(11) Uani 1 1 d . . . C52 C 0.7243(4) 0.4803(3) -0.0517(2) 0.0437(10) Uani 1 1 d . . . C53 C 0.2662(3) 0.3193(3) 0.2454(3) 0.0403(10) Uani 1 1 d . . . C54 C 0.4437(3) 0.2133(2) 0.2820(2) 0.0367(9) Uani 1 1 d . . . C55A C 0.9269(8) 0.1171(5) 0.3221(7) 0.038(2) Uani 0.53 1 d P E 1 C55B C 0.9533(14) 0.1188(9) 0.2600(15) 0.051(6) Uani 0.47 1 d P D 2 C56A C 0.9880(9) 0.0288(6) 0.3517(9) 0.073(4) Uani 0.53 1 d P E 1 C56B C 1.0249(10) 0.0314(6) 0.2786(9) 0.063(3) Uani 0.47 1 d P D 2 C57A C 0.9389(11) 0.1778(7) 0.3668(9) 0.087(4) Uani 0.53 1 d PD E 1 C57B C 0.9959(9) 0.1801(7) 0.2876(11) 0.078(4) Uani 0.47 1 d PD D 2 C58A C 0.9748(14) 0.1433(11) 0.2293(13) 0.074(6) Uani 0.53 1 d P E 1 C58B C 0.9608(11) 0.1435(8) 0.1624(9) 0.076(4) Uani 0.47 1 d P D 2 C59 C 1.1163(4) -0.5057(3) 0.4116(3) 0.0508(12) Uani 1 1 d . . . C60 C 1.2287(3) -0.4978(3) 0.3549(3) 0.0414(10) Uani 1 1 d . F . C61 C 1.1916(4) -0.4413(3) 0.2792(3) 0.0500(12) Uani 1 1 d . F . C62 C 1.0730(4) -0.3931(3) 0.3121(3) 0.0508(12) Uani 1 1 d . . . C63 C 0.7793(8) 0.7783(5) 0.0170(5) 0.078(2) Uani 0.74 1 d PDU C 8 C64 C 0.8302(6) 0.7022(3) 0.0719(4) 0.0481(15) Uani 0.74 1 d P C 8 C65 C 0.8383(8) 0.6324(4) 0.0329(4) 0.0500(17) Uani 0.74 1 d P C 8 C66 C 0.8578(6) 0.6747(4) -0.0580(4) 0.0545(19) Uani 0.74 1 d PD C 8 C69 C 0.9011(13) 0.6996(13) -0.0603(18) 0.089(10) Uiso 0.26 1 d PD C 9 C70 C 0.879(2) 0.6219(16) 0.0000(16) 0.072(9) Uiso 0.26 1 d PD C 9 C71 C 0.762(2) 0.6479(13) 0.0586(14) 0.069(6) Uiso 0.26 1 d PD C 9 C72 C 0.742(3) 0.7424(18) 0.0252(9) 0.127(13) Uiso 0.26 1 d PD C 9 O63A O 1.0378(11) -0.4337(8) 0.3890(10) 0.049(3) Uani 0.5 1 d P F 6 O63B O 1.0216(13) -0.4561(9) 0.3758(11) 0.052(4) Uani 0.5 1 d P F 7 O67 O 0.7958(3) 0.7577(2) -0.0583(3) 0.0829(12) Uani 1 1 d DU . . B1 B 0.4527(4) -0.2767(3) 0.2130(3) 0.0349(11) Uani 1 1 d D . . F1A F 0.3814(9) -0.3243(6) 0.2170(6) 0.059(3) Uani 0.36 1 d PDU G 4 F1B F 0.3899(4) -0.3159(3) 0.1856(3) 0.0363(11) Uani 0.64 1 d PDU G 3 F2A F 0.5590(7) -0.3171(5) 0.2237(6) 0.077(3) Uani 0.36 1 d PDU G 4 F2B F 0.5674(3) -0.3039(3) 0.1707(3) 0.0514(10) Uani 0.64 1 d PDU G 3 F3A F 0.4503(7) -0.2072(5) 0.1530(5) 0.065(2) Uani 0.36 1 d PDU G 4 F3B F 0.4131(4) -0.1945(3) 0.1973(4) 0.0763(15) Uani 0.64 1 d PDU G 3 F4A F 0.4057(7) -0.2356(5) 0.2843(4) 0.064(2) Uani 0.36 1 d PDU G 4 F4B F 0.4551(4) -0.3030(3) 0.2924(3) 0.0657(12) Uani 0.64 1 d PDU G 3 H12 H 0.4622 0.1133 0.0701 0.044 Uiso 1 1 calc R . . H13 H 0.2837 0.1242 0.1589 0.047 Uiso 1 1 calc R . . H14 H 0.2673 0.0441 0.289 0.044 Uiso 1 1 calc R . . H16 H 0.9206 -0.1655 0.1455 0.064 Uiso 1 1 calc R . . H17 H 0.757 -0.175 0.4262 0.055 Uiso 1 1 calc R . . H18 H 0.7283 -0.0318 0.1079 0.043 Uiso 1 1 calc R D . H19 H 0.4755 -0.1287 0.3599 0.041 Uiso 1 1 calc R . . H2 H 0.7937 -0.2695 0.2724 0.036 Uiso 1 1 calc R . . H20A H 0.9377 -0.0296 0.1297 0.128 Uiso 1 1 calc R D . H20B H 0.9918 -0.0613 0.0444 0.128 Uiso 1 1 calc R . . H20C H 1.0751 -0.0588 0.1008 0.128 Uiso 1 1 calc R . . H21A H 1.1667 -0.2105 0.0922 0.102 Uiso 1 1 calc R D . H21B H 1.0752 -0.2111 0.0413 0.102 Uiso 1 1 calc R . . H21C H 1.0882 -0.2758 0.1249 0.102 Uiso 1 1 calc R . . H22A H 0.8732 -0.1323 0.5275 0.123 Uiso 1 1 calc R D . H22B H 0.7372 -0.1254 0.5459 0.123 Uiso 1 1 calc R . . H22C H 0.7941 -0.0664 0.4687 0.123 