# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'K. Travis Holman' _publ_contact_author_email kth7@georgetown.edu loop_ _publ_author_name K.T.Holman S.T.Mough data_03107sq _database_code_depnum_ccdc_archive 'CCDC 655268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C78 H72 O18), 3(C3 H7 N O), (C4 H10 O)' _chemical_formula_sum 'C91 H103 N3 O22' _chemical_formula_weight 1590.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.862(4) _cell_length_b 17.512(3) _cell_length_c 24.050(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.469(3) _cell_angle_gamma 90.00 _cell_volume 8334(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4179 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.40 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8737 _exptl_absorpt_correction_T_max 0.9821 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1k CCD (Siemens)' _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 61481 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14666 _reflns_number_gt 7690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED, L.Barbour (1999); http://x-seed.net/' _computing_publication_material ? _refine_special_details ; A disordered molecule of diethyl ether was removed from the refinement model and was modelled with the SQUEEZE subroutine of PLATON. SQUEEZE estimates a residual electron density of 174 electrons/cell within a void volume of 649.5 cubic angstroms. This value compares well with 168 electrons per unit cell calulated for four molecules of ether per unit cell (one per formula unit). The diethyl ether was included in the formula and density calculation. References: P. Vandersluis, A. L. Spek, Acta Crystallogr. Sect. A. 1990, 46, 194-201. Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. The structure shows some residual electron density (0.68 e/A3) within 1.35 A of one of the methoxy substituents (C60). The density is indicative of some disorder of the methoxy group. Attempts to model this electron density as a disorderedmethoxy group do not give rise to a more agreeable model. 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^)+(0.0908P)^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 14666 _refine_ls_number_parameters 1036 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.33878(12) -0.00399(15) 0.53274(15) 0.0885(10) Uani 1 1 d . . . O2 O 0.45826(12) 0.05611(13) 0.55190(13) 0.0675(7) Uani 1 1 d . . . O3 O 0.75077(12) 0.19456(16) 0.59083(13) 0.0746(8) Uani 1 1 d . . . O4 O 0.76262(16) 0.2842(2) 0.65885(18) 0.1208(13) Uani 1 1 d . . . O5 O 0.50763(10) 0.34253(11) 0.68148(9) 0.0419(5) Uani 1 1 d . . . O6 O 0.46689(11) 0.48098(12) 0.64874(10) 0.0530(6) Uani 1 1 d . . . O7 O 0.44986(11) 0.43752(12) 0.51660(10) 0.0491(6) Uani 1 1 d . . . O8 O 0.33611(10) 0.50718(12) 0.47514(9) 0.0479(6) Uani 1 1 d . . . O9 O 0.38706(12) 0.82504(13) 0.61016(12) 0.0664(7) Uani 1 1 d . . . O10 O 0.43349(12) 0.77552(15) 0.54658(11) 0.0682(7) Uani 1 1 d . . . O11 O 0.13872(9) 0.60285(11) 0.59101(9) 0.0411(5) Uani 1 1 d . . . O12 O 0.06264(10) 0.48321(12) 0.57001(9) 0.0496(6) Uani 1 1 d . . . O13 O 0.02418(11) 0.32962(12) 0.34848(11) 0.0561(6) Uani 1 1 d . . . O14 O 0.02228(9) 0.18094(10) 0.37703(8) 0.0334(5) Uani 1 1 d . . . O15 O 0.05415(11) -0.16364(11) 0.46341(9) 0.0449(5) Uani 1 1 d . . . O16 O 0.11760(13) -0.15720(12) 0.55760(10) 0.0646(7) Uani 1 1 d . . . O17 O 0.19185(10) 0.11579(11) 0.63089(9) 0.0473(6) Uani 1 1 d . . . O18 O 0.31541(11) 0.07908(12) 0.68639(10) 0.0530(6) Uani 1 1 d . . . C1 C 0.24397(17) 0.13842(18) 0.34723(17) 0.0566(10) Uani 1 1 d . . . H1A H 0.2226 0.0886 0.3330 0.068 Uiso 1 1 calc R . . H1B H 0.2631 0.1582 0.3173 0.068 Uiso 1 1 calc R . . C2 C 0.30207(16) 0.12452(18) 0.40336(18) 0.0521(9) Uani 1 1 d . . . C3 C 0.29275(19) 0.07024(19) 0.4428(2) 0.0626(11) Uani 1 1 d . . . H3 H 0.2497 0.0468 0.4350 0.075 Uiso 1 1 calc R . . C4 C 0.34438(19) 0.0497(2) 0.4928(2) 0.0663(12) Uani 1 1 d . . . C5 C 0.40857(18) 0.08310(19) 0.50368(19) 0.0563(10) Uani 1 1 d . . . C6 C 0.41718(18) 0.13831(19) 0.46595(18) 0.0553(10) Uani 1 1 d . . . H6 H 0.4599 0.1626 0.4744 0.066 Uiso 1 1 calc R . . C7 C 0.36506(18) 0.16001(18) 0.41544(18) 0.0531(10) Uani 1 1 d . . . C8 C 0.2722(2) -0.0275(3) 0.5304(3) 0.123(2) Uani 1 1 d . . . H8A H 0.2446 0.0176 0.5308 0.184 Uiso 1 1 calc R . . H8B H 0.2749 -0.0596 0.5645 0.184 Uiso 1 1 calc R . . H8C H 0.2516 -0.0567 0.4944 0.184 Uiso 1 1 calc R . . C9 C 0.52738(17) 0.0673(2) 0.55352(19) 0.0651(11) Uani 1 1 d . . . H9A H 0.5285 0.0738 0.5130 0.078 Uiso 1 1 calc R . . H9B H 0.5538 0.0210 0.5700 0.078 Uiso 1 1 calc R . . C10 C 0.56031(16) 0.13565(18) 0.58953(15) 0.0475(8) Uani 1 1 d . . . C11 C 0.53127(17) 0.17549(18) 0.62553(15) 0.0496(9) Uani 1 1 d . . . H11 H 0.4866 0.1629 0.6246 0.060 Uiso 1 1 calc R . . C12 C 0.56530(18) 0.23235(18) 0.66228(14) 0.0468(8) Uani 1 1 d . . . C13 C 0.62969(18) 0.25127(18) 0.66264(15) 0.0531(9) Uani 1 1 d . . . H13 H 0.6538 0.2903 0.6882 0.064 Uiso 1 1 calc R . . C14 C 0.65985(16) 0.21392(18) 0.62607(15) 0.0475(8) Uani 1 1 d . . . C15 C 0.62466(16) 0.15588(19) 0.59004(15) 0.0480(9) Uani 1 1 d . . . H15 H 0.6450 0.1296 0.5654 0.058 Uiso 1 1 calc R . . C16 C 0.7297(2) 0.2360(3) 0.6279(2) 0.0688(11) Uani 1 1 d . . . C17 C 0.81748(19) 0.2113(3) 0.5878(2) 0.1069(17) Uani 1 1 d . . . H17A H 0.8238 0.2668 0.5876 0.160 Uiso 1 1 calc R . . H17B H 0.8222 0.1894 0.5518 0.160 Uiso 1 1 calc R . . H17C H 0.8516 0.1892 0.6218 0.160 Uiso 1 1 calc R . . C18 C 0.5332(2) 0.2690(2) 0.70291(15) 0.0623(11) Uani 1 1 d . . . H18A H 0.4958 0.2364 0.7063 0.075 Uiso 1 1 calc R . . H18B H 0.5669 0.2740 0.7424 0.075 Uiso 1 1 calc R . . C19 C 0.46101(14) 0.37314(16) 0.70503(12) 0.0342(7) Uani 1 1 d . . . C20 C 0.43558(13) 0.33644(16) 0.74428(12) 0.0317(7) Uani 1 1 d . . . H20 H 0.4528 0.2875 0.7584 0.038 Uiso 1 1 calc R . . C21 C 0.38552(13) 0.36863(15) 0.76395(11) 0.0292(7) Uani 1 1 d . . . C22 C 0.36156(14) 0.44198(16) 0.74497(12) 0.0331(7) Uani 1 1 d . . . C23 C 0.38943(14) 0.48011(16) 0.70603(12) 0.0357(7) Uani 1 1 d . . . H23 H 0.3742 0.5302 0.6933 0.043 Uiso 1 1 calc R . . C24 C 0.43764(15) 0.44721(17) 0.68605(13) 0.0375(7) Uani 1 1 d . . . C25 C 0.4344(2) 0.54669(19) 0.61731(16) 0.0604(10) Uani 1 1 d . . . H25A H 0.3863 0.5359 0.5986 0.091 Uiso 1 1 calc R . . H25B H 0.4551 0.5597 0.5872 0.091 Uiso 1 1 calc R . . H25C H 0.4395 0.5897 0.6445 0.091 Uiso 1 1 calc R . . C26 C 0.30626(14) 0.48190(16) 0.76218(12) 0.0345(7) Uani 1 1 d . . . H26A H 0.3192 0.5359 0.7716 0.041 Uiso 1 1 calc R . . H26B H 0.3017 0.4575 0.7979 0.041 Uiso 1 1 calc R . . C27 C 0.37922(17) 0.22308(18) 0.37740(16) 0.0539(10) Uani 1 1 d . . . H27A H 0.3513 0.2148 0.3361 0.065 Uiso 1 1 calc R . . H27B H 0.4273 0.2210 0.3794 0.065 Uiso 1 1 calc R . . C28 C 0.36359(16) 0.30182(17) 0.39738(15) 0.0435(8) Uani 1 1 d . . . C29 C 0.41432(16) 0.33481(17) 0.44474(15) 0.0456(8) Uani 1 1 d . . . H29 H 0.4567 0.3097 0.4597 0.055 Uiso 1 1 calc R . . C30 C 0.40418(16) 0.40263(17) 0.46999(14) 0.0408(8) Uani 1 1 d . . . C31 C 0.34225(16) 0.44021(17) 0.44712(14) 0.0398(8) Uani 1 1 d . . . C32 C 0.29285(16) 0.40973(17) 0.39943(14) 0.0433(8) Uani 1 1 d . . . H32 H 0.2513 0.4362 0.3834 0.052 Uiso 1 1 calc R . . C33 C 0.30307(16) 0.33989(17) 0.37409(14) 0.0413(8) Uani 1 1 d . . . C34 C 0.51327(16) 0.3997(2) 0.54263(15) 0.0542(9) Uani 1 1 d . . . H34A H 0.5051 0.3480 0.5544 0.081 Uiso 1 1 calc R . . H34B H 0.5401 0.4284 0.5771 0.081 Uiso 1 1 calc R . . H34C H 0.5379 0.3969 0.5141 0.081 Uiso 1 1 calc R . . C35 C 0.27486(17) 0.54855(18) 0.45412(14) 0.0485(9) Uani 1 1 d . . . H35A H 0.2358 0.5145 0.4502 0.058 Uiso 1 1 calc R . . H35B H 0.2702 0.5711 0.4153 0.058 Uiso 1 1 calc R . . C36 C 0.27791(15) 0.61046(17) 0.49845(13) 0.0396(8) Uani 1 1 d . . . C37 C 0.23071(15) 0.61162(17) 0.52815(13) 0.0396(8) Uani 1 1 d . . . H37 H 0.1961 0.5741 0.5193 0.048 Uiso 1 1 calc R . . C38 C 0.23292(15) 0.66630(16) 0.57050(13) 0.0360(7) Uani 1 1 d . . . C39 C 0.28435(15) 0.72034(17) 0.58342(14) 0.0410(8) Uani 1 1 d . . . H39 H 0.2868 0.7578 0.6126 0.049 Uiso 1 1 calc R . . C40 C 0.33230(15) 0.72034(17) 0.55427(13) 0.0388(7) Uani 1 1 d . . . C41 C 0.32843(15) 0.66548(17) 0.51154(13) 0.0399(8) Uani 1 1 d . . . H41 H 0.3607 0.6656 0.4911 0.048 Uiso 1 1 calc R . . C42 C 0.38943(17) 0.77572(19) 0.56860(15) 0.0478(8) Uani 1 1 d . . . C43 C 0.44088(19) 0.8809(2) 0.6284(2) 0.0812(13) Uani 1 1 d . . . H43A H 0.4844 0.8559 0.6334 0.122 Uiso 1 1 calc R . . H43B H 0.4412 0.9039 0.6656 0.122 Uiso 1 1 calc R . . H43C H 0.4335 0.9208 0.5984 0.122 Uiso 1 1 calc R . . C44 C 0.17978(15) 0.66970(16) 0.60065(14) 0.0421(8) Uani 1 1 d . . . H44A H 0.2021 0.6763 0.6433 0.051 Uiso 1 1 calc R . . H44B H 0.1506 0.7148 0.5862 0.051 Uiso 1 1 calc R . . C45 C 0.16142(14) 0.54189(16) 0.62855(13) 0.0342(7) Uani 1 1 d . . . C46 C 0.22122(14) 0.54045(16) 0.67505(13) 0.0349(7) Uani 1 1 d . . . H46 H 0.2513 0.5826 0.6806 0.042 Uiso 1 1 calc R . . C47 C 0.23872(14) 0.47897(16) 0.71399(12) 0.0318(7) Uani 1 1 d . . . C48 C 0.19408(14) 0.41766(16) 0.70638(12) 0.0318(7) Uani 1 1 d . . . C49 C 0.13466(14) 0.41821(16) 0.65734(13) 0.0360(7) Uani 1 1 d . . . H49 H 0.1046 0.3760 0.6510 0.043 Uiso 1 1 calc R . . C50 C 0.11925(14) 0.47865(16) 0.61848(13) 0.0354(7) Uani 1 1 d . . . C51 C 0.02729(19) 0.41463(19) 0.55103(16) 0.0707(12) Uani 1 1 d . . . H51A H 0.0579 0.3768 0.5431 0.106 Uiso 1 1 calc R . . H51B H -0.0104 0.4241 0.5152 0.106 Uiso 1 1 calc R . . H51C H 0.0098 0.3952 0.5816 0.106 Uiso 1 1 calc R . . C52 C 0.20420(14) 0.35061(16) 0.74863(12) 0.0346(7) Uani 1 1 d . . . H52A H 0.2314 0.3685 0.7881 0.041 Uiso 1 1 calc R . . H52B H 0.1594 0.3353 0.7509 0.041 Uiso 1 1 calc R . . C53 C 0.24536(16) 0.31073(19) 0.32234(14) 0.0488(9) Uani 1 1 d . . . H53A H 0.2639 0.2744 0.2998 0.059 Uiso 1 1 calc R . . H53B H 0.2260 0.3544 0.2963 0.059 Uiso 1 1 calc R . . C54 C 0.18858(15) 0.27117(17) 0.33870(13) 0.0391(8) Uani 1 1 d . . . C55 C 0.13415(15) 0.31549(17) 0.34071(12) 0.0403(8) Uani 1 1 d . . . H55 H 0.1344 0.3686 0.3327 0.048 Uiso 1 1 calc R . . C56 C 0.07967(14) 0.28515(16) 0.35390(12) 0.0342(7) Uani 1 1 d . . . C57 C 0.07975(14) 0.20712(16) 0.36668(11) 0.0296(7) Uani 1 1 d . . . C58 C 0.13386(14) 0.16294(16) 0.36569(12) 0.0358(7) Uani 1 1 d . . . H58 H 0.1342 0.1103 0.3752 0.043 Uiso 1 1 calc R . . C59 C 0.18869(15) 0.19326(17) 0.35102(13) 0.0395(8) Uani 1 1 d . . . C60 C 0.0110(2) 0.3464(3) 0.3989(2) 0.1001(16) Uani 1 1 d . . . H60A H -0.0151 0.3047 0.4084 0.150 Uiso 1 1 calc R . . H60B H -0.0151 0.3939 0.3938 0.150 Uiso 1 1 calc R . . H60C H 0.0536 0.3527 0.4308 0.150 Uiso 1 1 calc R . . C61 C 0.01427(14) 0.10036(15) 0.38069(12) 0.0324(7) Uani 1 1 d . . . H61A H 0.0309 0.0750 0.3511 0.039 Uiso 1 1 calc R . . H61B H -0.0344 0.0885 0.3711 0.039 Uiso 1 1 calc R . . C62 C 0.05158(13) 0.06829(15) 0.44042(11) 0.0275(6) Uani 1 1 d . . . C63 C 0.07650(13) 0.11557(16) 0.48911(12) 0.0310(7) Uani 1 1 d . . . H63 H 0.0744 0.1694 0.4842 0.037 Uiso 1 1 calc R . . C64 C 0.10439(14) 0.08461(17) 0.54466(12) 0.0333(7) Uani 1 1 d . . . C65 C 0.10971(14) 0.00568(17) 0.55133(12) 0.0345(7) Uani 1 1 d . . . H65 H 0.1298 -0.0158 0.5891 0.041 Uiso 1 1 calc R . . C66 C 0.08563(13) -0.04189(16) 0.50260(12) 0.0307(7) Uani 1 1 d . . . C67 C 0.05678(13) -0.01042(16) 0.44766(12) 0.0295(7) Uani 1 1 d . . . H67 H 0.0404 -0.0429 0.4145 0.035 Uiso 1 1 calc R . . C68 C 0.08852(15) -0.12555(17) 0.51172(14) 0.0383(7) Uani 1 1 d . . . C69 C 0.0488(2) -0.24578(17) 0.46876(17) 0.0627(10) Uani 1 1 d . . . H69A H 0.0941 -0.2685 0.4805 0.094 Uiso 1 1 calc R . . H69B H 0.0218 -0.2671 0.4309 0.094 Uiso 1 1 calc R . . H69C H 0.0270 -0.2572 0.4984 0.094 Uiso 1 1 calc R . . C70 C 0.12615(15) 0.13737(18) 0.59643(13) 0.0434(8) Uani 1 1 d . . . H70A H 0.1261 0.1909 0.5831 0.052 Uiso 1 1 calc R . . H70B H 0.0947 0.1334 0.6196 0.052 Uiso 1 1 calc R . . C71 C 0.22592(15) 0.16533(16) 0.67459(12) 0.0358(7) Uani 1 1 d . . . C72 C 0.19877(14) 0.23051(16) 0.69097(12) 0.0332(7) Uani 1 1 d . . . H72 H 0.1523 0.2418 0.6726 0.040 Uiso 1 1 calc R . . C73 C 0.23824(13) 0.28002(15) 0.73394(12) 0.0303(7) Uani 1 1 d . . . C74 C 0.30621(13) 0.26295(15) 0.76071(11) 0.0289(6) Uani 1 1 d . . . C75 C 0.33232(14) 0.19474(16) 0.74606(12) 0.0337(7) Uani 1 1 d . . . H75 H 0.3781 0.1818 0.7659 0.040 Uiso 1 1 calc R . . C76 C 0.29338(15) 0.14600(16) 0.70364(13) 0.0363(7) Uani 1 1 d . . . C77 C 0.38254(18) 0.0567(2) 0.71706(19) 0.0749(12) Uani 1 1 d . . . H77A H 0.4142 0.0920 0.7078 0.112 Uiso 1 1 calc R . . H77B H 0.3903 0.0048 0.7053 0.112 Uiso 1 1 calc R . . H77C H 0.3896 0.0577 0.7593 0.112 Uiso 1 1 calc R . . C78 C 0.35602(14) 0.31782(16) 0.80101(12) 0.0328(7) Uani 1 1 d . . . H78A H 0.3926 0.2889 0.8297 0.039 Uiso 1 1 calc R . . H78B H 0.3328 0.3494 0.8229 0.039 Uiso 1 1 calc R . . O1SA O 0.89401(17) 0.03697(18) 0.66833(14) 0.0949(10) Uani 1 1 d D . . N2SA N 0.85159(16) 0.01993(18) 0.74256(14) 0.0674(9) Uani 1 1 d D . . C1SA C 0.8586(2) -0.0151(3) 0.7983(2) 0.0943(15) Uani 1 1 d D . . H1S1 H 0.8981 -0.0489 0.8090 0.141 Uiso 1 1 calc R . . H1S2 H 0.8179 -0.0448 0.7955 0.141 Uiso 1 1 calc R . . H1S3 H 0.8647 0.0246 0.8282 0.141 Uiso 1 1 calc R . . C2SA C 0.7924(2) 0.0680(3) 0.7163(2) 0.1062(17) Uani 1 1 d D . . H2S1 H 0.7986 0.1174 0.7364 0.159 Uiso 1 1 calc R . . H2S2 H 0.7520 0.0428 0.7201 0.159 Uiso 1 1 calc R . . H2S3 H 0.7868 0.0760 0.6747 0.159 Uiso 1 1 calc R . . C3SA C 0.8958(2) 0.0087(2) 0.71505(18) 0.0649(11) Uani 1 1 d D . . H3SA H 0.9325 -0.0245 0.7331 0.078 Uiso 1 1 calc R . . O1SB O 1.0204(2) 0.2895(3) 0.6706(2) 0.166(2) Uani 1 1 d . . . N1SB N 0.9916(2) 0.2179(2) 0.73628(18) 0.0920(12) Uani 1 1 d . . . C1SB C 0.9483(4) 0.2043(4) 0.7714(3) 0.174(3) Uani 1 1 d . . . H1S4 H 0.9179 0.2479 0.7680 0.262 Uiso 1 1 calc R . . H1S5 H 0.9758 0.1977 0.8124 0.262 Uiso 1 1 calc R . . H1S6 H 0.9216 0.1580 0.7575 0.262 Uiso 1 1 calc R . . C2SB C 1.0420(4) 0.1633(4) 0.7348(4) 0.231(5) Uani 1 1 d . . . H2S4 H 1.0586 0.1749 0.7020 0.346 Uiso 1 1 calc R . . H2S5 H 1.0222 0.1120 0.7298 0.346 Uiso 1 1 calc R . . H2S6 H 1.0795 0.1657 0.7716 0.346 Uiso 1 1 calc R . . C3SB C 0.9824(3) 0.2786(3) 0.7038(3) 0.123(2) Uani 1 1 d . . . H3SB H 0.9485 0.3146 0.7042 0.148 Uiso 1 1 calc R . . O1SC O 0.1509(5) 