# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gong, Shuling' _publ_contact_author_email gongsl@whu.edu.cn _publ_section_title ; Pendant orientation and its influence on the formation of hydrogen-bonded thiacalixarene nanotubes ; loop_ _publ_author_name 'Yan Li' 'Weiping Yang' 'Yuanyin Chen' 'Shuling Gong' # Attachment '- data 1-5.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 760511' #TrackingRef '- data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H56 O12 S4, 4 (C2H5OH), 2 (H2O)' _chemical_formula_sum 'C56 H84 O18 S4' _chemical_formula_weight 1173.47 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5110(13) _cell_length_b 16.749(2) _cell_length_c 18.137(2) _cell_angle_alpha 88.538(2) _cell_angle_beta 77.585(2) _cell_angle_gamma 87.949(2) _cell_volume 3115.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4243 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9575 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17971 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.1356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10863 _reflns_number_gt 7702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+1.5362P] 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 10863 _refine_ls_number_parameters 741 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2330 _refine_ls_wR_factor_gt 0.2157 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 C1 C 0.4579(4) 0.8254(3) 0.2757(2) 0.0178(9) Uani 1 1 d . . . C2 C 0.4305(4) 0.7453(3) 0.2892(2) 0.0210(10) Uani 1 1 d . . . H2 H 0.3973 0.7170 0.2530 0.025 Uiso 1 1 calc R . . C3 C 0.4500(4) 0.7047(3) 0.3545(2) 0.0242(10) Uani 1 1 d . . . C4 C 0.5026(4) 0.7476(2) 0.4049(2) 0.0185(9) Uani 1 1 d . . . H4 H 0.5201 0.7213 0.4488 0.022 Uiso 1 1 calc R . . C5 C 0.5303(4) 0.8284(2) 0.3926(2) 0.0173(9) Uani 1 1 d . . . C6 C 0.5037(4) 0.8682(2) 0.3295(2) 0.0175(9) Uani 1 1 d . . . C7 C 0.4154(5) 0.6172(3) 0.3680(3) 0.0307(11) Uani 1 1 d . . . C8 C 0.4508(7) 0.5828(3) 0.4391(4) 0.0602(19) Uani 1 1 d . . . H8A H 0.5437 0.5897 0.4367 0.090 Uiso 1 1 calc R . . H8B H 0.4322 0.5257 0.4435 0.090 Uiso 1 1 calc R . . H8C H 0.3993 0.6105 0.4831 0.090 Uiso 1 1 calc R . . C9 C 0.4881(7) 0.5677(3) 0.3004(4) 0.0625(19) Uani 1 1 d . . . H9A H 0.5822 0.5742 0.2938 0.094 Uiso 1 1 calc R . . H9B H 0.4602 0.5862 0.2545 0.094 Uiso 1 1 calc R . . H9C H 0.4682 0.5111 0.3098 0.094 Uiso 1 1 calc R . . C10 C 0.2680(6) 0.6104(4) 0.3741(4) 0.064(2) Uani 1 1 d . . . H10A H 0.2428 0.5554 0.3878 0.095 Uiso 1 1 calc R . . H10B H 0.2466 0.6251 0.3254 0.095 Uiso 1 1 calc R . . H10C H 0.2207 0.6466 0.4130 0.095 Uiso 1 1 calc R . . C11 C 0.4029(4) 0.9931(3) 0.3493(3) 0.0253(10) Uani 1 1 d . . . H11A H 0.3764 0.9833 0.4045 0.030 Uiso 1 1 calc R . . H11B H 0.3332 0.9744 0.3255 0.030 Uiso 1 1 calc R . . C12 C 0.4211(4) 1.0814(3) 0.3333(2) 0.0223(10) Uani 1 1 d . . . C13 C 0.7293(4) 0.9242(3) 0.4210(2) 0.0175(9) Uani 1 1 d . . . C14 C 0.8366(4) 0.8788(3) 0.3836(2) 0.0180(9) Uani 1 1 d . . . C15 C 0.9523(4) 0.9168(3) 0.3534(2) 0.0186(9) Uani 1 1 d . . . C16 C 0.9622(4) 0.9983(3) 0.3656(2) 0.0205(10) Uani 1 1 d . . . H16 H 1.0426 1.0233 0.3462 0.025 Uiso 1 1 calc R . . C17 C 0.8574(4) 1.0437(3) 0.4054(2) 0.0184(9) Uani 1 1 d . . . C18 C 0.7400(4) 1.0047(3) 0.4310(2) 0.0183(9) Uani 1 1 d . . . H18 H 0.6654 1.0348 0.4559 0.022 Uiso 1 1 calc R . . C19 C 0.8654(4) 1.1330(3) 0.4208(2) 0.0226(10) Uani 1 1 d . . . C20 C 0.8286(5) 1.1448(3) 0.5062(3) 0.0324(12) Uani 1 1 d . . . H20A H 0.8894 1.1136 0.5304 0.049 Uiso 1 1 calc R . . H20B H 0.7398 1.1269 0.5258 0.049 Uiso 1 1 calc R . . H20C H 0.8332 1.2016 0.5170 0.049 Uiso 1 1 calc R . . C21 C 0.7691(5) 1.1816(3) 0.3834(3) 0.0355(12) Uani 1 1 d . . . H21A H 0.7705 1.2381 0.3960 0.053 Uiso 1 1 calc R . . H21B H 0.6810 1.1619 0.4018 0.053 Uiso 1 1 calc R . . H21C H 0.7941 1.1759 0.3285 0.053 Uiso 1 1 calc R . . C22 C 1.0020(5) 1.1638(3) 0.3918(3) 0.0365(13) Uani 1 1 d . . . H22A H 1.0635 1.1336 0.4163 0.055 Uiso 1 1 calc R . . H22B H 1.0030 1.2206 0.4033 0.055 Uiso 1 1 calc R . . H22C H 1.0274 1.1569 0.3370 0.055 Uiso 1 1 calc R . . C23 C 0.8638(5) 0.7526(3) 0.4372(3) 0.0313(11) Uani 1 1 d . . . H23A H 0.8016 0.7656 0.4849 0.038 Uiso 1 1 calc R . . H23B H 0.9516 0.7678 0.4423 0.038 Uiso 1 1 calc R . . C24 C 0.8645(6) 0.6654(3) 0.4246(3) 0.0418(14) Uani 1 1 d . . . C25 C 1.0528(4) 0.8199(3) 0.2278(2) 0.0174(9) Uani 1 1 d . . . C26 C 1.0812(4) 0.7396(3) 0.2149(2) 0.0221(10) Uani 1 1 d . . . H26 H 1.1141 0.7082 0.2514 0.027 Uiso 1 1 calc R . . C27 C 1.0629(4) 0.7030(3) 0.1497(2) 0.0241(10) Uani 1 1 d . . . C28 C 1.0096(4) 0.7496(3) 0.0993(2) 0.0214(10) Uani 1 1 d . . . H28 H 0.9931 0.7256 0.0555 0.026 Uiso 1 1 calc R . . C29 C 0.9796(4) 0.8299(3) 0.1106(2) 0.0180(9) Uani 1 1 d . . . C30 C 1.0063(4) 0.8672(2) 0.1742(2) 0.0178(9) Uani 1 1 d . . . C31 C 1.0996(5) 0.6144(3) 0.1365(3) 0.0345(12) Uani 1 1 d . . . C32 C 1.0213(9) 0.5642(4) 0.2018(4) 0.076(2) Uani 1 1 d . . . H32A H 1.0434 0.5791 0.2494 0.114 Uiso 1 1 calc R . . H32B H 1.0428 0.5074 0.1928 0.114 Uiso 1 1 calc R . . H32C H 0.9279 0.5742 0.2050 0.114 Uiso 1 1 calc R . . C33 C 1.2467(7) 0.6017(4) 0.1317(4) 0.064(2) Uani 1 1 d . . . H33A H 1.2951 0.6294 0.0867 0.096 Uiso 1 1 calc R . . H33B H 1.2693 0.5445 0.1287 0.096 Uiso 1 1 calc R . . H33C H 1.2693 0.6233 0.1768 0.096 Uiso 1 1 calc R . . C34 C 1.0706(7) 0.5854(3) 0.0636(3) 0.0513(16) Uani 1 1 d . . . H34A H 0.9766 0.5905 0.0659 0.077 Uiso 1 1 calc R . . H34B H 1.0993 0.5293 0.0566 0.077 Uiso 1 1 calc R . . H34C H 1.1171 0.6177 0.0211 0.077 Uiso 1 1 calc R . . C35 C 1.1020(4) 0.9903(3) 0.1535(3) 0.0277(11) Uani 1 1 d . . . H35A H 1.1280 0.9833 0.0983 0.033 Uiso 1 1 calc R . . H35B H 1.1731 0.9676 0.1764 0.033 Uiso 1 1 calc R . . C36 C 1.0837(5) 1.0775(3) 0.1701(3) 0.0268(11) Uani 1 1 d . . . C37 C 0.7754(4) 0.9337(3) 0.0823(2) 0.0180(9) Uani 1 1 d . . . C38 C 0.6720(4) 0.8885(3) 0.1210(2) 0.0187(9) Uani 1 1 d . . . C39 C 0.5534(4) 0.9277(3) 0.1499(2) 0.0199(9) Uani 1 1 d . . . C40 C 0.5368(4) 1.0093(3) 0.1366(2) 0.0189(9) Uani 1 1 d . . . H40 H 0.4547 1.0349 0.1558 0.023 Uiso 1 1 calc R . . C41 C 0.6387(4) 1.0543(3) 0.0953(2) 0.0194(9) Uani 1 1 d . . . C42 C 0.7586(4) 1.0145(3) 0.0701(2) 0.0196(9) Uani 1 1 d . . . H42 H 0.8305 1.0440 0.0438 0.024 Uiso 1 1 calc R . . C43 C 0.6249(4) 1.1440(3) 0.0785(2) 0.0217(10) Uani 1 1 d . . . C44 C 0.7208(5) 1.1903(3) 0.1138(3) 0.0400(13) Uani 1 1 d . . . H44A H 0.6938 1.1874 0.1690 0.060 Uiso 1 1 calc R . . H44B H 0.7206 1.2463 0.0969 0.060 Uiso 1 1 calc R . . H44C H 0.8087 1.1666 0.0980 0.060 Uiso 1 1 calc R . . C45 C 0.4862(5) 1.1768(3) 0.1090(3) 0.0331(12) Uani 1 1 d . . . H45A H 0.4251 1.1492 0.0853 0.050 Uiso 1 1 calc R . . H45B H 0.4817 1.2342 0.0975 0.050 Uiso 1 1 calc R . . H45C H 0.4629 1.1680 0.1638 0.050 Uiso 1 1 calc R . . C46 C 0.6565(5) 1.1564(3) -0.0070(3) 0.0330(12) Uani 1 1 d . . . H46A H 0.7486 1.1425 -0.0270 0.050 Uiso 1 1 calc R . . H46B H 0.6392 1.2126 -0.0193 0.050 Uiso 1 1 calc R . . H46C H 0.6020 1.1223 -0.0297 0.050 Uiso 1 1 calc R . . C47 C 0.6580(5) 0.7647(3) 0.0688(3) 0.0326(12) Uani 1 1 d . . . H47A H 0.7211 0.7789 0.0218 0.039 Uiso 1 1 calc R . . H47B H 0.5696 0.7809 0.0621 0.039 Uiso 1 1 calc R . . C48 C 0.6649(5) 0.6774(3) 0.0824(3) 0.0394(13) Uani 1 1 d . . . C49 C 0.0515(9) 0.3210(5) 0.1155(5) 0.097(3) Uani 1 1 d D . . H49A H 0.0565 0.3621 0.0769 0.145 Uiso 0.51 1 d PR A 1 H49B H 0.0485 0.2691 0.0939 0.145 Uiso 0.51 1 d PR A 1 H49C H -0.0255 0.3301 0.1539 0.145 Uiso 0.51 1 d PR A 1 H49D H -0.0295 0.3491 0.1149 0.145 Uiso 0.49 1 d PR A 2 H49E H 0.1215 0.3521 0.0889 0.145 Uiso 0.49 1 d PR A 2 H49F H 0.0535 0.2701 0.0919 0.145 Uiso 0.49 1 d PR A 2 C51 C 0.6733(8) 0.4344(4) 0.1446(5) 0.080(2) Uani 1 1 d . . . H51A H 0.7526 0.4237 0.1060 0.120 Uiso 1 1 calc R . . H51B H 0.6595 0.3897 0.1810 0.120 Uiso 1 1 calc R . . H51C H 0.6828 0.4836 0.1708 0.120 Uiso 1 1 calc R . . C52 C 0.5607(9) 0.4438(5) 0.1084(5) 0.089(3) Uani 1 1 d . . . H52A H 0.5306 0.3905 0.0985 0.107 Uiso 1 1 calc R . . H52B H 0.4881 0.4723 0.1425 0.107 Uiso 1 1 calc R . . C53 C 0.4495(8) 0.3232(5) 0.3784(4) 0.075(2) Uani 1 1 d . . . H53A H 0.3932 0.3624 0.4101 0.112 Uiso 1 1 calc R B 1 H53B H 0.5401 0.3399 0.3689 0.112 Uiso 1 1 calc R B 1 H53C H 0.4426 0.2709 0.4042 0.112 Uiso 1 1 calc R B 1 C50 C 0.1718(12) 0.3251(7) 0.1497(7) 0.055(3) Uani 0.51 1 d PD C 1 H50A H 0.2506 0.3168 0.1092 0.066 Uiso 0.51 1 calc PR C 1 H50B H 0.1749 0.3794 0.1695 0.066 Uiso 0.51 1 calc PR C 1 C54 C 0.4100(10) 0.3177(5) 0.3085(5) 0.097(3) Uani 1 1 d . D 1 H54A H 0.4800 0.2922 0.2702 0.116 Uiso 1 1 calc R D 1 H54B H 0.3889 0.3715 0.2896 0.116 Uiso 1 1 calc R D 1 C50' C 0.0660(13) 0.3095(9) 0.1967(7) 0.079(5) Uani 0.49 1 d PD C 2 H50C H 0.0614 0.3627 0.2199 0.095 Uiso 0.49 1 calc PR C 2 H50D H -0.0090 0.2793 0.2248 0.095 Uiso 0.49 1 calc PR C 2 O1 O 0.5217(3) 0.95005(17) 0.32016(16) 0.0200(7) Uani 1 1 d . . . O2 O 0.5221(3) 1.11147(19) 0.3024(2) 0.0329(8) Uani 1 1 d . . . O3 O 0.3114(3) 1.1205(2) 0.3582(2) 0.0419(10) Uani 1 1 d . . . H3 H 0.3220 1.1696 0.3494 0.063 Uiso 1 1 calc R . . O4 O 0.6867(3) 0.80679(17) 0.13056(16) 0.0208(7) Uani 1 1 d . . . O5 O 0.6948(5) 0.6467(2) 0.1402(2) 0.0543(12) Uani 1 1 d . . . O6 O 0.6373(6) 0.6372(3) 0.0302(2) 0.0805(17) Uani 1 1 d . . . H6 H 0.6427 0.5883 0.0408 0.121 Uiso 1 1 calc R . . O7 O 0.9854(3) 0.94808(16) 0.18253(16) 0.0189(7) Uani 1 1 d . . . O8 O 1.1789(3) 1.1188(2) 0.1535(2) 0.0467(10) Uani 1 1 d . . . O9 O 0.9693(3) 1.10876(19) 0.19957(19) 0.0334(8) Uani 1 1 d . . . H9 H 0.9136 1.0730 0.2063 0.050 Uiso 1 1 calc R . . O10 O 0.8279(3) 0.79738(17) 0.37648(16) 0.0218(7) Uani 1 1 d . . . O11 O 0.8278(5) 0.6373(2) 0.3691(2) 0.0629(13) Uani 1 1 d . . . H11 H 0.8059 0.6750 0.3424 0.094 Uiso 1 1 calc R . . O12 O 0.9007(6) 0.6213(3) 0.4738(3) 0.0813(17) Uani 1 1 d . . . O13 O 0.7579(3) 1.03492(19) 0.24696(17) 0.0273(7) Uani 1 1 d . . . H13A H 0.7891 0.9892 0.2437 0.041 Uiso 1 1 d R . . H13B H 0.6844 1.0332 0.2737 0.041 Uiso 1 1 d R . . O14 O 0.7582(3) 0.7165(2) 0.25555(19) 0.0359(8) Uani 1 1 d . . . H14A H 0.7461 0.6889 0.2212 0.054 Uiso 1 1 d R . . H14B H 0.7469 0.7634 0.2437 0.054 Uiso 1 1 d R . . O15 O 0.1755(5) 0.2715(3) 0.2057(3) 0.0747(15) Uani 1 1 d D . . H15 H 0.1747 0.2251 0.1892 0.112 Uiso 1 1 calc R C 1 O17 O 0.5958(6) 0.4871(3) 0.0401(3) 0.0877(17) Uani 1 1 d . . . H17 H 0.5312 0.4923 0.0199 0.132 Uiso 1 1 calc R . . O18 O 0.2942(5) 0.2688(3) 0.3246(3) 0.0782(15) Uani 1 1 d . . . H18A H 0.2667 0.2637 0.2849 0.117 Uiso 1 1 calc R D 1 S1 S 0.41428(10) 0.87328(7) 0.19516(6) 0.0218(3) Uani 1 1 d . . . S2 S 0.92692(10) 0.88621(7) 0.03764(6) 0.0210(3) Uani 1 1 d . . . S3 S 1.09451(10) 0.86185(7) 0.30844(6) 0.0223(3) Uani 1 1 d . . . S4 S 0.58118(10) 0.87833(7) 0.46616(6) 0.0200(3) Uani 1 1 d . . . C55 C 0.843(3) 0.4209(17) 0.3573(15) 0.130(8) Uani 0.52 1 d PD E 1 H55A H 0.7757 0.4052 0.4008 0.195 Uiso 0.52 1 calc PR E 1 H55B H 0.8644 0.3762 0.3223 0.195 Uiso 0.52 1 calc PR E 1 H55C H 0.8118 0.4671 0.3314 0.195 Uiso 0.52 1 calc PR E 1 C56 C 0.966(2) 0.4428(15) 0.3842(10) 0.105(6) Uani 0.52 1 d PD E 1 H56A H 1.0229 0.3944 0.3826 0.126 Uiso 0.52 1 calc PR E 1 H56B H 1.0132 0.4824 0.3481 0.126 Uiso 0.52 1 calc PR E 1 O16 O 0.9444(14) 0.4733(9) 0.4551(8) 0.125(4) Uani 0.52 1 d PD E 1 H16A H 1.0141 0.4705 0.4708 0.187 Uiso 0.52 1 calc PR E 1 C55' C 0.810(2) 0.443(2) 0.343(2) 0.130(8) Uani 0.48 1 d PD F 2 H55D H 0.8562 0.4734 0.2996 0.195 Uiso 0.48 1 calc PR F 2 H55E H 0.7394 0.4759 0.3726 0.195 Uiso 0.48 1 calc PR F 2 H55F H 0.7731 0.3955 0.3255 0.195 Uiso 0.48 1 calc PR F 2 C56' C 0.9046(17) 0.4158(18) 0.3926(11) 0.105(6) Uani 0.48 1 d PD F 2 H56C H 0.8927 0.4523 0.4358 0.126 Uiso 0.48 1 calc PR F 2 H56D H 0.8813 0.3617 0.4133 0.126 Uiso 0.48 1 calc PR F 2 O16' O 1.0332(14) 0.4138(10) 0.3574(9) 0.125(4) Uani 0.48 1 d PD F 2 H16' H 1.0463 0.3791 0.3237 0.187 Uiso 0.48 1 calc PR F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.012(2) 0.023(2) 0.019(2) 0.0044(17) -0.0036(17) -0.0078(17) C2 0.017(2) 0.025(2) 0.023(2) -0.0008(18) -0.0069(18) -0.0070(18) C3 0.022(2) 0.026(3) 0.025(2) 0.0046(19) -0.0042(19) -0.0073(19) C4 0.015(2) 0.019(2) 0.022(2) 0.0020(17) -0.0033(18) -0.0026(17) C5 0.010(2) 0.019(2) 0.021(2) -0.0016(17) 0.0004(17) -0.0024(16) C6 0.010(2) 0.019(2) 0.023(2) 