Uiso 1 1 calc R . . H23A H 0.8596 -0.3138 0.4639 0.086 Uiso 1 1 calc R D . H23B H 0.7722 -0.2779 0.5409 0.086 Uiso 1 1 calc R . . H23C H 0.9077 -0.2854 0.5278 0.086 Uiso 1 1 calc R . . H24A H 0.6313 -0.0398 0.0072 0.097 Uiso 1 1 calc R . . H24B H 0.7428 -0.0036 -0.0328 0.097 Uiso 1 1 calc R . . H24C H 0.6164 0.0578 -0.0251 0.097 Uiso 1 1 calc R . . H25A H 0.6614 0.144 0.054 0.065 Uiso 1 1 calc R . . H25B H 0.7918 0.0887 0.043 0.065 Uiso 1 1 calc R . . H25C H 0.7181 0.1008 0.1326 0.065 Uiso 1 1 calc R . . H26A H 0.5545 -0.0383 0.3977 0.061 Uiso 1 1 calc R . . H26B H 0.4659 -0.0723 0.4753 0.061 Uiso 1 1 calc R . . H26C H 0.4285 0.0194 0.4247 0.061 Uiso 1 1 calc R . . H27A H 0.2542 -0.0259 0.4178 0.066 Uiso 1 1 calc R . . H27B H 0.3036 -0.1211 0.4553 0.066 Uiso 1 1 calc R . . H27C H 0.2705 -0.0968 0.3669 0.066 Uiso 1 1 calc R . . H29 H 0.5265 0.5478 0.2934 0.027 Uiso 1 1 calc R . . H3 H 0.6056 -0.1965 0.2332 0.039 Uiso 1 1 calc R D . H30 H 0.4671 0.5299 0.1736 0.028 Uiso 1 1 calc R . . H33 H 0.6341 0.3265 0.5655 0.041 Uiso 1 1 calc R . . H34 H 0.8129 0.3533 0.545 0.045 Uiso 1 1 calc R D . H35 H 0.8999 0.4147 0.4179 0.043 Uiso 1 1 calc R . . H39 H 0.6331 0.3642 -0.0584 0.039 Uiso 1 1 calc R . . H40 H 0.4953 0.2873 -0.0281 0.041 Uiso 1 1 calc R . . H41 H 0.3918 0.2604 0.1044 0.041 Uiso 1 1 calc R . . H43 H 0.4622 0.3768 0.4099 0.037 Uiso 1 1 calc R . . H44 H 0.789 0.4609 0.2324 0.04 Uiso 1 1 calc R . . H45 H 0.6704 0.4811 0.0717 0.037 Uiso 1 1 calc R . . H46 H 0.4053 0.3409 0.2757 0.036 Uiso 1 1 calc R . . H47A H 0.5514 0.2339 0.4434 0.079 Uiso 1 1 calc R D . H47B H 0.4192 0.2544 0.4904 0.079 Uiso 1 1 calc R . . H47C H 0.5206 0.2406 0.5383 0.079 Uiso 1 1 calc R . . H48A H 0.4291 0.379 0.5801 0.068 Uiso 1 1 calc R D . H48B H 0.328 0.3933 0.5318 0.068 Uiso 1 1 calc R . . H48C H 0.4029 0.4603 0.5118 0.068 Uiso 1 1 calc R . . H49A H 0.9992 0.4244 0.2895 0.086 Uiso 1 1 calc R D . H49B H 0.9892 0.4541 0.1953 0.086 Uiso 1 1 calc R . . H49C H 0.9665 0.3662 0.2437 0.086 Uiso 1 1 calc R . . H50A H 0.7305 0.5832 0.2847 0.069 Uiso 1 1 calc R . . H50B H 0.8513 0.5825 0.2216 0.069 Uiso 1 1 calc R . . H50C H 0.8474 0.5613 0.3181 0.069 Uiso 1 1 calc R . . H51A H 0.8449 0.3377 0.0294 0.07 Uiso 1 1 calc R . . H51B H 0.7975 0.3576 0.1201 0.07 Uiso 1 1 calc R . . H51C H 0.8689 0.4156 0.0517 0.07 Uiso 1 1 calc R . . H52A H 0.7582 0.4386 -0.0872 0.066 Uiso 1 1 calc R . . H52B H 0.7783 0.5146 -0.0585 0.066 Uiso 1 1 calc R . . H52C H 0.6517 0.5155 -0.0665 0.066 Uiso 1 1 calc R . . H53A H 0.238 0.3751 0.2153 0.06 Uiso 1 1 calc R D . H53B H 0.2242 0.3148 0.3025 0.06 Uiso 1 1 calc R . . H53C H 0.2535 0.2781 0.2201 0.06 Uiso 1 1 calc R . . H54A H 0.4375 0.1757 0.2494 0.055 Uiso 1 1 calc R . . H54B H 0.3992 0.2017 0.3378 0.055 Uiso 1 1 calc R . . H54C H 0.525 0.205 0.2838 0.055 Uiso 1 1 calc R . . H56A H 1.106 0.0291 0.2522 0.095 Uiso 0.47 1 calc PR D 2 H56B H 0.9968 -0.0058 0.2577 0.095 Uiso 0.47 1 calc PR D 2 H56C H 1.0185 0.0141 0.3379 0.095 Uiso 0.47 1 calc PR D 2 H56D H 1.0703 0.025 0.3461 0.11 Uiso 0.53 1 calc PR E 1 H56E H 0.9793 -0.0076 0.3189 0.11 Uiso 0.53 1 calc PR E 1 H56F H 0.954 0.0116 0.4094 0.11 Uiso 0.53 1 calc PR E 1 H57A H 0.978 0.1719 0.3475 0.118 Uiso 0.47 1 calc PR D 2 H57B H 0.9575 0.2368 0.2651 0.118 Uiso 0.47 1 calc PR D 2 