0.3031(6) 0.5107(4) 0.0683(19) Uiso 0.28 1 d PD A 2 N1SC N 0.2664(6) 0.2943(11) 0.5529(9) 0.044(2) Uiso 0.28 1 d PD A 2 C1SC C 0.3285(8) 0.2577(10) 0.5555(9) 0.091(4) Uiso 0.28 1 d PD A 2 H2S7 H 0.3663 0.2852 0.5830 0.136 Uiso 0.28 1 calc PR A 2 H2S8 H 0.3339 0.2578 0.5165 0.136 Uiso 0.28 1 calc PR A 2 H2S9 H 0.3280 0.2049 0.5689 0.136 Uiso 0.28 1 calc PR A 2 C2SC C 0.2766(8) 0.3711(7) 0.5826(6) 0.058(3) Uiso 0.28 1 d PD A 2 H1S7 H 0.3248 0.3791 0.6029 0.087 Uiso 0.28 1 calc PR A 2 H1S8 H 0.2518 0.3728 0.6110 0.087 Uiso 0.28 1 calc PR A 2 H1S9 H 0.2597 0.4112 0.5532 0.087 Uiso 0.28 1 calc PR A 2 C3SC C 0.2053(6) 0.2694(8) 0.5202(6) 0.062(4) Uiso 0.28 1 d PD A 2 H3SC H 0.2036 0.2207 0.5025 0.074 Uiso 0.28 1 calc PR A 2 O1SE O 0.1419(5) 0.2959(6) 0.5299(4) 0.0683(19) Uiso 0.28 1 d PD B 3 N1SE N 0.2552(6) 0.2957(12) 0.5531(8) 0.044(2) Uiso 0.28 1 d PD B 3 C1SE C 0.3151(9) 0.3086(13) 0.6004(9) 0.118(6) Uiso 0.28 1 d PD B 3 H1SX H 0.3530 0.2825 0.5926 0.177 Uiso 0.28 1 calc PR B 3 H1SY H 0.3095 0.2888 0.6366 0.177 Uiso 0.28 1 calc PR B 3 H1SZ H 0.3244 0.3636 0.6044 0.177 Uiso 0.28 1 calc PR B 3 C2SE C 0.2593(10) 0.2363(9) 0.5136(8) 0.094(4) Uiso 0.28 1 d PD B 3 H2SX H 0.3068 0.2235 0.5199 0.141 Uiso 0.28 1 calc PR B 3 H2SY H 0.2384 0.2536 0.4731 0.141 Uiso 0.28 1 calc PR B 3 H2SZ H 0.2354 0.1909 0.5206 0.141 Uiso 0.28 1 calc PR B 3 C3SE C 0.1972(7) 0.3244(9) 0.5565(7) 0.092(5) Uiso 0.28 1 d PD B 3 H3SE H 0.1987 0.3682 0.5802 0.110 Uiso 0.28 1 calc PR B 3 O1SD O 0.1786(9) 0.4196(9) 0.4942(8) 0.101(3) Uiso 0.22 1 d PD C 4 N1SD N 0.2531(8) 0.3271(10) 0.5441(7) 0.045(3) Uiso 0.22 1 d PD C 4 C1SD C 0.3181(11) 0.3350(17) 0.5867(11) 0.118(6) Uiso 0.22 1 d PD C 4 H1SA H 0.3386 0.2844 0.5969 0.177 Uiso 0.22 1 calc PR C 4 H1SB H 0.3136 0.3596 0.6218 0.177 Uiso 0.22 1 calc PR C 4 H1SC H 0.3469 0.3664 0.5706 0.177 Uiso 0.22 1 calc PR C 4 C2SD C 0.2438(12) 0.2707(12) 0.4977(9) 0.094(4) Uiso 0.22 1 d PD C 4 H2SA H 0.2845 0.2685 0.4858 0.141 Uiso 0.22 1 calc PR C 4 H2SB H 0.2050 0.2852 0.4640 0.141 Uiso 0.22 1 calc PR C 4 H2SC H 0.2355 0.2205 0.5121 0.141 Uiso 0.22 1 calc PR C 4 C3SD C 0.2192(11) 0.3929(12) 0.5398(9) 0.117(8) Uiso 0.22 1 d PD C 4 H3SD H 0.2268 0.4219 0.5748 0.141 Uiso 0.22 1 calc PR C 4 O1SF O 0.1791(9) 0.3914(10) 0.4887(8) 0.101(3) Uiso 0.22 1 d PD D 5 N1SF N 0.2657(9) 0.3156(12) 0.5414(7) 0.045(3) Uiso 0.22 1 d PD D 5 C1SF C 0.3051(12) 0.2479(13) 0.5445(12) 0.091(4) Uiso 0.22 1 d PD D 5 H2SD H 0.2763 0.2073 0.5214 0.136 Uiso 0.22 1 calc PR D 5 H2SE H 0.3237 0.2315 0.5854 0.136 Uiso 0.22 1 calc PR D 5 H2SF H 0.3421 0.2584 0.5287 0.136 Uiso 0.22 1 calc PR D 5 C2SF C 0.2737(10) 0.3516(10) 0.5992(7) 0.058(3) Uiso 0.22 1 d PD D 5 H1SD H 0.3055 0.3944 0.6054 0.087 Uiso 0.22 1 calc PR D 5 H1SE H 0.2911 0.3138 0.6304 0.087 Uiso 0.22 1 calc PR D 5 H1SF H 0.2298 0.3704 0.6001 0.087 Uiso 0.22 1 calc PR D 5 C3SF C 0.2089(9) 0.3298(12) 0.4961(8) 0.088(6) Uiso 0.22 1 d PD D 5 H3SF H 0.1912 0.2901 0.4686 0.106 Uiso 0.22 1 calc PR D 5 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 O1 0.0439(16) 0.0607(17) 0.170(3) 0.0409(19) 0.0463(17) 0.0052(13) O2 0.0431(15) 0.0513(15) 0.115(2) -0.0035(15) 0.0341(15) -0.0014(12) O3 0.0463(16) 0.082(2) 0.107(2) 0.0186(17) 0.0407(16) 0.0029(14) O4 0.069(2) 0.103(3) 0.187(4) -0.041(3) 0.036(2) -0.039(2) O5 0.0470(13) 0.0384(12) 0.0430(13) 0.0083(10) 0.0179(10) 0.0131(10) O6 0.0589(15) 0.0507(14) 0.0584(15) 0.0263(12) 0.0313(12) 0.0134(11) O7 0.0425(13) 0.0431(13) 0.0591(15) -0.0089(12) 0.0124(11) 0.0021(11) O8 0.0422(13) 0.0389(13) 0.0598(15) -0.0138(11) 0.0121(11) 0.0050(10) O9 0.0567(16) 0.0520(15) 0.097(2) -0.0330(15) 0.0340(14) -0.0146(12) O10 0.0533(16) 0.0746(18) 0.0870(19) -0.0185(15) 0.0369(15) -0.0184(13) O11 0.0344(12) 0.0364(12) 0.0517(13) 0.0099(10) 0.0123(10) 0.0070(10) O12 0.0420(13) 0.0397(13) 0.0521(14) 0.0011(11) -0.0065(11) -0.0012(10) O13 0.0392(13) 0.0433(14) 0.0792(18) -0.0005(13) 0.0092(12) 0.0105(11) O14 0.0309(11) 0.0315(11) 0.0369(12) 0.0059(9) 0.0095(9) 0.0027(9) O15 0.0576(14) 0.0275(12) 0.0491(14) 0.0011(10) 0.0160(11) -0.0022(10) O16 0.108(2) 0.0400(14) 0.0392(14) 0.0111(12) 0.0143(14) 0.0158(13) O17 0.0486(14) 0.0308(12) 0.0445(13) -0.0051(10) -0.0108(11) -0.0032(10) O18 0.0463(14) 0.0389(13) 0.0621(15) -0.0095(11) 0.0007(11) 0.0046(11) C1 0.058(2) 0.038(2) 0.091(3) -0.0258(19) 0.049(2) -0.0154(17) C2 0.038(2) 0.0300(18) 0.097(3) -0.0180(19) 0.034(2) -0.0024(15) C3 0.044(2) 0.031(2) 0.126(4) -0.004(2) 0.046(2) -0.0037(17) C4 0.045(2) 0.039(2) 0.129(4) 0.006(2) 0.047(3) 0.0064(18) C5 0.045(2) 0.0323(19) 0.103(3) -0.013(2) 0.041(2) -0.0029(17) C6 0.043(2) 0.035(2) 0.100(3) -0.019(2) 0.040(2) -0.0080(16) C7 0.052(2) 0.0282(18) 0.097(3) -0.0203(19) 0.048(2) -0.0063(16) C8 0.055(3) 0.110(4) 0.217(6) 0.077(4) 0.064(3) 0.001(3) C9 0.041(2) 0.047(2) 0.114(3) -0.016(2) 0.034(2) -0.0034(17) C10 0.042(2) 0.0392(19) 0.069(2) -0.0012(17) 0.0286(18) 0.0058(15) C11 0.044(2) 0.044(2) 0.069(2) 0.0066(19) 0.0299(18) 0.0052(16) C12 0.057(2) 0.0382(19) 0.050(2) 0.0085(17) 0.0233(18) 0.0131(17) C13 0.063(2) 0.040(2) 0.050(2) 0.0031(17) 0.0078(19) 0.0080(17) C14 0.044(2) 0.0389(19) 0.060(2) 0.0108(18) 0.0172(17) 0.0021(16) C15 0.042(2) 0.046(2) 0.065(2) 0.0005(18) 0.0288(17) 0.0053(16) C16 0.051(3) 0.065(3) 0.091(3) 0.015(2) 0.024(2) -0.005(2) C17 0.052(3) 0.118(4) 0.167(5) 0.039(4) 0.058(3) 0.000(3) C18 0.088(3) 0.053(2) 0.053(2) 0.0157(19) 0.032(2) 0.035(2) C19 0.0306(16) 0.0368(18) 0.0323(17) 0.0000(14) 0.0059(14) 0.0017(14) C20 0.0280(16) 0.0307(16) 0.0296(16) -0.0014(13) -0.0003(13) -0.0024(13) C21 0.0267(15) 0.0322(16) 0.0235(15) -0.0028(13) 0.0006(12) -0.0073(13) C22 0.0289(16) 0.0375(18) 0.0274(16) -0.0046(14) 0.0011(13) -0.0019(13) C23 0.0358(17) 0.0288(16) 0.0389(18) 0.0054(14) 0.0068(14) 0.0016(13) C24 0.0424(19) 0.0361(18) 0.0339(17) 0.0067(14) 0.0119(15) -0.0004(15) C25 0.089(3) 0.043(2) 0.058(2) 0.0203(18) 0.037(2) 0.0165(19) C26 0.0392(18) 0.0282(16) 0.0332(17) -0.0029(13) 0.0075(14) -0.0033(13) C27 0.048(2) 0.049(2) 0.080(3) -0.0240(19) 0.0426(19) -0.0129(17) C28 0.050(2) 0.0350(18) 0.060(2) -0.0138(16) 0.0374(18) -0.0181(16) C29 0.047(2) 0.0349(18) 0.067(2) -0.0031(17) 0.0350(18) -0.0029(15) C30 0.043(2) 0.0335(18) 0.051(2) -0.0040(16) 0.0226(17) -0.0058(15) C31 0.045(2) 0.0310(17) 0.049(2) -0.0075(15) 0.0233(16) -0.0043(15) C32 0.044(2) 0.0412(19) 0.051(2) -0.0024(16) 0.0254(17) -0.0086(15) C33 0.049(2) 0.0384(19) 0.047(2) -0.0101(16) 0.0289(17) -0.0160(16) C34 0.047(2) 0.057(2) 0.058(2) 0.0005(18) 0.0152(17) 0.0108(17) C35 0.052(2) 0.044(2) 0.050(2) -0.0042(17) 0.0177(17) 0.0078(17) C36 0.0441(19) 0.0380(18) 0.0355(18) -0.0009(15) 0.0106(15) 0.0065(15) C37 0.0408(19) 0.0308(17) 0.0463(19) 0.0020(15) 0.0123(16) 0.0031(14) C38 0.0392(18) 0.0310(17) 0.0392(18) 0.0060(15) 0.0146(14) 0.0091(14) C39 0.0432(19) 0.0333(18) 0.0434(19) -0.0038(15) 0.0092(15) 0.0043(15) C40 0.0380(18) 0.0346(18) 0.0468(19) 0.0017(15) 0.0178(15) 0.0042(14) C41 0.0380(18) 0.0414(19) 0.0421(19) 0.0049(16) 0.0154(15) 0.0074(15) C42 0.041(2) 0.045(2) 0.058(2) -0.0042(18) 0.0167(18) 0.0016(16) C43 0.055(2) 0.058(3) 0.133(4) -0.037(3) 0.033(2) -0.014(2) C44 0.0425(19) 0.0292(17) 0.056(2) 0.0053(15) 0.0182(16) 0.0041(14) C45 0.0363(18) 0.0267(16) 0.0415(18) 0.0021(14) 0.0151(15) 0.0044(14) C46 0.0315(17) 0.0303(17) 0.0443(19) -0.0034(14) 0.0142(15) 0.0024(13) C47 0.0332(17) 0.0293(16) 0.0318(17) -0.0038(14) 0.0088(13) 0.0030(13) C48 0.0341(17) 0.0303(16) 0.0321(17) -0.0007(13) 0.0118(14) 0.0038(13) C49 0.0309(17) 0.0325(17) 0.0415(18) -0.0018(15) 0.0070(14) 0.0015(13) C50 0.0324(17) 0.0351(18) 0.0349(18) -0.0007(15) 0.0052(14) 0.0059(14) C51 0.074(3) 0.044(2) 0.066(3) 0.008(2) -0.018(2) -0.013(2) C52 0.0307(16) 0.0379(18) 0.0336(17) 0.0003(14) 0.0081(13) -0.0001(13) C53 0.058(2) 0.050(2) 0.046(2) -0.0084(17) 0.0270(17) -0.0157(17) C54 0.0454(19) 0.0383(19) 0.0353(18) -0.0079(15) 0.0153(15) -0.0108(15) C55 0.047(2) 0.0323(17) 0.0378(18) -0.0007(14) 0.0076(15) -0.0045(15) C56 0.0345(17) 0.0289(17) 0.0343(17) -0.0011(14) 0.0040(14) 0.0016(14) C57 0.0313(16) 0.0323(17) 0.0234(15) 0.0000(13) 0.0063(13) -0.0011(13) C58 0.0401(18) 0.0275(16) 0.0416(18) -0.0027(14) 0.0156(15) -0.0013(14) C59 0.0406(19) 0.0370(18) 0.0469(19) -0.0136(15) 0.0222(15) -0.0071(14) C60 0.086(3) 0.109(4) 0.110(4) -0.025(3) 0.038(3) 0.024(3) C61 0.0305(16) 0.0327(17) 0.0309(17) 0.0005(13) 0.0054(13) -0.0018(13) C62 0.0230(15) 0.0331(17) 0.0272(16) 0.0024(13) 0.0090(12) -0.0014(12) C63 0.0301(16) 0.0299(16) 0.0297(16) 0.0000(13) 0.0047(13) 0.0004(13) C64 0.0323(17) 0.0381(18) 0.0263(16) -0.0051(14) 0.0048(13) 0.0007(13) C65 0.0339(17) 0.0415(19) 0.0252(16) 0.0026(14) 0.0053(13) 0.0053(14) C66 0.0310(16) 0.0316(16) 0.0303(17) 0.0044(14) 0.0108(13) 0.0046(13) C67 0.0263(15) 0.0361(17) 0.0260(16) -0.0031(13) 0.0084(12) -0.0001(13) C68 0.0461(19) 0.0386(19) 0.0332(19) 0.0012(16) 0.0168(16) 0.0061(15) C69 0.088(3) 0.0299(19) 0.074(3) -0.0011(18) 0.032(2) -0.0082(18) C70 0.0405(19) 0.046(2) 0.0354(18) -0.0070(15) 0.0009(15) 0.0008(15) C71 0.0393(18) 0.0277(16) 0.0320(17) 0.0015(14) -0.0007(14) -0.0063(14) C72 0.0290(16) 0.0309(17) 0.0337(17) 0.0062(14) 0.0017(13) -0.0036(13) C73 0.0300(16) 0.0310(16) 0.0283(16) 0.0026(13) 0.0069(13) -0.0049(13) C74 0.0297(16) 0.0285(16) 0.0269(16) 0.0036(13) 0.0067(13) -0.0040(12) C75 0.0298(16) 0.0323(17) 0.0342(17) 0.0037(14) 0.0032(13) -0.0048(13) C76 0.0413(18) 0.0252(16) 0.0387(18) 0.0012(14) 0.0076(15) 0.0012(14) C77 0.050(2) 0.056(2) 0.108(3) -0.015(2) 0.010(2) 0.0154(19) C78 0.0304(16) 0.0362(17) 0.0261(16) 0.0003(13) 0.0010(13) -0.0045(13) O1SA 0.133(3) 0.091(2) 0.084(2) 0.0114(18) 0.066(2) 0.0385(19) N2SA 0.081(2) 0.065(2) 0.067(2) -0.0070(18) 0.0404(19) 0.0210(18) C1SA 0.104(4) 0.111(4) 0.083(3) 0.006(3) 0.052(3) 0.024(3) C2SA 0.123(4) 0.093(4) 0.122(4) 0.012(3) 0.065(3) 0.052(3) C3SA 0.075(3) 0.065(3) 0.058(3) -0.016(2) 0.026(2) 0.014(2) O1SB 0.155(4) 0.187(5) 0.137(4) 0.053(3) 0.021(3) -0.060(3) N1SB 0.118(3) 0.059(2) 0.111(3) 0.012(2) 0.052(3) 0.004(2) C1SB 0.251(8) 0.148(6) 0.203(7) -0.027(5) 0.183(7) -0.010(6) C2SB 0.298(10) 0.145(6) 0.360(12) 0.097(7) 0.261(10) 0.108(7) C3SB 0.115(5) 0.092(4) 0.156(6) 0.013(4) 0.032(4) -0.027(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C4 1.375(4) . ? O1 C8 1.433(4) . ? O2 C5 1.372(4) . ? O2 C9 1.444(4) . ? O3 C16 1.330(5) . ? O3 C17 1.447(4) . ? O4 C16 1.188(5) . ? O5 C19 1.380(3) . ? O5 C18 1.427(4) . ? O6 C24 1.369(3) . ? O6 C25 1.425(4) . ? O7 C30 1.364(4) . ? O7 C34 1.434(4) . ? O8 C31 1.379(3) . ? O8 C35 1.416(4) . ? O9 C42 1.334(4) . ? O9 C43 1.448(4) . ? O10 C42 1.197(4) . ? O11 C45 1.381(3) . ? O11 C44 1.426(3) . ? O12 C50 1.374(3) . ? O12 C51 1.408(4) . ? O13 C60 1.358(5) . ? O13 C56 1.367(3) . ? O14 C57 1.378(3) . ? O14 C61 1.427(3) . ? O15 C68 1.335(3) . ? O15 C69 1.452(3) . ? O16 C68 1.212(3) . ? O17 C71 1.374(3) . ? O17 C70 1.410(3) . ? O18 C76 1.370(3) . ? O18 C77 1.416(4) . ? C1 C2 1.521(5) . ? C1 C59 1.525(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.399(4) . ? C2 C3 1.399(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.408(5) . ? C5 C6 1.376(5) . ? C6 C7 1.402(5) . ? C6 H6 0.9500 . ? C7 C27 1.522(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.509(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.385(4) . ? C10 C11 1.391(4) . ? C11 C12 1.371(5) . ? C11 H11 0.9500 . ? C12 C13 1.381(5) . ? C12 C18 1.493(4) . ? C13 C14 1.396(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 C16 1.494(5) . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.380(4) . ? C19 C24 1.410(4) . ? C20 C21 1.395(4) . ? C20 H20 0.9500 . ? C21 C22 1.401(4) . ? C21 C78 1.521(4) . ? C22 C23 1.416(4) . ? C22 C26 1.514(4) . ? C23 C24 1.371(4) . ? C23 H23 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C47 1.515(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.529(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C33 1.380(4) . ? C28 C29 1.410(4) . ? C29 C30 1.380(4) . ? C29 H29 0.9500 . ? C30 C31 1.398(4) . ? C31 C32 1.383(4) . ? C32 C33 1.412(4) . ? C32 H32 0.9500 . ? C33 C53 1.520(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.508(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.388(4) . ? C36 C41 1.389(4) . ? C37 C38 1.388(4) . ? C37 H37 0.9500 . ? C38 C39 1.390(4) . ? C38 C44 1.506(4) . ? C39 C40 1.392(4) . ? C39 H39 0.9500 . ? C40 C41 1.390(4) . ? C40 C42 1.490(4) . ? C41 H41 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.387(4) . ? C45 C50 1.387(4) . ? C46 C47 1.397(4) . ? C46 H46 0.9500 . ? C47 C48 1.395(4) . ? C48 C49 1.415(4) . ? C48 C52 1.523(4) . ? C49 C50 1.381(4) . ? C49 H49 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C73 1.522(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.527(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.389(4) . ? C54 C59 1.396(4) . ? C55 C56 1.379(4) . ? C55 H55 0.9500 . ? C56 C57 1.401(4) . ? C57 C58 1.375(4) . ? C58 C59 1.404(4) . ? C58 H58 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.509(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C67 1.389(4) . ? C62 C63 1.393(4) . ? C63 C64 1.387(4) . ? C63 H63 0.9500 . ? C64 C65 1.392(4) . ? C64 C70 1.501(4) . ? C65 C66 1.395(4) . ? C65 H65 0.9500 . ? C66 C67 1.381(4) . ? C66 C68 1.480(4) . ? C67 H67 0.9500 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.386(4) . ? C71 C76 1.400(4) . ? C72 C73 1.400(4) . ? C72 H72 0.9500 . ? C73 C74 1.392(4) . ? C74 C75 1.403(4) . ? C74 C78 1.518(4) . ? C75 C76 1.380(4) . ? C75 H75 0.9500 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? O1SA C3SA 1.218(4) . ? N2SA C3SA 1.309(4) . ? N2SA C1SA 1.438(5) . ? N2SA C2SA 1.463(5) . ? C1SA H1S1 0.9800 . ? C1SA H1S2 0.9800 . ? C1SA H1S3 0.9800 . ? C2SA H2S1 0.9800 . ? C2SA H2S2 0.9800 . ? C2SA H2S3 0.9800 . ? C3SA H3SA 0.9500 . ? O1SB C3SB 1.306(7) . ? N1SB C3SB 1.296(6) . ? N1SB C2SB 1.429(6) . ? N1SB C1SB 1.439(6) . ? C1SB H1S4 0.9800 . ? C1SB H1S5 0.9800 . ? C1SB H1S6 0.9800 . ? C2SB H2S4 0.9800 . ? C2SB H2S5 0.9800 . ? C2SB H2S6 0.9800 . ? C3SB H3SB 0.9500 . ? O1SC C3SC 1.233(11) . ? N1SC C3SC 1.341(13) . ? N1SC C1SC 1.430(13) . ? N1SC C2SC 1.506(15) . ? C1SC H2S7 0.9800 . ? C1SC H2S8 0.9800 . ? C1SC H2S9 0.9800 . ? C2SC H1S7 0.9800 . ? C2SC H1S8 0.9800 . ? C2SC H1S9 0.9800 . ? C3SC H3SC 0.9500 . ? O1SE C3SE 1.235(12) . ? N1SE C3SE 1.335(13) . ? N1SE C1SE 1.417(13) . ? N1SE C2SE 1.431(15) . ? C1SE H1SX 0.9800 . ? C1SE H1SY 0.9800 . ? C1SE H1SZ 0.9800 . ? C2SE H2SX 0.9800 . ? C2SE H2SY 0.9800 . ? C2SE H2SZ 0.9800 . ? C3SE H3SE 0.9500 . ? O1SD C3SD 1.245(15) . ? N1SD C3SD 1.339(14) . ? N1SD C1SD 1.424(14) . ? N1SD C2SD 1.456(15) . ? C1SD H1SA 0.9800 . ? C1SD H1SB 0.9800 . ? C1SD H1SC 0.9800 . ? C2SD H2SA 0.9800 . ? C2SD H2SB 0.9800 . ? C2SD H2SC 0.9800 . ? C3SD H3SD 0.9500 . ? O1SF C3SF 1.230(14) . ? N1SF C3SF 1.354(14) . ? N1SF C1SF 1.432(14) . ? N1SF C2SF 1.489(15) . ? C1SF H2SD 0.9800 . ? C1SF H2SE 0.9800 . ? C1SF H2SF 0.9800 . ? C2SF H1SD 0.9800 . ? C2SF H1SE 0.9800 . ? C2SF H1SF 0.9800 . ? C3SF H3SF 0.9500 . ? 