0.0022(17) -0.0017(17) -0.0047(16) C7 0.039(3) 0.020(2) 0.036(3) 0.000(2) -0.012(2) -0.011(2) C8 0.101(6) 0.024(3) 0.066(4) 0.020(3) -0.040(4) -0.026(3) C9 0.097(6) 0.027(3) 0.061(4) -0.006(3) -0.011(4) -0.004(3) C10 0.058(4) 0.046(4) 0.093(5) 0.025(4) -0.029(4) -0.036(3) C11 0.018(2) 0.023(2) 0.030(3) -0.0007(19) 0.005(2) -0.0030(19) C12 0.017(2) 0.028(3) 0.021(2) 0.0040(19) -0.0033(19) 0.0004(19) C13 0.011(2) 0.025(2) 0.017(2) -0.0008(17) -0.0046(17) -0.0072(17) C14 0.018(2) 0.020(2) 0.017(2) -0.0003(17) -0.0080(18) -0.0028(18) C15 0.013(2) 0.030(3) 0.014(2) -0.0018(18) -0.0059(17) 0.0010(18) C16 0.013(2) 0.028(3) 0.021(2) -0.0006(18) -0.0044(18) -0.0057(18) C17 0.016(2) 0.022(2) 0.018(2) -0.0012(17) -0.0041(17) -0.0063(18) C18 0.013(2) 0.023(2) 0.020(2) -0.0062(18) -0.0040(17) -0.0030(17) C19 0.023(2) 0.021(2) 0.024(2) -0.0058(18) -0.0028(19) -0.0080(19) C20 0.033(3) 0.036(3) 0.030(3) -0.012(2) -0.009(2) -0.009(2) C21 0.040(3) 0.025(3) 0.044(3) 0.002(2) -0.015(3) -0.004(2) C22 0.028(3) 0.028(3) 0.051(3) -0.008(2) 0.000(2) -0.012(2) C23 0.035(3) 0.029(3) 0.033(3) 0.003(2) -0.014(2) -0.001(2) C24 0.057(4) 0.034(3) 0.038(3) 0.003(2) -0.020(3) 0.006(3) C25 0.010(2) 0.025(2) 0.016(2) -0.0012(17) -0.0006(17) 0.0004(17) C26 0.019(2) 0.021(2) 0.026(2) 0.0012(19) -0.0071(19) 0.0034(18) C27 0.019(2) 0.023(2) 0.027(2) -0.0011(19) 0.0005(19) 0.0023(19) C28 0.018(2) 0.024(2) 0.023(2) -0.0044(19) -0.0044(19) -0.0029(18) C29 0.012(2) 0.021(2) 0.019(2) 0.0026(17) 0.0007(17) -0.0021(17) C30 0.008(2) 0.019(2) 0.024(2) -0.0031(18) -0.0001(17) -0.0006(16) C31 0.050(3) 0.021(3) 0.033(3) -0.003(2) -0.011(2) 0.008(2) C32 0.120(7) 0.030(3) 0.065(5) 0.002(3) 0.004(4) 0.002(4) C33 0.066(5) 0.048(4) 0.082(5) -0.026(4) -0.025(4) 0.031(3) C34 0.069(4) 0.033(3) 0.057(4) -0.017(3) -0.025(3) 0.014(3) C35 0.016(2) 0.026(3) 0.038(3) 0.002(2) 0.001(2) -0.0067(19) C36 0.021(3) 0.026(3) 0.032(3) 0.004(2) -0.004(2) -0.008(2) C37 0.012(2) 0.026(2) 0.017(2) 0.0018(17) -0.0041(17) 0.0007(17) C38 0.021(2) 0.019(2) 0.018(2) 0.0037(17) -0.0067(18) -0.0025(18) C39 0.017(2) 0.029(3) 0.015(2) 0.0034(18) -0.0054(18) -0.0076(18) C40 0.015(2) 0.024(2) 0.018(2) 0.0027(17) -0.0041(17) -0.0011(18) C41 0.019(2) 0.025(2) 0.015(2) 0.0038(18) -0.0076(18) -0.0049(18) C42 0.015(2) 0.030(3) 0.013(2) 0.0043(18) -0.0009(17) -0.0056(18) C43 0.016(2) 0.023(2) 0.027(2) 0.0020(19) -0.0060(19) -0.0030(18) C44 0.040(3) 0.030(3) 0.055(3) 0.004(2) -0.022(3) 0.000(2) C45 0.029(3) 0.028(3) 0.038(3) 0.007(2) 0.002(2) 0.005(2) C46 0.032(3) 0.031(3) 0.034(3) 0.011(2) -0.003(2) 0.003(2) C47 0.038(3) 0.035(3) 0.032(3) -0.002(2) -0.020(2) -0.008(2) C48 0.040(3) 0.041(3) 0.042(3) -0.008(3) -0.016(3) -0.011(2) C49 0.130(8) 0.070(6) 0.105(7) -0.003(5) -0.061(6) 0.024(5) C51 0.095(6) 0.042(4) 0.093(6) -0.012(4) 0.002(5) 0.003(4) C52 0.094(7) 0.071(6) 0.100(7) 0.021(5) -0.017(5) -0.022(5) C53 0.084(6) 0.074(5) 0.081(5) -0.001(4) -0.047(4) -0.009(4) C50 0.085(10) 0.031(6) 0.054(8) 0.007(6) -0.024(7) -0.001(6) C54 0.152(9) 0.068(5) 0.081(6) 0.016(4) -0.040(6) -0.058(6) C50' 0.089(13) 0.068(11) 0.069(10) -0.034(8) 0.010(10) 0.002(9) O1 0.0137(15) 0.0171(15) 0.0281(17) 0.0020(12) -0.0016(13) -0.0043(12) O2 0.0227(18) 0.0229(18) 0.051(2) 0.0007(15) -0.0020(16) -0.0054(14) O3 0.0209(19) 0.0235(18) 0.074(3) 0.0040(18) 0.0056(18) 0.0018(14) O4 0.0195(16) 0.0196(16) 0.0255(16) 0.0030(13) -0.0100(13) -0.0028(12) O5 0.099(4) 0.025(2) 0.048(2) 0.0026(18) -0.034(2) -0.010(2) O6 0.159(5) 0.038(3) 0.061(3) -0.007(2) -0.053(3) -0.034(3) O7 0.0151(15) 0.0150(15) 0.0252(16) -0.0008(12) -0.0012(12) -0.0010(12) O8 0.027(2) 0.028(2) 0.082(3) -0.0071(19) -0.0024(19) -0.0114(16) O9 0.0215(18) 0.0252(18) 0.051(2) -0.0033(16) -0.0015(16) -0.0051(14) O10 0.0220(17) 0.0225(17) 0.0235(16) -0.0019(13) -0.0103(13) -0.0020(13) O11 0.117(4) 0.025(2) 0.055(3) 0.0039(19) -0.039(3) 0.002(2) O12 0.137(5) 0.052(3) 0.065(3) 0.013(2) -0.052(3) 0.027(3) O13 0.0189(17) 0.0326(18) 0.0289(17) -0.0023(14) -0.0013(13) -0.0012(14) O14 0.038(2) 0.0274(18) 0.043(2) -0.0042(16) -0.0108(17) -0.0021(16) O15 0.095(4) 0.043(3) 0.100(4) -0.007(3) -0.050(3) -0.007(3) O17 0.110(5) 0.070(4) 0.091(4) -0.017(3) -0.036(3) -0.018(3) O18 0.066(3) 0.037(3) 0.134(5) 0.008(3) -0.026(3) -0.013(2) S1 0.0138(6) 0.0309(6) 0.0220(6) 0.0093(5) -0.0062(4) -0.0087(4) S2 0.0160(6) 0.0277(6) 0.0181(6) 0.0037(4) -0.0013(4) 0.0007(4) S3 0.0136(5) 0.0316(6) 0.0227(6) -0.0064(5) -0.0055(4) 0.0025(4) S4 0.0161(6) 0.0251(6) 0.0184(6) -0.0034(4) -0.0009(4) -0.0080(4) C55 0.151(17) 0.092(18) 0.166(16) 0.068(13) -0.079(13) -0.053(14) C56 0.101(18) 0.101(18) 0.101(10) 0.000(9) 0.000(12) 0.000(12) O16 0.121(9) 0.121(8) 0.121(8) 0.000(6) 0.000(6) 0.000(7) C55' 0.151(17) 0.092(18) 0.166(16) 0.068(13) -0.079(13) -0.053(14) C56' 0.101(18) 0.101(18) 0.101(10) 0.000(9) 0.000(12) 0.000(12) O16' 0.121(9) 0.121(8) 0.121(8) 0.000(6) 0.000(6) 0.000(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 C1 C2 1.387(6) . ? C1 C6 1.401(6) . ? C1 S1 1.785(4) . ? C2 C3 1.399(6) . ? C2 H2 0.9500 . ? C3 C4 1.392(6) . ? C3 C7 1.524(6) . ? C4 C5 1.397(6) . ? C4 H4 0.9500 . ? C5 C6 1.385(6) . ? C5 S4 1.778(4) . ? C6 O1 1.391(5) . ? C7 C8 1.511(7) . ? C7 C10 1.537(8) . ? C7 C9 1.543(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O1 1.424(5) . ? C11 C12 1.510(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O2 1.210(5) . ? C12 O3 1.303(5) . ? C13 C18 1.377(6) . ? C13 C14 1.395(6) . ? C13 S4 1.786(4) . ? C14 O10 1.382(5) . ? C14 C15 1.391(6) . ? C15 C16 1.399(6) . ? C15 S3 1.778(4) . ? C16 C17 1.392(6) . ? C16 H16 0.9500 . ? C17 C18 1.400(6) . ? C17 C19 1.538(6) . ? C18 H18 0.9500 . ? C19 C22 1.522(6) . ? C19 C20 1.530(6) . ? C19 C21 1.535(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O10 1.427(5) . ? C23 C24 1.482(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O12 1.256(6) . ? C24 O11 1.260(7) . ? C25 C26 1.383(6) . ? C25 C30 1.396(6) . ? C25 S3 1.781(4) . ? C26 C27 1.396(6) . ? C26 H26 0.9500 . ? C27 C28 1.383(6) . ? C27 C31 1.532(6) . ? C28 C29 1.380(6) . ? C28 H28 0.9500 . ? C29 C30 1.410(6) . ? C29 S2 1.778(4) . ? C30 O7 1.372(5) . ? C31 C34 1.514(7) . ? C31 C33 1.537(8) . ? C31 C32 1.540(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 O7 1.430(5) . ? C35 C36 1.495(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O8 1.217(6) . ? C36 O9 1.304(5) . ? C37 C42 1.378(6) . ? C37 C38 1.396(6) . ? C37 S2 1.792(4) . ? C38 O4 1.383(5) . ? C38 C39 1.393(6) . ? C39 C40 1.393(6) . ? C39 S1 1.784(4) . ? C40 C41 1.400(6) . ? C40 H40 0.9500 . ? C41 C42 1.395(6) . ? C41 C43 1.533(6) . ? C42 H42 0.9500 . ? C43 C46 1.526(6) . ? C43 C45 1.532(6) . ? C43 C44 1.545(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 O4 1.430(5) . ? C47 C48 1.479(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O5 1.251(6) . ? C48 O6 1.263(6) . ? C49 C50' 1.521(12) . ? C49 C50 1.529(12) . ? C49 H49A 0.9632 . ? C49 H49B 0.9670 . ? C49 H49C 0.9575 . ? C49 H49D 0.9590 . ? C49 H49E 0.9528 . ? C49 H49F 0.9614 . ? C51 C52 1.474(11) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O17 1.403(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.421(10) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C50 O15 1.344(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C54 O18 1.464(9) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C50' O15 1.334(11) . ? C50' H50C 0.9900 . ? C50' H50D 0.9900 . ? O3 H3 0.8400 . ? O6 H6 0.8400 . ? O9 H9 0.8400 . ? O11 H11 0.8400 . ? O13 H13A 0.8199 . ? O13 H13B 0.8199 . ? O14 H14A 0.8200 . ? O14 H14B 0.8200 . ? O15 H15 0.8400 . ? O17 H17 0.8400 . ? O18 H18A 0.8400 . ? C55 C56 1.529(10) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 O16 1.367(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? O16 H16A 0.8400 . ? C55' C56' 1.526(10) . ? C55' H55D 0.9800 . ? C55' H55E 0.9800 . ? C55' H55F 0.9800 . ? C56' O16' 1.364(10) . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? O16' H16' 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.5(4) . . ? C2 C1 S1 118.2(3) . . ? C6 C1 S1 121.9(3) . . ? C1 C2 C3 122.2(4) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C4 C3 C2 117.1(4) . . ? C4 C3 C7 122.5(4) . . ? C2 C3 C7 120.4(4) . . ? C3 C4 C5 121.7(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 S4 122.6(3) . . ? C4 C5 S4 116.9(3) . . ? C5 C6 O1 120.1(4) . . ? C5 C6 C1 119.3(4) . . ? O1 C6 C1 120.6(4) . . ? C8 C7 C3 112.5(4) . . ? C8 C7 C10 109.2(5) . . ? C3 C7 C10 108.5(4) . . ? C8 C7 C9 108.5(5) . . ? C3 C7 C9 109.5(4) . . ? C10 C7 C9 108.6(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 109.8(3) . . ? O1 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O1 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O2 C12 O3 124.9(4) . . ? O2 C12 C11 125.3(4) . . ? O3 C12 C11 109.8(4) . . ? C18 C13 C14 120.3(4) . . ? C18 C13 S4 118.1(3) . . ? C14 C13 S4 121.3(3) . . ? O10 C14 C15 120.5(4) . . ? O10 C14 C13 120.4(4) . . ? C15 C14 C13 119.0(4) . . ? C14 C15 C16 119.8(4) . . ? C14 C15 S3 121.2(3) . . ? C16 C15 S3 118.6(3) . . ? C17 C16 C15 121.7(4) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 117.1(4) . . ? C16 C17 C19 123.1(4) . . ? C18 C17 C19 119.8(4) . . ? C13 C18 C17 121.9(4) . . ? C13 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C22 C19 C20 108.1(4) . . ? C22 C19 C21 109.2(4) . . ? C20 C19 C21 109.1(4) . . ? C22 C19 C17 112.2(4) . . ? C20 C19 C17 108.3(4) . . ? C21 C19 C17 109.8(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O10 C23 C24 111.4(4) . . ? O10 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? O10 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O12 C24 O11 122.1(5) . . ? O12 C24 C23 115.8(5) . . ? O11 C24 C23 122.1(5) . . ? C26 C25 C30 119.8(4) . . ? C26 C25 S3 118.0(3) . . ? C30 C25 S3 121.9(3) . . ? C25 C26 C27 122.0(4) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C28 C27 C26 117.4(4) . . ? C28 C27 C31 122.2(4) . . ? C26 C27 C31 120.3(4) . . ? C29 C28 C27 122.0(4) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 119.9(4) . . ? C28 C29 S2 118.2(3) . . ? C30 C29 S2 121.4(3) . . ? O7 C30 C25 121.6(4) . . ? O7 C30 C29 119.9(4) . . ? C25 C30 C29 118.6(4) . . ? C34 C31 C27 112.6(4) . . ? C34 C31 C33 107.6(5) . . ? C27 C31 C33 108.9(5) . . ? C34 C31 C32 107.8(5) . . ? C27 C31 C32 109.3(4) . . ? C33 C31 C32 110.6(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O7 C35 C36 111.5(4) . . ? O7 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? O7 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? O8 C36 O9 120.9(4) . . ? O8 C36 C35 117.7(4) . . ? O9 C36 C35 121.4(4) . . ? C42 C37 C38 120.7(4) . . ? C42 C37 S2 118.1(3) . . ? C38 C37 S2 120.8(3) . . ? O4 C38 C39 120.6(4) . . ? O4 C38 C37 120.9(4) . . ? C39 C38 C37 118.5(4) . . ? C40 C39 C38 120.4(4) . . ? C40 C39 S1 118.3(3) . . ? C38 C39 S1 121.0(3) . . ? C39 C40 C41 121.3(4) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 117.3(4) . . ? C42 C41 C43 119.5(4) . . ? C40 C41 C43 123.2(4) . . ? C37 C42 C41 121.8(4) . . ? C37 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C46 C43 C45 108.1(4) . . ? C46 C43 C41 108.0(4) . . ? C45 C43 C41 112.1(4) . . ? C46 C43 C44 109.8(4) . . ? C45 C43 C44 109.0(4) . . ? C41 C43 C44 109.9(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O4 C47 C48 110.8(4) . . ? O4 C47 H47A 109.5 . . ? C48 C47 H47A 109.5 . . ? O4 C47 H47B 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? O5 C48 O6 123.6(5) . . ? O5 C48 C47 122.9(5) . . ? O6 C48 C47 113.5(5) . . ? C50' C49 C50 49.6(8) . . ? C50' C49 H49A 140.4 . . ? C50 C49 H49A 108.3 . . ? C50' C49 H49B 108.7 . . ? C50 C49 H49B 110.0 . . ? H49A C49 H49B 110.1 . . ? C50' C49 H49C 63.