H57C H 1.0797 0.1711 0.2679 0.118 Uiso 0.47 1 calc PR D 2 H57D H 0.8953 0.1692 0.4232 0.131 Uiso 0.53 1 calc PR E 1 H57E H 0.9085 0.2344 0.3393 0.131 Uiso 0.53 1 calc PR E 1 H57F H 1.0207 0.1697 0.3671 0.131 Uiso 0.53 1 calc PR E 1 H58A H 1.0409 0.1432 0.1346 0.114 Uiso 0.47 1 calc PR D 2 H58B H 0.911 0.1991 0.1492 0.114 Uiso 0.47 1 calc PR D 2 H58C H 0.9351 0.1033 0.1441 0.114 Uiso 0.47 1 calc PR D 2 H58D H 0.9237 0.1953 0.2077 0.111 Uiso 0.53 1 calc PR E 1 H58E H 0.9786 0.0998 0.2001 0.111 Uiso 0.53 1 calc PR E 1 H58F H 1.0525 0.1514 0.2216 0.111 Uiso 0.53 1 calc PR E 1 H59A H 1.0936 -0.5544 0.4054 0.061 Uiso 1 1 calc R B 6 H59B H 1.1222 -0.512 0.4692 0.061 Uiso 1 1 calc R B 6 H6 H 1.1875 -0.1848 0.206 0.06 Uiso 1 1 calc R . . H60A H 1.2768 -0.5525 0.3426 0.05 Uiso 1 1 calc R . . H60B H 1.2728 -0.4729 0.3786 0.05 Uiso 1 1 calc R . . H61A H 1.2441 -0.4042 0.2527 0.06 Uiso 1 1 calc R . . H61B H 1.1896 -0.4736 0.2392 0.06 Uiso 1 1 calc R . . H62A H 1.0745 -0.3361 0.3138 0.061 Uiso 1 1 calc R A 6 H62B H 1.0192 -0.3895 0.2768 0.061 Uiso 1 1 calc R A 6 H63A H 0.6957 0.7983 0.0391 0.094 Uiso 0.74 1 calc PR C 8 H63B H 0.8179 0.8229 0.0123 0.094 Uiso 0.74 1 calc PR C 8 H64A H 0.9077 0.7034 0.077 0.058 Uiso 0.74 1 calc PR C 8 H64B H 0.78 0.6974 0.1271 0.058 Uiso 0.74 1 calc PR C 8 H65A H 0.7661 0.6133 0.0499 0.06 Uiso 0.74 1 calc PR C 8 H65B H 0.9043 0.5852 0.0448 0.06 Uiso 0.74 1 calc PR C 8 H66A H 0.941 0.6709 -0.0807 0.065 Uiso 0.74 1 calc PR C 8 H66B H 0.8282 0.6483 -0.0908 0.065 Uiso 0.74 1 calc PR C 8 H69A H 0.9568 0.721 -0.0442 0.107 Uiso 0.26 1 calc PR C 9 H69B H 0.9334 0.687 -0.1161 0.107 Uiso 0.26 1 calc PR C 9 H7 H 1.2073 -0.2035 0.3408 0.058 Uiso 1 1 calc R D . H70A H 0.9415 0.5975 0.0313 0.087 Uiso 0.26 1 calc PR C 9 H70B H 0.8758 0.58 -0.0297 0.087 Uiso 0.26 1 calc PR C 9 H71A H 0.7685 0.6334 0.1168 0.083 Uiso 0.26 1 calc PR C 9 H71B H 0.7011 0.625 0.0509 0.083 Uiso 0.26 1 calc PR C 9 H72A H 0.6582 0.7684 0.0317 0.152 Uiso 0.26 1 calc PR C 9 H72B H 0.7745 0.7677 0.0572 0.152 Uiso 0.26 1 calc PR C 9 H8 H 1.0499 -0.202 0.447 0.052 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 0.0281(3) 0.0164(2) 0.0466(3) -0.0072(2) -0.0201(2) -0.00012(18) Cu2 0.0370(3) 0.0164(2) 0.0417(3) -0.00790(19) -0.0247(2) 0.00108(18) S1A 0.0322(18) 0.0153(11) 0.041(2) -0.0055(13) -0.0195(15) -0.0009(12) S1B 0.043(2) 0.0305(15) 0.051(2) -0.0084(15) -0.0217(15) -0.0057(14) N1 0.0226(15) 0.0168(15) 0.0307(17) -0.0028(12) -0.0090(13) -0.0004(12) N2 0.0249(16) 0.0204(15) 0.0355(18) -0.0076(13) -0.0112(13) -0.0021(12) N3 0.0239(15) 0.0181(14) 0.0225(15) -0.0050(12) -0.0091(12) -0.0023(12) N4 0.0233(15) 0.0169(14) 0.0227(15) -0.0033(12) -0.0094(12) -0.0023(12) C1 0.0210(18) 0.0227(18) 0.029(2) -0.0048(15) -0.0075(15) -0.0021(15) C2 0.034(2) 0.0185(18) 0.039(2) -0.0067(16) -0.0113(18) -0.0057(16) C3 0.033(2) 0.0228(19) 0.049(2) -0.0122(17) -0.0125(18) -0.0083(16) C4 0.0254(19) 0.0136(17) 0.041(2) -0.0022(15) -0.0117(17) 0.0004(14) C5 0.029(2) 0.024(2) 0.049(3) 0.0087(18) -0.0081(19) -0.0018(16) C6 0.027(2) 0.029(2) 0.080(4) 0.016(2) -0.011(2) -0.0047(18) C7 0.035(2) 0.024(2) 0.094(4) -0.003(2) -0.036(3) -0.0026(18) C8 0.047(3) 0.027(2) 0.064(3) -0.018(2) -0.035(2) 0.0078(19) C9 0.035(2) 0.0189(19) 0.043(2) -0.0099(17) -0.0167(19) 0.0040(16) C10 