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 C4 O1 C8 117.7(3) . . ? C5 O2 C9 117.2(3) . . ? C16 O3 C17 116.9(4) . . ? C19 O5 C18 115.7(2) . . ? C24 O6 C25 117.4(2) . . ? C30 O7 C34 117.4(2) . . ? C31 O8 C35 118.3(2) . . ? C42 O9 C43 117.1(3) . . ? C45 O11 C44 117.7(2) . . ? C50 O12 C51 116.5(2) . . ? C60 O13 C56 116.3(3) . . ? C57 O14 C61 117.8(2) . . ? C68 O15 C69 116.9(3) . . ? C71 O17 C70 116.8(2) . . ? C76 O18 C77 116.8(2) . . ? C2 C1 C59 116.9(3) . . ? C2 C1 H1A 108.1 . . ? C59 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? C59 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C7 C2 C3 119.0(4) . . ? C7 C2 C1 123.1(3) . . ? C3 C2 C1 117.9(3) . . ? C4 C3 C2 121.9(3) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? O1 C4 C3 124.7(3) . . ? O1 C4 C5 116.2(4) . . ? C3 C4 C5 119.1(4) . . ? O2 C5 C6 125.3(3) . . ? O2 C5 C4 115.7(4) . . ? C6 C5 C4 119.0(4) . . ? C5 C6 C7 122.3(3) . . ? C5 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C2 C7 C6 118.6(3) . . ? C2 C7 C27 123.1(4) . . ? C6 C7 C27 118.2(3) . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 113.1(3) . . ? O2 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? O2 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C15 C10 C11 118.6(3) . . ? C15 C10 C9 118.1(3) . . ? C11 C10 C9 123.1(3) . . ? C12 C11 C10 121.8(3) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 118.8(3) . . ? C11 C12 C18 119.1(3) . . ? C13 C12 C18 122.0(3) . . ? C12 C13 C14 121.0(3) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 118.9(3) . . ? C15 C14 C16 121.8(3) . . ? C13 C14 C16 119.3(4) . . ? C10 C15 C14 120.9(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O4 C16 O3 123.9(4) . . ? O4 C16 C14 124.6(4) . . ? O3 C16 C14 111.4(4) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O5 C18 C12 110.2(3) . . ? O5 C18 H18A 109.6 . . ? C12 C18 H18A 109.6 . . ? O5 C18 H18B 109.6 . . ? C12 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C20 C19 O5 125.0(3) . . ? C20 C19 C24 118.8(3) . . ? O5 C19 C24 116.2(3) . . ? C19 C20 C21 122.4(3) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C20 C21 C22 119.2(3) . . ? C20 C21 C78 116.6(2) . . ? C22 C21 C78 124.0(3) . . ? C21 C22 C23 118.0(3) . . ? C21 C22 C26 123.9(3) . . ? C23 C22 C26 118.1(3) . . ? C24 C23 C22 122.3(3) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? O6 C24 C23 125.2(3) . . ? O6 C24 C19 115.4(3) . . ? C23 C24 C19 119.3(3) . . ? O6 C25 H25A 109.5 . . ? O6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 C47 112.3(2) . . ? C22 C26 H26A 109.1 . . ? C47 C26 H26A 109.1 . . ? C22 C26 H26B 109.1 . . ? C47 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C7 C27 C28 111.4(2) . . ? C7 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C7 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C33 C28 C29 119.1(3) . . ? C33 C28 C27 124.5(3) . . ? C29 C28 C27 116.3(3) . . ? C30 C29 C28 121.8(3) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? O7 C30 C29 125.6(3) . . ? O7 C30 C31 115.5(3) . . ? C29 C30 C31 118.9(3) . . ? O8 C31 C32 125.0(3) . . ? O8 C31 C30 115.2(3) . . ? C32 C31 C30 119.8(3) . . ? C31 C32 C33 121.1(3) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C28 C33 C32 119.1(3) . . ? C28 C33 C53 123.8(3) . . ? C32 C33 C53 117.1(3) . . ? O7 C34 H34A 109.5 . . ? O7 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O7 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O8 C35 C36 106.5(2) . . ? O8 C35 H35A 110.4 . . ? C36 C35 H35A 110.4 . . ? O8 C35 H35B 110.4 . . ? C36 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? C37 C36 C41 119.0(3) . . ? C37 C36 C35 119.8(3) . . ? C41 C36 C35 121.2(3) . . ? C36 C37 C38 121.6(3) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C37 C38 C39 118.5(3) . . ? C37 C38 C44 121.5(3) . . ? C39 C38 C44 120.0(3) . . ? C38 C39 C40 121.0(3) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 119.3(3) . . ? C41 C40 C42 118.4(3) . . ? C39 C40 C42 122.2(3) . . ? C36 C41 C40 120.6(3) . . ? C36 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? O10 C42 O9 123.3(3) . . ? O10 C42 C40 124.5(3) . . ? O9 C42 C40 112.2(3) . . ? O9 C43 H43A 109.5 . . ? O9 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O9 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O11 C44 C38 112.7(2) . . ? O11 C44 H44A 109.1 . . ? C38 C44 H44A 109.1 . . ? O11 C44 H44B 109.1 . . ? C38 C44 H44B 109.1 . . ? H44A C44 H44B 107.8 . . ? O11 C45 C46 125.1(3) . . ? O11 C45 C50 115.8(3) . . ? C46 C45 C50 119.0(3) . . ? C45 C46 C47 122.1(3) . . ? C45 C46 H46 118.9 . . ? C47 C46 H46 118.9 . . ? C48 C47 C46 118.9(3) . . ? C48 C47 C26 123.1(3) . . ? C46 C47 C26 117.9(2) . . ? C47 C48 C49 118.5(3) . . ? C47 C48 C52 124.1(2) . . ? C49 C48 C52 117.4(2) . . ? C50 C49 C48 121.6(3) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? O12 C50 C49 124.9(3) . . ? O12 C50 C45 115.4(3) . . ? C49 C50 C45 119.7(3) . . ? O12 C51 H51A 109.5 . . ? O12 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O12 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C73 C52 C48 116.6(2) . . ? C73 C52 H52A 108.1 . . ? C48 C52 H52A 108.1 . . ? C73 C52 H52B 108.1 . . ? C48 C52 H52B 108.1 . . ? H52A C52 H52B 107.3 . . ? C33 C53 C54 114.8(2) . . ? C33 C53 H53A 108.6 . . ? C54 C53 H53A 108.6 . . ? C33 C53 H53B 108.6 . . ? C54 C53 H53B 108.6 . . ? H53A C53 H53B 107.5 . . ? C55 C54 C59 119.0(3) . . ? C55 C54 C53 117.7(3) . . ? C59 C54 C53 123.3(3) . . ? C56 C55 C54 122.4(3) . . ? C56 C55 H55 118.8 . . ? C54 C55 H55 118.8 . . ? O13 C56 C55 119.6(3) . . ? O13 C56 C57 121.3(3) . . ? C55 C56 C57 118.8(3) . . ? C58 C57 O14 125.6(2) . . ? C58 C57 C56 119.3(3) . . ? O14 C57 C56 115.1(2) . . ? C57 C58 C59 122.0(3) . . ? C57 C58 H58 119.0 . . ? C59 C58 H58 119.0 . . ? C54 C59 C58 118.4(3) . . ? C54 C59 C1 123.6(3) . . ? C58 C59 C1 117.9(3) . . ? O13 C60 H60A 109.5 . . ? O13 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O13 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O14 C61 C62 113.1(2) . . ? O14 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? O14 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? C67 C62 C63 119.4(2) . . ? C67 C62 C61 119.0(2) . . ? C63 C62 C61 121.4(2) . . ? C64 C63 C62 120.5(3) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 119.5(3) . . ? C63 C64 C70 118.9(3) . . ? C65 C64 C70 121.6(3) . . ? C64 C65 C66 120.1(3) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C67 C66 C65 119.8(3) . . ? C67 C66 C68 121.5(3) . . ? C65 C66 C68 118.7(3) . . ? C66 C67 C62 120.6(3) . . ? C66 C67 H67 119.7 . . ? C62 C67 H67 119.7 . . ? O16 C68 O15 122.7(3) . . ? O16 C68 C66 125.0(3) . . ? O15 C68 C66 112.4(3) . . ? O15 C69 H69A 109.5 . . ? O15 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? O15 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O17 C70 C64 107.8(2) . . ? O17 C70 H70A 110.2 . . ? C64 C70 H70A 110.2 . . ? O17 C70 H70B 110.2 . . ? C64 C70 H70B 110.2 . . ? H70A C70 H70B 108.5 . . ? O17 C71 C72 125.3(3) . . ? O17 C71 C76 115.1(3) . . ? C72 C71 C76 119.6(3) . . ? C71 C72 C73 121.5(3) . . ? C71 C72 H72 119.3 . . ? C73 C72 H72 119.3 . . ? C74 C73 C72 118.9(3) . . ? C74 C73 C52 123.3(2) . . ? C72 C73 C52 117.8(2) . . ? C73 C74 C75 119.1(2) . . ? C73 C74 C78 123.4(3) . . ? C75 C74 C78 117.2(2) . . ? C76 C75 C74 121.9(3) . . ? C76 C75 H75 119.1 . . ? C74 C75 H75 119.1 . . ? O18 C76 C75 125.3(3) . . ? O18 C76 C71 115.9(3) . . ? C75 C76 C71 118.9(3) . . ? O18 C77 H77A 109.5 . . ? O18 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? O18 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C74 C78 C21 108.6(2) . . ? C74 C78 H78A 110.0 . . ? C21 C78 H78A 110.0 . . ? C74 C78 H78B 110.0 . . ? C21 C78 H78B 110.0 . . ? H78A C78 H78B 108.4 . . ? C3SA N2SA C1SA 121.8(3) . . ? C3SA N2SA C2SA 120.1(4) . . ? C1SA N2SA C2SA 118.1(3) . . ? N2SA C1SA H1S1 109.5 . . ? N2SA C1SA H1S2 109.5 . . ? H1S1 C1SA H1S2 109.5 . . ? N2SA C1SA H1S3 109.5 . . ? H1S1 C1SA H1S3 109.5 . . ? H1S2 C1SA H1S3 109.5 . . ? N2SA C2SA H2S1 109.5 . . ? N2SA C2SA H2S2 109.5 . . ? H2S1 C2SA H2S2 109.5 . . ? N2SA C2SA H2S3 109.5 . . ? H2S1 C2SA H2S3 109.5 . . ? H2S2 C2SA H2S3 109.5 . . ? O1SA C3SA N2SA 125.8(4) . . ? O1SA C3SA H3SA 117.1 . . ? N2SA C3SA H3SA 117.1 . . ? C3SB N1SB C2SB 120.3(5) . . ? C3SB N1SB C1SB 119.2(5) . . ? C2SB N1SB C1SB 120.5(5) . . ? N1SB C1SB H1S4 109.5 . . ? N1SB C1SB H1S5 109.5 . . ? H1S4 C1SB H1S5 109.5 . . ? N1SB C1SB H1S6 109.5 . . ? H1S4 C1SB H1S6 109.5 . . ? H1S5 C1SB H1S6 109.5 . . ? N1SB C2SB H2S4 109.5 . . ? N1SB C2SB H2S5 109.5 . . ? H2S4 C2SB H2S5 109.5 . . ? N1SB C2SB H2S6 109.5 . . ? H2S4 C2SB H2S6 109.5 . . ? H2S5 C2SB H2S6 109.5 . . ? N1SB C3SB O1SB 119.0(6) . . ? N1SB C3SB H3SB 120.5 . . ? O1SB C3SB H3SB 120.5 . . ? C3SC N1SC C1SC 124.1(13) . . ? C3SC N1SC C2SC 122.2(12) . . ? C1SC N1SC C2SC 112.9(12) . . ? N1SC C1SC H2S7 109.5 . . ? N1SC C1SC H2S8 109.5 . . ? H2S7 C1SC H2S8 109.5 . . ? N1SC C1SC H2S9 109.5 . . ? H2S7 C1SC H2S9 109.5 . . ? H2S8 C1SC H2S9 109.5 . . ? N1SC C2SC H1S7 109.5 . . ? N1SC C2SC H1S8 109.5 . . ? H1S7 C2SC H1S8 109.5 . . ? N1SC C2SC H1S9 109.5 . . ? H1S7 C2SC H1S9 109.5 . . ? H1S8 C2SC H1S9 109.5 . . ? O1SC C3SC N1SC 126.9(13) . . ? O1SC C3SC H3SC 116.5 . . ? N1SC C3SC H3SC 116.5 . . ? C3SE N1SE C1SE 118.5(15) . . ? C3SE N1SE C2SE 124.1(13) . . ? C1SE N1SE C2SE 115.2(14) . . ? N1SE C1SE H1SX 109.5 . . ? N1SE C1SE H1SY 109.5 . . ? H1SX C1SE H1SY 109.5 . . ? N1SE C1SE H1SZ 109.5 . . ? H1SX C1SE H1SZ 109.5 . . ? H1SY C1SE H1SZ 109.5 . . ? N1SE C2SE H2SX 109.5 . . ? N1SE C2SE H2SY 109.5 . . ? H2SX C2SE H2SY 109.5 . . ? N1SE C2SE H2SZ 109.5 . . ? H2SX C2SE H2SZ 109.5 . . ? H2SY C2SE H2SZ 109.5 . . ? O1SE C3SE N1SE 122.1(14) . . ? O1SE C3SE H3SE 118.9 . . ? N1SE C3SE H3SE 118.9 . . ? C3SD N1SD C1SD 109.3(16) . . ? C3SD N1SD C2SD 125.9(15) . . ? C1SD N1SD C2SD 118.8(15) . . ? N1SD C1SD H1SA 109.5 . . ? N1SD C1SD H1SB 109.5 . . ? H1SA C1SD H1SB 109.5 . . ? N1SD C1SD H1SC 109.5 . . ? H1SA C1SD H1SC 109.5 . . ? H1SB C1SD H1SC 109.5 . . ? N1SD C2SD H2SA 109.5 . . ? N1SD C2SD H2SB 109.5 . . ? H2SA C2SD H2SB 109.5 . . ? N1SD C2SD H2SC 109.5 . . ? H2SA C2SD H2SC 109.5 . . ? H2SB C2SD H2SC 109.5 . . ? O1SD C3SD N1SD 125.8(19) . . ? O1SD C3SD H3SD 117.1 . . ? N1SD C3SD H3SD 117.1 . . ? C3SF N1SF C1SF 122.3(16) . . ? C3SF N1SF C2SF 119.0(15) . . ? C1SF N1SF C2SF 114.2(15) . . ? N1SF C1SF H2SD 109.5 . . ? N1SF C1SF H2SE 109.5 . . ? H2SD C1SF H2SE 109.5 . . ? N1SF C1SF H2SF 109.5 . . ? H2SD C1SF H2SF 109.5 . . ? H2SE C1SF H2SF 109.5 . . ? N1SF C2SF H1SD 109.5 . . ? N1SF C2SF H1SE 109.5 . . ? H1SD C2SF H1SE 109.5 . . ? N1SF C2SF H1SF 109.5 . . ? H1SD C2SF H1SF 109.5 . . ? H1SE C2SF H1SF 109.5 . . ? O1SF C3SF N1SF 123.4(19) . . ? O1SF C3SF H3SF 118.3 . . ? N1SF C3SF H3SF 118.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.677 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.049 #===END data_05159s2 _database_code_depnum_ccdc_archive 'CCDC 655269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Cu 2+)1.5, (C75 H63 O18 3-), 3(C5 H5 N), 2(C3 H7 N O), 5(C H4 O)' _chemical_formula_sum 'C101 H112 Cu1.50 N5 O25' _chemical_formula_weight 1891.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 52.867(10) _cell_length_b 16.102(3) _cell_length_c 23.170(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.582(3) _cell_angle_gamma 90.00 _cell_volume 19250(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5479 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.96 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7972 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5374 _exptl_absorpt_correction_T_max 0.9295 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART 1k CCD' _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 49632 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16928 _reflns_number_gt 8710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, L. Barbour; http://www.xseed.com' _computing_publication_material SHELXL-97-2 _refine_special_details ; A refinement model that included encapsulated DMF molecules was treated with SQUEEZE in order to model highly disordered residual solvents in the lattice. The SQUEEZE calculation estimated a solvent accessible volume of 485 \%A^3^ per formula unit (3880 \%A3/cell, 20% of the crystal volume) The volume is occupied by a calculated 72 e- per formula unit. To account for the disordered solvents in the density calculation, one molecule of DMF and four molecules of methanol were included in the formulation (calc. 112 electrons). SQUEEZE was also used to treat a refinement model that did not model the disordered, encapsulated DMF. The SQUEEZE calculation estimated a total solvent accessible volume of 641 \%A^3^ per formula unit (5129 \%A3/cell) The molecular cavity containing the DMF molecule is therefore estimated to be approximately 641 - 485 = 156 \%A^3^. The volume is occupied by a calculated additional (compared to the SQUEEZE analysis above) 39 e- per formula unit (309 e-/cell), a value that agrees well with one molecule of DMF (41 e-). References: P. Vandersluis, A. L. Spek, Acta Crystallogr. Sect. A. 1990, 46, 194-201. Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. 