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.4 . . ? H49B C49 H49C 109.5 . . ? C50' C49 H49D 109.2 . . ? C50 C49 H49D 141.0 . . ? H49A C49 H49D 65.4 . . ? H49B C49 H49D 107.9 . . ? H49C C49 H49D 47.8 . . ? C50' C49 H49E 108.6 . . ? C50 C49 H49E 62.7 . . ? H49A C49 H49E 47.5 . . ? H49B C49 H49E 113.2 . . ? H49C C49 H49E 136.5 . . ? H49D C49 H49E 109.1 . . ? C50' C49 H49F 110.2 . . ? C50 C49 H49F 108.4 . . ? H49A C49 H49F 108.1 . . ? H49C C49 H49F 113.0 . . ? H49D C49 H49F 110.0 . . ? H49E C49 H49F 109.7 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O17 C52 C51 110.0(7) . . ? O17 C52 H52A 109.7 . . ? C51 C52 H52A 109.7 . . ? O17 C52 H52B 109.7 . . ? C51 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? O15 C50 C49 114.3(8) . . ? O15 C50 H49E 150.5 . . ? O15 C50 H50A 108.7 . . ? C49 C50 H50A 108.7 . . ? H49E C50 H50A 81.3 . . ? O15 C50 H50B 108.7 . . ? C49 C50 H50B 108.7 . . ? H49E C50 H50B 93.7 . . ? H50A C50 H50B 107.6 . . ? C53 C54 O18 105.6(6) . . ? C53 C54 H54A 110.6 . . ? O18 C54 H54A 110.6 . . ? C53 C54 H54B 110.6 . . ? O18 C54 H54B 110.6 . . ? H54A C54 H54B 108.8 . . ? O15 C50' C49 115.4(8) . . ? O15 C50' H49C 151.4 . . ? O15 C50' H50C 108.4 . . ? C49 C50' H50C 108.4 . . ? H49C C50' H50C 94.1 . . ? O15 C50' H50D 108.4 . . ? C49 C50' H50D 108.4 . . ? H49C C50' H50D 80.1 . . ? H50C C50' H50D 107.5 . . ? C6 O1 C11 110.3(3) . . ? C12 O3 H3 109.5 . . ? C38 O4 C47 111.4(3) . . ? C48 O6 H6 109.5 . . ? C30 O7 C35 111.3(3) . . ? C36 O9 H9 109.5 . . ? C14 O10 C23 112.7(3) . . ? C24 O11 H11 109.5 . . ? H9 O13 H13A 90.2 . . ? H9 O13 H13B 158.6 . . ? H13A O13 H13B 107.7 . . ? H14A O14 H14B 107.7 . . ? C50' O15 C50 57.0(9) . . ? C50' O15 H15 107.2 . . ? C50 O15 H15 109.5 . . ? C52 O17 H17 109.5 . . ? C54 O18 H18A 109.5 . . ? C39 S1 C1 105.60(19) . . ? C29 S2 C37 105.30(19) . . ? C15 S3 C25 104.96(19) . . ? C5 S4 C13 104.67(19) . . ? O16 C56 C55 115.5(11) . . ? O16 C56 H56A 108.4 . . ? C55 C56 H56A 108.4 . . ? O16 C56 H56B 108.4 . . ? C55 C56 H56B 108.4 . . ? H56A C56 H56B 107.5 . . ? C56 O16 H16A 109.5 . . ? C56' C55' H55D 109.5 . . ? C56' C55' H55E 109.5 . . ? H55D C55' H55E 109.5 . . ? C56' C55' H55F 109.5 . . ? H55D C55' H55F 109.5 . . ? H55E C55' H55F 109.5 . . ? O16' C56' C55' 115.5(11) . . ? O16' C56' H56C 108.4 . . ? C55' C56' H56C 108.4 . . ? O16' C56' H56D 108.4 . . ? C55' C56' H56D 108.4 . . ? H56C C56' H56D 107.5 . . ? C56' O16' H16' 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.7(6) . . . . ? S1 C1 C2 C3 -174.0(3) . . . . ? C1 C2 C3 C4 -2.0(6) . . . . ? C1 C2 C3 C7 178.5(4) . . . . ? C2 C3 C4 C5 2.3(6) . . . . ? C7 C3 C4 C5 -178.2(4) . . . . ? C3 C4 C5 C6 1.0(6) . . . . ? C3 C4 C5 S4 173.7(3) . . . . ? C4 C5 C6 O1 175.0(4) . . . . ? S4 C5 C6 O1 2.7(5) . . . . ? C4 C5 C6 C1 -4.7(6) . . . . ? S4 C5 C6 C1 -176.9(3) . . . . ? C2 C1 C6 C5 5.0(6) . . . . ? S1 C1 C6 C5 177.0(3) . . . . ? C2 C1 C6 O1 -174.6(4) . . . . ? S1 C1 C6 O1 -2.6(6) . . . . ? C4 C3 C7 C8 -2.8(7) . . . . ? C2 C3 C7 C8 176.7(5) . . . . ? C4 C3 C7 C10 118.1(5) . . . . ? C2 C3 C7 C10 -62.4(6) . . . . ? C4 C3 C7 C9 -123.6(5) . . . . ? C2 C3 C7 C9 55.9(6) . . . . ? O1 C11 C12 O2 -2.0(7) . . . . ? O1 C11 C12 O3 178.3(4) . . . . ? C18 C13 C14 O10 177.1(4) . . . . ? S4 C13 C14 O10 4.3(5) . . . . ? C18 C13 C14 C15 -3.2(6) . . . . ? S4 C13 C14 C15 -176.0(3) . . . . ? O10 C14 C15 C16 -175.7(4) . . . . ? C13 C14 C15 C16 4.6(6) . . . . ? O10 C14 C15 S3 -2.8(5) . . . . ? C13 C14 C15 S3 177.5(3) . . . . ? C14 C15 C16 C17 -2.1(6) . . . . ? S3 C15 C16 C17 -175.2(3) . . . . ? C15 C16 C17 C18 -1.9(6) . . . . ? C15 C16 C17 C19 179.2(4) . . . . ? C14 C13 C18 C17 -0.9(6) . . . . ? S4 C13 C18 C17 172.2(3) . . . . ? C16 C17 C18 C13 3.4(6) . . . . ? C19 C17 C18 C13 -177.6(4) . . . . ? C16 C17 C19 C22 -3.5(6) . . . . ? C18 C17 C19 C22 177.5(4) . . . . ? C16 C17 C19 C20 -122.8(4) . . . . ? C18 C17 C19 C20 58.3(5) . . . . ? C16 C17 C19 C21 118.1(5) . . . . ? C18 C17 C19 C21 -60.8(5) . . . . ? O10 C23 C24 O12 177.0(5) . . . . ? O10 C23 C24 O11 -4.8(8) . . . . ? C30 C25 C26 C27 -1.0(6) . . . . ? S3 C25 C26 C27 -174.1(3) . . . . ? C25 C26 C27 C28 -2.7(7) . . . . ? C25 C26 C27 C31 178.1(4) . . . . ? C26 C27 C28 C29 2.4(7) . . . . ? C31 C27 C28 C29 -178.4(4) . . . . ? C27 C28 C29 C30 1.5(6) . . . . ? C27 C28 C29 S2 173.8(3) . . . . ? C26 C25 C30 O7 -175.5(4) . . . . ? S3 C25 C30 O7 -2.6(6) . . . . ? C26 C25 C30 C29 5.0(6) . . . . ? S3 C25 C30 C29 177.8(3) . . . . ? C28 C29 C30 O7 175.2(4) . . . . ? S2 C29 C30 O7 3.2(5) . . . . ? C28 C29 C30 C25 -5.2(6) . . . . ? S2 C29 C30 C25 -177.2(3) . . . . ? C28 C27 C31 C34 -0.2(7) . . . . ? C26 C27 C31 C34 179.0(5) . . . . ? C28 C27 C31 C33 119.2(5) . . . . ? C26 C27 C31 C33 -61.7(6) . . . . ? C28 C27 C31 C32 -120.0(6) . . . . ? C26 C27 C31 C32 59.2(7) . . . . ? O7 C35 C36 O8 174.4(4) . . . . ? O7 C35 C36 O9 -7.3(6) . . . . ? C42 C37 C38 O4 177.2(4) . . . . ? S2 C37 C38 O4 4.7(6) . . . . ? C42 C37 C38 C39 -2.9(6) . . . . ? S2 C37 C38 C39 -175.4(3) . . . . ? O4 C38 C39 C40 -176.4(4) . . . . ? C37 C38 C39 C40 3.6(6) . . . . ? O4 C38 C39 S1 -3.8(6) . . . . ? C37 C38 C39 S1 176.3(3) . . . . ? C38 C39 C40 C41 -1.3(6) . . . . ? S1 C39 C40 C41 -174.1(3) . . . . ? C39 C40 C41 C42 -1.9(6) . . . . ? C39 C40 C41 C43 179.4(4) . . . . ? C38 C37 C42 C41 -0.3(6) . . . . ? S2 C37 C42 C41 172.4(3) . . . . ? C40 C41 C42 C37 2.7(6) . . . . ? C43 C41 C42 C37 -178.5(4) . . . . ? C42 C41 C43 C46 59.9(5) . . . . ? C40 C41 C43 C46 -121.4(4) . . . . ? C42 C41 C43 C45 178.8(4) . . . . ? C40 C41 C43 C45 -2.5(6) . . . . ? C42 C41 C43 C44 -59.9(5) . . . . ? C40 C41 C43 C44 118.9(5) . . . . ? O4 C47 C48 O5 -1.4(8) . . . . ? O4 C47 C48 O6 178.5(5) . . . . ? C50' C49 C50 O15 37.1(9) . . . . ? C50 C49 C50' O15 -37.8(9) . . . . ? C5 C6 O1 C11 -93.8(4) . . . . ? C1 C6 O1 C11 85.8(5) . . . . ? C12 C11 O1 C6 -175.5(3) . . . . ? C39 C38 O4 C47 91.5(5) . . . . ? C37 C38 O4 C47 -88.6(5) . . . . ? C48 C47 O4 C38 -175.9(4) . . . . ? C25 C30 O7 C35 85.8(5) . . . . ? C29 C30 O7 C35 -94.6(4) . . . . ? C36 C35 O7 C30 -173.7(4) . . . . ? C15 C14 O10 C23 89.4(5) . . . . ? C13 C14 O10 C23 -90.9(5) . . . . ? C24 C23 O10 C14 -175.1(4) . . . . ? C49 C50' O15 C50 39.3(9) . . . . ? C49 C50 O15 C50' -38.6(9) . . . . ? C40 C39 S1 C1 -125.0(3) . . . . ? C38 C39 S1 C1 62.3(4) . . . . ? C2 C1 S1 C39 -133.7(3) . . . . ? C6 C1 S1 C39 54.2(4) . . . . ? C28 C29 S2 C37 126.4(3) . . . . ? C30 C29 S2 C37 -61.4(4) . . . . ? C42 C37 S2 C29 130.6(3) . . . . ? C38 C37 S2 C29 -56.7(4) . . . . ? C14 C15 S3 C25 64.0(4) . . . . ? C16 C15 S3 C25 -123.0(3) . . . . ? C26 C25 S3 C15 -131.9(3) . . . . ? C30 C25 S3 C15 55.1(4) . . . . ? C6 C5 S4 C13 -59.9(4) . . . . ? C4 C5 S4 C13 127.7(3) . . . . ? C18 C13 S4 C5 127.4(3) . . . . ? C14 C13 S4 C5 -59.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O18 H18A O15 0.84 1.89 2.713(7) 166.3 . O14 H14B O4 0.82 2.36 2.909(4) 124.6 . O14 H14A O5 0.82 1.84 2.641(5) 166.7 . O13 H13B O2 0.82 2.10 2.751(4) 136.7 . O13 H13B O1 0.82 2.25 2.948(4) 142.9 . O13 H13A O7 0.82 2.22 2.799(4) 128.1 . O11 H11 O14 0.84 1.87 2.641(5) 152.9 . O9 H9 O13 0.84 1.78 2.554(4) 152.9 . O6 H6 O17 0.84 1.78 2.563(7) 153.6 . O16 H16A O16 0.84 1.80 2.40(3) 127.8 2_766 O16 H16A O12 0.84 2.10 2.728(15) 131.8 2_766 O15 H15 O8 0.84 1.91 2.745(6) 177.7 1_445 O3 H3 O18 0.84 1.74 2.552(5) 161.4 1_565 C22 H22A O3 0.98 2.60 3.236(6) 123.1 1_655 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.194 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.097 data_2 _database_code_depnum_ccdc_archive 'CCDC 760512' #TrackingRef '- data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H60 N4 O12 S4, 2(C H2 Cl2)' _chemical_formula_sum 'C52 H64 Cl4 N4 O12 S4' _chemical_formula_weight 1207.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'c 2/c' _symmetry_space_group_name_HALL '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.4396(7) _cell_length_b 14.2832(3) _cell_length_c 21.6031(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.638(4) _cell_angle_gamma 90.00 _cell_volume 11601.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7025 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9016 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55715 _diffrn_reflns_av_R_equivalents 0.2234 _diffrn_reflns_av_sigmaI/netI 0.1083 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.10 _reflns_number_total 10327 _reflns_number_gt 7998 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1109P)^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 10327 _refine_ls_number_parameters 750 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.022 _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 C1 C 0.10548(7) 0.6687(2) -0.09565(14) 0.0202(6) Uani 1 1 d . . . C2 C 0.12868(8) 0.6953(2) -0.12082(14) 0.0216(6) Uani 1 1 d . . . C3 C 0.15464(8) 0.6322(2) -0.11868(15) 0.0245(7) Uani 1 1 d . . . H3 H 0.1701 0.6510 -0.1359 0.029 Uiso 1 1 calc R . . C4 C 0.15776(8) 0.5433(2) -0.09175(15) 0.0243(7) Uani 1 1 d . A . C5 C 0.13351(7) 0.5168(2) -0.06860(15) 0.0216(6) Uani 1 1 d . . . H5 H 0.1347 0.4566 -0.0512 0.026 Uiso 1 1 calc R . . C6 C 0.10750(7) 0.5780(2) -0.07078(14) 0.0210(6) Uani 1 1 d . . . C7 C 0.18731(8) 0.4767(2) -0.08640(18) 0.0340(8) Uani 1 1 d D . . C8 C 0.2171(3) 0.5196(7) -0.0891(8) 0.075(4) Uani 0.578(11) 1 d P A 1 H8A H 0.2333 0.4720 -0.0882 0.113 Uiso 0.578(11) 1 calc PR A 1 H8B H 0.2291 0.5601 -0.0495 0.113 Uiso 0.578(11) 1 calc PR A 1 H8C H 0.2090 0.5555 -0.1313 0.113 Uiso 0.578(11) 1 calc PR A 1 C9 C 0.2033(3) 0.4289(9) -0.0099(5) 0.077(4) Uani 0.578(11) 1 d P A 1 H9A H 0.2224 0.3875 -0.0034 0.116 Uiso 0.578(11) 1 calc PR A 1 H9B H 0.1849 0.3941 -0.0061 0.116 Uiso 0.578(11) 1 calc PR A 1 H9C H 0.2120 0.4768 0.0253 0.116 Uiso 0.578(11) 1 calc PR A 1 C10 C 0.1710(2) 0.3961(7) -0.1349(6) 0.077(4) Uani 0.578(11) 1 d P A 1 H10A H 0.1625 0.4168 -0.1822 0.116 Uiso 0.578(11) 1 calc PR A 1 H10B H 0.1515 0.3718 -0.1289 0.116 Uiso 0.578(11) 1 calc PR A 1 H10C H 0.1885 0.3480 -0.1247 0.116 Uiso 0.578(11) 1 calc PR A 1 C13 C 0.02631(7) 0.9261(2) -0.04794(16) 0.0233(6) Uani 1 1 d . . . C14 C 0.12443(7) 0.8926(2) -0.10858(15) 0.0209(6) Uani 1 1 d . . . C11 C 0.04762(8) 0.7390(2) -0.14906(16) 0.0299(7) Uani 1 1 d . . . H11A H 0.0364 0.6778 -0.1579 0.036 Uiso 1 1 calc R . . H11B H 0.0496 0.7579 -0.1903 0.036 Uiso 1 1 calc R . . C12 C 0.02508(8) 0.8088(2) -0.13476(16) 0.0276(7) Uani 1 1 d . . . C15 C 0.14666(7) 0.89512(19) -0.03680(14) 0.0182(6) Uani 1 1 d . . . C16 C 0.14894(7) 0.97677(19) 0.00000(14) 0.0182(6) Uani 1 1 d . . . C17 C 0.12820(8) 1.0540(2) -0.03485(15) 0.0212(6) Uani 1 1 d . . . H17 H 0.1299 1.1083 -0.0098 0.025 Uiso 1 1 calc R . . C18 C 0.10494(8) 1.0519(2) -0.10638(15) 0.0220(6) Uani 1 1 d . . . C19 C 0.10343(8) 0.9698(2) -0.14261(15) 0.0244(7) Uani 1 1 d . . . H19 H 0.0882 0.9666 -0.1903 0.029 Uiso 1 1 calc R . . C20 C 0.08127(9) 1.1347(2) -0.14464(15) 0.0302(7) Uani 1 1 d . . . C21 C 0.09147(9) 1.2233(2) -0.10066(18) 0.0351(8) Uani 1 1 d . . . H21A H 0.0888 1.2133 -0.0594 0.053 Uiso 1 1 calc R . . H21B H 0.0763 1.2738 -0.1273 0.053 Uiso 1 1 calc R . . H21C H 0.1158 1.2389 -0.0875 0.053 Uiso 1 1 calc R . . C22 C 0.08409(17) 1.1548(3) -0.2121(2) 0.0829(19) Uani 1 1 d . . . H22A H 0.1085 1.1656 -0.2007 0.124 Uiso 1 1 calc R . . H22B H 0.0703 1.2092 -0.2347 0.124 Uiso 1 1 calc R . . H22C H 0.0753 1.1020 -0.2430 0.124 Uiso 1 1 calc R . . C23 C 0.04309(9) 1.1082(3) -0.1637(2) 0.0535(11) Uani 1 1 d . . . H23A H 0.0363 1.0540 -0.1934 0.080 Uiso 1 1 calc R . . H23B H 0.0276 1.1594 -0.1879 0.080 Uiso 1 1 calc R . . H23C H 0.0413 1.0946 -0.1219 0.080 Uiso 1 1 calc R . . C24 C 0.20091(7) 0.8096(2) 0.00575(16) 0.0255(7) Uani 1 1 d . . . H24A H 0.2144 0.8652 0.0287 0.031 Uiso 1 1 calc R . . H24B H 0.2001 0.8044 -0.0398 0.031 Uiso 1 1 calc R . . C25 C 0.21852(8) 0.7233(2) 0.04941(16) 0.0292(7) Uani 1 1 d . . . C26 C 0.18621(7) 0.8959(2) 0.13733(14) 0.0196(6) Uani 1 1 d . . . C27 C 0.15802(7) 0.85750(19) 0.14539(13) 0.0180(6) Uani 1 1 d . . . C28 C 0.16441(7) 0.77810(19) 0.18741(14) 0.0196(6) Uani 1 1 d . . . C29 C 0.19894(7) 0.7448(2) 0.22451(14) 0.0220(6) Uani 1 1 d . . . H29 H 0.2029 0.6929 0.2532 0.026 Uiso 1 1 calc R . . C30 C 0.22804(7) 0.7849(2) 0.22106(15) 0.0245(7) Uani 1 1 d . . . C31 C 0.22050(7) 0.8597(2) 0.17512(14) 0.0221(6) Uani 1 1 d . . . H31 H 0.2389 0.8865 0.1693 0.027 Uiso 1 1 calc R . . C32 C 0.26534(8) 0.7450(3) 0.26534(16) 0.0330(8) Uani 1 1 d . . . C33 C 0.27528(9) 0.7580(3) 0.34299(17) 0.0438(9) Uani 1 1 d . . . H33A H 0.2756 0.8235 0.3531 0.066 Uiso 1 1 calc R . . H33B H 0.2984 0.7317 0.3715 0.066 Uiso 1 1 calc R . . H33C H 0.2581 0.7268 0.3528 0.066 Uiso 1 1 calc R . . C34 C 0.26537(10) 0.6399(3) 0.24970(19) 0.0454(9) Uani 1 1 d . . . H34A H 0.2889 0.6152 0.2764 0.068 Uiso 1 1 calc R . . H34B H 0.2579 0.6313 0.2008 0.068 Uiso 1 1 calc R . . H34C H 0.2493 0.6077 0.2622 0.068 Uiso 1 1 calc R . . C35 C 0.29288(8) 0.7950(3) 0.24991(19) 0.0461(10) Uani 1 1 d . . . H35A H 0.2924 0.8609 0.2581 0.069 Uiso 1 1 calc R . . H35B