0.026(2) 0.0179(18) 0.046(2) -0.0084(17) -0.0193(17) -0.0014(15) C11 0.032(2) 0.029(2) 0.040(2) -0.0124(18) -0.0168(18) -0.0051(16) C12 0.042(2) 0.026(2) 0.046(3) -0.0038(18) -0.026(2) -0.0044(17) C13 0.035(2) 0.026(2) 0.062(3) -0.010(2) -0.028(2) 0.0017(17) C14 0.026(2) 0.028(2) 0.059(3) -0.009(2) -0.0165(19) -0.0040(16) C15 0.028(2) 0.0249(19) 0.048(2) -0.0104(18) -0.0193(18) -0.0042(16) C16 0.038(2) 0.059(3) 0.037(3) 0.013(2) -0.001(2) 0.003(2) C17 0.047(3) 0.049(3) 0.034(2) -0.013(2) -0.019(2) 0.013(2) C18 0.038(2) 0.035(2) 0.034(2) -0.0042(18) -0.0151(18) -0.0043(18) C19 0.030(2) 0.026(2) 0.047(3) -0.0059(18) -0.0114(18) -0.0039(16) C20 0.075(4) 0.053(3) 0.064(4) 0.027(3) 0.015(3) 0.024(3) C21 0.064(3) 0.063(3) 0.046(3) 0.008(2) -0.002(2) 0.009(3) C22 0.114(5) 0.054(3) 0.059(3) -0.029(3) -0.011(3) 0.016(3) C23 0.056(3) 0.050(3) 0.049(3) -0.009(2) 0.000(2) 0.003(2) C24 0.059(3) 0.086(4) 0.055(3) -0.030(3) -0.016(3) -0.007(3) C25 0.044(2) 0.040(2) 0.043(3) -0.001(2) -0.011(2) -0.008(2) C26 0.038(2) 0.041(2) 0.046(3) -0.009(2) -0.013(2) -0.0097(19) C27 0.033(2) 0.042(2) 0.057(3) -0.007(2) -0.011(2) -0.0109(19) C28 0.0231(18) 0.0230(18) 0.0198(18) -0.0052(14) -0.0075(14) -0.0061(14) C29 0.0265(19) 0.0151(17) 0.028(2) -0.0052(14) -0.0109(15) -0.0020(14) C30 0.0239(18) 0.0159(17) 0.0267(19) -0.0025(14) -0.0090(15) 0.0013(14) C31 0.030(2) 0.0160(17) 0.027(2) -0.0099(15) -0.0153(16) 0.0034(14) C32 0.037(2) 0.0153(17) 0.027(2) -0.0043(15) -0.0130(17) -0.0009(15) C33 0.054(3) 0.0207(19) 0.027(2) -0.0037(16) -0.0175(19) 0.0013(18) C34 0.049(3) 0.027(2) 0.039(2) -0.0110(18) -0.029(2) 0.0065(18) C35 0.034(2) 0.031(2) 0.050(3) -0.0189(19) -0.0234(19) 0.0040(17) C36 0.0267(19) 0.0222(18) 0.037(2) -0.0135(16) -0.0133(17) 0.0000(15) C37 0.0256(19) 0.0177(17) 0.027(2) -0.0048(14) -0.0148(16) 0.0006(14) C38 0.030(2) 0.0192(18) 0.027(2) -0.0048(15) -0.0141(16) 0.0029(15) C39 0.044(2) 0.030(2) 0.023(2) -0.0043(16) -0.0153(17) -0.0019(18) C40 0.050(2) 0.030(2) 0.029(2) -0.0096(17) -0.0217(19) -0.0051(18) C41 0.041(2) 0.028(2) 0.042(2) -0.0090(18) -0.0230(19) -0.0067(17) C42 0.029(2) 0.0193(18) 0.032(2) -0.0032(15) -0.0150(16) -0.0014(15) C43 0.040(2) 0.0237(19) 0.028(2) -0.0005(16) -0.0095(17) -0.0082(17) C44 0.032(2) 0.040(2) 0.034(2) -0.0096(18) -0.0087(17) -0.0120(18) C45 0.035(2) 0.031(2) 0.028(2) -0.0092(16) -0.0089(17) -0.0053(17) C46 0.031(2) 0.031(2) 0.036(2) -0.0088(17) -0.0129(17) -0.0104(16) C47 0.050(3) 0.030(2) 0.074(3) -0.008(2) -0.002(2) -0.015(2) C48 0.047(3) 0.043(3) 0.045(3) -0.013(2) -0.010(2) -0.005(2) C49 0.042(3) 0.060(3) 0.065(3) -0.018(3) -0.004(2) -0.005(2) C50 0.053(3) 0.041(3) 0.045(3) -0.007(2) -0.002(2) -0.020(2) C51 0.036(2) 0.058(3) 0.048(3) -0.005(2) -0.017(2) -0.011(2) C52 0.051(3) 0.045(3) 0.035(2) -0.001(2) -0.012(2) -0.014(2) C53 0.029(2) 0.042(2) 0.050(3) -0.010(2) -0.0099(19) -0.0076(18) C54 0.041(2) 0.038(2) 0.034(2) -0.0015(18) -0.0137(18) -0.0135(19) C55A 0.029(5) 0.022(4) 0.068(7) -0.001(5) -0.025(5) -0.007(3) C55B 0.034(10) 0.018(7) 0.108(18) 0.005(9) -0.046(13) -0.004(5) C56A 0.044(6) 0.027(5) 0.152(11) 0.008(7) -0.062(7) 0.003(4) C56B 0.045(7) 0.027(5) 0.130(11) -0.014(7) -0.046(8) -0.003(5) C57A 0.086(9) 0.052(6) 0.161(13) -0.034(8) -0.083(9) -0.011(6) C57B 0.044(7) 0.040(6) 