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^)+(0.1118P)^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 16928 _refine_ls_number_parameters 1068 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.280921(11) 0.41607(4) -0.15969(3) 0.0514(2) Uani 1 1 d . . . O1 O 0.21778(6) 0.51491(18) 0.04625(12) 0.0437(8) Uani 1 1 d . . . C1 C 0.21986(8) 0.8223(3) 0.05181(18) 0.0353(10) Uani 1 1 d . . . H1A H 0.2219 0.8664 0.0823 0.042 Uiso 1 1 calc R . . H1B H 0.2364 0.8189 0.0384 0.042 Uiso 1 1 calc R . . Cu2 Cu 0.0000 0.83513(5) 0.2500 0.0420(2) Uani 1 2 d S . . O2 O 0.20080(5) 0.50617(18) 0.14439(12) 0.0424(7) Uani 1 1 d . . . C2 C 0.21553(7) 0.7396(3) 0.08068(17) 0.0325(10) Uani 1 1 d . B . O3 O 0.20737(7) 0.1912(2) 0.17950(15) 0.0558(9) Uani 1 1 d . . . C3 C 0.21923(7) 0.6657(3) 0.05190(17) 0.0327(10) Uani 1 1 d . . . H3 H 0.2249 0.6691 0.0158 0.039 Uiso 1 1 calc R B . O4 O 0.16969(8) 0.1359(2) 0.14073(18) 0.0804(12) Uani 1 1 d . . . C4 C 0.21505(7) 0.5892(3) 0.07302(18) 0.0336(10) Uani 1 1 d . B . O5 O 0.09037(6) 0.4186(2) 0.17680(14) 0.0495(8) Uani 1 1 d . . . C5 C 0.20664(7) 0.5841(3) 0.12649(18) 0.0346(10) Uani 1 1 d . B . O6 O 0.06171(17) 0.5523(5) 0.1451(4) 0.053(2) Uani 0.70 1 d P A 1 C6 C 0.20394(7) 0.6560(3) 0.15629(18) 0.0355(10) Uani 1 1 d . . . H6 H 0.1995 0.6521 0.1938 0.043 Uiso 1 1 calc R D . O7 O 0.11257(7) 0.7225(2) 0.18949(18) 0.0731(11) Uani 1 1 d . . . C7 C 0.20739(7) 0.7350(3) 0.13381(18) 0.0345(10) Uani 1 1 d . B . O8 O 0.08959(6) 0.7969(2) 0.09484(15) 0.0612(10) Uani 1 1 d . D . C8 C 0.21706(11) 0.5182(3) -0.0158(2) 0.0599(14) Uani 1 1 d . B 10 H8A H 0.2030 0.5550 -0.0352 0.090 Uiso 1 1 calc R B 10 H8B H 0.2141 0.4623 -0.0327 0.090 Uiso 1 1 calc R B 10 H8C H 0.2336 0.5395 -0.0221 0.090 Uiso 1 1 calc R B 10 O9 O 0.00962(6) 0.83665(19) 0.17263(13) 0.0442(8) Uani 1 1 d . C 1 C9 C 0.18504(8) 0.5050(3) 0.18746(19) 0.0420(11) Uani 1 1 d . D 11 H9A H 0.1722 0.5505 0.1794 0.050 Uiso 1 1 calc R D 11 H9B H 0.1960 0.5135 0.2275 0.050 Uiso 1 1 calc R D 11 O10 O -0.02751(6) 0.7918(2) 0.11614(14) 0.0581(9) Uani 1 1 d . C 2 C10 C 0.17134(8) 0.4228(3) 0.18483(18) 0.0372(10) Uani 1 1 d . . . O11 O 0.00650(5) 0.72170(18) -0.13055(12) 0.0408(7) Uani 1 1 d . D . C11 C 0.14548(8) 0.4208(3) 0.18818(18) 0.0384(10) Uani 1 1 d . D . H11 H 0.1368 0.4717 0.1915 0.046 Uiso 1 1 calc R . . O12 O 0.03305(18) 0.6979(6) -0.2118(4) 0.034(2) Uani 0.50 1 d PU D 2 C12 C 0.13202(8) 0.3474(3) 0.18687(18) 0.0399(11) Uani 1 1 d . . . O13 O 0.14510(7) 0.9269(2) -0.14933(15) 0.0672(10) Uani 1 1 d . . . C13 C 0.14420(9) 0.2741(3) 0.17820(18) 0.0422(11) Uani 1 1 d . D . H13 H 0.1348 0.2234 0.1743 0.051 Uiso 1 1 calc R . . O14 O 0.18795(6) 0.84279(18) -0.16399(13) 0.0483(8) Uani 1 1 d . F . C14 C 0.17010(8) 0.2739(3) 0.17516(18) 0.0389(11) Uani 1 1 d . . . O15 O 0.26259(6) 0.51803(18) -0.14740(14) 0.0473(8) Uani 1 1 d . F . C15 C 0.18369(8) 0.3486(3) 0.18046(18) 0.0412(11) Uani 1 1 d . D . H15 H 0.2017 0.3484 0.1811 0.049 Uiso 1 1 calc R . . O16 O 0.23309(6) 0.42426(19) -0.18426(15) 0.0541(9) Uani 1 1 d . . . C16 C 0.18282(11) 0.1947(3) 0.1649(2) 0.0470(12) Uani 1 1 d . D . C17 C 0.10492(8) 0.3453(3) 0.1973(2) 0.0484(12) Uani 1 1 d . D . H17A H 0.0957 0.2963 0.1769 0.058 Uiso 1 1 calc R . . H17B H 0.1058 0.3387 0.2402 0.058 Uiso 1 1 calc R . . O18 O 0.16448(5) 0.4037(2) -0.01803(13) 0.0519(9) Uani 1 1 d . . . C18 C 0.07775(8) 0.4215(3) 0.11809(19) 0.0401(11) Uani 1 1 d . A . C19 C 0.08101(8) 0.3657(3) 0.0750(2) 0.0425(11) Uani 1 1 d . . . H19 H 0.0934 0.3224 0.0852 0.051 Uiso 1 1 calc R . . C20 C 0.06641(7) 0.3711(3) 0.0160(2) 0.0369(10) Uani 1 1 d . . . C21 C 0.04727(8) 0.4308(3) 0.0029(2) 0.0410(11) Uani 1 1 d . . . C22 C 0.04552(8) 0.4896(3) 0.0463(2) 0.0473(12) Uani 1 1 d . A . H22 H 0.0332 0.5330 0.0365 0.057 Uiso 1 1 calc R . . C23 C 0.06071(9) 0.4877(3) 0.1022(2) 0.0482(12) Uani 1 1 d . . . C24 C 0.05574(18) 0.6325(5) 0.1237(4) 0.070(2) Uani 0.70 1 d P A 1 H24A H 0.0611 0.6726 0.1559 0.105 Uiso 0.70 1 calc PR A 1 H24B H 0.0370 0.6371 0.1080 0.105 Uiso 0.70 1 calc PR A 1 H24C H 0.0649 0.6443 0.0921 0.105 Uiso 0.70 1 calc PR A 1 C25 C 0.02761(8) 0.4362(3) -0.0558(2) 0.0441(12) Uani 1 1 d . D . H25A H 0.0282 0.3835 -0.0775 0.053 Uiso 1 1 calc R . . H25B H 0.0101 0.4409 -0.0473 0.053 Uiso 1 1 calc R . . C26 C 0.19905(8) 0.8088(3) 0.16650(18) 0.0389(11) Uani 1 1 d . . . H26A H 0.2042 0.7997 0.2097 0.047 Uiso 1 1 calc R D . H26B H 0.2076 0.8601 0.1568 0.047 Uiso 1 1 calc R . . C27 C 0.16969(8) 0.8174(3) 0.14751(19) 0.0394(11) Uani 1 1 d . D . C28 C 0.15490(9) 0.7708(3) 0.1788(2) 0.0429(11) Uani 1 1 d . . . H28 H 0.1633 0.7418 0.2133 0.051 Uiso 1 1 calc R D . C29 C 0.12848(9) 0.7658(3) 0.1609(2) 0.0523(13) Uani 1 1 d . D . C30 C 0.11610(9) 0.8079(3) 0.1098(2) 0.0490(12) Uani 1 1 d . . . C31 C 0.13059(8) 0.8560(3) 0.0797(2) 0.0461(12) Uani 1 1 d . D . H31 H 0.1221 0.8857 0.0456 0.055 Uiso 1 1 calc R . . C32 C 0.15763(8) 0.8620(3) 0.0983(2) 0.0403(11) Uani 1 1 d . . . C33 C 0.12499(13) 0.6757(5) 0.2412(4) 0.123(3) Uani 1 1 d . E 1 H33A H 0.1354 0.6309 0.2294 0.184 Uiso 1 1 calc R E 1 H33B H 0.1118 0.6519 0.2601 0.184 Uiso 1 1 calc R E 1 H33C H 0.1363 0.7125 0.2692 0.184 Uiso 1 1 calc R E 1 C34 C 0.07591(9) 0.8335(4) 0.0416(2) 0.0584(14) Uani 1 1 d . . . H34A H 0.0827 0.8126 0.0077 0.070 Uiso 1 1 calc R D . H34B H 0.0780 0.8946 0.0435 0.070 Uiso 1 1 calc R . . C35 C 0.04762(8) 0.8105(3) 0.0341(2) 0.0446(11) Uani 1 1 d . D . C36 C 0.03374(8) 0.7806(3) -0.0194(2) 0.0461(12) Uani 1 1 d . . . H36 H 0.0422 0.7731 -0.0511 0.055 Uiso 1 1 calc R D . C37 C 0.00761(8) 0.7613(2) -0.02760(18) 0.0333(10) Uani 1 1 d . D . C38 C -0.00464(8) 0.7717(2) 0.01919(18) 0.0335(10) Uani 1 1 d . . . H38 H -0.0226 0.7596 0.0139 0.040 Uiso 1 1 calc R D . C39 C 0.00925(8) 0.7999(2) 0.07406(18) 0.0334(10) Uani 1 1 d . C . C40 C 0.03539(8) 0.8193(3) 0.08076(19) 0.0404(11) Uani 1 1 d . . . H40 H 0.0449 0.8388 0.1178 0.048 Uiso 1 1 calc R D . C41 C -0.00432(9) 0.8101(3) 0.12405(19) 0.0358(10) Uani 1 1 d . . . C42 C -0.00842(8) 0.7360(3) -0.08759(17) 0.0398(11) Uani 1 1 d . . . H42A H -0.0181 0.6847 -0.0829 0.048 Uiso 1 1 calc R D . H42B H -0.0212 0.7802 -0.1021 0.048 Uiso 1 1 calc R . . C43 C 0.01969(8) 0.6471(3) -0.12896(18) 0.0364(10) Uani 1 1 d . . . C44 C 0.01828(8) 0.5816(3) -0.09248(19) 0.0391(11) Uani 1 1 d . D . H44 H 0.0081 0.5869 -0.0636 0.047 Uiso 1 1 calc R . . C45 C 0.03125(8) 0.5072(3) -0.09608(19) 0.0383(11) Uani 1 1 d . . . C46 C 0.04674(7) 0.4999(3) -0.13739(18) 0.0371(11) Uani 1 1 d . D . C47 C 0.04867(8) 0.5683(3) -0.17333(18) 0.0415(11) Uani 1 1 d . . . H47 H 0.0594 0.5639 -0.2011 0.050 Uiso 1 1 calc R D . C48 C 0.03577(8) 0.6411(3) -0.17023(19) 0.0422(11) Uani 1 1 d . D . C49 C 0.0462(3) 0.6912(11) -0.2582(6) 0.063(5) Uani 0.50 1 d P D 2 H49A H 0.0647 0.6833 -0.2419 0.095 Uiso 0.50 1 calc PR D 2 H49B H 0.0436 0.7421 -0.2820 0.095 Uiso 0.50 1 calc PR D 2 H49C H 0.0394 0.6436 -0.2832 0.095 Uiso 0.50 1 calc PR D 2 C50 C 0.06030(8) 0.4200(3) -0.1469(2) 0.0449(11) Uani 1 1 d . . . H50A H 0.0613 0.4166 -0.1889 0.054 Uiso 1 1 calc R D . H50B H 0.0496 0.3726 -0.1387 0.054 Uiso 1 1 calc R . . C51 C 0.17198(9) 0.9207(3) 0.0654(2) 0.0433(11) Uani 1 1 d . D . H51A H 0.1890 0.9334 0.0917 0.052 Uiso 1 1 calc R . . H51B H 0.1621 0.9734 0.0589 0.052 Uiso 1 1 calc R . . C52 C 0.17690(8) 0.8921(3) 0.0059(2) 0.0403(11) Uani 1 1 d . . . C53 C 0.15893(9) 0.9147(3) -0.0456(2) 0.0480(12) Uani 1 1 d . D . H53 H 0.1437 0.9436 -0.0420 0.058 Uiso 1 1 calc R . . C54 C 0.16258(9) 0.8966(3) -0.1007(2) 0.0477(12) Uani 1 1 d . D . C55 C 0.18471(9) 0.8545(3) -0.10706(19) 0.0411(11) Uani 1 1 d . . . C56 C 0.20198(8) 0.8296(2) -0.05656(18) 0.0346(10) Uani 1 1 d . D . H56 H 0.2168 0.7986 -0.0606 0.042 Uiso 1 1 calc R . . C57 C 0.19881(7) 0.8480(2) 0.00024(18) 0.0326(10) Uani 1 1 d . D . C59 C 0.20837(9) 0.7906(3) -0.17291(19) 0.0436(11) Uani 1 1 d . . . H59A H 0.2244 0.8061 -0.1442 0.052 Uiso 1 1 calc R F . H59B H 0.2113 0.8007 -0.2131 0.052 Uiso 1 1 calc R . . C60 C 0.20331(9) 0.6998(3) -0.16637(17) 0.0378(10) Uani 1 1 d . F . C61 C 0.17867(9) 0.6702(3) -0.16361(18) 0.0405(11) Uani 1 1 d . . . H61 H 0.1651 0.7086 -0.1631 0.049 Uiso 1 1 calc R F . C62 C 0.17387(8) 0.5868(3) -0.16165(19) 0.0398(11) Uani 1 1 d . F . C63 C 0.19350(8) 0.5307(3) -0.16284(19) 0.0420(11) Uani 1 1 d . . . H63 H 0.1901 0.4728 -0.1624 0.050 Uiso 1 1 calc R F . C64 C 0.21819(8) 0.5584(3) -0.16470(18) 0.0361(10) Uani 1 1 d . F . C65 C 0.22288(8) 0.6433(2) -0.16579(17) 0.0347(10) Uani 1 1 d . . . H65 H 0.2398 0.6626 -0.1662 0.042 Uiso 1 1 calc R F . C66 C 0.23896(9) 0.4956(3) -0.16556(19) 0.0388(11) Uani 1 1 d . F . O67 O 0.15269(6) 0.4984(2) -0.10811(14) 0.0565(9) Uani 1 1 d . F . C67 C 0.14786(9) 0.5535(3) -0.1566(2) 0.0501(12) Uani 1 1 d . . . H67A H 0.1364 0.5992 -0.1498 0.060 Uiso 1 1 calc R F . H67B H 0.1395 0.5239 -0.1933 0.060 Uiso 1 1 calc R . . C68 C 0.13246(8) 0.4534(3) -0.09552(19) 0.0430(11) Uani 1 1 d . . . C69 C 0.10713(8) 0.4552(3) -0.12646(19) 0.0422(11) Uani 1 1 d . D . H69 H 0.1028 0.4879 -0.1614 0.051 Uiso 1 1 calc R . . C70 C 0.08747(8) 0.4111(3) -0.10860(19) 0.0378(10) Uani 1 1 d . D . C71 C 0.09378(8) 0.3627(2) -0.0578(2) 0.0361(10) Uani 1 1 d . . . C72 C 0.11975(8) 0.3591(3) -0.02733(19) 0.0358(10) Uani 1 1 d . D . H72 H 0.1242 0.3251 0.0069 0.043 Uiso 1 1 calc R . . C25S C 0.13904(8) 0.4029(3) -0.04512(19) 0.0396(11) Uani 1 1 d . D . C74 C 0.17095(10) 0.3661(3) 0.0381(2) 0.0657(15) Uani 1 1 d . . . H74A H 0.1593 0.3866 0.0626 0.098 Uiso 1 1 calc R . . H74B H 0.1889 0.3798 0.0570 0.098 Uiso 1 1 calc R . . H74C H 0.1691 0.3057 0.0337 0.098 Uiso 1 1 calc R . . C75 C 0.07394(8) 0.3174(3) -0.0306(2) 0.0426(11) Uani 1 1 d . D . H75A H 0.0584 0.3042 -0.0616 0.051 Uiso 1 1 calc R . . H75B H 0.0814 0.2645 -0.0127 0.051 Uiso 1 1 calc R . . O6A O 0.0541(4) 0.5258(13) 0.1419(11) 0.056(6) Uani 0.30 1 d PU A 2 O12A O 0.0388(2) 0.7206(6) -0.1980(4) 0.041(3) Uani 0.50 1 d PU D 1 C24A C 0.0721(4) 0.5944(14) 0.1570(9) 0.043(5) Uani 0.30 1 d P A 2 H24D H 0.0873 0.5761 0.1864 0.064 Uiso 0.30 1 calc PR A 2 H24E H 0.0636 0.6401 0.1734 0.064 Uiso 0.30 1 calc PR A 2 H24F H 0.0775 0.6136 0.1214 0.064 Uiso 0.30 1 calc PR A 2 C49A C 0.0569(3) 0.7197(11) -0.2349(7) 0.058(4) Uani 0.50 1 d P D 1 H49D H 0.0744 0.7105 -0.2108 0.087 Uiso 0.50 1 calc PR D 1 H49E H 0.0564 0.7730 -0.2555 0.087 Uiso 0.50 1 calc PR D 1 H49F H 0.0526 0.6749 -0.2640 0.087 Uiso 0.50 1 calc PR D 1 C58A C 0.13225(17) 0.8629(6) -0.1906(4) 0.149(4) Uani 1 1 d . F 2 H58A H 0.1442 0.8428 -0.2143 0.223 Uiso 1 1 calc R F 2 H58B H 0.1169 0.8866 -0.2167 0.223 Uiso 1 1 calc R F 2 H58C H 0.1271 0.8166 -0.1682 0.223 Uiso 1 1 calc R F 2 N7S N 0.28759(8) 0.4689(2) -0.23250(17) 0.0491(10) Uani 1 1 d . G -1 C8S C 0.31082(11) 0.5030(3) -0.2330(3) 0.0592(14) Uani 1 1 d . . . H8S H 0.3242 0.4971 -0.1986 0.071 Uiso 1 1 calc R G . C9S C 0.31631(15) 0.5457(4) -0.2797(3) 0.089(2) Uani 1 1 d . G . H9S H 0.3331 0.5678 -0.2788 0.106 Uiso 1 1 calc R . . C10S C 0.2969(2) 0.5545(5) -0.3266(4) 0.133(3) Uani 1 1 d . . . H10S H 0.2998 0.5844 -0.3599 0.160 Uiso 1 1 calc R G . C11S C 0.27237(17) 0.5210(6) -0.3283(3) 0.124(3) Uani 1 1 d . G . H11S H 0.2587 0.5276 -0.3622 0.149 Uiso 1 1 calc R . . C12S C 0.26865(12) 0.4790(4) -0.2801(2) 0.0692(16) Uani 1 1 d . . . H12S H 0.2521 0.4562 -0.2804 0.083 Uiso 1 1 calc R G . N13S N 0.27427(18) 0.3657(6) -0.0857(4) 0.044(3) Uiso 0.40 1 d PG G 1 C18S C 0.2734(2) 0.4171(6) -0.0380(5) 0.080(5) Uiso 0.40 1 d PG G 1 H18S H 0.2776 0.4743 -0.0395 0.097 Uiso 0.40 1 calc PR G 1 C17S C 0.2663(3) 0.3849(11) 0.0119(4) 0.201(13) Uiso 0.40 1 d PG G 1 H17S H 0.2657 0.4200 0.0445 0.241 Uiso 0.40 1 calc PR G 1 C16S C 0.2602(4) 0.3012(12) 0.0141(6) 0.184(11) Uiso 0.40 1 d PG G 1 H16S H 0.2553 0.2791 0.0482 0.221 Uiso 0.40 1 calc PR G 1 C15S C 0.2611(3) 0.2497(7) -0.0336(8) 0.175(10) Uiso 0.40 1 d PG G 1 H15S H 0.2568 0.1925 -0.0321 0.210 Uiso 0.40 1 calc PR G 1 C14S C 0.2681(2) 0.2820(6) -0.0835(5) 0.101(6) Uiso 0.40 1 d PG G 1 H14S H 0.2687 0.2468 -0.1161 0.121 Uiso 0.40 1 calc PR G 1 N19S N 0.28426(15) 0.3853(5) -0.0760(3) 0.086(3) Uiso 0.60 1 d PG G 2 C24S C 0.28298(15) 0.4444(4) -0.0331(3) 0.073(3) Uiso 0.60 1 d PG G 2 H24S H 0.2834 0.5019 -0.0422 0.087 Uiso 0.60 1 calc PR G 2 C23S C 0.28112(17) 0.4195(5) 0.0233(3) 0.114(4) Uiso 0.60 1 d PG G 2 H23S H 0.2802 0.4600 0.0527 0.136 Uiso 0.60 1 calc PR G 2 C22S C 0.28055(19) 0.3355(6) 0.0367(3) 0.121(4) Uiso 0.60 1 d PG G 2 H22S H 0.2793 0.3185 0.0752 0.145 Uiso 0.60 1 calc PR G 2 C21S C 0.28183(19) 0.2764(4) -0.0063(4) 0.134(5) Uiso 0.60 1 d PG G 2 H21S H 0.2814 0.2190 0.0029 0.161 Uiso 0.60 1 calc PR G 2 C20S C 0.28369(17) 0.3013(4) -0.0626(4) 0.112(4) Uiso 0.60 1 d PG G 2 H20S H 0.2846 0.2608 -0.0920 0.135 Uiso 0.60 1 calc PR G 2 N25S N 0.0000 0.9598(3) 0.2500 0.0426(13) Uani 0.50 2 d SP . 1 C26S C 0.0128(3) 0.9964(10) 0.2186(6) 0.056(4) Uani 0.35 1 d P H 1 H26S H 0.0222 0.9650 0.1955 0.067 Uiso 0.35 1 calc PR H 1 C27S C 0.0135(3) 1.0862(9) 0.2167(7) 0.065(4) Uani 0.35 1 d P H 1 H27S H 0.0233 1.1131 0.1924 0.078 Uiso 0.35 1 calc PR H 1 C28S C 0.0000 1.1330(5) 0.2500 0.069(2) Uani 0.50 2 d SP . 1 H28S H 0.0000 1.1920 0.2500 0.082 Uiso 0.50 2 calc SPR . 1 N29S N 0.0000 0.9598(3) 0.2500 0.0426(13) Uani 0.50 2 d SP . 2 C30S C 0.01273(17) 1.0059(5) 0.2961(4) 0.057(2) Uani 0.65 1 d P I 2 H30S H 0.0219 0.9777 0.3303 0.069 Uiso 0.65 1 calc PR I 2 C31S C 0.01314(18) 1.0947(5) 0.2961(4) 0.070(2) Uani 0.65 1 d P I 2 H31S H 0.0228 1.1248 0.3290 0.083 Uiso 0.65 1 calc PR I 2 C32S C 0.0000 1.1330(5) 0.2500 0.069(2) Uani 0.50 2 d SP . 2 H32S H 0.0000 1.1920 0.2500 0.082 Uiso 0.50 2 calc SPR . 