H 0.2873 0.7847 0.2020 0.069 Uiso 1 1 calc R . . H35C H 0.3161 0.7706 0.2799 0.069 Uiso 1 1 calc R . . C36 C 0.10750(8) 0.9250(2) 0.15013(15) 0.0223(6) Uani 1 1 d . . . H36A H 0.1217 0.9034 0.1977 0.027 Uiso 1 1 calc R . . H36B H 0.0847 0.8932 0.1314 0.027 Uiso 1 1 calc R . . C37 C 0.10132(7) 1.0289(2) 0.15148(14) 0.0207(6) Uani 1 1 d . . . C38 C 0.11475(7) 1.1829(2) 0.11589(14) 0.0217(6) Uani 1 1 d . . . C39 C 0.09711(7) 0.68787(19) 0.12176(14) 0.0195(6) Uani 1 1 d . . . C40 C 0.10201(7) 0.63547(19) 0.07250(14) 0.0181(6) Uani 1 1 d . . . C41 C 0.07229(7) 0.60648(19) 0.01167(14) 0.0195(6) Uani 1 1 d . . . C42 C 0.03819(7) 0.6263(2) 0.00245(15) 0.0215(6) Uani 1 1 d . . . H42 H 0.0186 0.6076 -0.0386 0.026 Uiso 1 1 calc R . . C43 C 0.03277(7) 0.6734(2) 0.05313(15) 0.0202(6) Uani 1 1 d . . . C44 C 0.06287(7) 0.70495(19) 0.11209(15) 0.0201(6) Uani 1 1 d . . . H44 H 0.0599 0.7384 0.1460 0.024 Uiso 1 1 calc R . . C45 C -0.00446(7) 0.6907(2) 0.04618(16) 0.0241(7) Uani 1 1 d . . . C46 C -0.03331(8) 0.6417(3) -0.01749(17) 0.0369(8) Uani 1 1 d . . . H46A H -0.0334 0.6657 -0.0591 0.055 Uiso 1 1 calc R . . H46B H -0.0560 0.6529 -0.0194 0.055 Uiso 1 1 calc R . . H46C H -0.0287 0.5756 -0.0142 0.055 Uiso 1 1 calc R . . C47 C -0.00580(8) 0.6518(3) 0.11121(16) 0.0322(8) Uani 1 1 d . . . H47A H -0.0290 0.6626 0.1073 0.048 Uiso 1 1 calc R . . H47B H 0.0118 0.6827 0.1521 0.048 Uiso 1 1 calc R . . H47C H -0.0010 0.5858 0.1148 0.048 Uiso 1 1 calc R . . C48 C -0.01225(10) 0.7953(2) 0.0392(2) 0.0473(10) Uani 1 1 d . . . H48A H -0.0103 0.8193 -0.0003 0.071 Uiso 1 1 calc R . . H48B H 0.0045 0.8267 0.0808 0.071 Uiso 1 1 calc R . . H48C H -0.0359 0.8059 0.0328 0.071 Uiso 1 1 calc R . . C49 C 0.15599(8) 0.5458(2) 0.13126(17) 0.0273(7) Uani 1 1 d . . . H49A H 0.1603 0.5684 0.1768 0.033 Uiso 1 1 calc R . . H49B H 0.1789 0.5386 0.1320 0.033 Uiso 1 1 calc R . . C50 C 0.13798(8) 0.4512(2) 0.11838(15) 0.0242(7) Uani 1 1 d . . . C51 C 0.07552(12) 0.5105(3) 0.7262(2) 0.0568(11) Uani 1 1 d . . . H51A H 0.0721 0.4812 0.6829 0.068 Uiso 1 1 calc R . . H51B H 0.1004 0.5278 0.7520 0.068 Uiso 1 1 calc R . . C8' C 0.1860(3) 0.3825(6) -0.0629(8) 0.083(6) Uani 0.422(11) 1 d PD A 2 H8'1 H 0.1658 0.3503 -0.0980 0.124 Uiso 0.422(11) 1 calc PR A 2 H8'2 H 0.1842 0.3851 -0.0203 0.124 Uiso 0.422(11) 1 calc PR A 2 H8'3 H 0.2073 0.3497 -0.0547 0.124 Uiso 0.422(11) 1 calc PR A 2 C9' C 0.2228(3) 0.5243(9) -0.0420(7) 0.084(7) Uani 0.422(11) 1 d PD A 2 H9'1 H 0.2417 0.4793 -0.0285 0.125 Uiso 0.422(11) 1 calc PR A 2 H9'2 H 0.2229 0.5502 -0.0009 0.125 Uiso 0.422(11) 1 calc PR A 2 H9'3 H 0.2263 0.5735 -0.0684 0.125 Uiso 0.422(11) 1 calc PR A 2 C10' C 0.1850(3) 0.4722(9) -0.1620(4) 0.068(5) Uani 0.422(11) 1 d PD A 2 H10D H 0.1834 0.5345 -0.1798 0.101 Uiso 0.422(11) 1 calc PR A 2 H10E H 0.1643 0.4371 -0.1927 0.101 Uiso 0.422(11) 1 calc PR A 2 H10F H 0.2059 0.4421 -0.1590 0.101 Uiso 0.422(11) 1 calc PR A 2 Cl1 Cl 0.04964(3) 0.61217(7) 0.70608(5) 0.0559(3) Uani 1 1 d . . . Cl2 Cl 0.06590(5) 0.43005(9) 0.77438(6) 0.1018(6) Uani 1 1 d . . . C52 C 0.1943(10) 0.0460(9) 0.8989(9) 0.152(6) Uani 0.573(5) 1 d PD B 1 H52A H 0.1709 0.0235 0.8894 0.182 Uiso 0.573(5) 1 calc PR B 1 H52B H 0.2115 0.0005 0.9292 0.182 Uiso 0.573(5) 1 calc PR B 1 Cl3 Cl 0.20175(10) 0.1473(3) 0.9426(4) 0.187(3) Uani 0.573(5) 1 d PD B 1 Cl4 Cl 0.19634(13) 0.0492(4) 0.8201(2) 0.159(3) Uani 0.573(5) 1 d PD B 1 C52' C 0.1989(12) 0.0293(8) 0.8894(7) 0.152(6) Uani 0.427(5) 1 d PD B 2 H52C H 0.1885 0.0109 0.9191 0.182 Uiso 0.427(5) 1 calc PR B 2 H52D H 0.2234 0.0084 0.9118 0.182 Uiso 0.427(5) 1 calc PR B 2 Cl3' Cl 0.19858(17) 0.1492(3) 0.8849(3) 0.1193(19) Uani 0.427(5) 1 d PD B 2 Cl4' Cl 0.17663(8) -0.0284(3) 0.81041(19) 0.0814(16) Uani 0.427(5) 1 d PD B 2 N1 N 0.11509(6) 1.08501(17) 0.11921(12) 0.0221(5) Uani 1 1 d . . . H1 H 0.1253 1.0568 0.0982 0.027 Uiso 1 1 calc R . . N2 N 0.04161(6) 0.86046(17) -0.07497(12) 0.0243(6) Uani 1 1 d . . . H2 H 0.0642 0.8519 -0.0508 0.029 Uiso 1 1 calc R . . N3 N 0.10177(7) 1.22864(18) 0.15209(13) 0.0269(6) Uani 1 1 d . . . H3A H 0.1018 1.2888 0.1523 0.032 Uiso 1 1 calc R . . H3B H 0.0933 1.1982 0.1754 0.032 Uiso 1 1 calc R . . N4 N -0.00742(6) 0.94860(18) -0.08832(13) 0.0283(6) Uani 1 1 d . . . H4A H -0.0179 0.9880 -0.0738 0.034 Uiso 1 1 calc R . . H4B H -0.0189 0.9238 -0.1291 0.034 Uiso 1 1 calc R . . O1 O 0.08234(5) 0.73381(14) -0.09038(10) 0.0225(4) Uani 1 1 d . . . O2 O -0.00656(6) 0.81491(18) -0.17618(12) 0.0435(6) Uani 1 1 d . . . O3 O 0.04472(6) 0.95786(16) 0.01077(11) 0.0335(5) Uani 1 1 d . . . O4 O 0.16595(5) 0.81597(13) -0.00177(10) 0.0206(4) Uani 1 1 d . . . O5 O 0.19801(6) 0.66617(15) 0.06354(11) 0.0320(5) Uani 1 1 d . . . H5A H 0.1776 0.6867 0.0458 0.048 Uiso 1 1 calc R . . O6 O 0.24952(6) 0.7078(2) 0.07031(13) 0.0484(7) Uani 1 1 d . . . O7 O 0.12501(5) 0.89908(13) 0.10953(9) 0.0189(4) Uani 1 1 d . . . O8 O 0.08506(5) 1.05750(15) 0.18173(11) 0.0272(5) Uani 1 1 d . . . O9 O 0.12741(6) 1.22017(14) 0.08092(11) 0.0285(5) Uani 1 1 d . . . O10 O 0.13537(5) 0.61476(13) 0.07911(10) 0.0210(4) Uani 1 1 d . . . O11 O 0.14736(6) 0.39427(15) 0.08278(12) 0.0333(5) Uani 1 1 d . . . H11 H 0.1369 0.3443 0.0774 0.050 Uiso 1 1 calc R . . O12 O 0.11744(6) 0.43189(15) 0.14101(13) 0.0365(6) Uani 1 1 d . . . S1 S 0.12477(2) 0.80258(5) -0.16459(4) 0.0282(2) Uani 1 1 d . . . S2 S 0.181541(18) 0.99853(5) 0.08768(4) 0.02086(19) Uani 1 1 d . . . S3 S 0.132095(19) 0.72053(5) 0.20426(4) 0.02102(19) Uani 1 1 d . . . S4 S 0.07496(2) 0.53018(5) -0.05010(4) 0.0251(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0178(14) 0.0228(16) 0.0140(14) -0.0062(11) 0.0023(11) 0.0017(12) C2 0.0230(15) 0.0231(16) 0.0132(14) -0.0042(11) 0.0038(12) -0.0022(12) C3 0.0228(15) 0.0304(18) 0.0219(15) -0.0084(13) 0.0118(13) -0.0044(13) C4 0.0226(15) 0.0220(17) 0.0229(15) -0.0082(12) 0.0061(13) -0.0006(12) C5 0.0215(15) 0.0188(15) 0.0210(15) -0.0032(12) 0.0069(12) 0.0003(12) C6 0.0203(14) 0.0247(16) 0.0130(14) -0.0069(11) 0.0036(12) -0.0056(12) C7 0.0249(17) 0.0313(19) 0.044(2) -0.0101(15) 0.0144(15) 0.0026(14) C8 0.054(6) 0.045(6) 0.148(12) 0.019(7) 0.065(8) 0.018(4) C9 0.068(6) 0.106(9) 0.056(6) 0.030(5) 0.029(5) 0.059(6) C10 0.050(5) 0.065(7) 0.094(8) -0.051(6) 0.015(5) 0.019(4) C13 0.0190(15) 0.0267(17) 0.0228(16) 0.0000(12) 0.0084(13) 0.0017(12) C14 0.0227(15) 0.0210(16) 0.0178(14) 0.0006(12) 0.0083(12) -0.0023(12) C11 0.0237(16) 0.0341(18) 0.0200(16) -0.0066(13) 0.0002(13) 0.0051(14) C12 0.0236(16) 0.0314(18) 0.0213(16) -0.0015(13) 0.0048(13) 0.0025(13) C15 0.0160(13) 0.0197(15) 0.0174(14) 0.0031(11) 0.0064(12) 0.0011(11) C16 0.0155(13) 0.0208(15) 0.0167(14) 0.0012(11) 0.0062(12) -0.0014(11) C17 0.0242(15) 0.0215(16) 0.0179(14) 0.0010(12) 0.0098(12) 0.0023(12) C18 0.0225(15) 0.0248(16) 0.0196(15) 0.0061(12) 0.0104(12) 0.0034(12) C19 0.0253(16) 0.0304(17) 0.0128(14) 0.0040(12) 0.0049(12) 0.0017(13) C20 0.0425(19) 0.0317(18) 0.0183(15) 0.0104(13) 0.0158(14) 0.0169(15) C21 0.0371(19) 0.0285(18) 0.041(2) 0.0111(15) 0.0189(16) 0.0120(15) C22 0.171(6) 0.057(3) 0.052(3) 0.042(2) 0.078(4) 0.065(3) C23 0.032(2) 0.051(2) 0.048(2) -0.0093(19) -0.0056(17) 0.0198(18) C24 0.0173(15) 0.0323(18) 0.0237(16) 0.0004(13) 0.0066(13) 0.0012(12) C25 0.0240(17) 0.042(2) 0.0191(16) 0.0026(14) 0.0078(13) 0.0090(14) C26 0.0201(14) 0.0223(15) 0.0115(13) -0.0023(11) 0.0032(11) -0.0015(12) C27 0.0162(14) 0.0193(15) 0.0098(13) -0.0030(11) -0.0011(11) 0.0010(11) C28 0.0205(14) 0.0202(15) 0.0123(13) -0.0030(11) 0.0027(12) -0.0034(12) C29 0.0214(15) 0.0219(16) 0.0155(14) 0.0043(12) 0.0023(12) 0.0007(12) C30 0.0174(15) 0.0300(17) 0.0159(14) 0.0015(12) -0.0010(12) 0.0012(12) C31 0.0140(14) 0.0295(17) 0.0160(14) -0.0018(12) 0.0012(11) -0.0054(12) C32 0.0166(15) 0.046(2) 0.0238(17) 0.0082(15) -0.0018(13) 0.0072(14) C33 0.0236(17) 0.066(3) 0.0246(18) 0.0050(17) -0.0036(14) 0.0010(17) C34 0.0342(19) 0.053(2) 0.037(2) 0.0098(18) 0.0061(16) 0.0204(17) C35 0.0183(17) 0.074(3) 0.033(2) 0.0164(19) 0.0013(15) 0.0085(17) C36 0.0193(14) 0.0252(17) 0.0213(15) 0.0035(12) 0.0087(12) 0.0018(12) C37 0.0135(14) 0.0265(16) 0.0138(14) -0.0003(12) -0.0006(11) 0.0005(12) C38 0.0202(15) 0.0222(16) 0.0150(14) -0.0031(12) 0.0015(12) 0.0013(12) C39 0.0207(15) 0.0159(15) 0.0170(14) 0.0035(11) 0.0047(12) -0.0010(11) C40 0.0166(14) 0.0166(15) 0.0196(14) 0.0030(11) 0.0073(12) -0.0010(11) C41 0.0211(14) 0.0155(15) 0.0189(14) -0.0006(11) 0.0067(12) -0.0025(11) C42 0.0164(14) 0.0220(16) 0.0204(14) -0.0004(12) 0.0037(12) 0.0001(11) C43 0.0186(14) 0.0195(15) 0.0199(15) 0.0047(12) 0.0067(12) -0.0003(11) C44 0.0212(15) 0.0205(15) 0.0192(15) -0.0013(11) 0.0099(12) -0.0002(12) C45 0.0169(14) 0.0273(17) 0.0279(16) 0.0044(13) 0.0102(13) 0.0008(12) C46 0.0161(15) 0.062(2) 0.0266(18) 0.0021(16) 0.0049(14) 0.0024(15) C47 0.0191(15) 0.047(2) 0.0279(17) 0.0029(15) 0.0086(14) -0.0024(14) C48 0.033(2) 0.032(2) 0.086(3) 0.0121(19) 0.036(2) 0.0098(16) C49 0.0205(15) 0.0226(16) 0.0307(17) 0.0027(13) 0.0050(13) 0.0043(12) C50 0.0200(15) 0.0216(16) 0.0242(16) 0.0043(13) 0.0044(13) 0.0062(12) C51 0.062(3) 0.042(2) 0.057(3) 0.005(2) 0.020(2) 0.002(2) C8' 0.079(11) 0.055(8) 0.15(2) 0.023(9) 0.083(13) 0.029(7) C9' 0.023(5) 0.084(10) 0.114(13) -0.051(11) 0.006(8) 0.017(5) C10' 0.073(8) 0.076(9) 0.068(8) -0.014(6) 0.045(7) 0.037(7) Cl1 0.0698(7) 0.0549(6) 0.0352(5) -0.0001(4) 0.0177(5) 0.0141(5) Cl2 0.1549(14) 0.0633(8) 0.0306(6) 0.0056(5) -0.0048(7) -0.0532(9) C52 0.114(9) 0.154(9) 0.170(10) 0.063(8) 0.051(8) -0.015(8) Cl3 0.075(2) 0.113(3) 0.355(10) 0.068(5) 0.083(4) 0.010(2) Cl4 0.149(4) 0.218(5) 0.146(4) 0.111(4) 0.099(3) 0.053(4) C52' 0.114(9) 0.154(9) 0.170(10) 0.063(8) 0.051(8) -0.015(8) Cl3' 0.150(4) 0.088(3) 0.114(4) 0.013(3) 0.057(3) -0.011(3) Cl4' 0.0488(18) 0.111(3) 0.084(2) -0.013(2) 0.0303(16) 0.0040(17) N1 0.0247(13) 0.0202(13) 0.0210(13) -0.0014(10) 0.0102(11) 0.0011(10) N2 0.0175(12) 0.0297(15) 0.0190(13) -0.0045(10) 0.0028(10) 0.0040(10) N3 0.0350(15) 0.0194(13) 0.0250(14) -0.0007(10) 0.0127(12) 0.0035(11) N4 0.0204(13) 0.0351(15) 0.0240(14) -0.0031(11) 0.0056(11) 0.0092(11) O1 0.0184(10) 0.0247(11) 0.0180(10) -0.0047(8) 0.0031(8) 0.0025(8) O2 0.0243(12) 0.0562(17) 0.0314(13) -0.0164(11) -0.0029(11) 0.0102(11) O3 0.0251(11) 0.0416(14) 0.0265(12) -0.0102(10) 0.0058(10) 0.0046(10) O4 0.0185(10) 0.0191(10) 0.0213(10) 0.0025(8) 0.0067(8) 0.0027(8) O5 0.0258(11) 0.0313(13) 0.0325(13) 0.0055(10) 0.0082(10) 0.0088(10) O6 0.0256(13) 0.077(2) 0.0410(15) 0.0231(13) 0.0146(12) 0.0209(12) O7 0.0126(9) 0.0227(11) 0.0153(10) 0.0015(8) 0.0014(8) 0.0032(8) O8 0.0262(11) 0.0278(12) 0.0286(12) -0.0010(9) 0.0137(10) 0.0027(9) O9 0.0414(13) 0.0211(11) 0.0252(12) -0.0021(9) 0.0173(10) -0.0017(10) O10 0.0155(10) 0.0216(11) 0.0230(11) 0.0019(8) 0.0064(8) 0.0028(8) O11 0.0449(13) 0.0214(12) 0.0369(13) 0.0000(10) 0.0217(11) 0.0008(10) O12 0.0367(13) 0.0278(13) 0.0510(15) -0.0052(11) 0.0256(12) -0.0014(10) S1 0.0436(5) 0.0244(4) 0.0163(4) -0.0004(3) 0.0138(4) -0.0001(3) S2 0.0198(4) 0.0204(4) 0.0158(4) 0.0001(3) 0.0026(3) -0.0035(3) S3 0.0213(4) 0.0230(4) 0.0139(4) 0.0011(3) 0.0041(3) -0.0029(3) S4 0.0236(4) 0.0246(4) 0.0277(4) -0.0099(3) 0.0124(3) -0.0077(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(4) . ? C1 C6 1.390(4) . ? C1 O1 1.395(3) . ? C2 C3 1.408(4) . ? C2 S1 1.767(3) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.389(4) . ? C4 C7 1.535(4) . ? C5 C6 1.392(4) . ? C5 H5 0.9300 . ? C6 S4 1.774(3) . ? C7 C8 1.431(9) . ? C7 C8' 1.448(7) . ? C7 C10 1.493(8) . ? C7 C9' 1.521(7) . ? C7 C10' 1.591(7) . ? C7 C9 1.619(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C13 O3 1.227(4) . ? C13 N4 1.325(4) . ? C13 N2 1.412(4) . ? C14 C15 1.392(4) . ? C14 C19 1.394(4) . ? C14 S1 1.771(3) . ? C11 O1 1.432(3) . ? C11 C12 1.510(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.223(4) . ? C12 N2 1.365(4) . ? C15 C16 1.389(4) . ? C15 O4 1.395(3) . ? C16 C17 1.394(4) . ? C16 S2 1.780(3) . ? C17 C18 1.396(4) . ? C17 H17 0.9300 . ? C18 C19 1.394(4) . ? C18 C20 1.524(4) . ? C19 H19 0.9300 . ? C20 C21 1.520(5) . ? C20 C23 1.523(5) . ? C20 C22 1.544(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O4 1.419(3) . ? C24 C25 1.521(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O6 1.197(4) . ? C25 O5 1.328(4) . ? C26 C31 1.396(4) . ? C26 C27 1.398(4) . ? C26 S2 1.773(3) . ? C27 O7 1.382(3) . ? C27 C28 1.398(4) . ? C28 C29 1.388(4) . ? C28 S3 1.776(3) . ? C29 C30 1.395(4) . ? C29 H29 0.9300 . ? C30 C31 1.390(4) . ? C30 C32 1.530(4) . ? C31 H31 0.9300 . ? C32 C35 1.532(5) . ? C32 C34 1.539(5) . ? C32 C33 1.539(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O7 1.436(3) . ? C36 C37 1.510(4) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O8 1.220(3) . ? C37 N1 1.359(4) . ? C38 O9 1.232(3) . ? C38 N3 1.320(4) . ? C38 N1 1.400(4) . ? C39 C44 1.390(4) . ? C39 C40 1.393(4) . ? C39 S3 1.773(3) . ? C40 O10 1.387(3) . ? C40 C41 1.397(4) . ? C41 C42 1.395(4) . ? C41 S4 1.767(3) . ? C42 C43 1.392(4) . ? C42 H42 0.9300 . ? C43 C44 1.396(4) . ? C43 C45 1.536(4) . ? C44 H44 0.9300 . ? C45 C46 1.523(4) . ? C45 C48 1.523(4) . ? C45 C47 1.536(4) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 O10 1.446(3) . ? C49 C50 1.514(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 O12 1.212(4) . ? C50 O11 1.302(4) . ? C51 Cl2 1.723(4) . ? C51 Cl1 1.749(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C8' H8'1 0.9600 . ? C8' H8'2 0.9600 . ? C8' H8'3 0.9600 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C52 Cl3 1.676(9) . ? C52 Cl4 1.746(10) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C52' Cl3' 1.714(10) . ? C52' Cl4' 1.729(10) . ? C52' H52C 0.9700 . ? C52' H52D 0.9700 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? O5 H5A 0.8200 . ? O11 H11 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.8(3) . . ? C2 C1 O1 120.4(3) . . ? C6 C1 O1 120.6(2) . . ? C1 C2 C3 120.1(3) . . ? C1 C2 S1 122.9(2) . . ? C3 C2 S1 116.8(2) . . ? C4 C3 C2 121.7(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 117.5(3) . . ? C3 C4 C7 121.2(3) . . ? C5 C4 C7 121.3(3) . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 120.3(3) . . ? C1 C6 S4 122.7(2) . . ? C5 C6 S4 116.6(2) . . ? C8 C7 C8' 126.1(6) . . ? C8 C7 C10 115.7(7) . . ? C8' C7 C9' 112.4(6) . . ? C10 C7 C9' 142.1(6) . . ? C8 C7 C4 116.0(5) . . ? C8' C7 C4 116.1(5) . . ? C10 C7 C4 109.1(4) . . ? C9' C7 C4 107.8(5) . . ? C8' C7 C10' 109.1(6) . . ? C9' C7 C10' 103.8(6) . . ? C4 C7 C10' 106.8(4) . . ? C8 C7 C9 105.2(7) . . ? C8' C7 C9 46.8(6) . . ? C10 C7 C9 103.2(7) . . ? C4 C7 C9 106.2(4) . . ? C10' C7 C9 145.9(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? O3 C13 N4 124.5(3) . . ? O3 C13 N2 118.6(3) . . ? N4 C13 N2 116.9(3) . . ? C15 C14 C19 120.3(3) . . ? C15 C14 S1 124.3(2) . . ? C19 C14 S1 114.8(2) . . ? O1 C11 C12 110.0(2) . . ? O1 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O1 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O2 C12 N2 124.2(3) . . ? O2 C12 C11 118.8(3) . . ? N2 C12 C11 117.0(3) . . ? C16 C15 C14 119.3(3) . . ? C16 C15 O4 120.2(2) . . ? C14 C15 O4 120.5(2) . . ? C15 C16 C17 119.8(3) . . ? C15 C16 S2 124.7(2) . . ? C17 C16 S2 114.9(2) . . ? C16 C17 C18 121.7(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 117.7(3) . . ? C19 C18 C20 120.1(3) . . ? C17 C18 C20 122.2(3) . . ? C14 C19 C18 121.1(3) . . ? C14 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C21 C20 C23 109.5(3) . . ? C21 C20 C18 112.5(3) . . ? C23 C20 C18 107.7(3) . . ? C21 C20 C22 108.2(3) . . ? C23 C20 C22 109.2(4) . . ? C18 C20 C22 109.6(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 C25 108.1(2) . . ? O4 C24 H24A 110.1 . . ? C25 C24 H24A 110.1 . . ? O4 C24 H24B 110.1 . . ? C25 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? O6 C25 O5 121.6(3) . . ? O6 C25 C24 121.4(3) . . ? O5 C25 C24 117.0(3) . . ? C31 C26 C27 120.1(3) . . ? C31 C26 S2 117.0(2) . . ? C27 C26 S2 122.5(2) . . ? O7 C27 C26 117.7(2) . . ? O7 C27 C28 123.6(2) . . ? C26 C27 C28 118.6(2) . . ? C29 C28 C27 119.2(3) . . ? C29 C28 S3 115.6(2) . . ? C27 C28 S3 125.0(2) . . ? C28 C29 C30 123.5(3) . . ? C28 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C31 C30 C29 116.0(3) . . ? C31 C30 C32 124.1(3) . . ? C29 C30 C32 119.9(3) . . ? C30 C31 C26 122.3(3) . . ? C30 C31 H31 118.9 . . ? C26 C31 H31 118.9 . . ? C30 C32 C35 111.3(3) . . ? C30 C32 C34 109.4(3) . . ? C35 C32 C34 109.1(3) . . ? C30 C32 C33 108.5(3) . . ? C35 C32 C33 109.3(3) . . ? C34 C32 C33 109.2(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O7 C36 C37 114.1(2) . . ? O7 C36 H36A 108.7 . . ? C37 C36 H36A 108.7 . . ? O7 C36 H36B 108.7 . . ? C37 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? O8 C37 N1 124.2(3) . . ? O8 C37 C36 119.1(3) . . ? N1 C37 C36 116.7(2) . . ? O9 C38 N3 124.8(3) . . ? O9 C38 N1 117.8(3) . . ? N3 C38 N1 117.5(3) . . ? C44 C39 C40 119.7(3) . . ? C44 C39 S3 115.8(2) . . ? C40 C39 S3 123.8(2) . . ? O10 C40 C39 122.9(2) . . ? O10 C40 C41 117.8(2) . . ? C39 C40 C41 119.2(2) . . ? C42 C41 C40 119.9(3) . . ? C42 C41 S4 116.3(2) . . ? C40 C41 S4 123.2(2) . . ? C43 C42 C41 121.7(3) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C44 117.3(2) . . ? C42 C43 C45 122.6(3) . . ? C44 C43 C45 120.1(3) . . ? C39 C44 C43 122.1(3) . . ? C39 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C46 C45 C48 108.4(3) . . ? C46 C45 C43 112.0(2) . . ? C48 C45 C43 109.5(2) . . ? C46 C45 C47 107.7(2) . . ? C48 C45 C47 110.3(3) . . ? C43 C45 C47 109.0(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O10 C49 C50 113.2(2) . . ? O10 C49 H49A 108.9 . . ? C50 C49 H49A 108.9 . . ? O10 C49 H49B 108.9 . . ? C50 C49 H49B 108.9 . . ? H49A C49 H49B 107.8 . . ? O12 C50 O11 124.8(3) . . ? O12 C50 C49 121.7(3) . . ? O11 C50 C49 113.5(3) . . ? Cl2 C51 Cl1 114.0(3) . . ? Cl2 C51 H51A 108.8 . . ? Cl1 C51 H51A 108.8 . . ? Cl2 C51 H51B 108.8 . . ? Cl1 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? C7 C8' H8'1 109.5 . . ? C7 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7 C9' H9'1 109.5 . . ? C7 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C7 C10' H10D 109.5 . . ? C7 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? Cl3 C52 Cl4 116.4(8) . . ? Cl3 C52 H52A 108.2 . . ? Cl4 C52 H52A 108.2 . . ? Cl3 C52 H52B 108.2 . . ? Cl4 C52 H52B 108.2 . . ? H52A C52 H52B 107.3 . . ? Cl3' C52' Cl4' 115.7(9) . . ? Cl3' C52' H52C 108.3 . . ? Cl4' C52' H52C 108.3 . . ? Cl3' C52' H52D 108.3 . . ? Cl4' C52' H52D 108.3 . . ? H52C C52' H52D 107.4 . . ? C37 N1 C38 128.2(3) . . ? C37 N1 H1 115.9 . . ? C38 N1 H1 115.9 . . ? C12 N2 C13 128.1(2) . . ? C12 N2 H2 116.0 . . ? C13 N2 H2 116.0 . . ? C38 N3 H3A 120.0 . . ? C38 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C13 N4 H4A 120.0 . . ? C13 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C1 O1 C11 115.9(2) . . ? C15 O4 C24 115.7(2) . . ? C25 O5 H5A 109.5 . . ? C27 O7 C36 116.5(2) . . ? C40 O10 C49 116.4(2) . . ? C50 O11 H11 109.5 . . ? C2 S1 C14 107.00(13) . . ? C26 S2 C16 108.24(13) . . ? C39 S3 C28 106.38(13) . . ? C41 S4 C6 106.43(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.3(4) . . . . ? O1 C1 C2 C3 172.9(2) . . . . ? C6 C1 C2 S1 171.0(2) . . . . ? O1 C1 C2 S1 -13.8(4) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? S1 C2 C3 C4 -173.9(2) . . . . ? C2 C3 C4 C5 2.0(4) . . . . ? C2 C3 C4 C7 -177.0(3) . . . . ? C3 C4 C5 C6 -1.5(4) . . . . ? C7 C4 C5 C6 177.5(3) . . . . ? C2 C1 C6 C5 2.8(4) . . . . ? O1 C1 C6 C5 -172.4(2) . . . . ? C2 C1 C6 S4 -169.8(2) . . . . ? O1 C1 C6 S4 15.0(4) . . . . ? C4 C5 C6 C1 -0.9(4) . . . . ? C4 C5 C6 S4 172.2(2) . . . . ? C3 C4 C7 C8 19.3(8) . . . . ? C5 C4 C7 C8 -159.6(7) . . . . ? C3 C4 C7 C8' -174.9(8) . . . . ? C5 C4 C7 C8' 6.2(8) . . . . ? C3 C4 C7 C10 -113.5(6) . . . . ? C5 C4 C7 C10 67.5(6) . . . . ? C3 C4 C7 C9' 58.0(8) . . . . ? C5 C4 C7 C9' -120.9(7) . . . . ? C3 C4 C7 C10' -53.0(6) . . . . ? C5 C4 C7 C10' 128.1(6) . . . . ? C3 C4 C7 C9 135.8(6) . . . . ? C5 C4 C7 C9 -43.1(6) . . . . ? O1 C11 C12 O2 -172.2(3) . . . . ? O1 C11 C12 N2 6.7(4) . . . . ? C19 C14 C15 C16 -2.9(4) . . . . ? S1 C14 C15 C16 167.9(2) . . . . ? C19 C14 C15 O4 175.8(2) . . . . ? S1 C14 C15 O4 -13.4(4) . . . . ? C14 C15 C16 C17 2.0(4) . . . . ? O4 C15 C16 C17 -176.7(2) . . . . ? C14 C15 C16 S2 -168.2(2) . . . . ? O4 C15 C16 S2 13.1(4) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? S2 C16 C17 C18 171.1(2) . . . . ? C16 C17 C18 C19 -1.0(4) . . . . ? C16 C17 C18 C20 178.1(3) . . . . ? C15 C14 C19 C18 2.0(4) . . . . ? S1 C14 C19 C18 -169.7(2) . . . . ? C17 C18 C19 C14 0.0(4) . . . . ? C20 C18 C19 C14 -179.1(3) . . . . ? C19 C18 C20 C21 -169.0(3) . . . . ? C17 C18 C20 C21 12.0(4) . . . . ? C19 C18 C20 C23 70.2(3) . . . . ? C17 C18 C20 C23 -108.8(3) . . . . ? C19 C18 C20 C22 -48.6(4) . . . . ? C17 C18 C20 C22 132.4(4) . . . . ? O4 C24 C25 O6 -171.2(3) . . . . ? O4 C24 C25 O5 8.5(4) . . . . ? C31 C26 C27 O7 176.7(2) . . . . ? S2 C26 C27 O7 3.9(3) . . . . ? C31 C26 C27 C28 -5.1(4) . . . . ? S2 C26 C27 C28 -177.9(2) . . . . ? O7 C27 C28 C29 -176.3(2) . . . . ? C26 C27 C28 C29 5.6(4) . . . . ? O7 C27 C28 S3 -2.4(4) . . . . ? C26 C27 C28 S3 179.4(2) . . . . ? C27 C28 C29 C30 -1.7(4) . . . . ? S3 C28 C29 C30 -176.1(2) . . . . ? C28 C29 C30 C31 -2.7(4) . . . . ? C28 C29 C30 C32 178.4(3) . . . . ? C29 C30 C31 C26 3.3(4) . . . . ? C32 C30 C31 C26 -177.9(3) . . . . ? C27 C26 C31 C30 0.6(4) . . . . ? S2 C26 C31 C30 173.8(2) . . . . ? C31 C30 C32 C35 -2.7(5) . . . . ? C29 C30 C32 C35 176.1(3) . . . . ? C31 C30 C32 C34 -123.4(3) . . . . ? C29 C30 C32 C34 55.4(4) . . . . ? C31 C30 C32 C33 117.6(3) . . . . ? C29 C30 C32 C33 -63.6(4) . . . . ? O7 C36 C37 O8 176.4(2) . . . . ? O7 C36 C37 N1 -4.7(3) . . . . ? C44 C39 C40 O10 -179.2(2) . . . . ? S3 C39 C40 O10 -9.3(4) . . . . ? C44 C39 C40 C41 4.4(4) . . . . ? S3 C39 C40 C41 174.4(2) . . . . ? O10 C40 C41 C42 -179.5(2) . . . . ? C39 C40 C41 C42 -3.0(4) . . . . ? O10 C40 C41 S4 10.1(4) . . . . ? C39 C40 C41 S4 -173.4(2) . . . . ? C40 C41 C42 C43 -1.1(4) . . . . ? S4 C41 C42 C43 170.0(2) . . . . ? C41 C42 C43 C44 3.6(4) . . . . ? C41 C42 C43 C45 -176.1(3) . . . . ? C40 C39 C44 C43 -1.9(4) . . . . ? S3 C39 C44 C43 -172.6(2) . . . . ? C42 C43 C44 C39 -2.1(4) . . . . ? C45 C43 C44 C39 177.6(3) . . . . ? C42 C43 C45 C46 6.1(4) . . . . ? C44 C43 C45 C46 -173.6(3) . . . . ? C42 C43 C45 C48 -114.1(3) . . . . ? C44 C43 C45 C48 66.2(4) . . . . ? C42 C43 C45 C47 125.2(3) . . . . ? C44 C43 C45 C47 -54.5(4) . . . . ? O10 C49 C50 O12 -88.1(4) . . . . ? O10 C49 C50 O11 93.3(3) . . . . ? O8 C37 N1 C38 2.3(4) . . . . ? C36 C37 N1 C38 -176.5(3) . . . . ? O9 C38 N1 C37 -176.7(3) . . . . ? N3 C38 N1 C37 5.1(4) . . . . ? O2 C12 N2 C13 2.6(5) . . . . ? C11 C12 N2 C13 -176.3(3) . . . . ? O3 C13 N2 C12 171.7(3) . . . . ? N4 C13 N2 C12 -7.8(5) . . . . ? C2 C1 O1 C11 93.3(3) . . . . ? C6 C1 O1 C11 -91.6(3) . . . . ? C12 C11 O1 C1 177.4(2) . . . . ? C16 C15 O4 C24 -88.5(3) . . . . ? C14 C15 O4 C24 92.8(3) . . . . ? C25 C24 O4 C15 175.9(2) . . . . ? C26 C27 O7 C36 -127.5(3) . . . . ? C28 C27 O7 C36 54.4(3) . . . . ? C37 C36 O7 C27 116.9(3) . . . . ? C39 C40 O10 C49 73.0(3) . . . . ? C41 C40 O10 C49 -110.7(3) . . . . ? C50 C49 O10 C40 60.3(3) . . . . ? C1 C2 S1 C14 55.0(3) . . . . ? C3 C2 S1 C14 -131.5(2) . . . . ? C15 C14 S1 C2 42.2(3) . . . . ? C19 C14 S1 C2 -146.5(2) . . . . ? C31 C26 S2 C16 126.2(2) . . . . ? C27 C26 S2 C16 -60.7(3) . . . . ? C15 C16 S2 C26 -43.4(3) . . . . ? C17 C16 S2 C26 146.1(2) . . . . ? C44 C39 S3 C28 -135.7(2) . . . . ? C40 C39 S3 C28 54.0(3) . . . . ? C29 C28 S3 C39 -128.3(2) . . . . ? C27 C28 S3 C39 57.7(3) . . . . ? C42 C41 S4 C6 137.9(2) . . . . ? C40 C41 S4 C6 -51.4(3) . . . . ? C1 C6 S4 C41 -56.1(3) . . . . ? C5 C6 S4 C41 131.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C36 H36A S3 0.97 2.64 3.139(3) 112.2 . C49 H49A S3 0.97 2.68 3.351(3) 127.1 . C17 H17 O9 0.93 2.57 3.459(4) 160.7 . O5 H5A O10 0.82 2.45 2.924(3) 117.9 . O5 H5A O4 0.82 2.06 2.577(3) 120.8 . N4 H4B O2 0.86 2.05 2.704(3) 131.7 . N3 H3B O8 0.86 2.06 2.704(3) 131.5 . N2 H2 O1 0.86 2.19 2.628(3) 111.5 . N1 H1 O7 0.86 2.27 2.712(3) 112.3 . N1 H1 S2 0.86 2.63 3.424(2) 153.2 . O11 H11 O9 0.82 1.83 2.621(3) 162.6 1_545 N4 H4B O8 0.86 2.51 2.961(3) 113.8 5_575 N4 H4A O3 0.86 2.28 3.091(3) 157.7 5_575 N3 H3A O12 0.86 2.20 3.013(3) 158.2 1_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.041 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.112 # start Validation Reply Form _vrf_PLAT222_2 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.21 Ratio RESPONSE: This is due to the disorder of the tertiary butyl group. ; _vrf_PLAT213_2 ; PROBLEM: Atom C22 has ADP max/min Ratio ..... 