0.173(15) -0.043(9) -0.049(8) 0.001(5) C58A 0.031(6) 0.056(12) 0.114(17) -0.018(12) 0.022(8) -0.008(7) C58B 0.056(8) 0.052(7) 0.095(11) -0.007(8) 0.018(8) -0.010(6) C59 0.052(3) 0.056(3) 0.047(3) 0.008(2) -0.023(2) -0.021(2) C60 0.035(2) 0.037(2) 0.055(3) -0.020(2) -0.011(2) -0.0008(18) C61 0.053(3) 0.040(3) 0.046(3) -0.006(2) 0.010(2) -0.013(2) C62 0.045(3) 0.044(3) 0.053(3) 0.014(2) -0.013(2) -0.013(2) C63 0.094(4) 0.073(4) 0.076(4) -0.017(3) -0.034(3) -0.015(4) C64 0.066(4) 0.041(3) 0.040(3) -0.008(3) -0.023(3) -0.006(3) C65 0.063(5) 0.044(4) 0.039(4) -0.019(3) -0.006(4) -0.002(3) C66 0.036(4) 0.085(5) 0.039(4) -0.026(4) -0.019(3) 0.012(4) O63A 0.026(6) 0.041(7) 0.055(6) 0.004(5) 0.009(5) 0.003(4) O63B 0.033(4) 0.040(7) 0.074(8) 0.029(5) -0.017(4) -0.021(4) O67 0.078(2) 0.073(2) 0.094(3) 0.010(2) -0.032(2) -0.019(2) B1 0.037(3) 0.026(2) 0.042(3) 0.002(2) -0.019(2) -0.006(2) F1A 0.058(4) 0.057(4) 0.064(4) -0.011(2) -0.014(2) -0.017(2) F1B 0.0365(17) 0.0430(18) 0.0356(18) -0.0121(15) -0.0082(14) -0.0141(13) F2A 0.073(3) 0.074(3) 0.085(3) -0.012(2) -0.018(2) -0.020(2) F2B 0.0422(17) 0.0644(18) 0.0525(18) -0.0170(15) -0.0091(14) -0.0157(14) F3A 0.073(3) 0.061(3) 0.058(3) -0.0099(19) -0.0113(19) -0.0145(19) F3B 0.074(2) 0.063(2) 0.090(2) -0.0061(17) -0.0188(17) -0.0181(16) F4A 0.063(3) 0.071(3) 0.064(3) -0.0186(19) -0.0127(19) -0.0202(19) F4B 0.080(2) 0.0673(19) 0.0519(18) -0.0151(15) -0.0173(15) -0.0150(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 C1 1.894(3) . ? Cu1 S1A 2.185(4) . ? Cu1 S1B 2.136(6) . ? Cu2 C28 1.891(3) . ? Cu2 S1A 2.164(4) . ? Cu2 S1B 2.178(6) . ? N1 C1 1.356(4) . ? N1 C2 1.385(4) . ? N1 C4 1.443(4) . ? N3 C28 1.361(4) . ? N3 C29 1.379(4) . ? N3 C31 1.443(4) . ? N4 C37 1.447(4) . ? C1 N2 1.358(4) . ? C2 C3 1.338(5) . ? C2 H2 0.95 . ? C3 H3 0.95 . ? C3 N2 1.387(4) . ? C4 C5 1.401(5) . ? C4 C9 1.389(5) . ? C5 C16 1.512(6) . ? C5 C6 1.398(6) . ? C6 H6 0.95 . ? C7 C6 1.386(7) . ? C7 H7 0.95 . ? C8 C7 1.364(6) . ? C8 C9 1.391(5) . ? C8 H8 0.95 . ? C10 C15 1.394(5) . ? C10 N2 1.453(4) . ? C11 C10 1.391(5) . ? C11 C12 1.401(5) . ? C11 C18 1.518(5) . ? C12 C13 1.380(6) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 C13 1.377(6) . ? C14 C15 1.392(5) . ? C14 H14 0.95 . ? C16 H16 1 . ? C17 C22 1.525(6) . ? C17 C23 1.515(6) . ? C17 C9 1.517(6) . ? C17 H17 1 . ? C18 C24 1.528(6) . ? C18 C25 1.531(6) . ? C18 H18 1 . ? C19 C15 1.524(5) . ? C19 C26 1.534(5) . ? C19 C27 1.535(5) . ? C19 H19 1 . ? C20 C16 1.524(7) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C16 1.526(6) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 N4 1.358(4) . ? C29 H29 0.95 . ? C30 C29 1.335(5) . ? C30 H30 0.95 . ? C30 N4 1.386(4) . ? C31 C32 1.389(5) . ? C31 C36 1.410(5) . ? C33 C32 1.404(5) . ? C33 C34 1.371(6) . ? C33 H33 0.95 . ? C34 C35 1.384(6) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 C35 1.392(5) . ? C36 C44 1.520(5) . ? C38 C37 1.391(5) . ? C38 C39 1.394(5) . ? C38 C45 1.522(5) . ? C39 H39 0.95 . ? C40 C39 1.389(5) . ? C40 C41 1.378(5) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? C42 C37 1.405(5) . ? C42 C41 1.396(5) . ? C42 C46 1.520(5) . ? C43 C32 1.517(5) . ? C43 C47 1.525(5) . ? C43 C48 1.520(5) . ? C43 H43 1 . ? C44 C49 1.521(6) . ? C44 H44 1 . ? C45 C51 1.530(5) . ? C45 C52 1.522(5) . ? C45 H45 1 . ? C46 C53 1.530(5) . ? C46 H46 1 . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 C44 1.521(5) . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? C54 C46 1.538(5) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55A C56A 1.508(12) . ? C55A C57A 1.494(13) . ? C55A C58A 1.55(2) . ? C55A S1A 1.845(9) . ? C55B C56B 1.504(17) . ? C55B C57B 1.52(2) . ? C55B C58B 1.61(3) . ? C55B S1B 1.835(18) . ? C56A H56D 0.98 . ? C56A H56E 0.98 . ? C56A H56F 0.98 . ? C56B H56A 0.98 . ? C56B H56B 0.98 . ? C56B H56C 0.98 . ? C57A H57D 0.98 . ? C57A H57E 0.98 . ? C57A H57F 0.98 . ? C57B H57A 0.98 . ? C57B H57B 0.98 . ? C57B H57C 0.98 . ? C58A H58D 0.98 . ? C58A H58E 0.98 . ? C58A H58F 0.98 . ? C58B H58A 0.98 . ? C58B H58B 0.98 . ? C58B H58C 0.98 . ? C59 H59A 0.99 . ? C59 H59B 0.99 . ? C59 O63A 1.369(16) . ? C59 O63B 1.415(17) . ? C60 C59 1.497(6) . ? C60 C61 1.509(6) . ? C60 H60A 0.99 . ? C60 H60B 0.99 . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C62 C61 1.496(6) . ? C62 H62A 0.99 . ? C62 H62B 0.99 . ? C62 O63A 1.361(17) . ? C62 O63B 1.496(15) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? C63 O67 1.372(6) . ? C64 C63 1.488(10) . ? C64 H64A 0.99 . ? C64 H64B 0.99 . ? C65 C64 1.474(8) . ? C65 C66 1.543(10) . ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 H66A 0.99 . ? C66 H66B 0.99 . ? C69 H69A 0.99 . ? C69 H69B 0.99 . ? C70 C69 1.52(2) . ? C70 H70A 0.99 . ? C70 H70B 0.99 . ? C71 C70 1.55(2) . ? C71 C72 1.55(2) . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C72 H72A 0.99 . ? C72 H72B 0.99 . ? O67 C66 1.403(6) . ? O67 C69 1.384(9) . ? O67 C72 1.412(10) . ? B1 F1A 1.345(9) . ? B1 F1B 1.387(6) . ? B1 F2A 1.329(8) . ? B1 F2B 1.413(6) . ? B1 F3A 1.372(8) . ? B1 F3B 1.332(6) . ? B1 F4A 1.464(8) . ? B1 F4B 1.333(6) . ? 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 Cu1 S1B Cu2 119.8(2) . . ? Cu2 S1A Cu1 118.19(18) . . ? S1A Cu2 S1B 12.90(16) . . ? S1B Cu1 S1A 12.90(16) . . ? C1 Cu1 S1B 172.22(17) . . ? C1 Cu1 S1A 166.63(14) . . ? C1 N1 C2 111.3(3) . . ? C1 N1 C4 123.9(3) . . ? C1 N2 C3 111.3(3) . . ? C1 N2 C10 125.9(3) . . ? C28 Cu2 S1A 167.02(14) . . ? C28 Cu2 S1B 174.12(18) . . ? C28 N3 C29 111.8(3) . . ? C28 N3 C31 122.5(3) . . ? C28 N4 C30 111.2(3) . . ? C28 N4 C37 124.7(3) . . ? N1 C2 H2 126.6 . . ? N1 C1 N2 103.9(3) . . ? N1 C1 Cu1 125.5(2) . . ? N2 C1 Cu1 130.4(2) . . ? N2 C3 H3 126.6 . . ? N3 C28 Cu2 125.6(2) . . ? N3 C29 H29 126.7 . . ? N4 C30 H30 126.5 . . ? N4 C28 N3 103.4(3) . . ? N4 C28 Cu2 130.9(2) . . ? C2 N1 C4 124.6(3) . . ? C2 C3 N2 106.7(3) . . ? C2 C3 H3 126.6 . . ? C3 C2 N1 106.8(3) . . ? C3 C2 H2 126.6 . . ? C3 N2 C10 122.8(3) . . ? C4 C5 C16 122.0(3) . . ? C4 C9 C8 117.3(4) . . ? C4 C9 C17 122.2(3) . . ? C5 C4 N1 117.8(3) . . ? C5 C16 C20 110.1(4) . . ? C5 C16 C21 112.1(4) . . ? C5 C16 H16 108.1 . . ? C5 C6 H6 120 . . ? C6 C5 C4 117.3(4) . . ? C6 C5 C16 120.7(4) . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 121.2(4) . . ? C7 C8 H8 119.4 . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120 . . ? C8 C7 C6 121.1(4) . . ? C8 C7 H7 119.4 . . ? C8 C9 C17 120.4(4) . . ? C9 C4 C5 123.0(3) . . ? C9 C4 N1 119.2(3) . . ? C9 C8 H8 119.4 . . ? C9 C17 C22 112.2(4) . . ? C9 C17 H17 107.4 . . ? C10 C11 C12 116.5(4) . . ? C10 C11 C18 124.2(3) . . ? C10 C15 C19 121.8(3) . . ? C11 C12 H12 119.4 . . ? C11 C10 C15 123.9(3) . . ? C11 C10 N2 117.7(3) . . ? C11 C18 C24 112.6(3) . . ? C11 C18 C25 110.2(3) . . ? C11 C18 H18 107.8 . . ? C12 C11 C18 119.3(3) . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 121.4(4) . . ? C13 C14 H14 119.3 . . ? C13 C12 C11 121.2(4) . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C14 C15 C10 116.8(4) . . ? C14 C15 C19 121.4(4) . . ? C15 C14 H14 119.3 . . ? C15 C19 C26 110.8(3) . . ? C15 C19 C27 113.5(3) . . ? C15 C19 H19 107.5 . . ? C15 C10 N2 118.3(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? C20 C16 C21 110.1(4) . . ? C20 C16 H16 108.1 . . ? C21 C16 H16 108.1 . . ? C22 C17 H17 107.4 . . ? C23 C17 C9 110.7(3) . . ? C23 C17 C22 111.6(4) . . ? C23 C17 H17 107.4 . . ? C24 C18 C25 110.3(4) . . ? C24 C18 H18 107.8 . . ? C25 C18 H18 107.8 . . ? C26 C19 C27 109.8(3) . . ? C26 C19 H19 107.5 . . ? C27 C19 H19 107.5 . . ? C29 C30 N4 107.0(3) . . ? C29 C30 H30 126.5 . . ? C29 N3 C31 125.7(3) . . ? C30 N4 C37 124.1(3) . . ? C30 C29 N3 106.6(3) . . ? C30 C29 H29 126.7 . . ? C31 C36 C44 122.3(3) . . ? C31 C32 C33 117.0(3) . . ? C31 C32 C43 122.9(3) . . ? C32 C31 C36 123.8(3) . . ? C32 C31 N3 118.5(3) . . ? C32 C43 C48 111.8(3) . . ? C32 C43 C47 111.3(3) . . ? C32 C43 H43 107.8 . . ? C32 C33 H33 119.8 . . ? C33 C32 C43 120.2(3) . . ? C33 C34 C35 121.5(3) . . ? C33 C34 H34 119.3 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C34 C35 C36 120.8(4) . . ? C34 C35 H35 119.6 . . ? C35 C36 C31 116.4(3) . . ? C35 C36 C44 121.1(3) . . ? C35 C34 H34 119.3 . . ? C36 C31 N3 117.7(3) . . ? C36 C44 C49 112.6(3) . . ? C36 C44 C50 110.2(3) . . ? C36 C44 H44 107.9 . . ? C36 C35 H35 119.6 . . ? C37 C38 C39 117.1(3) . . ? C37 C38 C45 121.7(3) . . ? C37 C42 C46 123.1(3) . . ? C38 C37 C42 123.6(3) . . ? C38 C37 N4 118.3(3) . . ? C38 C45 C51 110.7(3) . . ? C38 C45 H45 107.2 . . ? C38 C39 H39 119.5 . . ? C39 C38 C45 121.2(3) . . ? C39 C40 H40 119.8 . . ? C40 C39 C38 121.0(4) . . ? C40 C39 H39 119.5 . . ? C40 C41 C42 121.3(4) . . ? C40 C41 H41 119.3 . . ? C41 C40 C39 120.3(3) . . ? C41 C40 H40 119.8 . . ? C41 C42 C37 116.6(3) . . ? C41 C42 C46 120.3(3) . . ? C42 C46 C53 112.2(3) . . ? C42 C46 C54 110.3(3) . . ? C42 C46 H46 108.1 . . ? C42 C37 N4 118.0(3) . . ? C42 C41 H41 119.3 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? C45 C52 H52A 109.5 . . ? C45 C52 H52B 109.5 . . ? C45 C52 H52C 109.5 . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? C46 C53 H53A 109.5 . . ? C46 C53 H53B 109.5 . . ? C46 C53 H53C 109.5 . . ? C47 C43 H43 107.8 . . ? C48 C43 C47 110.1(3) . . ? C48 C43 H43 107.8 . . ? C49 C44 C50 110.3(3) . . ? C49 C44 H44 107.9 . . ? C50 C44 H44 107.9 . . ? C51 C45 H45 107.2 . . ? C52 C45 C38 113.9(3) . . ? C52 C45 C51 110.3(3) . . ? C52 C45 H45 107.2 . . ? C53 C46 C54 110.1(3) . . ? C53 C46 H46 108.1 . . ? C54 C46 H46 108.1 . . ? C55A S1A Cu2 104.8(3) . . ? C55A S1A Cu1 108.2(3) . . ? C55B C58B H58A 109.5 . . ? C55B C58B H58B 109.5 . . ? C55B C58B H58C 109.5 . . ? C55B C57B H57A 109.5 . . ? C55B C57B H57B 109.5 . . ? C55B C57B H57C 109.5 . . ? C55B C56B H56A 109.5 . . ? C55B C56B H56B 109.5 . . ? C55B C56B H56C 109.5 . . ? C55B S1B Cu1 107.8(7) . . ? C55B S1B Cu2 109.1(5) . . ? C56A C55A C58A 110.0(11) . . ? C56A C55A S1A 109.1(7) . . ? C56B C55B