2 N33S N 0.0000 0.7077(3) 0.2500 0.0399(13) Uani 1 2 d S . . C34S C 0.01365(9) 0.6643(3) 0.2191(2) 0.0483(12) Uani 1 1 d . . . H34S H 0.0238 0.6940 0.1967 0.058 Uiso 1 1 calc R C . C35S C 0.01416(9) 0.5789(3) 0.2172(2) 0.0495(12) Uani 1 1 d . C . H35S H 0.0241 0.5506 0.1937 0.059 Uiso 1 1 calc R . . C36S C 0.0000 0.5361(4) 0.2500 0.0494(18) Uani 1 2 d S . . H36S H 0.0000 0.4771 0.2500 0.059 Uiso 1 2 calc SR C . O37S O 0.04803(8) 0.8404(2) 0.29331(18) 0.0791(11) Uani 1 1 d . J -1 H37S H 0.0417 0.8161 0.3189 0.095 Uiso 1 1 calc R J -1 C38S C 0.06842(13) 0.7928(4) 0.2810(3) 0.099(2) Uani 1 1 d . . . H38A H 0.0661 0.7346 0.2912 0.148 Uiso 1 1 calc R J . H39A H 0.0849 0.8134 0.3045 0.148 Uiso 1 1 calc R . . H40A H 0.0685 0.7971 0.2389 0.148 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 0.0560(4) 0.0506(4) 0.0512(4) 0.0006(3) 0.0195(3) 0.0162(3) O1 0.057(2) 0.0401(18) 0.0382(18) 0.0002(14) 0.0194(15) -0.0006(15) C1 0.034(2) 0.041(3) 0.034(2) -0.003(2) 0.014(2) -0.0082(19) Cu2 0.0520(5) 0.0429(5) 0.0331(4) 0.000 0.0138(4) 0.000 O2 0.0443(18) 0.0411(18) 0.0450(18) 0.0104(15) 0.0171(15) 0.0018(14) C2 0.026(2) 0.039(3) 0.032(2) -0.003(2) 0.0048(18) -0.0085(18) O3 0.057(2) 0.050(2) 0.065(2) 0.0028(17) 0.0223(19) 0.0181(17) C3 0.027(2) 0.045(3) 0.025(2) 0.002(2) 0.0044(18) -0.0058(19) O4 0.083(3) 0.060(3) 0.088(3) -0.018(2) -0.004(2) 0.017(2) C4 0.029(2) 0.038(3) 0.033(2) -0.002(2) 0.0042(19) -0.0031(19) O5 0.0409(18) 0.062(2) 0.047(2) 0.0044(17) 0.0137(15) 0.0059(16) C5 0.028(2) 0.044(3) 0.030(2) 0.011(2) 0.0036(18) 0.0010(19) O6 0.067(7) 0.035(5) 0.059(4) -0.008(4) 0.017(5) 0.005(4) C6 0.031(2) 0.047(3) 0.030(2) -0.004(2) 0.0099(19) 0.000(2) O7 0.054(2) 0.085(3) 0.089(3) 0.025(2) 0.036(2) -0.0026(19) C7 0.026(2) 0.042(3) 0.034(2) -0.001(2) 0.0045(19) -0.0037(19) O8 0.0287(18) 0.090(3) 0.068(2) 0.008(2) 0.0158(17) -0.0037(17) C8 0.089(4) 0.054(3) 0.042(3) -0.003(2) 0.026(3) -0.004(3) O9 0.0485(19) 0.052(2) 0.0350(17) -0.0067(15) 0.0154(15) -0.0112(15) C9 0.046(3) 0.040(3) 0.044(3) 0.006(2) 0.018(2) -0.002(2) O10 0.041(2) 0.088(3) 0.049(2) -0.0212(18) 0.0184(16) -0.0236(18) C10 0.039(3) 0.039(3) 0.033(2) 0.009(2) 0.009(2) 0.008(2) O11 0.0399(17) 0.052(2) 0.0328(16) 0.0041(14) 0.0126(14) 0.0131(15) C11 0.044(3) 0.038(3) 0.036(2) 0.005(2) 0.014(2) 0.007(2) O12 0.035(4) 0.036(4) 0.032(4) 0.001(3) 0.009(3) 0.000(3) C12 0.043(3) 0.044(3) 0.035(2) 0.012(2) 0.014(2) 0.002(2) O13 0.063(2) 0.088(3) 0.049(2) 0.012(2) 0.0094(19) 0.029(2) C13 0.044(3) 0.044(3) 0.038(3) 0.003(2) 0.007(2) -0.007(2) O14 0.067(2) 0.0427(19) 0.0374(18) 0.0066(15) 0.0163(16) 0.0146(16) C14 0.046(3) 0.033(3) 0.037(3) 0.006(2) 0.008(2) 0.006(2) O15 0.0355(18) 0.0480(19) 0.057(2) -0.0098(16) 0.0075(15) -0.0023(15) C15 0.036(3) 0.054(3) 0.034(2) 0.009(2) 0.008(2) 0.004(2) O16 0.0468(19) 0.0379(19) 0.082(2) -0.0139(18) 0.0243(18) -0.0067(15) C16 0.060(4) 0.045(3) 0.035(3) 0.001(2) 0.007(2) 0.006(3) C17 0.042(3) 0.058(3) 0.050(3) 0.011(2) 0.018(2) -0.003(2) O18 0.0275(17) 0.078(2) 0.049(2) 0.0142(18) 0.0048(15) 0.0004(15) C18 0.034(3) 0.052(3) 0.038(3) 0.004(2) 0.017(2) -0.001(2) C19 0.031(2) 0.040(3) 0.058(3) 0.014(2) 0.015(2) 0.000(2) C20 0.022(2) 0.036(3) 0.054(3) 0.004(2) 0.012(2) -0.0054(19) C21 0.030(2) 0.047(3) 0.051(3) 0.008(2) 0.019(2) -0.006(2) C22 0.035(3) 0.054(3) 0.060(3) 0.015(3) 0.025(2) 0.009(2) C23 0.045(3) 0.058(3) 0.046(3) -0.001(3) 0.018(3) 0.009(2) C24 0.081(6) 0.054(5) 0.077(6) -0.005(5) 0.024(5) -0.005(5) C25 0.026(2) 0.050(3) 0.059(3) 0.002(2) 0.014(2) 0.003(2) C26 0.040(3) 0.048(3) 0.030(2) -0.007(2) 0.011(2) -0.013(2) C27 0.037(3) 0.043(3) 0.041(3) -0.012(2) 0.016(2) -0.004(2) C28 0.043(3) 0.046(3) 0.044(3) -0.007(2) 0.018(2) 0.001(2) C29 0.046(3) 0.057(3) 0.063(3) -0.004(3) 0.031(3) -0.004(2) C30 0.033(3) 0.064(3) 0.054(3) -0.004(3) 0.017(2) -0.003(2) C31 0.034(3) 0.065(3) 0.041(3) -0.004(2) 0.010(2) 0.005(2) C32 0.035(3) 0.046(3) 0.045(3) -0.008(2) 0.020(2) 0.000(2) C33 0.080(5) 0.146(7) 0.157(7) 0.097(6) 0.058(5) 0.013(4) C34 0.041(3) 0.090(4) 0.049(3) 0.000(3) 0.019(2) -0.010(3) C35 0.033(3) 0.055(3) 0.047(3) -0.004(2) 0.012(2) -0.008(2) C36 0.040(3) 0.064(3) 0.041(3) 0.002(2) 0.024(2) 0.004(2) C37 0.038(3) 0.031(2) 0.032(2) 0.0054(19) 0.011(2) 0.0071(19) C38 0.028(2) 0.036(2) 0.039(3) 0.003(2) 0.011(2) 0.0023(18) C39 0.040(3) 0.028(2) 0.035(2) 0.0004(19) 0.013(2) 0.0005(19) C40 0.039(3) 0.044(3) 0.037(2) -0.005(2) 0.006(2) -0.006(2) C41 0.047(3) 0.032(2) 0.033(3) 0.000(2) 0.020(2) 0.003(2) C42 0.040(3) 0.050(3) 0.032(2) 0.000(2) 0.014(2) 0.010(2) C43 0.029(2) 0.051(3) 0.029(2) -0.001(2) 0.0050(19) 0.004(2) C44 0.033(2) 0.049(3) 0.037(3) 0.001(2) 0.013(2) 0.002(2) C45 0.026(2) 0.048(3) 0.040(3) -0.003(2) 0.003(2) -0.002(2) C46 0.019(2) 0.056(3) 0.034(2) -0.012(2) 0.0009(18) -0.0006(19) C47 0.033(3) 0.061(3) 0.032(2) 0.002(2) 0.010(2) 0.008(2) C48 0.037(3) 0.057(3) 0.035(3) 0.008(2) 0.014(2) 0.012(2) C49 0.057(11) 0.101(14) 0.042(9) 0.030(8) 0.032(7) 0.035(8) C50 0.031(2) 0.058(3) 0.042(3) -0.009(2) 0.002(2) 0.007(2) C51 0.042(3) 0.039(3) 0.052(3) -0.001(2) 0.018(2) 0.006(2) C52 0.042(3) 0.034(3) 0.047(3) 0.000(2) 0.015(2) -0.004(2) C53 0.043(3) 0.051(3) 0.052(3) 0.008(2) 0.016(2) 0.014(2) C54 0.045(3) 0.055(3) 0.043(3) 0.011(2) 0.011(2) 0.011(2) C55 0.053(3) 0.035(3) 0.036(3) 0.005(2) 0.012(2) -0.003(2) C56 0.037(2) 0.026(2) 0.040(3) 0.002(2) 0.008(2) -0.0007(19) C57 0.030(2) 0.029(2) 0.040(3) -0.0022(19) 0.0093(19) -0.0064(18) C59 0.058(3) 0.040(3) 0.034(3) 0.006(2) 0.014(2) 0.006(2) C60 0.046(3) 0.042(3) 0.026(2) -0.001(2) 0.010(2) 0.003(2) C61 0.047(3) 0.042(3) 0.033(2) -0.001(2) 0.012(2) 0.009(2) C62 0.031(2) 0.051(3) 0.037(3) -0.004(2) 0.008(2) 0.003(2) C63 0.048(3) 0.038(3) 0.041(3) -0.004(2) 0.011(2) -0.002(2) C64 0.036(3) 0.040(3) 0.034(2) -0.005(2) 0.013(2) -0.002(2) C65 0.044(3) 0.035(3) 0.027(2) -0.0061(19) 0.0114(19) -0.002(2) C66 0.045(3) 0.036(3) 0.039(3) -0.004(2) 0.018(2) -0.006(2) O67 0.0322(18) 0.090(3) 0.049(2) 0.0226(19) 0.0113(15) -0.0037(17) C67 0.046(3) 0.061(3) 0.043(3) 0.007(3) 0.009(2) 0.008(2) C68 0.030(3) 0.059(3) 0.042(3) 0.004(2) 0.013(2) 0.005(2) C69 0.035(3) 0.059(3) 0.033(2) 0.004(2) 0.008(2) 0.008(2) C70 0.033(2) 0.045(3) 0.037(3) -0.009(2) 0.009(2) 0.008(2) C71 0.027(2) 0.031(2) 0.050(3) -0.011(2) 0.009(2) 0.0002(18) C72 0.035(3) 0.035(3) 0.036(2) 0.000(2) 0.005(2) 0.0035(19) C25S 0.025(2) 0.050(3) 0.045(3) 0.002(2) 0.010(2) 0.003(2) C74 0.048(3) 0.072(4) 0.066(4) 0.023(3) -0.012(3) -0.007(3) C75 0.036(3) 0.036(3) 0.054(3) -0.001(2) 0.006(2) -0.003(2) O6A 0.056(7) 0.056(8) 0.058(7) -0.003(5) 0.017(5) -0.003(5) O12A 0.043(4) 0.045(4) 0.041(4) 0.005(3) 0.019(3) 0.000(3) C24A 0.044(12) 0.039(13) 0.051(13) 0.007(10) 0.023(10) 0.018(10) C49A 0.054(10) 0.074(10) 0.052(10) 0.017(8) 0.024(7) 0.011(7) C58A 0.125(7) 0.189(10) 0.107(6) -0.022(7) -0.031(6) 0.052(7) N7S 0.058(3) 0.042(2) 0.049(3) -0.0073(19) 0.016(2) 0.003(2) C8S 0.065(4) 0.047(3) 0.066(4) -0.015(3) 0.018(3) -0.011(3) C9S 0.104(5) 0.093(5) 0.072(4) -0.006(4) 0.027(4) -0.033(4) C10S 0.182(9) 0.129(7) 0.085(6) 0.038(5) 0.022(6) -0.068(7) C11S 0.124(7) 0.163(8) 0.073(5) 0.042(5) -0.006(5) -0.036(6) C12S 0.071(4) 0.083(4) 0.052(3) 0.006(3) 0.011(3) -0.005(3) N25S 0.040(3) 0.046(3) 0.045(3) 0.000 0.016(3) 0.000 C26S 0.062(11) 0.079(12) 0.033(8) -0.005(8) 0.023(8) -0.005(8) C27S 0.087(13) 0.036(9) 0.080(12) 0.004(8) 0.038(10) -0.009(8) C28S 0.065(6) 0.053(5) 0.087(7) 0.000 0.013(5) 0.000 N29S 0.040(3) 0.046(3) 0.045(3) 0.000 0.016(3) 0.000 C30S 0.069(6) 0.051(5) 0.054(5) -0.011(4) 0.014(4) -0.002(4) C31S 0.075(7) 0.052(6) 0.086(7) -0.029(5) 0.027(5) -0.006(5) C32S 0.065(6) 0.053(5) 0.087(7) 0.000 0.013(5) 0.000 N33S 0.045(3) 0.043(3) 0.035(3) 0.000 0.017(3) 0.000 C34S 0.048(3) 0.056(3) 0.041(3) 0.002(2) 0.012(2) 0.007(2) C35S 0.050(3) 0.049(3) 0.049(3) 0.002(3) 0.012(2) 0.009(2) C36S 0.040(4) 0.043(4) 0.055(4) 0.000 -0.010(3) 0.000 O37S 0.082(3) 0.083(3) 0.080(3) 0.001(2) 0.033(2) 0.000(2) C38S 0.083(5) 0.099(5) 0.128(6) -0.002(4) 0.052(4) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3 1.924(3) 7 ? Cu1 O15 1.958(3) . ? Cu1 N19S 1.971(6) . ? Cu1 N7S 1.988(4) . ? Cu1 N13S 1.996(8) . ? Cu1 C66 2.539(4) . ? O1 C4 1.370(5) . ? O1 C8 1.432(5) . ? C1 C57 1.502(6) . ? C1 C2 1.530(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? Cu2 O9 1.967(3) . ? Cu2 O9 1.967(3) 2 ? Cu2 N25S 2.007(5) . ? Cu2 N33S 2.052(5) . ? O2 C5 1.377(5) . ? O2 C9 1.433(5) . ? C2 C7 1.392(5) . ? C2 C3 1.398(5) . ? O3 C16 1.270(5) . ? O3 Cu1 1.924(3) 7 ? C3 C4 1.361(5) . ? C3 H3 0.9500 . ? O4 C16 1.235(6) . ? C4 C5 1.407(5) . ? O5 C18 1.379(5) . ? O5 C17 1.433(5) . ? C5 C6 1.372(6) . ? O6 C24 1.395(11) . ? O6 C23 1.431(9) . ? C6 C7 1.401(6) . ? C6 H6 0.9500 . ? O7 C29 1.371(5) . ? O7 C33 1.447(7) . ? C7 C26 1.525(6) . ? O8 C30 1.380(5) . ? O8 C34 1.415(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C41 1.277(5) . ? C9 C10 1.504(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 C41 1.235(5) . ? C10 C15 1.375(6) . ? C10 C11 1.386(6) . ? O11 C43 1.385(5) . ? O11 C42 1.417(4) . ? C11 C12 1.377(6) . ? C11 H11 0.9500 . ? O12 C48 1.312(10) . ? O12 C49 1.406(17) . ? C12 C13 1.380(6) . ? C12 C17 1.504(6) . ? O13 C54 1.381(5) . ? O13 C58A 1.467(9) . ? C13 C14 1.386(6) . ? C13 H13 0.9500 . ? O14 C55 1.380(5) . ? O14 C59 1.418(5) . ? C14 C15 1.393(6) . ? C14 C16 1.485(6) . ? O15 C66 1.281(5) . ? C15 H15 0.9500 . ? O16 C66 1.243(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O18 C25S 1.355(5) . ? O18 C74 1.406(5) . ? C18 C19 1.382(6) . ? C18 C23 1.392(6) . ? C19 C20 1.419(6) . ? C19 H19 0.9500 . ? C20 C21 1.380(6) . ? C20 C75 1.503(6) . ? C21 C22 1.400(6) . ? C21 C25 1.523(6) . ? C22 C23 1.367(6) . ? C22 H22 0.9500 . ? C23 O6A 1.22(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C45 1.515(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.525(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.381(6) . ? C27 C28 1.394(6) . ? C28 C29 1.370(6) . ? C28 H28 0.9500 . ? C29 C30 1.397(7) . ? C30 C31 1.379(6) . ? C31 C32 1.404(6) . ? C31 H31 0.9500 . ? C32 C51 1.517(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.513(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.381(6) . ? C35 C40 1.383(6) . ? C36 C37 1.388(6) . ? C36 H36 0.9500 . ? C37 C38 1.388(5) . ? C37 C42 1.518(6) . ? C38 C39 1.398(6) . ? C38 H38 0.9500 . ? C39 C40 1.392(6) . ? C39 C41 1.498(5) . ? C40 H40 0.9500 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.364(6) . ? C43 C48 1.414(6) . ? C44 C45 1.391(6) . ? C44 H44 0.9500 . ? C45 C46 1.393(6) . ? C46 C47 1.397(6) . ? C46 C50 1.513(6) . ? C47 C48 1.367(6) . ? C47 H47 0.9500 . ? C48 O12A 1.457(11) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C70 1.522(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.530(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C57 1.389(6) . ? C52 C53 1.402(6) . ? C53 C54 1.363(6) . ? C53 H53 0.9500 . ? C54 C55 1.388(6) . ? C55 C56 1.378(6) . ? C56 C57 1.394(6) . ? C56 H56 0.9500 . ? C59 C60 1.500(6) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C65 1.375(6) . ? C60 C61 1.402(6) . ? C61 C62 1.369(6) . ? C61 H61 0.9500 . ? C62 C63 1.381(6) . ? C62 C67 1.504(6) . ? C63 C64 1.389(6) . ? C63 H63 0.9500 . ? C64 C65 1.391(6) . ? C64 C66 1.497(6) . ? C65 H65 0.9500 . ? O67 C68 1.374(5) . ? O67 C67 1.411(5) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.375(6) . ? C68 C25S 1.404(6) . ? C69 C70 1.394(6) . ? C69 H69 0.9500 . ? C70 C71 1.390(6) . ? C71 C72 1.402(6) . ? C71 C75 1.523(6) . ? C72 C25S 1.375(6) . ? C72 H72 0.9500 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? O6A C24A 1.45(2) . ? O12A C49A 1.418(18) . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C49A H49D 0.9800 . ? C49A H49E 0.9800 . ? C49A H49F 0.9800 . ? C58A H58A 0.9800 . ? C58A H58B 0.9800 . ? C58A H58C 0.9800 . ? N7S C12S 1.328(6) . ? N7S C8S 1.348(6) . ? C8S C9S 1.366(8) . ? C8S H8S 0.9500 . ? C9S C10S 1.328(10) . ? C9S H9S 0.9500 . ? C10S C11S 1.398(11) . ? C10S H10S 0.9500 . ? C11S C12S 1.356(8) . ? C11S H11S 0.9500 . ? C12S H12S 0.9500 . ? N13S C18S 1.3900 . ? N13S C14S 1.3900 . ? C18S C17S 1.3900 . ? C18S H18S 0.9500 . ? C17S C16S 1.3900 . ? C17S H17S 0.9500 . ? C16S C15S 1.3900 . ? C16S H16S 0.9500 . ? C15S C14S 1.3900 . ? C15S H15S 0.9500 . ? C14S H14S 0.9500 . ? N19S C24S 1.3900 . ? N19S C20S 1.3900 . ? C24S C23S 1.3900 . ? C24S H24S 0.9500 . ? C23S C22S 1.3900 . ? C23S H23S 0.9500 . ? C22S C21S 1.3900 . ? C22S H22S 0.9500 . ? C21S C20S 1.3900 . ? C21S H21S 0.9500 . ? C20S H20S 0.9500 . ? N25S C26S 1.244(14) . ? N25S C26S 1.244(14) 2 ? C26S C27S 1.45(2) . ? C26S H26S 0.9500 . ? C27S C28S 1.382(16) . ? C27S H27S 0.9500 . ? C28S C27S 1.382(16) 2 ? C28S H28S 0.9500 . ? C30S C31S 1.431(11) . ? C30S H30S 0.9500 . ? C31S H31S 0.9500 . ? N33S C34S 1.322(5) 2 ? N33S C34S 1.322(5) . ? C34S C35S 1.376(6) . ? C34S H34S 0.9500 . ? C35S C36S 1.364(6) . ? C35S H35S 0.9500 . ? C36S C35S 1.364(6) 2 ? C36S H36S 0.9500 . ? O37S C38S 1.401(6) . ? O37S H37S 0.8400 . ? C38S H38A 0.9800 . ? C38S H39A 0.9800 . ? C38S H40A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cu1 O15 169.24(14) 7 . ? O3 Cu1 N19S 92.5(2) 7 . ? O15 Cu1 N19S 90.5(2) . . ? O3 Cu1 N7S 93.21(14) 7 . ? O15 Cu1 N7S 87.10(14) . . ? N19S Cu1 N7S 161.4(3) . . ? O3 Cu1 N13S 88.0(3) 7 . ? O15 Cu1 N13S 91.8(3) . . ? N19S Cu1 N13S 17.8(3) . . ? N7S Cu1 N13S 178.7(3) . . ? O3 Cu1 C66 139.69(15) 7 . ? O15 Cu1 C66 29.66(12) . . ? N19S Cu1 C66 94.0(2) . . ? N7S Cu1 C66 93.05(15) . . ? N13S Cu1 C66 86.3(3) . . ? C4 O1 C8 116.2(3) . . ? C57 C1 C2 115.6(3) . . ? C57 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? C57 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? O9 Cu2 O9 178.58(18) . 2 ? O9 Cu2 N25S 89.29(9) . . ? O9 Cu2 N25S 89.29(9) 2 . ? O9 Cu2 N33S 90.71(9) . . ? O9 Cu2 N33S 90.71(9) 2 . ? N25S Cu2 N33S 180.000(1) . . ? C5 O2 C9 115.1(3) . . ? C7 C2 C3 118.6(4) . . ? C7 C2 C1 122.5(4) . . ? C3 C2 C1 118.9(3) . . ? C16 O3 Cu1 109.9(3) . 7 ? C4 C3 C2 123.2(4) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C3 C4 O1 125.9(4) . . ? C3 C4 C5 118.5(4) . . ? O1 C4 C5 115.6(4) . . ? C18 O5 C17 117.7(4) . . ? C6 C5 O2 124.3(4) . . ? C6 C5 C4 118.7(4) . . ? O2 C5 C4 117.0(4) . . ? C24 O6 C23 117.1(7) . . ? C5 C6 C7 122.9(4) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C29 O7 C33 116.8(4) . . ? C2 C7 C6 117.9(4) . . ? C2 C7 C26 125.2(4) . . ? C6 C7 C26 116.6(3) . . ? C30 O8 C34 117.6(4) . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? C41 O9 Cu2 125.8(3) . . ? O2 C9 C10 109.4(3) . . ? O2 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O2 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C15 C10 C11 118.4(4) . . ? C15 C10 C9 122.3(4) . . ? C11 C10 C9 119.3(4) . . ? C43 O11 C42 118.4(3) . . ? C12 C11 C10 121.9(4) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C48 O12 C49 121.0(10) . . ? C11 C12 C13 118.8(4) . . ? C11 C12 C17 121.4(4) . . ? C13 C12 C17 119.7(4) . . ? C54 O13 C58A 114.6(5) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C55 O14 C59 118.5(3) . . ? C13 C14 C15 119.3(4) . . ? C13 C14 C16 119.8(4) . . ? C15 C14 C16 120.9(4) . . ? C66 O15 Cu1 101.2(3) . . ? C10 C15 C14 120.8(4) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O4 C16 O3 121.8(5) . . ? O4 C16 C14 120.2(5) . . ? O3 C16 C14 117.9(4) . . ? O5 C17 C12 112.9(4) . . ? O5 C17 H17A 109.0 . . ? C12 C17 H17A 109.0 . . ? O5 C17 H17B 109.0 . . ? C12 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C25S O18 C74 116.2(3) . . ? O5 C18 C19 125.5(4) . . ? O5 C18 C23 115.6(4) . . ? C19 C18 C23 118.9(4) . . ? C18 C19 C20 121.9(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C19 118.3(4) . . ? C21 C20 C75 122.6(4) . . ? C19 C20 C75 118.8(4) . . ? C20 C21 C22 118.2(4) . . ? C20 C21 C25 124.2(4) . . ? C22 C21 C25 117.7(4) . . ? C23 C22 C21 123.3(4) . . ? C23 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? O6A C23 C22 119.8(12) . . ? O6A C23 C18 117.5(12) . . ? C22 C23 C18 118.7(5) . . ? C22 C23 O6 124.5(5) . . ? C18 C23 O6 116.7(5) . . ? C45 C25 C21 116.0(4) . . ? C45 C25 H25A 108.3 . . ? C21 C25 H25A 108.3 . . ? C45 C25 H25B 108.3 . . ? C21 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C7 108.3(3) . . ? C27 C26 H26A 110.0 . . ? C7 C26 H26A 110.0 . . ? C27 C26 H26B 110.0 . . ? C7 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? C32 C27 C28 119.9(4) . . ? C32 C27 C26 122.9(4) . . ? C28 C27 C26 116.9(4) . . ? C29 C28 C27 121.6(4) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 O7 125.2(5) . . ? C28 C29 C30 119.1(4) . . ? O7 C29 C30 115.7(4) . . ? C31 C30 O8 126.2(4) . . ? C31 C30 C29 119.4(4) . . ? O8 C30 C29 114.4(4) . . ? C30 C31 C32 121.6(4) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C27 C32 C31 118.3(4) . . ? C27 C32 C51 123.2(4) . . ? C31 C32 C51 118.5(4) . . ? O7 C33 H33A 109.5 . . ? O7 C33 H33B 109.5 . . ? O7 C33 H33C 109.5 . . ? O8 C34 C35 107.7(4) . . ? O8 C34 H34A 110.2 . . ? C35 C34 H34A 110.2 . . ? O8 C34 H34B 110.2 . . ? C35 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C36 C35 C40 119.3(4) . . ? C36 C35 C34 120.5(4) . . ? C40 C35 C34 120.2(4) . . ? C35 C36 C37 121.3(4) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C36 C37 C38 119.0(4) . . ? C36 C37 C42 121.7(4) . . ? C38 C37 C42 119.0(4) . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.1(4) . . ? C40 C39 C41 121.3(4) . . ? C38 C39 C41 119.6(4) . . ? C35 C40 C39 120.8(4) . . ? C35 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? O10 C41 O9 125.0(4) . . ? O10 C41 C39 119.1(4) . . ? O9 C41 C39 115.9(4) . . ? O11 C42 C37 113.7(3) . . ? O11 C42 H42A 108.8 . . ? C37 C42 H42A 108.8 . . ? O11 C42 H42B 108.8 . . ? C37 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 C43 O11 126.3(4) . . ? C44 C43 C48 119.2(4) . . ? O11 C43 C48 114.4(4) . . ? C43 C44 C45 122.3(4) . . ? C43 C44 H44 118.9 . . ? C45 C44 H44 118.9 . . ? C44 C45 C46 119.0(4) . . ? C44 C45 C25 118.8(4) . . ? C46 C45 C25 122.1(4) . . ? C45 C46 C47 118.2(4) . . ? C45 C46 C50 122.7(4) . . ? C47 C46 C50 119.0(4) . . ? C48 C47 C46 122.9(4) . . ? C48 C47 H47 118.6 . . ? C46 C47 H47 118.6 . . ? O12 C48 C47 122.4(6) . . ? O12 C48 C43 117.6(6) . . ? C47 C48 C43 118.3(4) . . ? C47 C48 O12A 128.8(5) . . ? C43 C48 O12A 112.3(5) . . ? O12 C49 H49A 109.5 . . ? O12 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O12 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C46 C50 C70 114.4(3) . . ? C46 C50 H50A 108.7 . . ? C70 C50 H50A 108.7 . . ? C46 C50 H50B 108.7 . . ? C70 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C32 C51 C52 117.8(4) . . ? C32 C51 H51A 107.8 . . ? C52 C51 H51A 107.8 . . ? C32 C51 H51B 107.8 . . ? C52 C51 H51B 107.8 . . ? H51A C51 H51B 107.2 . . ? C57 C52 C53 118.5(4) . . ? C57 C52 C51 123.2(4) . . ? C53 C52 C51 118.2(4) . . ? C54 C53 C52 122.3(4) . . ? C54 C53 H53 118.9 . . ? C52 C53 H53 118.9 . . ? C53 C54 O13 118.8(4) . . ? C53 C54 C55 119.9(4) . . ? O13 C54 C55 121.0(4) . . ? C56 C55 O14 125.1(4) . . ? C56 C55 C54 118.0(4) . . ? O14 C55 C54 116.8(4) . . ? C55 C56 C57 123.1(4) . . ? C55 C56 H56 118.4 . . ? C57 C56 H56 118.4 . . ? C52 C57 C56 118.1(4) . . ? C52 C57 C1 123.6(4) . . ? C56 C57 C1 118.2(4) . . ? O14 C59 C60 113.8(4) . . ? O14 C59 H59A 108.8 . . ? C60 C59 H59A 108.8 . . ? O14 C59 H59B 108.8 . . ? C60 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C65 C60 C61 118.6(4) . . ? C65 C60 C59 119.7(4) . . ? C61 C60 C59 121.6(4) . . ? C62 C61 C60 121.1(4) . . ? C62 C61 H61 119.5 . . ? C60 C61 H61 119.5 . . ? C61 C62 C63 119.7(4) . . ? C61 C62 C67 122.2(4) . . ? C63 C62 C67 118.1(4) . . ? C62 C63 C64 120.4(4) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C63 C64 C65 119.2(4) . . ? C63 C64 C66 118.7(4) . . ? C65 C64 C66 122.1(4) . . ? C60 C65 C64 120.9(4) . . ? C60 C65 H65 119.5 . . ? C64 C65 H65 119.5 . . ? O16 C66 O15 121.8(4) . . ? O16 C66 C64 120.1(4) . . ? O15 C66 C64 118.1(4) . . ? O16 C66 Cu1 72.6(2) . . ? O15 C66 Cu1 49.2(2) . . ? C64 C66 Cu1 167.2(3) . . ? C68 O67 C67 119.1(3) . . ? O67 C67 C62 106.0(4) . . ? O67 C67 H67A 110.5 . . ? C62 C67 H67A 110.5 . . ? O67 C67 H67B 110.5 . . ? C62 C67 H67B 110.5 . . ? H67A C67 H67B 108.7 . . ? O67 C68 C69 126.4(4) . . ? O67 C68 C25S 114.8(4) . . ? C69 C68 C25S 118.9(4) . . ? C68 C69 C70 122.6(4) . . ? C68 C69 H69 118.7 . . ? C70 C69 H69 118.7 . . ? C71 C70 C69 118.7(4) . . ? C71 C70 C50 124.6(4) . . ? C69 C70 C50 116.7(4) . . ? C70 C71 C72 118.5(4) . . ? C70 C71 C75 124.0(4) . . ? C72 C71 C75 117.3(4) . . ? C25S C72 C71 122.5(4) . . ? C25S C72 H72 118.8 . . ? C71 C72 H72 118.8 . . ? O18 C25S C72 126.3(4) . . ? O18 C25S C68 114.9(4) . . ? C72 C25S C68 118.8(4) . . ? O18 C74 H74A 109.5 . . ? O18 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? O18 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C20 C75 C71 109.6(3) . . ? C20 C75 H75A 109.8 . . ? C71 C75 H75A 109.8 . . ? C20 C75 H75B 109.8 . . ? C71 C75 H75B 109.8 . . ? H75A C75 H75B 108.2 . . ? C23 O6A C24A 106.5(19) . . ? C49A O12A C48 114.3(10) . . ? O6A C24A H24D 109.5 . . ? O6A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? O6A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? O13 C58A H58A 109.5 . . ? O13 C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? O13 C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? C12S N7S C8S 117.8(5) . . ? C12S N7S Cu1 121.1(4) . . ? C8S N7S Cu1 120.8(4) . . ? N7S C8S C9S 124.3(6) . . ? N7S C8S H8S 117.9 . . ? C9S C8S H8S 117.9 . . ? C10S C9S C8S 116.2(7) . . ? C10S C9S H9S 121.9 . . ? C8S C9S H9S 121.9 . . ? C9S C10S C11S 121.9(7) . . ? C9S C10S H10S 119.0 . . ? C11S C10S H10S 119.0 . . ? C12S C11S C10S 118.0(7) . . ? C12S C11S H11S 121.0 . . ? C10S C11S H11S 121.0 . . ? N7S C12S C11S 121.8(6) . . ? N7S C12S H12S 119.1 . . ? C11S C12S H12S 119.1 . . ? C18S N13S C14S 120.0 . . ? C18S N13S Cu1 118.9(6) . . ? C14S N13S Cu1 120.8(6) . . ? N13S C18S C17S 120.0 . . ? N13S C18S H18S 120.0 . . ? C17S C18S H18S 120.0 . . ? C16S C17S C18S 120.0 . . ? C16S C17S H17S 120.0 . . ? C18S C17S H17S 120.0 . . ? C17S C16S C15S 120.0 . . ? C17S C16S H16S 120.0 . . ? C15S C16S H16S 120.0 . . ? C16S C15S C14S 120.0 . . ? C16S C15S H15S 120.0 . . ? C14S C15S H15S 120.0 . . ? C15S C14S N13S 120.0 . . ? C15S C14S H14S 120.0 . . ? N13S C14S H14S 120.0 . . ? C24S N19S C20S 120.0 . . ? C24S N19S Cu1 121.6(4) . . ? C20S N19S Cu1 117.6(4) . . ? C23S C24S N19S 120.0 . . ? C23S C24S H24S 120.0 . . ? N19S C24S H24S 120.0 . . ? C24S C23S C22S 120.0 . . ? C24S C23S H23S 120.0 . . ? C22S C23S H23S 120.0 . . ? C21S C22S C23S 120.0 . . ? C21S C22S H22S 120.0 . . ? C23S C22S H22S 120.0 . . ? C20S C21S C22S 120.0 . . ? C20S C21S H21S 120.0 . . ? C22S C21S H21S 120.0 . . ? C21S C20S N19S 120.0 . . ? C21S C20S H20S 120.0 . . ? N19S C20S H20S 120.0 . . ? C26S N25S C26S 123.4(15) . 2 ? C26S N25S Cu2 118.3(8) . . ? C26S N25S Cu2 118.3(8) 2 . ? N25S C26S C27S 120.8(13) . . ? N25S C26S H26S 119.6 . . ? C27S C26S H26S 119.6 . . ? C28S C27S C26S 120.5(13) . . ? C28S C27S H27S 119.7 . . ? C26S C27S H27S 119.7 . . ? C27S C28S C27S 113.9(13) 2 . ? C27S C28S H28S 123.1 2 . ? C27S C28S H28S 123.1 . . ? C31S C30S H30S 118.2 . . ? C30S C31S H31S 121.0 . . ? C34S N33S C34S 116.2(6) 2 . ? C34S N33S Cu2 121.9(3) 2 . ? C34S N33S Cu2 121.9(3) . . ? N33S C34S C35S 124.2(5) . . ? N33S C34S H34S 117.9 . . ? C35S C34S H34S 117.9 . . ? C36S C35S C34S 118.0(5) . . ? C36S C35S H35S 121.0 . . ? C34S C35S H35S 121.0 . . ? C35S C36S C35S 119.4(7) 2 . ? C35S C36S H36S 120.3 2 . ? C35S C36S H36S 120.3 . . ? C38S O37S H37S 109.5 . . ? H38A C38S H39A 109.5 . . ? H38A C38S H40A 109.5 . . ? H39A C38S H40A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.649 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.078 #===END data_06070s2 _database_code_depnum_ccdc_archive 'CCDC 655270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Cu 2+)1.5, (C75 H63 O18 3-), 2.15(C5 H5 N), 2(C3 H7 N O), 1(C H4 O)' _chemical_formula_sum 'C93.25 H93.75 Cu1.50 N4.15 O21.50' _chemical_formula_weight 1711.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 53.319(6) _cell_length_b 15.9118(16) _cell_length_c 22.444(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.719(2) _cell_angle_gamma 90.00 _cell_volume 18574(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6330 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 19.95 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7182 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5599 _exptl_absorpt_correction_T_max 0.9439 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1k CCD (Siemens)' _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 51505 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.10 _reflns_number_total 11478 _reflns_number_gt 4431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, L. Barbour; http://www.xseed.com' _computing_publication_material SHELXL-97-2 _refine_special_details ; A refinement model that included encapsulated DMF molecules was treated with SQUEEZE in order to model highly disordered residual solvents in the lattice. The SQUEEZE calculation estimated a solvent accessible volume of 374 \%A^3^ per formula unit (2992 \%A^3^/cell, or 16% of the crystal volume). The volume is occupied by a calculated 57e- per formula unit. To account for the disordered solvents in the density calculation, one molecule of DMF and one molecule of methanol were inluded in the formulation (calc. 58 electrons). SQUEEZE was also used to treat a refinemnt model that did not model the disordered, encapsulated DMF. The SQUEEZE calculation estimated a total solvent accessible volume of 523 \%A^3^ per formula unit (4185 \%A3/cell) The molecular cavity containing the DMF molecule is therefore estimated to be approximately 523 - 374 = 149 \%A^3^. The volume is occupied by a calculated additional (compared to the SQUEEZE analysis above) 30 e- per formula unit (237 e-/cell), a value that is 72% of what would be expected for one molecule of DMF (41 e-). References: P. Vandersluis, A. L. Spek, Acta Crystallogr. Sect. A. 1990, 46, 194-201. Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. 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^)+(0.1710P)^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 11478 _refine_ls_number_parameters 958 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1775 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2815 _refine_ls_wR_factor_gt 0.2458 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.28196(3) 0.39508(7) -0.14468(7) 0.1146(6) Uani 1 1 d . . . O1 O 0.22111(11) 0.5239(4) 0.0594(3) 0.0917(18) Uani 1 1 d . . . C1 C 0.22181(16) 0.8320(5) 0.0511(4) 0.071(2) Uani 1 1 d . . . H1A H 0.2383 0.8258 0.0380 0.086 Uiso 1 1 calc R . . H1B H 0.2238 0.8795 0.0803 0.086 Uiso 1 1 calc R . . Cu2 Cu 0.0000 0.84736(12) 0.2500 0.1040(7) Uani 1 2 d S . . O2 O 0.20269(11) 0.5240(4) 0.1575(3) 0.095(2) Uani 1 1 d . . . C2 C 0.21735(15) 0.7547(5) 0.0837(4) 0.062(2) Uani 1 1 d . B . O3 O 0.20880(16) 0.2158(4) 0.1716(3) 0.112(2) Uani 1 1 d . . . C3 C 0.22185(14) 0.6790(6) 0.0591(4) 0.067(2) Uani 1 1 d . . . H3 H 0.2283 0.6793 0.0228 0.081 Uiso 1 1 calc R B . O4 O 0.17070(16) 0.1560(5) 0.1311(4) 0.127(3) Uani 1 1 d . . . C4 C 0.21774(16) 0.6033(6) 0.0835(4) 0.076(2) Uani 1 1 d . B . O5 O 0.09359(13) 0.4270(4) 0.1954(4) 0.096(2) Uani 1 1 d . D . C5 C 0.20804(15) 0.6013(7) 0.1377(4) 0.077(3) Uani 1 1 d . B . O6 O 0.06006(12) 0.5457(5) 0.1651(4) 0.114(2) Uani 1 1 d . . . C6 C 0.20442(16) 0.6759(7) 0.1625(4) 0.083(3) Uani 1 1 d . . . H6 H 0.1986 0.6755 0.1996 0.100 Uiso 1 1 calc R D . O7 O 0.11343(15) 0.7517(6) 0.1893(4) 0.153(3) Uani 1 1 d . . . C7 C 0.20850(15) 0.7534(6) 0.1383(4) 0.075(2) Uani 1 1 d . B . O8 O 0.0900(2) 0.8643(8) 0.0833(6) 0.077(4) Uiso 0.50 1 d P A 1 C8 C 0.2359(4) 0.5212(10) 0.0146(8) 0.112(7) Uani 0.65 1 d P B 9 H8A H 0.2350 0.4648 -0.0032 0.168 Uiso 0.65 1 calc PR B 9 H8B H 0.2538 0.5348 0.0334 0.168 Uiso 0.65 1 calc PR B 9 H8C H 0.2292 0.5623 -0.0175 0.168 Uiso 0.65 1 calc PR B 9 O9 O 0.0131(2) 0.8295(11) 0.1770(6) 0.100(4) Uani 0.70 1 d P C 2 C9 C 0.18497(16) 0.5253(6) 0.1988(4) 0.081(3) Uani 1 1 d . D 11 H9A H 0.1718 0.5696 0.1865 0.098 Uiso 1 1 calc R D 11 H9B H 0.1944 0.5362 0.2412 0.098 Uiso 1 1 calc R D 11 O10 O -0.0115(7) 0.7601(18) 0.1385(13) 0.118(11) Uiso 0.30 1 d P C 1 C10 C 0.17258(18) 0.4397(7) 0.1937(4) 0.086(3) Uani 1 1 d . . . O11 O 0.01013(11) 0.7163(4) -0.1345(2) 0.0859(17) Uani 1 1 d . . . C11 C 0.14749(19) 0.4369(7) 0.2036(4) 0.096(3) Uani 1 1 d . D . H11 H 0.1393 0.4867 0.2128 0.115 Uiso 1 1 calc R . . O12 O 0.03436(11) 0.6860(4) -0.2172(3) 0.0966(19) Uani 1 1 d . E . C12 C 0.1348(2) 0.3591(7) 0.1995(4) 0.092(3) Uani 1 1 d . . . O13 O 0.14691(17) 0.9106(5) -0.1620(4) 0.126(2) Uiso 1 1 d . . . C13 C 0.1466(2) 0.2901(6) 0.1843(4) 0.099(3) Uani 1 1 d . D . H13 H 0.1376 0.2382 0.1787 0.119 Uiso 1 1 calc R . . O14 O 0.18831(13) 0.8221(4) -0.1709(3) 0.0909(18) Uani 1 1 d . G . C14 C 0.1717(2) 0.2936(7) 0.1768(4) 0.087(3) Uani 1 1 d . . . O15 O 0.26112(12) 0.4904(4) -0.1322(3) 0.097(2) Uani 1 1 d . G . C15 C 0.18380(17) 0.3666(7) 0.1804(4) 0.081(3) Uani 1 1 d . D . H15 H 0.2008 0.3684 0.1736 0.097 Uiso 1 1 calc R . . O16 O 0.23083(12) 0.3958(4) -0.1647(4) 0.135(3) Uani 1 1 d . G . C16 C 0.1835(3) 0.2150(7) 0.1568(5) 0.096(3) Uani 1 1 d . D . O17 O 0.14347(11) 0.4625(4) -0.1428(3) 0.099(2) Uani 1 1 d . G . C17 C 0.10916(18) 0.3536(6) 0.2150(5) 0.109(4) Uani 1 1 d . D . H17A H 0.1001 0.3031 