4.30 prola RESPONSE: This is due to the disorder of the tertiary butyl group. ; _vrf_PLAT220_2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.69 Ratio RESPONSE: This is due to the disorder of the tertiary butyl group. ; _vrf_PLAT242_2 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C7 RESPONSE: This is due to the disorder of the tertiary butyl group. ; # end Validation Reply Form data_3 _database_code_depnum_ccdc_archive 'CCDC 760513' #TrackingRef '- data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H60 N4 O12 S4' _chemical_formula_weight 1037.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 24.5640(7) _cell_length_b 20.0520(5) _cell_length_c 10.7714(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.394(2) _cell_angle_gamma 90.00 _cell_volume 5296.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3339 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 21.25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9623 _exptl_absorpt_correction_T_max 0.9809 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15406 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4648 _reflns_number_gt 3483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+10.8217P] 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 4648 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.2161 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.51653(17) 0.1759(2) 0.4180(4) 0.0464(11) Uani 1 1 d . . . C2 C 0.48463(18) 0.1226(2) 0.3764(4) 0.0486(11) Uani 1 1 d . . . C3 C 0.44166(18) 0.1013(2) 0.4444(5) 0.0521(12) Uani 1 1 d . . . H3 H 0.4212 0.0648 0.4159 0.062 Uiso 1 1 calc R . . C4 C 0.42833(16) 0.1323(2) 0.5527(4) 0.0436(10) Uani 1 1 d . . . C5 C 0.45897(18) 0.1872(2) 0.5893(4) 0.0470(11) Uani 1 1 d . . . H5 H 0.4500 0.2102 0.6602 0.056 Uiso 1 1 calc R . . C6 C 0.50273(17) 0.2098(2) 0.5247(4) 0.0460(11) Uani 1 1 d . . . C7 C 0.38144(19) 0.1083(2) 0.6297(5) 0.0560(13) Uani 1 1 d . . . C8 C 0.4051(3) 0.0894(3) 0.7599(6) 0.0852(19) Uani 1 1 d . . . H8A H 0.3764 0.0730 0.8085 0.128 Uiso 1 1 calc R . . H8B H 0.4213 0.1281 0.7996 0.128 Uiso 1 1 calc R . . H8C H 0.4322 0.0555 0.7532 0.128 Uiso 1 1 calc R . . C9 C 0.3522(3) 0.0490(5) 0.5735(8) 0.140(4) Uani 1 1 d . . . H9A H 0.3253 0.0340 0.6282 0.209 Uiso 1 1 calc R . . H9B H 0.3779 0.0139 0.5616 0.209 Uiso 1 1 calc R . . H9C H 0.3347 0.0613 0.4948 0.209 Uiso 1 1 calc R . . C10 C 0.3413(3) 0.1660(4) 0.6432(8) 0.109(3) Uani 1 1 d . . . H10A H 0.3245 0.1770 0.5631 0.163 Uiso 1 1 calc R . . H10B H 0.3606 0.2042 0.6770 0.163 Uiso 1 1 calc R . . H10C H 0.3138 0.1530 0.6980 0.163 Uiso 1 1 calc R . . C11 C 0.6075(2) 0.1631(3) 0.3735(6) 0.0783(17) Uani 1 1 d . . . H11A H 0.6009 0.1157 0.3639 0.094 Uiso 1 1 calc R . . H11B H 0.6222 0.1712 0.4578 0.094 Uiso 1 1 calc R . . C12 C 0.6485(2) 0.1862(3) 0.2806(5) 0.0690(15) Uani 1 1 d . . . C13 C 0.56472(17) 0.3281(2) 0.4862(4) 0.0424(10) Uani 1 1 d . . . C14 C 0.52689(16) 0.3660(2) 0.4182(4) 0.0436(10) Uani 1 1 d . . . C15 C 0.54528(18) 0.4131(2) 0.3363(4) 0.0474(11) Uani 1 1 d . . . C16 C 0.60092(18) 0.4240(2) 0.3306(4) 0.0466(11) Uani 1 1 d . . . H16 H 0.6128 0.4554 0.2747 0.056 Uiso 1 1 calc R . . C17 C 0.63907(16) 0.3899(2) 0.4048(4) 0.0383(9) Uani 1 1 d . . . C18 C 0.61943(17) 0.3407(2) 0.4794(4) 0.0433(10) Uani 1 1 d . . . H18 H 0.6442 0.3149 0.5271 0.052 Uiso 1 1 calc R . . C19 C 0.70032(17) 0.4072(3) 0.4121(4) 0.0536(12) Uani 1 1 d . . . C20 C 0.7355(2) 0.3452(4) 0.4207(7) 0.092(2) Uani 1 1 d . . . H20A H 0.7316 0.3211 0.3437 0.139 Uiso 1 1 calc R . . H20B H 0.7243 0.3174 0.4871 0.139 Uiso 1 1 calc R . . H20C H 0.7730 0.3577 0.4367 0.139 Uiso 1 1 calc R . . C21 C 0.7162(2) 0.4461(4) 0.3003(6) 0.091(2) Uani 1 1 d . . . H21A H 0.7538 0.4589 0.3112 0.137 Uiso 1 1 calc R . . H21B H 0.6939 0.4854 0.2912 0.137 Uiso 1 1 calc R . . H21C H 0.7110 0.4190 0.2272 0.137 Uiso 1 1 calc R . . C22 C 0.7103(3) 0.4495(4) 0.5296(7) 0.114(3) Uani 1 1 d . . . H22A H 0.7481 0.4618 0.5386 0.171 Uiso 1 1 calc R . . H22B H 0.7009 0.4241 0.6008 0.171 Uiso 1 1 calc R . . H22C H 0.6883 0.4890 0.5231 0.171 Uiso 1 1 calc R . . C23 C 0.4564(2) 0.3984(4) 0.5402(7) 0.097(2) Uani 1 1 d . . . H23A H 0.4572 0.4453 0.5181 0.116 Uiso 1 1 calc R . . H23B H 0.4830 0.3914 0.6093 0.116 Uiso 1 1 calc R . . C24 C 0.4001(2) 0.3808(3) 0.5809(6) 0.0772(17) Uani 1 1 d . . . C25 C 0.3173(2) 0.3208(3) 0.5103(6) 0.0663(15) Uani 1 1 d . . . N1 N 0.37072(16) 0.3431(2) 0.5004(4) 0.0630(11) Uani 1 1 d . . . H1 H 0.3864 0.3311 0.4347 0.076 Uiso 1 1 calc R . . N2 N 0.29225(19) 0.3383(3) 0.6101(5) 0.0898(17) Uani 1 1 d . . . H2A H 0.2593 0.3254 0.6192 0.108 Uiso 1 1 calc R . . H2B H 0.3088 0.3627 0.6662 0.108 Uiso 1 1 calc R . . O1 O 0.55879(12) 0.19835(16) 0.3514(3) 0.0547(8) Uani 1 1 d . . . O2 O 0.6877(2) 0.1544(3) 0.2661(5) 0.122(2) Uani 1 1 d . . . O3 O 0.63512(16) 0.2410(2) 0.2248(4) 0.0856(13) Uani 1 1 d . . . H3A H 0.6584 0.2509 0.1764 0.128 Uiso 1 1 calc R . . O4 O 0.47163(12) 0.35922(17) 0.4358(3) 0.0634(10) Uani 1 1 d . . . O5 O 0.38473(18) 0.4031(3) 0.6771(5) 0.1123(18) Uani 1 1 d . . . O6 O 0.29589(14) 0.2851(2) 0.4239(4) 0.0826(12) Uani 1 1 d . . . S1 S 0.5000 0.07082(8) 0.2500 0.0721(7) Uani 1 2 d S . . S2 S 0.54500(6) 0.27081(8) 0.59993(11) 0.0750(5) Uani 1 1 d . . . S3 S 0.5000 0.46706(9) 0.2500 0.0862(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(2) 0.050(3) 0.049(3) 0.022(2) 0.0118(19) -0.004(2) C2 0.050(3) 0.038(2) 0.060(3) 0.010(2) 0.018(2) 0.000(2) C3 0.050(3) 0.036(2) 0.073(3) 0.001(2) 0.020(2) -0.011(2) C4 0.037(2) 0.039(2) 0.055(3) 0.007(2) 0.0078(19) -0.0028(18) C5 0.049(3) 0.057(3) 0.036(2) 0.006(2) 0.0090(19) -0.008(2) C6 0.047(2) 0.053(3) 0.038(2) 0.011(2) 0.0058(19) -0.013(2) C7 0.046(3) 0.055(3) 0.070(3) 0.009(2) 0.021(2) -0.012(2) C8 0.083(4) 0.087(4) 0.089(4) 0.036(4) 0.031(3) -0.011(3) C9 0.124(6) 0.169(8) 0.133(7) -0.050(6) 0.070(5) -0.103(6) C10 0.062(4) 0.116(6) 0.154(7) 0.043(5) 0.051(4) 0.023(4) C11 0.051(3) 0.109(5) 0.076(4) 0.026(3) 0.020(3) 0.003(3) C12 0.051(3) 0.085(4) 0.072(4) 0.005(3) 0.006(3) 0.009(3) C13 0.046(2) 0.046(3) 0.036(2) -0.0021(18) 0.0028(18) -0.0151(19) C14 0.034(2) 0.041(2) 0.056(3) -0.014(2) 0.0024(19) -0.0102(18) C15 0.046(3) 0.032(2) 0.062(3) -0.008(2) -0.014(2) -0.0025(19) C16 0.049(3) 0.040(2) 0.049(3) 0.010(2) -0.004(2) -0.0152(19) C17 0.035(2) 0.043(2) 0.037(2) -0.0024(18) -0.0005(17) -0.0065(17) C18 0.040(2) 0.052(3) 0.037(2) 0.0100(19) -0.0048(17) -0.0077(19) C19 0.034(2) 0.073(3) 0.055(3) 0.004(2) 0.0073(19) -0.016(2) C20 0.039(3) 0.119(5) 0.119(5) 0.026(4) 0.003(3) 0.008(3) C21 0.055(3) 0.114(5) 0.107(5) 0.033(4) 0.032(3) -0.012(3) C22 0.066(4) 0.173(7) 0.104(5) -0.057(5) 0.012(4) -0.070(5) C23 0.055(3) 0.106(5) 0.133(6) -0.054(5) 0.035(4) -0.017(3) C24 0.071(4) 0.072(4) 0.091(4) -0.021(3) 0.027(3) -0.002(3) C25 0.044(3) 0.082(4) 0.075(4) -0.006(3) 0.016(3) -0.002(3) N1 0.043(2) 0.073(3) 0.075(3) -0.011(2) 0.013(2) -0.004(2) N2 0.062(3) 0.121(4) 0.091(4) -0.027(3) 0.037(3) -0.017(3) O1 0.0450(18) 0.067(2) 0.0540(19) 0.0205(16) 0.0164(14) -0.0077(15) O2 0.077(3) 0.152(5) 0.141(4) 0.046(4) 0.047(3) 0.042(3) O3 0.074(3) 0.088(3) 0.099(3) 0.026(2) 0.042(2) 0.008(2) O4 0.0312(16) 0.072(2) 0.087(2) -0.0250(19) 0.0047(15) -0.0142(15) O5 0.082(3) 0.141(4) 0.118(4) -0.063(3) 0.041(3) -0.012(3) O6 0.044(2) 0.114(3) 0.092(3) -0.014(3) 0.0229(19) -0.008(2) S1 0.0994(15) 0.0339(9) 0.0886(14) 0.000 0.0525(12) 0.000 S2 0.0869(10) 0.1003(11) 0.0368(7) 0.0152(7) -0.0031(6) -0.0557(9) S3 0.0772(14) 0.0330(9) 0.140(2) 0.000 -0.0610(14) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.372(5) . ? C1 C2 1.384(6) . ? C1 C6 1.394(6) . ? C2 C3 1.387(6) . ? C2 S1 1.771(5) . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(6) . ? C4 C7 1.537(6) . ? C5 C6 1.390(6) . ? C5 H5 0.9300 . ? C6 S2 1.769(5) . ? C7 C9 1.497(8) . ? C7 C10 1.532(8) . ? C7 C8 1.533(8) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.399(6) . ? C11 C12 1.532(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.173(7) . ? C12 O3 1.286(6) . ? C13 C18 1.373(6) . ? C13 C14 1.377(6) . ? C13 S2 1.768(4) . ? C14 C15 1.386(6) . ? C14 O4 1.388(5) . ? C15 C16 1.389(6) . ? C15 S3 1.775(4) . ? C16 C17 1.376(6) . ? C16 H16 0.9300 . ? C17 C18 1.379(6) . ? C17 C19 1.542(6) . ? C18 H18 0.9300 . ? C19 C21 1.506(7) . ? C19 C20 1.515(8) . ? C19 C22 1.530(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O4 1.439(7) . ? C23 C24 1.517(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O5 1.209(6) . ? C24 N1 1.332(7) . ? C25 O6 1.264(6) . ? C25 N2 1.318(7) . ? C25 N1 1.396(6) . ? N1 H1 0.8600 . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? O3 H3A 0.8200 . ? S1 C2 1.771(5) 2_655 ? S3 C15 1.775(4) 2_655 ? 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 O1 C1 C2 121.0(4) . . ? O1 C1 C6 119.9(4) . . ? C2 C1 C6 118.9(4) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 S1 124.0(3) . . ? C3 C2 S1 115.3(3) . . ? C4 C3 C2 122.2(4) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 116.7(4) . . ? C5 C4 C7 120.7(4) . . ? C3 C4 C7 122.6(4) . . ? C4 C5 C6 122.9(4) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 119.1(4) . . ? C5 C6 S2 116.5(3) . . ? C1 C6 S2 123.4(3) . . ? C9 C7 C10 110.0(6) . . ? C9 C7 C8 108.7(5) . . ? C10 C7 C8 108.0(5) . . ? C9 C7 C4 112.8(4) . . ? C10 C7 C4 108.7(4) . . ? C8 C7 C4 108.4(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 109.0(4) . . ? O1 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O1 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O2 C12 O3 126.3(6) . . ? O2 C12 C11 119.9(6) . . ? O3 C12 C11 113.9(5) . . ? C18 C13 C14 120.2(4) . . ? C18 C13 S2 117.7(3) . . ? C14 C13 S2 121.5(3) . . ? C13 C14 C15 118.6(4) . . ? C13 C14 O4 120.5(4) . . ? C15 C14 O4 120.8(4) . . ? C14 C15 C16 119.6(4) . . ? C14 C15 S3 122.1(3) . . ? C16 C15 S3 117.9(3) . . ? C17 C16 C15 122.2(4) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C18 116.4(4) . . ? C16 C17 C19 123.2(4) . . ? C18 C17 C19 120.3(4) . . ? C13 C18 C17 122.6(4) . . ? C13 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C21 C19 C20 107.5(5) . . ? C21 C19 C22 109.8(5) . . ? C20 C19 C22 109.9(5) . . ? C21 C19 C17 111.9(4) . . ? C20 C19 C17 111.7(4) . . ? C22 C19 C17 106.0(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C23 C24 112.4(5) . . ? O4 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O4 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? O5 C24 N1 125.7(5) . . ? O5 C24 C23 119.9(6) . . ? N1 C24 C23 114.4(5) . . ? O6 C25 N2 123.9(5) . . ? O6 C25 N1 118.5(5) . . ? N2 C25 N1 117.6(5) . . ? C24 N1 C25 127.5(5) . . ? C24 N1 H1 116.3 . . ? C25 N1 H1 116.3 . . ? C25 N2 H2A 120.0 . . ? C25 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C1 O1 C11 114.4(4) . . ? C12 O3 H3A 109.5 . . ? C14 O4 C23 110.8(3) . . ? C2 S1 C2 108.2(3) 2_655 . ? C13 S2 C6 108.00(19) . . ? C15 S3 C15 104.8(3) 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.2(4) . . . . ? C6 C1 C2 C3 -3.7(7) . . . . ? O1 C1 C2 S1 9.7(6) . . . . ? C6 C1 C2 S1 -174.8(3) . . . . ? C1 C2 C3 C4 1.4(7) . . . . ? S1 C2 C3 C4 173.2(4) . . . . ? C2 C3 C4 C5 1.7(7) . . . . ? C2 C3 C4 C7 -178.9(4) . . . . ? C3 C4 C5 C6 -2.4(7) . . . . ? C7 C4 C5 C6 178.2(4) . . . . ? C4 C5 C6 C1 0.1(7) . . . . ? C4 C5 C6 S2 -168.6(4) . . . . ? O1 C1 C6 C5 178.5(4) . . . . ? C2 C1 C6 C5 3.0(6) . . . . ? O1 C1 C6 S2 -13.6(6) . . . . ? C2 C1 C6 S2 170.9(3) . . . . ? C5 C4 C7 C9 178.7(6) . . . . ? C3 C4 C7 C9 -0.7(8) . . . . ? C5 C4 C7 C10 56.3(7) . . . . ? C3 C4 C7 C10 -123.0(6) . . . . ? C5 C4 C7 C8 -60.9(6) . . . . ? C3 C4 C7 C8 119.8(5) . . . . ? O1 C11 C12 O2 -164.9(6) . . . . ? O1 C11 C12 O3 15.1(7) . . . . ? C18 C13 C14 C15 4.9(6) . . . . ? S2 C13 C14 C15 175.8(3) . . . . ? C18 C13 C14 O4 -172.1(4) . . . . ? S2 C13 C14 O4 -1.1(5) . . . . ? C13 C14 C15 C16 -4.2(6) . . . . ? O4 C14 C15 C16 172.8(4) . . . . ? C13 C14 C15 S3 -176.9(3) . . . . ? O4 C14 C15 S3 0.1(6) . . . . ? C14 C15 C16 C17 -0.6(7) . . . . ? S3 C15 C16 C17 172.4(3) . . . . ? C15 C16 C17 C18 4.5(6) . . . . ? C15 C16 C17 C19 -172.1(4) . . . . ? C14 C13 C18 C17 -0.9(7) . . . . ? S2 C13 C18 C17 -172.2(3) . . . . ? C16 C17 C18 C13 -3.7(6) . . . . ? C19 C17 C18 C13 172.9(4) . . . . ? C16 C17 C19 C21 -20.7(7) . . . . ? C18 C17 C19 C21 162.9(5) . . . . ? C16 C17 C19 C20 -141.3(5) . . . . ? C18 C17 C19 C20 42.3(6) . . . . ? C16 C17 C19 C22 99.0(6) . . . . ? C18 C17 C19 C22 -77.5(6) . . . . ? O4 C23 C24 O5 170.3(6) . . . . ? O4 C23 C24 N1 -12.7(9) . . . . ? O5 C24 N1 C25 -1.1(11) . . . . ? C23 C24 N1 C25 -177.9(6) . . . . ? O6 C25 N1 C24 180.0(6) . . . . ? N2 C25 N1 C24 -0.1(9) . . . . ? C2 C1 O1 C11 -83.8(6) . . . . ? C6 C1 O1 C11 100.8(5) . . . . ? C12 C11 O1 C1 171.9(4) . . . . ? C13 C14 O4 C23 83.1(6) . . . . ? C15 C14 O4 C23 -93.8(6) . . . . ? C24 C23 O4 C14 -167.1(5) . . . . ? C1 C2 S1 C2 -48.6(3) . . . 