C57B 112.0(11) . . ? C56B C55B C58B 108.1(15) . . ? C56B C55B S1B 109.7(10) . . ? C57A C55A C56A 113.4(9) . . ? C57A C55A C58A 108.3(10) . . ? C57A C55A S1A 108.3(8) . . ? C57B C55B C58B 109.2(14) . . ? C57B C55B S1B 109.6(15) . . ? C58A C55A S1A 107.5(9) . . ? C58B C55B S1B 108.2(8) . . ? C59 C60 C61 103.2(3) . . ? C59 C60 H60A 111.1 . . ? C59 C60 H60B 111.1 . . ? C59 O63B C62 103.1(9) . . ? C60 C61 H61A 111.2 . . ? C60 C61 H61B 111.2 . . ? C60 C59 H59A 110.7 . . ? C60 C59 H59B 110.7 . . ? C61 C60 H60A 111.1 . . ? C61 C60 H60B 111.1 . . ? C61 C62 O63B 103.8(7) . . ? C61 C62 H62A 110.2 . . ? C61 C62 H62B 110.2 . . ? C62 C61 C60 102.9(3) . . ? C62 C61 H61A 111.2 . . ? C62 C61 H61B 111.2 . . ? C62 O63A C59 113.3(10) . . ? C63 C64 H64A 110.6 . . ? C63 C64 H64B 110.6 . . ? C63 O67 C69 100.5(14) . . ? C63 O67 C66 110.7(5) . . ? C63 O67 C72 34.9(13) . . ? C64 C65 C66 100.0(5) . . ? C64 C65 H65A 111.8 . . ? C64 C65 H65B 111.8 . . ? C64 C63 H63A 110.3 . . ? C64 C63 H63B 110.3 . . ? C65 C64 C63 105.5(5) . . ? C65 C64 H64A 110.6 . . ? C65 C64 H64B 110.6 . . ? C65 C66 H66A 110.8 . . ? C65 C66 H66B 110.8 . . ? C66 C65 H65A 111.8 . . ? C66 C65 H65B 111.8 . . ? C66 O67 C72 93.6(12) . . ? C69 O67 C66 31.9(11) . . ? C69 O67 C72 102.2(19) . . ? C69 C70 C71 107.4(19) . . ? C69 C70 H70A 110.2 . . ? C69 C70 H70B 110.2 . . ? C70 C71 C72 96.2(18) . . ? C70 C71 H71A 112.5 . . ? C70 C71 H71B 112.5 . . ? C70 C69 H69A 110.3 . . ? C70 C69 H69B 110.3 . . ? C71 C70 H70A 110.2 . . ? C71 C70 H70B 110.2 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? C72 C71 H71A 112.5 . . ? C72 C71 H71B 112.5 . . ? O63A C62 C61 107.4(7) . . ? O63A C62 O63B 23.3(8) . . ? O63A C62 H62A 110.2 . . ? O63A C62 H62B 110.2 . . ? O63A C59 O63B 24.4(7) . . ? O63A C59 C60 105.1(7) . . ? O63A C59 H59A 110.7 . . ? O63A C59 H59B 110.7 . . ? O63B C62 H62A 130.9 . . ? O63B C62 H62B 91 . . ? O63B C59 C60 110.9(7) . . ? O63B C59 H59A 86.8 . . ? O63B C59 H59B 125.9 . . ? O67 C63 C64 107.2(6) . . ? O67 C63 H63A 110.3 . . ? O67 C63 H63B 110.3 . . ? O67 C66 C65 105.0(5) . . ? O67 C66 H66A 110.8 . . ? O67 C66 H66B 110.8 . . ? O67 C69 C70 107.0(16) . . ? O67 C69 H69A 110.3 . . ? O67 C69 H69B 110.3 . . ? O67 C72 C71 110.7(17) . . ? O67 C72 H72A 109.5 . . ? O67 C72 H72B 109.5 . . ? F1A B1 F3A 117.8(6) . . ? F1A B1 F4A 105.9(6) . . ? F1B B1 F2B 103.8(4) . . ? F2A B1 F1A 115.8(6) . . ? F2A B1 F3A 113.0(6) . . ? F2A B1 F4A 102.6(6) . . ? F3A B1 F4A 98.4(5) . . ? F3B B1 F4B 110.4(5) . . ? F3B B1 F1B 111.1(4) . . ? F3B B1 F2B 112.7(4) . . ? F4B B1 F1B 112.7(4) . . ? F4B B1 F2B 105.8(4) . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? H56A C56B H56B 109.5 . . ? H56A C56B H56C 109.5 . . ? H56B C56B H56C 109.5 . . ? H57A C57B H57B 109.5 . . ? H57A C57B H57C 109.5 . . ? H57B C57B H57C 109.5 . . ? H58A C58B H58B 109.5 . . ? H58A C58B H58C 109.5 . . ? H58B C58B H58C 109.5 . . ? H59A C59 H59B 108.8 . . ? H60A C60 H60B 109.1 . . ? H61A C61 H61B 109.1 . . ? H62A C62 H62B 108.5 . . ? H63A C63 H63B 108.5 . . ? H64A C64 H64B 108.8 . . ? H65A C65 H65B 109.5 . . ? H66A C66 H66B 108.8 . . ? H69A C69 H69B 108.6 . . ? H70A C70 H70B 108.5 . . ? H71A C71 H71B 110 . . ? H72A C72 H72B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.564 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.070