0.1954 0.130 Uiso 1 1 calc R . . H17B H 0.1115 0.3471 0.2598 0.130 Uiso 1 1 calc R . . O18 O 0.16003(13) 0.3965(4) -0.0310(4) 0.106(2) Uani 1 1 d . . . C18 C 0.07983(19) 0.4284(7) 0.1358(6) 0.081(3) Uani 1 1 d . . . C19 C 0.08272(17) 0.3726(6) 0.0907(6) 0.080(3) Uani 1 1 d . E . H19 H 0.0960 0.3315 0.1000 0.096 Uiso 1 1 calc R . . C20 C 0.0668(2) 0.3739(6) 0.0315(6) 0.081(3) Uani 1 1 d . . . C21 C 0.04758(18) 0.4340(6) 0.0172(5) 0.076(3) Uani 1 1 d . E . C22 C 0.04565(18) 0.4911(6) 0.0614(6) 0.080(3) Uani 1 1 d . . . H22 H 0.0325 0.5324 0.0522 0.096 Uiso 1 1 calc R E . C23 C 0.0617(2) 0.4922(7) 0.1189(6) 0.090(3) Uani 1 1 d . E . C24 C 0.0391(4) 0.6078(10) 0.1564(7) 0.160(6) Uani 0.80 1 d P E 2 H24A H 0.0385 0.6386 0.1183 0.240 Uiso 0.80 1 calc PR E 2 H24B H 0.0422 0.6472 0.1908 0.240 Uiso 0.80 1 calc PR E 2 H24C H 0.0227 0.5788 0.1543 0.240 Uiso 0.80 1 calc PR E 2 C25 C 0.02810(17) 0.4350(6) -0.0415(5) 0.083(3) Uani 1 1 d . . . H25A H 0.0279 0.3784 -0.0599 0.100 Uiso 1 1 calc R E . H25B H 0.0111 0.4437 -0.0318 0.100 Uiso 1 1 calc R . . C26 C 0.20008(15) 0.8310(5) 0.1671(4) 0.071(2) Uani 1 1 d . . . H26A H 0.2092 0.8808 0.1561 0.085 Uiso 1 1 calc R D . H26B H 0.2044 0.8253 0.2122 0.085 Uiso 1 1 calc R . . C27 C 0.17130(18) 0.8428(6) 0.1448(5) 0.073(2) Uani 1 1 d . A . C28 C 0.1561(2) 0.7969(6) 0.1776(4) 0.091(3) Uani 1 1 d . . . H28 H 0.1644 0.7673 0.2133 0.109 Uiso 1 1 calc R D . C29 C 0.1309(3) 0.7935(7) 0.1608(6) 0.102(3) Uani 1 1 d . A . C30 C 0.11903(18) 0.8386(8) 0.1106(6) 0.103(4) Uani 1 1 d . . . C31 C 0.1333(2) 0.8878(7) 0.0774(4) 0.102(3) Uani 1 1 d . A . H31 H 0.1247 0.9204 0.0435 0.123 Uiso 1 1 calc R . . C32 C 0.15998(18) 0.8882(6) 0.0946(5) 0.073(2) Uani 1 1 d . . . C33 C 0.1272(7) 0.696(2) 0.2494(17) 0.202(14) Uiso 0.50 1 d P F 1 H33A H 0.1220 0.7172 0.2857 0.303 Uiso 0.50 1 calc PR F 1 H33B H 0.1459 0.6994 0.2553 0.303 Uiso 0.50 1 calc PR F 1 H33C H 0.1218 0.6368 0.2429 0.303 Uiso 0.50 1 calc PR F 1 C34 C 0.0779(3) 0.8599(12) 0.0372(8) 0.069(5) Uiso 0.50 1 d P A 1 H34A H 0.0875 0.8294 0.0110 0.083 Uiso 0.50 1 calc PR A 1 H34B H 0.0746 0.9175 0.0205 0.083 Uiso 0.50 1 calc PR A 1 C35 C 0.05125(16) 0.8150(7) 0.0323(5) 0.108(3) Uani 1 1 d . . . C36 C 0.0369(2) 0.7834(6) -0.0232(4) 0.097(3) Uani 1 1 d . A . H36 H 0.0450 0.7752 -0.0564 0.116 Uiso 1 1 calc R . . C37 C 0.01120(17) 0.7640(5) -0.0305(5) 0.074(2) Uani 1 1 d . . . C38 C 0.00039(17) 0.7750(5) 0.0200(5) 0.077(3) Uani 1 1 d . A . H38 H -0.0173 0.7619 0.0159 0.092 Uiso 1 1 calc R . . C39 C 0.01386(18) 0.8035(5) 0.0748(4) 0.071(2) Uani 1 1 d . . . C40 C 0.03875(18) 0.8229(6) 0.0835(4) 0.100(3) Uani 1 1 d . A . H40 H 0.0481 0.8416 0.1222 0.120 Uiso 1 1 calc R . . C41 C -0.0010(3) 0.8127(6) 0.1260(6) 0.084(3) Uani 1 1 d . C . C42 C -0.00425(16) 0.7385(6) -0.0899(4) 0.086(3) Uani 1 1 d . A . H42A H -0.0149 0.6898 -0.0837 0.103 Uiso 1 1 calc R . . H42B H -0.0161 0.7851 -0.1063 0.103 Uiso 1 1 calc R . . C43 C 0.02160(15) 0.6390(6) -0.1293(4) 0.066(2) Uani 1 1 d . E . C44 C 0.01999(14) 0.5798(6) -0.0882(4) 0.073(2) Uani 1 1 d . . . H44 H 0.0112 0.5931 -0.0568 0.088 Uiso 1 1 calc R E . C45 C 0.03079(15) 0.4973(6) -0.0888(5) 0.082(3) Uani 1 1 d . E . C46 C 0.04298(15) 0.4804(6) -0.1379(5) 0.084(3) Uani 1 1 d . . . C47 C 0.04416(16) 0.5413(7) -0.1801(5) 0.086(3) Uani 1 1 d . E . H47 H 0.0520 0.5283 -0.2131 0.103 Uiso 1 1 calc R . . C48 C 0.03449(16) 0.6198(7) -0.1766(4) 0.083(3) Uani 1 1 d . . . C49 C 0.0436(2) 0.6675(7) -0.2705(5) 0.137(4) Uani 1 1 d . . . H49A H 0.0625 0.6662 -0.2601 0.206 Uiso 1 1 calc R E . H49B H 0.0378 0.7110 -0.3014 0.206 Uiso 1 1 calc R . . H49C H 0.0370 0.6127 -0.2867 0.206 Uiso 1 1 calc R . . C50 C 0.05511(17) 0.3964(6) -0.1421(4) 0.090(3) Uani 1 1 d . E . H50A H 0.0449 0.3533 -0.1260 0.108 Uiso 1 1 calc R . . H50B H 0.0540 0.3835 -0.1857 0.108 Uiso 1 1 calc R . . C51 C 0.17488(16) 0.9412(5) 0.0605(4) 0.081(3) Uani 1 1 d . A . H51A H 0.1921 0.9515 0.0868 0.097 Uiso 1 1 calc R . . H51B H 0.1662 0.9963 0.0522 0.097 Uiso 1 1 calc R . . C52 C 0.1783(2) 0.9035(6) -0.0009(5) 0.085(3) Uani 1 1 d . . . C53 C 0.1607(2) 0.9215(6) -0.0537(6) 0.088(3) Uani 1 1 d . A . H53 H 0.1458 0.9537 -0.0520 0.106 Uiso 1 1 calc R . . C54 C 0.1642(2) 0.8941(6) -0.1072(5) 0.087(3) Uani 1 1 d . A . C55 C 0.1850(2) 0.8473(6) -0.1135(5) 0.080(3) Uani 1 1 d . . . C56 C 0.20311(18) 0.8258(5) -0.0614(5) 0.067(2) Uani 1 1 d . A . H56 H 0.2171 0.7908 -0.0649 0.081 Uiso 1 1 calc R . . C57 C 0.20121(19) 0.8546(5) -0.0039(5) 0.073(2) Uani 1 1 d . A . C58 C 0.1271(4) 0.9563(15) -0.1615(10) 0.172(9) Uiso 0.60 1 d P G 1 H58A H 0.1226 0.9886 -0.1996 0.258 Uiso 0.60 1 calc PR G 1 H58B H 0.1309 0.9949 -0.1267 0.258 Uiso 0.60 1 calc PR G 1 H58C H 0.1126 0.9202 -0.1580 0.258 Uiso 0.60 1 calc PR G 1 C59 C 0.20805(18) 0.7656(5) -0.1773(4) 0.077(2) Uani 1 1 d . . . H59A H 0.2244 0.7846 -0.1508 0.092 Uiso 1 1 calc R G . H59B H 0.2101 0.7672 -0.2201 0.092 Uiso 1 1 calc R . . C60 C 0.20307(16) 0.6775(5) -0.1612(4) 0.071(2) Uani 1 1 d . G . C61 C 0.17963(18) 0.6516(5) -0.1513(3) 0.078(2) Uani 1 1 d . . . H61 H 0.1664 0.6917 -0.1518 0.093 Uiso 1 1 calc R G . C62 C 0.17524(16) 0.5673(6) -0.1404(4) 0.076(3) Uani 1 1 d . G . C63 C 0.19365(16) 0.5086(5) -0.1401(4) 0.074(2) Uani 1 1 d . . . H63 H 0.1901 0.4511 -0.1339 0.088 Uiso 1 1 calc R G . C64 C 0.21747(16) 0.5322(6) -0.1486(4) 0.077(3) Uani 1 1 d . G . C65 C 0.22208(16) 0.6149(6) -0.1588(4) 0.076(2) Uani 1 1 d . . . H65 H 0.2386 0.6308 -0.1643 0.091 Uiso 1 1 calc R G . C66 C 0.23711(19) 0.4682(6) -0.1492(4) 0.083(3) Uani 1 1 d . . . C67 C 0.14993(16) 0.5409(6) -0.1250(5) 0.092(3) Uani 1 1 d . . . H67A H 0.1515 0.5455 -0.0804 0.111 Uiso 1 1 calc R G . H67B H 0.1361 0.5797 -0.1453 0.111 Uiso 1 1 calc R . . C68 C 0.1257(2) 0.4276(6) -0.1133(5) 0.082(3) Uani 1 1 d . . . C69 C 0.10084(18) 0.4278(5) -0.1399(4) 0.083(3) Uani 1 1 d . E . H69 H 0.0951 0.4533 -0.1787 0.099 Uiso 1 1 calc R . . C70 C 0.08239(19) 0.3887(6) -0.1090(6) 0.082(3) Uani 1 1 d . . . C71 C 0.09012(18) 0.3532(6) -0.0540(6) 0.081(3) Uani 1 1 d . E . C72 C 0.11653(19) 0.3505(5) -0.0260(5) 0.099(3) Uani 1 1 d . . . H72 H 0.1224 0.3216 0.0115 0.119 Uiso 1 1 calc R E . C73 C 0.13463(17) 0.3934(6) -0.0563(6) 0.084(3) Uani 1 1 d . E . C74 C 0.1678(2) 0.3755(9) 0.0314(6) 0.145(5) Uani 1 1 d . . . H74A H 0.1559 0.4007 0.0540 0.217 Uiso 1 1 calc R . . H74B H 0.1852 0.3969 0.0476 0.217 Uiso 1 1 calc R . . H74C H 0.1677 0.3142 0.0360 0.217 Uiso 1 1 calc R . . C75 C 0.07276(16) 0.3124(5) -0.0175(4) 0.087(3) Uani 1 1 d . E . H75A H 0.0812 0.2613 0.0029 0.105 Uiso 1 1 calc R . . H75B H 0.0565 0.2952 -0.0453 0.105 Uiso 1 1 calc R . . O8A O 0.0939(2) 0.8168(8) 0.0990(6) 0.079(4) Uiso 0.50 1 d P A 2 C8A C 0.2182(6) 0.524(2) -0.0031(17) 0.094(13) Uiso 0.35 1 d P B 10 H8A1 H 0.2009 0.5441 -0.0223 0.141 Uiso 0.35 1 calc PR B 10 H8A2 H 0.2206 0.4670 -0.0172 0.141 Uiso 0.35 1 calc PR B 10 H8A3 H 0.2311 0.5615 -0.0142 0.141 Uiso 0.35 1 calc PR B 10 O9A O 0.0077(6) 0.8719(16) 0.1662(14) 0.090(12) Uiso 0.30 1 d P C 1 O10A O -0.02500(17) 0.7992(7) 0.1138(4) 0.082(3) Uani 0.70 1 d P C 2 C24A C 0.0603(14) 0.639(4) 0.133(3) 0.17(3) Uiso 0.20 1 d P E 3 H24D H 0.0701 0.6779 0.1631 0.248 Uiso 0.20 1 calc PR E 3 H24E H 0.0426 0.6589 0.1198 0.248 Uiso 0.20 1 calc PR E 3 H24F H 0.0683 0.6342 0.0980 0.248 Uiso 0.20 1 calc PR E 3 C33A C 0.1173(6) 0.677(2) 0.2057(15) 0.158(11) Uiso 0.50 1 d P F 2 H33D H 0.1229 0.6456 0.1735 0.237 Uiso 0.50 1 calc PR F 2 H33E H 0.1014 0.6531 0.2131 0.237 Uiso 0.50 1 calc PR F 2 H33F H 0.1307 0.6751 0.2433 0.237 Uiso 0.50 1 calc PR F 2 C34A C 0.0809(3) 0.8023(13) 0.0501(8) 0.078(5) Uiso 0.50 1 d P A 2 H34C H 0.0840 0.7427 0.0414 0.094 Uiso 0.50 1 calc PR A 2 H34D H 0.0881 0.8361 0.0207 0.094 Uiso 0.50 1 calc PR A 2 C58A C 0.1305(7) 0.863(2) -0.1867(15) 0.159(12) Uiso 0.40 1 d P G 2 H58D H 0.1188 0.8510 -0.1596 0.238 Uiso 0.40 1 calc PR G 2 H58E H 0.1385 0.8104 -0.1961 0.238 Uiso 0.40 1 calc PR G 2 H58F H 0.1208 0.8882 -0.2247 0.238 Uiso 0.40 1 calc PR G 2 N7S N 0.28672(18) 0.4493(3) -0.2211(3) 0.096(3) Uani 1 1 d G H -1 C8S C 0.31117(14) 0.4760(4) -0.2247(4) 0.113(4) Uani 1 1 d G H -1 H8S H 0.3255 0.4635 -0.1925 0.136 Uiso 1 1 calc R H -1 C9S C 0.31464(18) 0.5211(4) -0.2754(5) 0.137(5) Uani 1 1 d G H -1 H9S H 0.3313 0.5393 -0.2778 0.164 Uiso 1 1 calc R H -1 C10S C 0.2937(3) 0.5394(4) -0.3224(4) 0.135(5) Uani 1 1 d G H -1 H10S H 0.2960 0.5702 -0.3571 0.162 Uiso 1 1 calc R H -1 C11S C 0.2692(2) 0.5127(6) -0.3189(4) 0.154(5) Uani 1 1 d G H -1 H11S H 0.2549 0.5252 -0.3510 0.184 Uiso 1 1 calc R H -1 C12S C 0.26574(13) 0.4677(5) -0.2682(5) 0.120(4) Uani 1 1 d G H -1 H12S H 0.2490 0.4494 -0.2658 0.144 Uiso 1 1 calc R H -1 N13S N 0.2796(3) 0.3520(9) -0.0703(6) 0.025(4) Uiso 0.30 1 d PG H -2 C14S C 0.2843(5) 0.2690(8) -0.0518(10) 0.122(12) Uiso 0.30 1 d PG H -2 H14S H 0.2850 0.2265 -0.0811 0.147 Uiso 0.30 1 calc PR H -2 C15S C 0.2879(6) 0.2481(14) 0.0097(12) 0.23(3) Uiso 0.30 1 d PG H -2 H15S H 0.2911 0.1914 0.0223 0.277 Uiso 0.30 1 calc PR H -2 C16S C 0.2868(6) 0.310(2) 0.0526(7) 0.142(14) Uiso 0.30 1 d PG H -2 H16S H 0.2893 0.2960 0.0946 0.170 Uiso 0.30 1 calc PR H -2 C17S C 0.2822(6) 0.3932(19) 0.0341(8) 0.23(2) Uiso 0.30 1 d PG H -2 H17S H 0.2814 0.4357 0.0634 0.272 Uiso 0.30 1 calc PR H -2 C18S C 0.2786(4) 0.4141(10) -0.0274(10) 0.119(12) Uiso 0.30 1 d PG H -2 H18S H 0.2754 0.4708 -0.0400 0.143 Uiso 0.30 1 calc PR H -2 N19S N 0.2919(3) 0.3575(9) -0.0427(6) 0.028(4) Uiso 0.30 1 d PG H -1 C20S C 0.3144(3) 0.3678(12) 0.0017(9) 0.151(15) Uiso 0.30 1 d PG H -1 H20S H 0.3270 0.4071 -0.0044 0.182 Uiso 0.30 1 calc PR H -1 C21S C 0.3184(4) 0.3205(15) 0.0550(8) 0.085(9) Uiso 0.30 1 d PG H -1 H21S H 0.3338 0.3275 0.0854 0.102 Uiso 0.30 1 calc PR H -1 C22S C 0.3000(6) 0.2630(15) 0.0640(9) 0.21(2) Uiso 0.30 1 d PG H -1 H22S H 0.3028 0.2307 0.1005 0.253 Uiso 0.30 1 calc PR H -1 C23S C 0.2775(5) 0.2528(16) 0.0196(12) 0.161(19) Uiso 0.30 1 d PG H -1 H23S H 0.2649 0.2135 0.0257 0.193 Uiso 0.30 1 calc PR H -1 C24S C 0.2734(4) 0.3000(14) -0.0338(10) 0.28(4) Uiso 0.30 1 d PG H -1 H24S H 0.2581 0.2930 -0.0641 0.340 Uiso 0.30 1 calc PR H -1 N25S N 0.0056(4) 0.9671(6) 0.2610(9) 0.084(6) Uiso 0.35 1 d PG C -1 C26S C -0.0077(4) 1.0093(10) 0.2094(8) 0.129(7) Uiso 0.35 1 d PG C -1 H26S H -0.0167 0.9785 0.1751 0.155 Uiso 0.35 1 calc PR C -1 C27S C -0.0079(4) 1.0967(10) 0.2082(8) 0.186(10) Uiso 0.35 1 d PG C -1 H27S H -0.0170 1.1255 0.1729 0.223 Uiso 0.35 1 calc PR C -1 C28S C 0.0053(4) 1.1418(6) 0.2584(11) 0.063(6) Uiso 0.35 1 d PG C -1 H28S H 0.0052 1.2015 0.2575 0.076 Uiso 0.35 1 calc PR C -1 C29S C 0.0186(4) 1.0996(10) 0.3100(9) 0.186(10) Uiso 0.35 1 d PG C -1 H29S H 0.0276 1.1305 0.3443 0.223 Uiso 0.35 1 calc PR C -1 C30S C 0.0188(4) 1.0123(10) 0.3113(8) 0.129(7) Uiso 0.35 1 d PG C -1 H30S H 0.0279 0.9834 0.3465 0.155 Uiso 0.35 1 calc PR C -1 N31S N 0.0016(3) 0.7239(9) 0.2522(11) 0.109(9) Uiso 0.20 1 d PG C -1 C32S C 0.0177(5) 0.6845(11) 0.2197(11) 0.161(12) Uiso 0.20 1 d PG C -1 H32S H 0.0296 0.7168 0.2034 0.193 Uiso 0.20 1 calc PR C -1 C33S C 0.0163(6) 0.5980(12) 0.2110(17) 0.132(13) Uiso 0.20 1 d PG C -1 H33S H 0.0272 0.5711 0.1888 0.159 Uiso 0.20 1 calc PR C -1 C34S C -0.0012(7) 0.5509(10) 0.2348(19) 0.103(16) Uiso 0.20 1 d PG C -1 H34S H -0.0021 0.4918 0.2289 0.124 Uiso 0.20 1 calc PR C -1 C35S C -0.0172(6) 0.5903(15) 0.2673(19) 0.132(13) Uiso 0.20 1 d PG C -1 H35S H -0.0291 0.5581 0.2836 0.159 Uiso 0.20 1 calc PR C -1 C36S C -0.0158(5) 0.6768(15) 0.2760(17) 0.161(12) Uiso 0.20 1 d PG C -1 H36S H -0.0268 0.7037 0.2983 0.193 Uiso 0.20 1 calc PR C -1 O37S O 0.0310(3) 0.8089(7) 0.2782(6) 0.149(6) Uiso 0.50 1 d PG C -1 H37S H 0.0354 0.7587 0.2749 0.179 Uiso 0.50 1 calc PR C -1 C38S C 0.0507(3) 0.8521(9) 0.3072(7) 0.120(7) Uiso 0.50 1 d PG C -1 H38A H 0.0465 0.9121 0.3047 0.179 Uiso 0.50 1 calc PR C -1 H38B H 0.0654 0.8419 0.2885 0.179 Uiso 0.50 1 calc PR C -1 H38C H 0.0552 0.8347 0.3501 0.179 Uiso 0.50 1 calc PR C -1 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 0.1362(11) 0.0761(8) 0.1642(13) -0.0124(8) 0.1039(10) 0.0041(8) O1 0.096(4) 0.084(5) 0.109(5) 0.006(4) 0.052(4) 0.001(3) C1 0.075(6) 0.067(6) 0.081(6) -0.022(5) 0.038(6) -0.017(5) Cu2 0.1185(14) 0.1220(15) 0.0883(12) 0.000 0.0590(11) 0.000 O2 0.111(5) 0.077(4) 0.127(5) 0.031(4) 0.090(4) 0.022(4) C2 0.069(5) 0.045(5) 0.077(6) -0.015(5) 0.028(5) -0.009(4) O3 0.110(6) 0.126(6) 0.103(5) -0.022(4) 0.029(5) 0.041(5) C3 0.063(5) 0.071(6) 0.076(6) 0.014(5) 0.032(4) -0.007(5) O4 0.154(7) 0.078(5) 0.145(7) -0.009(5) 0.025(5) 0.018(5) C4 0.091(6) 0.055(6) 0.093(7) -0.003(6) 0.046(5) 0.014(5) O5 0.078(4) 0.128(6) 0.094(5) 0.024(5) 0.042(4) 0.014(4) C5 0.072(6) 0.091(8) 0.080(7) 0.010(6) 0.041(5) 0.019(5) O6 0.091(5) 0.122(6) 0.133(6) 0.026(5) 0.033(5) 0.032(5) C6 0.091(7) 0.095(8) 0.080(6) -0.010(6) 0.055(5) 0.001(6) O7 0.145(7) 0.150(8) 0.208(9) -0.004(7) 0.132(7) -0.020(6) C7 0.060(6) 0.079(7) 0.097(7) 0.001(6) 0.038(5) 0.004(5) C8 0.18(2) 0.080(11) 0.116(15) -0.016(10) 0.112(16) -0.012(13) O9 0.101(9) 0.132(12) 0.079(8) -0.006(9) 0.048(7) 0.003(9) C9 0.086(6) 0.085(7) 0.084(6) 0.012(5) 0.043(5) 0.025(5) C10 0.080(7) 0.095(8) 0.095(7) 0.016(6) 0.048(5) 0.023(6) O11 0.092(4) 0.097(5) 0.079(4) -0.009(3) 0.041(3) 0.015(4) C11 0.094(8) 0.094(8) 0.112(8) 0.042(6) 0.051(6) 0.039(6) O12 0.090(4) 0.128(6) 0.083(4) 0.012(4) 0.043(4) 0.019(4) C12 0.103(8) 0.078(7) 0.102(8) 0.027(6) 0.036(6) 0.028(7) C13 0.109(9) 0.076(7) 0.123(8) 0.008(6) 0.050(7) 0.000(7) O14 0.135(6) 0.063(4) 0.079(5) 0.008(3) 0.033(4) -0.012(4) C14 0.088(8) 0.073(7) 0.102(7) -0.001(6) 0.025(6) 0.015(6) O15 0.071(4) 0.089(4) 0.145(6) -0.046(4) 0.050(4) -0.017(4) C15 0.072(6) 0.082(7) 0.101(7) 0.001(6) 0.045(5) 0.019(6) O16 0.073(4) 0.084(5) 0.271(9) -0.071(6) 0.084(5) -0.023(4) C16 0.133(11) 0.064(7) 0.094(8) 0.011(6) 0.033(8) 0.010(8) O17 0.078(4) 0.080(4) 0.166(6) -0.023(4) 0.082(4) -0.020(4) C17 0.083(7) 0.105(8) 0.151(10) 0.066(7) 0.057(7) 0.024(6) O18 0.065(5) 0.124(5) 0.138(6) 0.011(5) 0.040(4) 0.002(4) C18 0.059(7) 0.095(8) 0.105(10) 0.016(8) 0.052(7) -0.002(6) C19 0.048(6) 0.089(8) 0.116(9) 0.034(7) 0.043(7) -0.001(5) C20 0.069(7) 0.067(7) 0.120(9) 0.015(6) 0.048(7) -0.009(6) C21 0.053(6) 0.078(7) 0.107(8) 0.017(7) 0.037(6) -0.003(6) C22 0.056(6) 