2_655 ? C3 C2 S1 C2 139.9(4) . . . 2_655 ? C18 C13 S2 C6 -127.1(4) . . . . ? C14 C13 S2 C6 61.8(4) . . . . ? C5 C6 S2 C13 -142.2(4) . . . . ? C1 C6 S2 C13 49.7(4) . . . . ? C14 C15 S3 C15 -57.8(3) . . . 2_655 ? C16 C15 S3 C15 129.3(4) . . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.86 2.53 3.170(6) 132.3 2_655 N1 H1 O4 0.86 2.17 2.634(5) 113.7 . O3 H3A O6 0.82 1.74 2.557(5) 170.6 2_655 N2 H2A O2 0.86 2.47 3.154(6) 137.2 8_456 N2 H2B O5 0.86 2.03 2.679(7) 131.5 . C5 H5 S2 0.93 2.85 3.750(5) 163.0 2_656 C11 H11A S1 0.97 2.85 3.429(6) 119.5 . C23 H23B S2 0.97 2.86 3.395(8) 115.4 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.556 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.073 data_5 _database_code_depnum_ccdc_archive 'CCDC 760514' #TrackingRef '- data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C52 H64 N8 O12 S4), H2 O, 2(C4 H8 0)' _chemical_formula_sum 'C112 H146 N16 O27 S8' _chemical_formula_weight 2404.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.9385(5) _cell_length_b 25.0431(8) _cell_length_c 15.9995(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.281(2) _cell_angle_gamma 90.00 _cell_volume 5984.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6785 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 24.57 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37926 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10509 _reflns_number_gt 7690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10509 _refine_ls_number_parameters 744 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.45426(18) 0.17226(11) 0.31288(18) 0.0245(7) Uani 1 1 d . . . C2 C 0.48260(18) 0.14847(11) 0.23891(19) 0.0251(7) Uani 1 1 d . . . C3 C 0.51867(18) 0.09716(11) 0.24123(18) 0.0258(7) Uani 1 1 d . . . H3 H 0.5388 0.0821 0.1920 0.031 Uiso 1 1 calc R . . C4 C 0.52550(19) 0.06762(11) 0.31527(18) 0.0260(7) Uani 1 1 d . . . C5 C 0.49537(19) 0.09190(11) 0.38718(18) 0.0271(7) Uani 1 1 d . . . H5 H 0.4979 0.0729 0.4371 0.033 Uiso 1 1 calc R . . C6 C 0.46142(18) 0.14380(11) 0.38758(18) 0.0248(7) Uani 1 1 d . . . C7 C 0.5674(2) 0.01197(11) 0.31353(19) 0.0292(7) Uani 1 1 d . . . C8 C 0.5291(3) -0.02139(13) 0.2411(2) 0.0496(10) Uani 1 1 d . . . H8A H 0.4654 -0.0244 0.2462 0.074 Uiso 1 1 calc R . . H8B H 0.5555 -0.0563 0.2426 0.074 Uiso 1 1 calc R . . H8C H 0.5424 -0.0044 0.1891 0.074 Uiso 1 1 calc R . . C9 C 0.6685(2) 0.01878(14) 0.3057(3) 0.0493(10) Uani 1 1 d . . . H9A H 0.6808 0.0383 0.2556 0.074 Uiso 1 1 calc R . . H9B H 0.6964 -0.0157 0.3033 0.074 Uiso 1 1 calc R . . H9C H 0.6918 0.0380 0.3533 0.074 Uiso 1 1 calc R . . C10 C 0.5500(3) -0.01910(14) 0.3940(2) 0.0486(9) Uani 1 1 d . . . H10A H 0.5734 0.0006 0.4411 0.073 Uiso 1 1 calc R . . H10B H 0.5790 -0.0533 0.3915 0.073 Uiso 1 1 calc R . . H10C H 0.4868 -0.0241 0.3998 0.073 Uiso 1 1 calc R . . C11 C 0.4795(2) 0.26402(11) 0.3330(2) 0.0365(8) Uani 1 1 d . . . H11A H 0.5281 0.2646 0.2938 0.044 Uiso 1 1 calc R . . H11B H 0.5048 0.2570 0.3883 0.044 Uiso 1 1 calc R . . C12 C 0.4328(2) 0.31743(12) 0.3324(2) 0.0325(7) Uani 1 1 d . . . C13 C 0.2904(2) 0.36157(11) 0.29078(19) 0.0312(7) Uani 1 1 d . . . C14 C 0.37927(18) 0.20628(10) 0.11815(17) 0.0216(6) Uani 1 1 d . . . C15 C 0.37180(19) 0.25601(11) 0.08095(18) 0.0256(7) Uani 1 1 d . . . H15 H 0.4227 0.2772 0.0772 0.031 Uiso 1 1 calc R . . C16 C 0.29107(19) 0.27539(11) 0.04905(17) 0.0244(6) Uani 1 1 d . . . C17 C 0.21562(18) 0.24449(11) 0.06083(16) 0.0226(6) Uani 1 1 d . . . H17 H 0.1602 0.2573 0.0424 0.027 Uiso 1 1 calc R . . C18 C 0.22041(18) 0.19483(11) 0.09942(17) 0.0218(6) Uani 1 1 d . . . C19 C 0.30326(18) 0.17415(11) 0.12518(16) 0.0221(6) Uani 1 1 d . . . C20 C 0.28707(19) 0.32926(11) 0.00268(18) 0.0272(7) Uani 1 1 d . . . C21 C 0.3178(3) 0.31933(13) -0.0869(2) 0.0453(9) Uani 1 1 d . . . H21A H 0.2750 0.2970 -0.1158 0.068 Uiso 1 1 calc R . . H21B H 0.3751 0.3019 -0.0853 0.068 Uiso 1 1 calc R . . H21C H 0.3226 0.3528 -0.1157 0.068 Uiso 1 1 calc R . . C22 C 0.1931(2) 0.35233(13) 0.0004(2) 0.0455(9) Uani 1 1 d . . . H22A H 0.1944 0.3876 -0.0231 0.068 Uiso 1 1 calc R . . H22B H 0.1709 0.3540 0.0561 0.068 Uiso 1 1 calc R . . H22C H 0.1547 0.3300 -0.0334 0.068 Uiso 1 1 calc R . . C23 C 0.3504(2) 0.36974(12) 0.0451(2) 0.0366(8) Uani 1 1 d . . . H23A H 0.3436 0.4039 0.0184 0.055 Uiso 1 1 calc R . . H23B H 0.4111 0.3578 0.0405 0.055 Uiso 1 1 calc R . . H23C H 0.3360 0.3729 0.1031 0.055 Uiso 1 1 calc R . . C24 C 0.34613(19) 0.08514(11) 0.09970(18) 0.0262(7) Uani 1 1 d . . . H24A H 0.3682 0.0539 0.1295 0.031 Uiso 1 1 calc R . . H24B H 0.3957 0.1013 0.0708 0.031 Uiso 1 1 calc R . . C25 C 0.2734(2) 0.06908(11) 0.03736(19) 0.0269(7) Uani 1 1 d . . . C26 C 0.1286(2) 0.01884(11) 0.03634(19) 0.0271(7) Uani 1 1 d . . . C27 C 0.09772(18) 0.14244(11) 0.20760(17) 0.0209(6) Uani 1 1 d . . . C28 C 0.10497(17) 0.18019(10) 0.27165(17) 0.0205(6) Uani 1 1 d . . . C29 C 0.07877(18) 0.16524(11) 0.35141(17) 0.0230(6) Uani 1 1 d . . . C30 C 0.04109(18) 0.11551(11) 0.36540(17) 0.0242(6) Uani 1 1 d . . . H30 H 0.0237 0.1066 0.4191 0.029 Uiso 1 1 calc R . . C31 C 0.02868(18) 0.07861(10) 0.30144(17) 0.0219(6) Uani 1 1 d . . . C32 C 0.06040(18) 0.09270(10) 0.22332(17) 0.0217(6) Uani 1 1 d . . . H32 H 0.0565 0.0679 0.1801 0.026 Uiso 1 1 calc R . . C33 C -0.01588(19) 0.02437(11) 0.31611(18) 0.0254(7) Uani 1 1 d . . . C34 C 0.0538(3) -0.01820(15) 0.3216(4) 0.106(2) Uani 1 1 d . . . H34A H 0.0893 -0.0135 0.3718 0.159 Uiso 1 1 calc R . . H34B H 0.0916 -0.0160 0.2740 0.159 Uiso 1 1 calc R . . H34C H 0.0253 -0.0526 0.3226 0.159 Uiso 1 1 calc R . . C35 C -0.0807(3) 0.01175(19) 0.2445(3) 0.0948(19) Uani 1 1 d . . . H35A H -0.0477 0.0025 0.1958 0.142 Uiso 1 1 calc R . . H35B H -0.1173 0.0425 0.2327 0.142 Uiso 1 1 calc R . . H35C H -0.1181 -0.0177 0.2598 0.142 Uiso 1 1 calc R . . C36 C -0.0715(4) 0.02382(18) 0.3922(3) 0.103(2) Uani 1 1 d . . . H36A H -0.1065 -0.0083 0.3931 0.154 Uiso 1 1 calc R . . H36B H -0.1106 0.0542 0.3915 0.154 Uiso 1 1 calc R . . H36C H -0.0332 0.0252 0.4412 0.154 Uiso 1 1 calc R . . C37 C 0.0781(2) 0.26603(11) 0.21466(19) 0.0316(7) Uani 1 1 d . . . H37A H 0.0465 0.2464 0.1708 0.038 Uiso 1 1 calc R . . H37B H 0.1116 0.2945 0.1888 0.038 Uiso 1 1 calc R . . C38 C 0.0110(2) 0.28972(13) 0.2738(2) 0.0353(8) Uani 1 1 d . . . C39 C -0.0049(3) 0.36103(17) 0.3814(2) 0.0573(12) Uani 1 1 d . . . C40 C 0.19184(19) 0.23074(11) 0.45669(17) 0.0240(6) Uani 1 1 d . . . C41 C 0.20193(19) 0.28092(11) 0.49357(18) 0.0265(7) Uani 1 1 d . . . H41 H 0.1526 0.3035 0.4956 0.032 Uiso 1 1 calc R . . C42 C 0.2831(2) 0.29808(11) 0.52727(18) 0.0276(7) Uani 1 1 d . . . C43 C 0.35683(19) 0.26425(11) 0.51913(18) 0.0285(7) Uani 1 1 d . . . H43 H 0.4128 0.2752 0.5392 0.034 Uiso 1 1 calc R . . C44 C 0.34771(19) 0.21440(12) 0.48137(18) 0.0275(7) Uani 1 1 d . . . C45 C 0.2656(2) 0.19705(11) 0.45057(17) 0.0247(7) Uani 1 1 d . . . C46 C 0.2921(2) 0.35087(12) 0.5760(2) 0.0353(8) Uani 1 1 d . . . C47 C 0.2805(4) 0.33864(17) 0.6677(3) 0.0944(19) Uani 1 1 d . . . H47A H 0.2247 0.3204 0.6751 0.142 Uiso 1 1 calc R . . H47B H 0.2806 0.3714 0.6990 0.142 Uiso 1 1 calc R . . H47C H 0.3289 0.3164 0.6874 0.142 Uiso 1 1 calc R . . C48 C 0.2194(3) 0.39133(14) 0.5497(3) 0.0685(13) Uani 1 1 d . . . H48A H 0.2203 0.3964 0.4902 0.103 Uiso 1 1 calc R . . H48B H 0.2308 0.4248 0.5772 0.103 Uiso 1 1 calc R . . H48C H 0.1618 0.3781 0.5652 0.103 Uiso 1 1 calc R . . C49 C 0.3808(2) 0.37819(15) 0.5617(3) 0.0581(11) Uani 1 1 d . . . H49A H 0.4287 0.3557 0.5818 0.087 Uiso 1 1 calc R . . H49B H 0.3825 0.4116 0.5912 0.087 Uiso 1 1 calc R . . H49C H 0.3874 0.3846 0.5030 0.087 Uiso 1 1 calc R . . C50 C 0.2428(2) 0.10564(11) 0.47513(18) 0.0317(7) Uani 1 1 d . . . H50A H 0.1822 0.1087 0.4951 0.038 Uiso 1 1 calc R . . H50B H 0.2837 0.1104 0.5225 0.038 Uiso 1 1 calc R . . C51 C 0.25594(19) 0.05117(11) 0.43861(19) 0.0282(7) Uani 1 1 d . . . C52 C 0.28119(19) 0.00149(11) 0.30735(19) 0.0258(7) Uani 1 1 d . . . N1 N 0.34776(18) 0.31795(9) 0.29950(17) 0.0327(6) Uani 1 1 d D . . H1A H 0.326(2) 0.2876(9) 0.2863(19) 0.039 Uiso 1 1 d D . . N2 N 0.3179(2) 0.40719(10) 0.32360(18) 0.0406(7) Uani 1 1 d D . . H2A H 0.3671(16) 0.4102(13) 0.3538(19) 0.049 Uiso 1 1 d D . . H2B H 0.2810(19) 0.4332(10) 0.315(2) 0.049 Uiso 1 1 d D . . N3 N 0.21325(16) 0.03353(9) 0.06819(15) 0.0278(6) Uani 1 1 d D . . H3A H 0.224(2) 0.0284(12) 0.1197(12) 0.033 Uiso 1 1 d D . . N4 N 0.1052(2) 0.03807(12) -0.03819(18) 0.0417(7) Uani 1 1 d D . . H4A H 0.138(2) 0.0629(11) -0.057(2) 0.050 Uiso 1 1 d D . . H4B H 0.0520(14) 0.0306(13) -0.055(2) 0.050 Uiso 1 1 d D . . N5 N 0.0418(2) 0.33142(11) 0.32045(18) 0.0398(7) Uani 1 1 d D . . H5A H 0.0984(13) 0.3361(14) 0.314(2) 0.048 Uiso 1 1 d D . . N6 N -0.0879(3) 0.34582(18) 0.3941(3) 0.0766(12) Uani 1 1 d D . . H6A H -0.123(3) 0.3630(16) 0.428(2) 0.092 Uiso 1 1 d D . . H6B H -0.110(3) 0.3186(14) 0.366(3) 0.092 Uiso 1 1 d D . . N7 N 0.26891(16) 0.04810(9) 0.35508(15) 0.0260(6) Uani 1 1 d D . . N8 N 0.29544(19) -0.04300(10) 0.34932(18) 0.0327(6) Uani 1 1 d D . . H8D H 0.301(2) -0.0730(9) 0.3218(18) 0.039 Uiso 1 1 d D . . H8E H 0.286(2) -0.0426(13) 0.4015(12) 0.047(11) Uiso 1 1 d D . . O1 O 0.41777(13) 0.22278(7) 0.31048(12) 0.0290(5) Uani 1 1 d . . . O2 O 0.47313(16) 0.35646(9) 0.35841(16) 0.0487(7) Uani 1 1 d . . . O3 O 0.21896(15) 0.35588(8) 0.25203(15) 0.0395(6) Uani 1 1 d . . . O4 O 0.30920(12) 0.12301(7) 0.15815(12) 0.0236(4) Uani 1 1 d . . . O5 O 0.26835(15) 0.08781(9) -0.03277(13) 0.0424(6) Uani 1 1 d . . . O6 O 0.08201(13) -0.01015(8) 0.07902(13) 0.0334(5) Uani 1 1 d . . . O7 O 0.13915(12) 0.23065(7) 0.25846(12) 0.0255(5) Uani 1 1 d . . . H7A H 0.2673(19) 0.0769(9) 0.3249(17) 0.031 Uiso 1 1 d D . . O8 O -0.06380(17) 0.27085(11) 0.27769(18) 0.0625(8) Uani 1 1 d . . . O9 O 0.0343(2) 0.39766(13) 0.41622(19) 0.0846(10) Uani 1 1 d . . . O10 O 0.25823(13) 0.14671(7) 0.41475(12) 0.0267(5) Uani 1 1 d . . . O11 O 0.25382(17) 0.01277(8) 0.48473(14) 0.0455(6) Uani 1 1 d . . . O12 O 0.28035(14) 0.00506(8) 0.23109(13) 0.0343(5) Uani 1 1 d . . . S1 S 0.44363(5) 0.17186(3) 0.48807(5) 0.0329(2) Uani 1 1 d . . . S2 S 0.48961(5) 0.18489(3) 0.14445(5) 0.02738(19) Uani 1 1 d . . . S3 S 0.12014(5) 0.15636(3) 0.10082(4) 0.02319(18) Uani 1 1 d . . . S4 S 0.07943(5) 0.21130(3) 0.43616(5) 0.0286(2) Uani 1 1 d . . . O13 O 0.0516(7) 0.4981(4) 0.5047(7) 0.177(5) Uani 0.50 1 d P A -1 H3B H 0.0044 0.4816 0.5359 0.212 Uiso 0.50 1 d PR A -1 H3C H 0.0951 0.4811 0.4895 0.212 Uiso 0.50 1 d PR A -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 C1 0.0177(15) 0.0220(15) 0.0335(18) -0.0027(12) -0.0045(13) 0.0036(12) C2 0.0175(15) 0.0257(16) 0.0317(17) 0.0016(13) -0.0054(13) 0.0003(12) C3 0.0229(16) 0.0282(16) 0.0262(17) -0.0021(12) 0.0004(13) 0.0037(12) C4 0.0201(15) 0.0277(16) 0.0300(17) -0.0018(13) -0.0060(13) 0.0017(12) C5 0.0243(16) 0.0288(16) 0.0279(17) 0.0045(13) -0.0048(13) 0.0009(13) C6 0.0153(15) 0.0294(16) 0.0293(17) -0.0030(13) -0.0048(12) 0.0018(12) C7 0.0294(17) 0.0276(16) 0.0305(18) 0.0010(13) -0.0025(14) 0.0054(13) C8 0.061(2) 0.0295(18) 0.057(2) -0.0073(16) -0.0098(19) 0.0109(17) C9 0.038(2) 0.041(2) 0.070(3) 0.0033(18) 0.0064(18) 0.0148(16) C10 0.059(2) 0.037(2) 0.050(2) 0.0066(16) 0.0027(19) 0.0164(18) C11 0.0318(18) 0.0264(17) 0.051(2) -0.0020(15) -0.0001(16) -0.0006(14) C12 0.0337(19) 0.0292(17) 0.0346(19) -0.0003(14) 0.0038(15) 0.0012(14) C13 0.037(2) 0.0179(15) 0.039(2) 0.0043(13) 0.0026(16) 0.0015(13) C14 0.0193(15) 0.0237(15) 0.0215(15) 0.0005(12) -0.0018(12) -0.0004(12) C15 0.0200(15) 0.0286(16) 0.0282(17) 0.0046(13) 0.0036(12) -0.0064(12) C16 0.0286(17) 0.0225(15) 0.0220(16) 0.0010(12) 0.0023(13) -0.0001(12) C17 0.0192(15) 0.0271(15) 0.0214(16) 0.0029(12) -0.0014(12) 0.0021(12) C18 0.0199(15) 0.0265(15) 0.0190(15) 0.0014(11) 0.0018(12) -0.0042(12) C19 0.0257(16) 0.0243(15) 0.0163(15) 0.0011(11) 0.0003(12) -0.0019(12) C20 0.0269(17) 