0.080(7) 0.114(9) 0.002(7) 0.043(7) 0.010(5) C23 0.063(7) 0.104(9) 0.112(10) -0.007(8) 0.042(7) 0.002(7) C24 0.190(17) 0.136(14) 0.166(15) 0.039(12) 0.066(13) 0.046(13) C25 0.060(6) 0.083(7) 0.119(8) 0.017(6) 0.047(6) 0.009(5) C26 0.065(6) 0.082(6) 0.070(6) -0.027(5) 0.022(4) -0.007(5) C27 0.080(7) 0.072(6) 0.080(7) -0.024(6) 0.047(6) -0.010(5) C28 0.060(7) 0.118(8) 0.103(8) -0.007(6) 0.040(6) 0.006(6) C29 0.121(11) 0.109(9) 0.096(9) -0.012(7) 0.063(8) 0.004(8) C30 0.046(6) 0.154(11) 0.121(9) -0.048(9) 0.041(7) -0.022(7) C31 0.084(8) 0.140(9) 0.095(7) -0.016(6) 0.047(6) -0.001(7) C32 0.067(7) 0.082(6) 0.082(7) -0.019(6) 0.040(6) -0.007(5) C35 0.044(6) 0.178(11) 0.113(9) -0.026(8) 0.042(6) -0.005(6) C36 0.085(8) 0.143(9) 0.070(7) -0.004(6) 0.033(6) 0.019(7) C37 0.049(6) 0.094(7) 0.090(7) 0.005(6) 0.038(6) 0.012(5) C38 0.075(6) 0.075(6) 0.094(7) 0.012(6) 0.047(6) 0.012(5) C39 0.074(7) 0.081(6) 0.068(6) -0.012(5) 0.039(5) -0.006(5) C40 0.069(7) 0.160(10) 0.079(7) -0.032(6) 0.035(5) -0.026(6) C41 0.131(11) 0.043(6) 0.094(9) -0.010(6) 0.061(9) -0.024(6) C42 0.071(6) 0.110(7) 0.082(7) -0.006(6) 0.028(6) 0.031(5) C43 0.068(6) 0.066(6) 0.070(6) -0.003(5) 0.027(5) 0.013(5) C44 0.040(5) 0.103(8) 0.080(6) -0.001(6) 0.021(4) 0.005(5) C45 0.050(5) 0.080(7) 0.116(8) -0.006(6) 0.019(5) 0.002(5) C46 0.061(6) 0.086(7) 0.116(8) -0.019(7) 0.045(6) 0.011(5) C47 0.071(6) 0.087(7) 0.112(8) 0.008(7) 0.048(6) 0.025(6) C48 0.051(6) 0.120(9) 0.081(7) 0.007(7) 0.022(5) -0.010(6) C49 0.123(9) 0.186(12) 0.131(9) 0.021(8) 0.089(8) 0.048(8) C50 0.068(7) 0.100(7) 0.118(8) -0.011(6) 0.051(6) 0.001(6) C51 0.095(7) 0.067(6) 0.095(7) -0.012(5) 0.054(6) -0.001(5) C52 0.084(7) 0.070(6) 0.109(9) 0.032(6) 0.038(7) -0.009(6) C53 0.104(8) 0.073(7) 0.102(9) 0.024(7) 0.054(8) 0.008(6) C54 0.085(7) 0.083(7) 0.091(9) 0.024(6) 0.015(7) -0.001(6) C55 0.100(8) 0.066(6) 0.077(8) 0.018(6) 0.023(7) 0.003(6) C56 0.085(7) 0.042(5) 0.083(7) -0.005(5) 0.037(6) -0.013(5) C57 0.090(7) 0.049(5) 0.092(8) 0.003(5) 0.044(6) -0.004(5) C59 0.102(7) 0.070(6) 0.067(6) 0.008(5) 0.036(5) 0.000(6) C60 0.074(6) 0.073(6) 0.081(6) -0.014(5) 0.051(5) -0.020(5) C61 0.111(7) 0.060(6) 0.075(6) -0.005(5) 0.048(5) 0.000(5) C62 0.084(6) 0.066(6) 0.099(7) -0.007(5) 0.063(5) -0.015(5) C63 0.073(6) 0.051(5) 0.110(7) -0.015(5) 0.049(5) 0.001(5) C64 0.076(6) 0.060(6) 0.116(7) -0.030(5) 0.065(5) -0.017(5) C65 0.073(6) 0.081(7) 0.088(6) -0.015(5) 0.050(5) -0.017(6) C66 0.069(7) 0.067(7) 0.125(8) -0.046(6) 0.045(6) -0.025(6) C67 0.074(6) 0.077(7) 0.145(9) -0.014(6) 0.067(6) 0.008(5) C68 0.061(7) 0.075(6) 0.121(9) 0.025(6) 0.041(7) 0.014(5) C69 0.057(6) 0.085(6) 0.120(8) -0.005(6) 0.050(6) 0.010(5) C70 0.067(7) 0.064(6) 0.126(9) -0.009(6) 0.045(7) 0.002(5) C71 0.047(6) 0.064(6) 0.145(10) -0.009(6) 0.046(6) -0.005(5) C72 0.088(8) 0.068(6) 0.162(9) 0.003(6) 0.071(7) 0.010(6) C73 0.033(6) 0.075(6) 0.153(10) 0.002(7) 0.041(6) 0.001(5) C74 0.087(8) 0.227(15) 0.124(10) 0.021(10) 0.028(7) -0.024(8) C75 0.065(6) 0.076(6) 0.133(8) 0.014(6) 0.046(6) -0.010(5) O10A 0.053(6) 0.115(8) 0.090(7) -0.018(6) 0.044(5) -0.022(6) N7S 0.108(6) 0.067(5) 0.137(7) -0.021(5) 0.078(6) 0.009(5) C8S 0.132(10) 0.065(6) 0.176(11) -0.005(7) 0.104(8) 0.013(6) C9S 0.198(14) 0.084(8) 0.162(12) -0.016(8) 0.114(12) -0.020(9) C10S 0.184(14) 0.100(9) 0.138(12) -0.008(8) 0.071(11) -0.028(10) C11S 0.207(17) 0.143(12) 0.111(10) 0.017(8) 0.034(10) -0.048(11) C12S 0.097(9) 0.104(9) 0.167(12) -0.035(9) 0.046(10) -0.006(7) _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 N13S 1.834(13) . ? Cu1 O15 1.937(5) . ? Cu1 O3 1.963(6) 7 ? Cu1 N7S 1.987(6) . ? Cu1 N19S 2.311(14) . ? O1 C8A 1.38(4) . ? O1 C4 1.402(9) . ? O1 C8 1.408(13) . ? C1 C2 1.476(10) . ? C1 C57 1.505(11) . ? Cu2 O37S 1.744(15) 2 ? Cu2 N25S 1.936(11) . ? Cu2 N25S 1.936(11) 2 ? Cu2 O9 1.937(11) 2 ? Cu2 O9 1.937(11) . ? Cu2 N31S 1.966(15) 2 ? Cu2 N31S 1.966(15) . ? Cu2 O9A 2.05(3) 2 ? Cu2 O9A 2.05(3) . ? O2 C5 1.360(10) . ? O2 C9 1.462(8) . ? C2 C3 1.368(10) . ? C2 C7 1.407(10) . ? O3 C16 1.316(12) . ? O3 Cu1 1.963(6) 7 ? C3 C4 1.360(10) . ? O4 C16 1.228(11) . ? C4 C5 1.423(10) . ? O5 C18 1.376(11) . ? O5 C17 1.445(10) . ? C5 C6 1.344(11) . ? O6 C23 1.359(11) . ? O6 C24 1.472(15) . ? O6 C24A 1.64(7) . ? C6 C7 1.384(11) . ? O7 C33A 1.24(3) . ? O7 C29 1.408(12) . ? O7 C33 1.65(3) . ? C7 C26 1.508(10) . ? O8 C34 1.096(16) . ? O8 C30 1.587(17) . ? O9 C41 1.253(14) . ? C9 C10 1.507(12) . ? O10 C41 1.08(3) . ? C10 C15 1.371(11) . ? C10 C11 1.404(11) . ? O11 C43 1.368(9) . ? O11 C42 1.434(8) . ? C11 C12 1.405(12) . ? O12 C48 1.391(10) . ? O12 C49 1.422(9) . ? C12 C13 1.348(12) . ? C12 C17 1.484(12) . ? O13 C58A 1.20(3) . ? O13 C58 1.28(2) . ? O13 C54 1.390(11) . ? C13 C14 1.385(12) . ? O14 C55 1.397(10) . ? O14 C59 1.415(9) . ? C14 C15 1.322(11) . ? C14 C16 1.514(13) . ? O15 C66 1.302(9) . ? O16 C66 1.229(9) . ? O17 C67 1.332(9) . ? O17 C68 1.387(9) . ? O18 C73 1.349(10) . ? O18 C74 1.410(11) . ? C18 C19 1.380(12) . ? C18 C23 1.396(13) . ? C19 C20 1.411(12) . ? C20 C21 1.388(12) . ? C20 C75 1.556(12) . ? C21 C22 1.365(11) . ? C21 C25 1.487(12) . ? C22 C23 1.383(13) . ? C25 C45 1.482(11) . ? C26 C27 1.517(11) . ? C27 C32 1.362(11) . ? C27 C28 1.413(11) . ? C28 C29 1.315(13) . ? C29 C30 1.367(13) . ? C30 O8A 1.354(14) . ? C30 C31 1.414(14) . ? C31 C32 1.388(12) . ? C32 C51 1.482(11) . ? C34 C35 1.571(18) . ? C35 C36 1.405(12) . ? C35 C40 1.454(11) . ? C35 C34A 1.555(18) . ? C36 C37 1.379(11) . ? C37 C38 1.390(11) . ? C37 C42 1.461(11) . ? C38 C39 1.359(11) . ? C39 C40 1.334(11) . ? C39 C41 1.542(11) . ? C41 O10A 1.265(14) . ? C41 O9A 1.32(3) . ? C43 C44 1.334(10) . ? C43 C48 1.419(11) . ? C44 C45 1.435(11) . ? C45 C46 1.424(11) . ? C46 C47 1.366(11) . ? C46 C50 1.497(11) . ? C47 C48 1.360(12) . ? C50 C70 1.486(12) . ? C51 C52 1.551(12) . ? C52 C53 1.371(12) . ? C52 C57 1.463(12) . ? C53 C54 1.329(12) . ? C54 C55 1.368(12) . ? C55 C56 1.387(11) . ? C56 C57 1.393(10) . ? C59 C60 1.485(10) . ? C60 C61 1.380(10) . ? C60 C65 1.413(11) . ? C61 C62 1.392(10) . ? C62 C63 1.354(10) . ? C62 C67 1.524(10) . ? C63 C64 1.378(10) . ? C64 C65 1.367(10) . ? C64 C66 1.463(11) . ? C68 C69 1.327(11) . ? C68 C73 1.376(12) . ? C69 C70 1.462(11) . ? C70 C71 1.338(12) . ? C71 C72 1.410(12) . ? C71 C75 1.511(11) . ? C72 C73 1.466(12) . ? O8A C34A 1.186(17) . ? N7S C8S 1.3900 . ? N7S C12S 1.3900 . ? C8S C9S 1.3900 . ? C9S C10S 1.3900 . ? C10S C11S 1.3900 . ? C11S C12S 1.3900 . ? N13S C14S 1.3900 . ? N13S C18S 1.3900 . ? C14S C15S 1.3900 . ? C15S C16S 1.3900 . ? C16S C17S 1.3900 . ? C17S C18S 1.3900 . ? N19S C20S 1.3900 . ? N19S C24S 1.3900 . ? C20S C21S 1.3900 . ? C21S C22S 1.3900 . ? C22S C23S 1.3900 . ? C23S C24S 1.3900 . ? N25S C26S 1.3900 . ? N25S C30S 1.3900 . ? C26S C27S 1.3900 . ? C27S C28S 1.3900 . ? C28S C29S 1.3900 . ? C29S C30S 1.3900 . ? N31S C32S 1.3900 . ? N31S C36S 1.3900 . ? C32S C33S 1.3900 . ? C33S C34S 1.3900 . ? C34S C35S 1.3900 . ? C35S C36S 1.3900 . ? O37S C38S 1.3068 . ? 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 N13S Cu1 O15 90.3(5) . . ? N13S Cu1 O3 90.9(5) . 7 ? O15 Cu1 O3 160.0(3) . 7 ? N13S Cu1 N7S 174.8(5) . . ? O15 Cu1 N7S 88.4(3) . . ? O3 Cu1 N7S 92.1(3) 7 . ? N13S Cu1 N19S 17.9(5) . . ? O15 Cu1 N19S 94.2(4) . . ? O3 Cu1 N19S 93.1(4) 7 . ? N7S Cu1 N19S 157.3(5) . . ? C8A O1 C4 113.3(16) . . ? C4 O1 C8 116.2(8) . . ? C2 C1 C57 115.9(7) . . ? O37S Cu2 N25S 119.9(11) 2 . ? O37S Cu2 N25S 101.1(10) 2 2 ? N25S Cu2 N25S 20.4(12) . 2 ? O37S Cu2 O9 76.5(19) 2 2 ? N25S Cu2 O9 96.3(8) . 2 ? N25S Cu2 O9 100.2(8) 2 2 ? O37S Cu2 O9 97.5(19) 2 . ? N25S Cu2 O9 100.2(8) . . ? N25S Cu2 O9 96.3(8) 2 . ? O9 Cu2 O9 163.2(10) 2 . ? O37S Cu2 N31S 66.8(10) 2 2 ? N25S Cu2 N31S 172.4(8) . 2 ? N25S Cu2 N31S 167.2(8) 2 2 ? O9 Cu2 N31S 81.5(9) 2 2 ? O9 Cu2 N31S 81.6(9) . 2 ? O37S Cu2 N31S 72.0(8) 2 . ? N25S Cu2 N31S 167.2(8) . . ? N25S Cu2 N31S 172.4(8) 2 . ? O9 Cu2 N31S 81.6(9) 2 . ? O9 Cu2 N31S 81.5(9) . . ? N31S Cu2 N31S 5.3(10) 2 . ? O37S Cu2 O9A 92(2) 2 2 ? N25S Cu2 O9A 75.7(10) . 2 ? N25S Cu2 O9A 82.7(10) 2 2 ? O9 Cu2 O9A 21.5(8) 2 2 ? O9 Cu2 O9A 170.5(11) . 2 ? N31S Cu2 O9A 101.3(11) 2 2 ? N31S Cu2 O9A 100.6(11) . 2 ? O37S Cu2 O9A 96(2) 2 . ? N25S Cu2 O9A 82.7(10) . . ? N25S Cu2 O9A 75.7(10) 2 . ? O9 Cu2 O9A 170.5(11) 2 . ? O9 Cu2 O9A 21.5(8) . . ? N31S Cu2 O9A 100.6(11) 2 . ? N31S Cu2 O9A 101.3(11) . . ? O9A Cu2 O9A 158.1(15) 2 . ? C5 O2 C9 114.0(6) . . ? C3 C2 C7 117.4(7) . . ? C3 C2 C1 118.2(7) . . ? C7 C2 C1 124.4(7) . . ? C16 O3 Cu1 103.0(7) . 7 ? C4 C3 C2 124.0(7) . . ? C3 C4 O1 126.7(8) . . ? C3 C4 C5 119.0(8) . . ? O1 C4 C5 114.3(8) . . ? C18 O5 C17 117.2(8) . . ? C6 C5 O2 127.1(8) . . ? C6 C5 C4 116.6(9) . . ? O2 C5 C4 116.2(8) . . ? C23 O6 C24 119.6(10) . . ? C23 O6 C24A 103(3) . . ? C24 O6 C24A 54(3) . . ? C5 C6 C7 125.0(8) . . ? C33A O7 C29 120.0(17) . . ? C29 O7 C33 114.1(16) . . ? C6 C7 C2 117.9(8) . . ? C6 C7 C26 118.3(8) . . ? C2 C7 C26 123.3(8) . . ? C34 O8 C30 132.2(14) . . ? C41 O9 Cu2 123.2(9) . . ? O2 C9 C10 105.9(7) . . ? C15 C10 C11 118.9(10) . . ? C15 C10 C9 125.3(8) . . ? C11 C10 C9 115.7(9) . . ? C43 O11 C42 117.4(6) . . ? C10 C11 C12 118.8(9) . . ? C48 O12 C49 116.2(8) . . ? C13 C12 C11 119.2(9) . . ? C13 C12 C17 121.2(10) . . ? C11 C12 C17 119.6(9) . . ? C58A O13 C58 81.0(19) . . ? C58A O13 C54 124.3(18) . . ? C58 O13 C54 119.2(14) . . ? C12 C13 C14 121.1(10) . . ? C55 O14 C59 121.6(7) . . ? C15 C14 C13 120.0(9) . . ? C15 C14 C16 121.0(10) . . ? C13 C14 C16 118.6(11) . . ? C66 O15 Cu1 107.7(5) . . ? C14 C15 C10 121.9(9) . . ? O4 C16 O3 124.1(11) . . ? O4 C16 C14 123.1(12) . . ? O3 C16 C14 112.8(11) . . ? C67 O17 C68 113.1(7) . . ? O5 C17 C12 112.1(7) . . ? C73 O18 C74 117.3(8) . . ? O5 C18 C19 125.4(10) . . ? O5 C18 C23 117.7(11) . . ? C19 C18 C23 116.9(11) . . ? C18 C19 C20 122.7(10) . . ? C21 C20 C19 119.3(10) . . ? C21 C20 C75 121.7(11) . . ? C19 C20 C75 118.8(10) . . ? C22 C21 C20 117.4(10) . . ? C22 C21 C25 119.1(10) . . ? C20 C21 C25 123.3(11) . . ? C21 C22 C23 123.8(10) . . ? O6 C23 C22 126.1(11) . . ? O6 C23 C18 113.9(12) . . ? C22 C23 C18 119.6(11) . . ? C45 C25 C21 118.9(7) . . ? C7 C26 C27 109.5(6) . . ? C32 C27 C28 120.3(9) . . ? C32 C27 C26 124.8(8) . . ? C28 C27 C26 114.8(10) . . ? C29 C28 C27 122.6(10) . . ? C28 C29 C30 118.2(10) . . ? C28 C29 O7 128.7(13) . . ? C30 C29 O7 113.0(12) . . ? O8A C30 C29 106.4(13) . . ? O8A C30 C31 131.8(14) . . ? C29 C30 C31 121.3(10) . . ? C29 C30 O8 133.5(11) . . ? C31 C30 O8 104.3(12) . . ? C32 C31 C30 119.6(10) . . ? C27 C32 C31 117.9(9) . . ? C27 C32 C51 122.6(9) . . ? C31 C32 C51 119.4(10) . . ? O8 C34 C35 115.5(15) . . ? C36 C35 C40 118.5(8) . . ? C36 C35 C34A 120.3(10) . . ? C40 C35 C34A 115.2(11) . . ? C36 C35 C34 122.1(10) . . ? C40 C35 C34 118.1(11) . . ? C37 C36 C35 121.2(8) . . ? C36 C37 C38 117.1(9) . . ? C36 C37 C42 121.0(8) . . ? C38 C37 C42 121.8(8) . . ? C39 C38 C37 123.3(8) . . ? C40 C39 C38 121.3(8) . . ? C40 C39 C41 121.9(10) . . ? C38 C39 C41 116.8(9) . . ? C39 C40 C35 118.6(8) . . ? O10 C41 O9 100(2) . . ? O10 C41 O10A 50.8(17) . . ? O9 C41 O10A 127.6(10) . . ? O10 C41 O9A 120(2) . . ? O10A C41 O9A 117.4(16) . . ? O10 C41 C39 120.1(17) . . ? O9 C41 C39 113.4(12) . . ? O10A C41 C39 118.9(11) . . ? O9A C41 C39 114.5(15) . . ? O11 C42 C37 115.2(7) . . ? C44 C43 O11 126.7(8) . . ? C44 C43 C48 118.8(9) . . ? O11 C43 C48 114.2(9) . . ? C43 C44 C45 123.5(8) . . ? C46 C45 C44 115.6(9) . . ? C46 C45 C25 124.1(9) . . ? C44 C45 C25 120.2(8) . . ? C47 C46 C45 120.1(8) . . ? C47 C46 C50 120.2(8) . . ? C45 C46 C50 119.7(10) . . ? C48 C47 C46 122.4(9) . . ? C47 C48 O12 127.2(9) . . ? C47 C48 C43 119.5(9) . . ? O12 C48 C43 113.2(9) . . ? C70 C50 C46 115.5(8) . . ? C32 C51 C52 114.9(7) . . ? C53 C52 C57 119.5(9) . . ? C53 C52 C51 119.6(9) . . ? C57 C52 C51 120.7(10) . . ? C54 C53 C52 120.3(10) . . ? C53 C54 C55 123.5(10) . . ? C53 C54 O13 122.6(11) . . ? C55 C54 O13 113.9(11) . . ? C54 C55 C56 118.4(9) . . ? C54 C55 O14 121.5(10) . . ? C56 C55 O14 120.1(9) . . ? C55 C56 C57 121.4(9) . . ? C56 C57 C52 116.7(9) . . ? C56 C57 C1 119.6(8) . . ? C52 C57 C1 123.7(9) . . ? O14 C59 C60 113.5(7) . . ? C61 C60 C65 116.8(8) . . ? C61 C60 C59 122.5(8) . . ? C65 C60 C59 120.6(7) . . ? C60 C61 C62 120.6(8) . . ? C63 C62 C61 121.1(7) . . ? C63 C62 C67 119.0(8) . . ? C61 C62 C67 119.8(8) . . ? C62 C63 C64 120.0(8) . . ? C65 C64 C63 119.4(8) . . ? C65 C64 C66 120.9(8) . . ? C63 C64 C66 119.7(8) . . ? C64 C65 C60 122.1(7) . . ? O16 C66 O15 121.8(8) . . ? O16 C66 C64 120.3(8) . . ? O15 C66 C64 117.9(8) . . ? O17 C67 C62 111.9(7) . . ? C69 C68 C73 121.8(9) . . ? C69 C68 O17 120.3(10) . . ? C73 C68 O17 117.9(9) . . ? C68 C69 C70 119.6(9) . . ? C71 C70 C69 121.0(9) . . ? C71 C70 C50 124.4(9) . . ? C69 C70 C50 114.5(10) . . ? C70 C71 C72 119.9(9) . . ? C70 C71 C75 125.5(9) . . ? C72 C71 C75 114.6(10) . . ? C71 C72 C73 118.3(10) . . ? O18 C73 C68 119.2(9) . . ? O18 C73 C72 121.6(11) . . ? C68 C73 C72 119.1(9) . . ? C71 C75 C20 110.9(7) . . ? C34A O8A C30 125.4(14) . . ? C41 O9A Cu2 112.3(17) . . ? O8A C34A C35 124.4(15) . . ? C8S N7S C12S 120.0 . . ? C8S N7S Cu1 118.9(6) . . ? C12S N7S Cu1 120.9(6) . . ? N7S C8S C9S 120.0 . . ? C10S C9S C8S 120.0 . . ? C9S C10S C11S 120.0 . . ? C10S C11S C12S 120.0 . . ? C11S C12S N7S 120.0 . . ? C14S N13S C18S 120.0 . . ? C14S N13S Cu1 125.7(11) . . ? C18S N13S Cu1 112.7(11) . . ? N13S C14S C15S 120.0 . . ? C14S C15S C16S 120.0 . . ? C17S C16S C15S 120.0 . . ? C16S C17S C18S 120.0 . . ? C17S C18S N13S 120.0 . . ? C20S N19S C24S 120.0 . . ? C20S N19S Cu1 130.8(10) . . ? C24S N19S Cu1 107.4(10) . . ? C21S C20S N19S 120.0 . . ? C20S C21S C22S 120.0 . . ? C23S C22S C21S 120.0 . . ? C22S C23S C24S 120.0 . . ? C23S C24S N19S 120.0 . . ? C26S N25S C30S 120.0 . . ? C26S N25S Cu2 109.5(10) . . ? C30S N25S Cu2 130.4(11) . . ? N25S C26S C27S 120.0 . . ? C28S C27S C26S 120.0 . . ? C27S C28S C29S 120.0 . . ? C28S C29S C30S 120.0 . . ? C29S C30S N25S 120.0 . . ? C32S N31S C36S 120.0 . . ? C32S N31S Cu2 117.8(10) . . ? C36S N31S Cu2 121.3(9) . . ? C33S C32S N31S 120.0 . . ? C32S C33S C34S 120.0 . . ? C35S C34S C33S 120.0 . . ? C36S C35S C34S 120.0 . . ? C35S C36S N31S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.961 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.082 #===END