0.0253(16) 0.0292(17) 0.0071(13) 0.0004(13) 0.0001(13) C21 0.069(3) 0.0377(19) 0.0290(19) 0.0101(15) -0.0004(17) -0.0077(18) C22 0.040(2) 0.0316(18) 0.065(3) 0.0182(17) -0.0035(18) 0.0031(15) C23 0.043(2) 0.0276(17) 0.039(2) 0.0065(14) 0.0016(16) -0.0033(15) C24 0.0243(16) 0.0248(15) 0.0294(17) 0.0063(13) 0.0024(13) -0.0003(12) C25 0.0297(17) 0.0230(15) 0.0282(18) 0.0017(13) 0.0050(13) -0.0020(13) C26 0.0303(17) 0.0247(15) 0.0262(17) -0.0045(13) -0.0040(14) -0.0019(13) C27 0.0154(14) 0.0259(15) 0.0212(15) 0.0016(12) -0.0019(12) 0.0000(11) C28 0.0173(15) 0.0191(14) 0.0252(16) 0.0016(12) 0.0000(12) -0.0015(11) C29 0.0204(15) 0.0263(15) 0.0223(16) -0.0053(12) -0.0020(12) -0.0022(12) C30 0.0220(16) 0.0318(16) 0.0188(15) 0.0028(12) 0.0029(12) -0.0023(12) C31 0.0181(15) 0.0215(15) 0.0260(16) 0.0015(12) 0.0005(12) 0.0003(12) C32 0.0220(15) 0.0201(14) 0.0229(16) -0.0027(11) -0.0011(12) -0.0018(12) C33 0.0245(16) 0.0247(15) 0.0272(17) -0.0007(12) 0.0021(13) -0.0040(12) C34 0.044(3) 0.029(2) 0.245(7) 0.037(3) 0.016(3) -0.0004(19) C35 0.114(4) 0.088(3) 0.080(3) 0.037(3) -0.042(3) -0.081(3) C36 0.169(5) 0.057(3) 0.086(4) -0.019(2) 0.083(4) -0.061(3) C37 0.0358(18) 0.0216(16) 0.0373(19) 0.0028(13) 0.0012(15) -0.0016(13) C38 0.0294(19) 0.0334(18) 0.043(2) 0.0011(15) 0.0057(15) 0.0063(15) C39 0.077(3) 0.060(3) 0.035(2) -0.0049(19) -0.010(2) 0.034(2) C40 0.0240(16) 0.0297(16) 0.0183(15) -0.0016(12) -0.0012(12) -0.0001(12) C41 0.0237(16) 0.0279(16) 0.0280(17) -0.0059(13) 0.0009(13) 0.0028(13) C42 0.0265(17) 0.0329(17) 0.0234(16) -0.0071(13) 0.0025(13) -0.0029(13) C43 0.0219(16) 0.0358(17) 0.0276(17) -0.0098(13) -0.0064(13) -0.0037(13) C44 0.0258(17) 0.0337(17) 0.0229(16) -0.0045(13) 0.0005(13) 0.0040(13) C45 0.0312(17) 0.0232(15) 0.0196(15) -0.0046(12) 0.0009(13) -0.0021(13) C46 0.0345(19) 0.0351(18) 0.036(2) -0.0126(14) -0.0018(15) -0.0040(14) C47 0.192(6) 0.056(3) 0.036(3) -0.022(2) 0.017(3) -0.026(3) C48 0.049(2) 0.041(2) 0.116(4) -0.037(2) -0.013(2) 0.0067(18) C49 0.039(2) 0.049(2) 0.086(3) -0.034(2) 0.003(2) -0.0094(18) C50 0.0378(19) 0.0315(17) 0.0257(17) -0.0020(13) -0.0004(14) 0.0028(14) C51 0.0272(17) 0.0297(17) 0.0277(18) 0.0024(14) -0.0038(13) -0.0033(13) C52 0.0237(16) 0.0232(16) 0.0302(19) 0.0021(13) -0.0021(13) -0.0021(12) N1 0.0366(16) 0.0188(13) 0.0425(17) -0.0016(12) -0.0034(13) -0.0010(12) N2 0.051(2) 0.0249(15) 0.0455(18) -0.0061(13) -0.0155(15) 0.0070(13) N3 0.0305(15) 0.0289(14) 0.0237(14) 0.0032(11) -0.0034(12) -0.0074(11) N4 0.0387(18) 0.0516(18) 0.0342(17) 0.0087(14) -0.0125(14) -0.0204(14) N5 0.0431(17) 0.0372(16) 0.0392(17) -0.0057(13) 0.0028(15) 0.0130(14) N6 0.063(3) 0.103(3) 0.064(3) -0.018(2) 0.021(2) 0.033(2) N7 0.0316(14) 0.0190(13) 0.0274(15) 0.0017(10) -0.0025(11) -0.0014(11) N8 0.0465(17) 0.0219(14) 0.0295(17) 0.0015(12) -0.0014(14) 0.0018(12) O1 0.0270(11) 0.0229(11) 0.0368(12) -0.0017(9) -0.0048(9) 0.0057(9) O2 0.0451(15) 0.0293(13) 0.0712(18) -0.0081(12) -0.0104(13) -0.0048(11) O3 0.0379(14) 0.0259(12) 0.0544(15) 0.0037(10) -0.0072(12) -0.0014(10) O4 0.0260(11) 0.0183(10) 0.0265(11) 0.0050(8) 0.0014(9) -0.0005(8) O5 0.0415(14) 0.0586(15) 0.0270(13) 0.0115(11) -0.0001(10) -0.0177(12) O6 0.0308(12) 0.0353(12) 0.0340(13) 0.0082(10) -0.0030(10) -0.0128(10) O7 0.0219(11) 0.0211(10) 0.0335(12) -0.0011(8) 0.0021(9) -0.0054(8) O8 0.0318(15) 0.0734(19) 0.083(2) -0.0109(15) 0.0149(14) -0.0029(13) O9 0.111(3) 0.082(2) 0.060(2) -0.0367(17) -0.0249(18) 0.031(2) O10 0.0330(12) 0.0231(11) 0.0239(11) -0.0057(8) -0.0006(9) -0.0001(9) O11 0.0725(18) 0.0313(12) 0.0327(13) 0.0053(10) 0.0017(12) -0.0033(12) O12 0.0503(14) 0.0261(11) 0.0263(13) 0.0005(9) -0.0003(10) -0.0043(10) S1 0.0301(4) 0.0400(5) 0.0282(4) -0.0062(3) -0.0072(3) 0.0111(4) S2 0.0178(4) 0.0330(4) 0.0313(4) 0.0074(3) -0.0004(3) -0.0006(3) S3 0.0205(4) 0.0279(4) 0.0211(4) 0.0024(3) -0.0007(3) -0.0056(3) S4 0.0225(4) 0.0354(4) 0.0280(4) -0.0125(3) 0.0028(3) -0.0035(3) O13 0.187(11) 0.168(9) 0.175(10) -0.072(7) -0.002(10) -0.056(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.378(3) . ? C1 C6 1.393(4) . ? C1 C2 1.399(4) . ? C2 C3 1.394(4) . ? C2 S2 1.770(3) . ? C3 C4 1.398(4) . ? C3 H3 0.9300 . ? C4 C5 1.385(4) . ? C4 C7 1.528(4) . ? C5 C6 1.395(4) . ? C5 H5 0.9300 . ? C6 S1 1.780(3) . ? C7 C9 1.528(4) . ? C7 C8 1.529(4) . ? C7 C10 1.531(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.426(3) . ? C11 C12 1.509(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.217(4) . ? C12 N1 1.364(4) . ? C13 O3 1.230(4) . ? C13 N2 1.319(4) . ? C13 N1 1.394(4) . ? C14 C15 1.384(4) . ? C14 C19 1.398(4) . ? C14 S2 1.775(3) . ? C15 C16 1.387(4) . ? C15 H15 0.9300 . ? C16 C17 1.384(4) . ? C16 C20 1.540(4) . ? C17 C18 1.390(4) . ? C17 H17 0.9300 . ? C18 C19 1.395(4) . ? C18 S3 1.782(3) . ? C19 O4 1.387(3) . ? C20 C22 1.517(4) . ? C20 C23 1.534(4) . ? C20 C21 1.536(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O4 1.450(3) . ? C24 C25 1.513(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O5 1.217(3) . ? C25 N3 1.365(4) . ? C26 O6 1.224(3) . ? C26 N4 1.326(4) . ? C26 N3 1.402(4) . ? C27 C32 1.390(4) . ? C27 C28 1.397(4) . ? C27 S3 1.783(3) . ? C28 O7 1.381(3) . ? C28 C29 1.394(4) . ? C29 C30 1.387(4) . ? C29 S4 1.780(3) . ? C30 C31 1.388(4) . ? C30 H30 0.9300 . ? C31 C32 1.392(4) . ? C31 C33 1.533(4) . ? C32 H32 0.9300 . ? C33 C36 1.490(5) . ? C33 C34 1.491(5) . ? C33 C35 1.516(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 O7 1.442(3) . ? C37 C38 1.515(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O8 1.216(4) . ? C38 N5 1.357(4) . ? C39 O9 1.216(5) . ? C39 N6 1.317(6) . ? C39 N5 1.420(5) . ? C40 C45 1.393(4) . ? C40 C41 1.395(4) . ? C40 S4 1.772(3) . ? C41 C42 1.385(4) . ? C41 H41 0.9300 . ? C42 C43 1.397(4) . ? C42 C46 1.539(4) . ? C43 C44 1.392(4) . ? C43 H43 0.9300 . ? C44 C45 1.382(4) . ? C44 S1 1.787(3) . ? C45 O10 1.388(3) . ? C46 C47 1.513(5) . ? C46 C49 1.514(5) . ? C46 C48 1.536(5) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 O10 1.433(3) . ? C50 C51 1.499(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O11 1.213(3) . ? C51 N7 1.357(4) . ? C52 O12 1.223(3) . ? C52 N8 1.316(4) . ? C52 N7 1.409(4) . ? N1 H1A 0.853(17) . ? N2 H2A 0.873(18) . ? N2 H2B 0.864(18) . ? N3 H3A 0.844(17) . ? N4 H4A 0.853(18) . ? N4 H4B 0.854(18) . ? N5 H5A 0.862(18) . ? N6 H6A 0.88(4) . ? N6 H6B 0.88(4) . ? N7 H7A 0.869(17) . ? N8 H8D 0.876(17) . ? N8 H8E 0.852(18) . ? O13 H3B 0.9657 . ? O13 H3C 0.8193 . ? 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 O1 C1 C6 121.1(3) . . ? O1 C1 C2 119.6(3) . . ? C6 C1 C2 119.3(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 S2 117.9(2) . . ? C1 C2 S2 121.8(2) . . ? C2 C3 C4 122.1(3) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C7 123.8(3) . . ? C3 C4 C7 119.3(3) . . ? C4 C5 C6 122.5(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 119.6(3) . . ? C1 C6 S1 124.2(2) . . ? C5 C6 S1 115.7(2) . . ? C4 C7 C9 107.8(2) . . ? C4 C7 C8 111.5(2) . . ? C9 C7 C8 110.6(3) . . ? C4 C7 C10 111.8(3) . . ? C9 C7 C10 108.2(3) . . ? C8 C7 C10 107.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 110.1(2) . . ? O1 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? O1 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.2 . . ? O2 C12 N1 125.1(3) . . ? O2 C12 C11 118.9(3) . . ? N1 C12 C11 116.0(3) . . ? O3 C13 N2 124.1(3) . . ? O3 C13 N1 119.0(3) . . ? N2 C13 N1 116.9(3) . . ? C15 C14 C19 119.7(2) . . ? C15 C14 S2 116.0(2) . . ? C19 C14 S2 124.0(2) . . ? C14 C15 C16 122.3(3) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C17 C16 C15 117.3(2) . . ? C17 C16 C20 122.2(2) . . ? C15 C16 C20 120.5(2) . . ? C16 C17 C18 121.8(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 120.0(2) . . ? C17 C18 S3 117.0(2) . . ? C19 C18 S3 122.4(2) . . ? O4 C19 C18 120.2(2) . . ? O4 C19 C14 121.1(2) . . ? C18 C19 C14 118.6(2) . . ? C22 C20 C23 108.7(3) . . ? C22 C20 C21 109.6(3) . . ? C23 C20 C21 109.0(3) . . ? C22 C20 C16 111.8(2) . . ? C23 C20 C16 110.4(2) . . ? C21 C20 C16 107.4(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 C25 108.7(2) . . ? O4 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O4 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? O5 C25 N3 123.8(3) . . ? O5 C25 C24 122.3(3) . . ? N3 C25 C24 113.8(2) . . ? O6 C26 N4 125.1(3) . . ? O6 C26 N3 118.2(3) . . ? N4 C26 N3 116.7(3) . . ? C32 C27 C28 119.9(3) . . ? C32 C27 S3 115.7(2) . . ? C28 C27 S3 123.9(2) . . ? O7 C28 C29 119.9(2) . . ? O7 C28 C27 122.0(2) . . ? C29 C28 C27 118.1(2) . . ? C30 C29 C28 120.8(2) . . ? C30 C29 S4 117.0(2) . . ? C28 C29 S4 121.8(2) . . ? C29 C30 C31 121.8(3) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C32 116.8(2) . . ? C30 C31 C33 121.9(2) . . ? C32 C31 C33 121.3(2) . . ? C27 C32 C31 122.4(3) . . ? C27 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C36 C33 C34 110.3(4) . . ? C36 C33 C35 104.9(4) . . ? C34 C33 C35 109.2(4) . . ? C36 C33 C31 112.7(3) . . ? C34 C33 C31 109.7(2) . . ? C35 C33 C31 109.9(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O7 C37 C38 110.9(2) . . ? O7 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? O7 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.0 . . ? O8 C38 N5 124.8(3) . . ? O8 C38 C37 120.1(3) . . ? N5 C38 C37 115.1(3) . . ? O9 C39 N6 126.3(4) . . ? O9 C39 N5 118.0(5) . . ? N6 C39 N5 115.7(4) . . ? C45 C40 C41 119.8(3) . . ? C45 C40 S4 124.6(2) . . ? C41 C40 S4 114.8(2) . . ? C42 C41 C40 122.0(3) . . ? C42 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? C41 C42 C43 117.4(3) . . ? C41 C42 C46 121.9(3) . . ? C43 C42 C46 120.6(3) . . ? C44 C43 C42 121.0(3) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C45 C44 C43 120.9(3) . . ? C45 C44 S1 122.6(2) . . ? C43 C44 S1 116.0(2) . . ? C44 C45 O10 119.6(3) . . ? C44 C45 C40 118.8(2) . . ? O10 C45 C40 121.6(2) . . ? C47 C46 C49 110.9(3) . . ? C47 C46 C48 107.7(4) . . ? C49 C46 C48 106.0(3) . . ? C47 C46 C42 107.9(3) . . ? C49 C46 C42 112.2(3) . . ? C48 C46 C42 112.1(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O10 C50 C51 111.5(2) . . ? O10 C50 H50A 109.3 . . ? C51 C50 H50A 109.3 . . ? O10 C50 H50B 109.3 . . ? C51 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? O11 C51 N7 124.1(3) . . ? O11 C51 C50 118.6(3) . . ? N7 C51 C50 117.3(2) . . ? O12 C52 N8 124.7(3) . . ? O12 C52 N7 118.8(2) . . ? N8 C52 N7 116.5(3) . . ? C12 N1 C13 127.7(3) . . ? C12 N1 H1A 116(2) . . ? C13 N1 H1A 116(2) . . ? C13 N2 H2A 123(2) . . ? C13 N2 H2B 113(2) . . ? H2A N2 H2B 123(3) . . ? C25 N3 C26 129.5(3) . . ? C25 N3 H3A 110(2) . . ? C26 N3 H3A 117(2) . . ? C26 N4 H4A 116(2) . . ? C26 N4 H4B 116(2) . . ? H4A N4 H4B 126(3) . . ? C38 N5 C39 127.9(3) . . ? C38 N5 H5A 111(2) . . ? C39 N5 H5A 120(2) . . ? C39 N6 H6A 122(3) . . ? C39 N6 H6B 119(4) . . ? H6A N6 H6B 118(5) . . ? C51 N7 C52 127.1(2) . . ? C51 N7 H7A 120(2) . . ? C52 N7 H7A 113(2) . . ? C52 N8 H8D 119(2) . . ? C52 N8 H8E 117(2) . . ? H8D N8 H8E 122(3) . . ? C1 O1 C11 113.9(2) . . ? C19 O4 C24 112.4(2) . . ? C28 O7 C37 113.9(2) . . ? C45 O10 C50 112.7(2) . . ? C6 S1 C44 108.48(13) . . ? C2 S2 C14 106.59(13) . . ? C18 S3 C27 107.08(12) . . ? C40 S4 C29 107.97(13) . . ? H3B O13 H3C 121.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -179.4(2) . . . . ? C6 C1 C2 C3 -0.9(4) . . . . ? O1 C1 C2 S2 10.1(4) . . . . ? C6 C1 C2 S2 -171.5(2) . . . . ? C1 C2 C3 C4 1.8(4) . . . . ? S2 C2 C3 C4 172.6(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C2 C3 C4 C7 -178.9(3) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? C7 C4 C5 C6 176.8(3) . . . . ? O1 C1 C6 C5 177.4(2) . . . . ? C2 C1 C6 C5 -1.0(4) . . . . ? O1 C1 C6 S1 -11.1(4) . . . . ? C2 C1 C6 S1 170.5(2) . . . . ? C4 C5 C6 C1 2.2(4) . . . . ? C4 C5 C6 S1 -170.0(2) . . . . ? C5 C4 C7 C9 -103.8(3) . . . . ? C3 C4 C7 C9 74.3(3) . . . . ? C5 C4 C7 C8 134.6(3) . . . . ? C3 C4 C7 C8 -47.2(4) . . . . ? C5 C4 C7 C10 14.9(4) . . . . ? C3 C4 C7 C10 -166.9(3) . . . . ? O1 C11 C12 O2 172.6(3) . . . . ? O1 C11 C12 N1 -9.5(4) . . . . ? C19 C14 C15 C16 -0.7(4) . . . . ? S2 C14 C15 C16 173.0(2) . . . . ? C14 C15 C16 C17 4.4(4) . . . . ? C14 C15 C16 C20 -175.7(3) . . . . ? C15 C16 C17 C18 -3.0(4) . . . . ? C20 C16 C17 C18 177.1(3) . . . . ? C16 C17 C18 C19 -2.0(4) . . . . ? C16 C17 C18 S3 -173.7(2) . . . . ? C17 C18 C19 O4 -175.3(2) . . . . ? S3 C18 C19 O4 -4.0(4) . . . . ? C17 C18 C19 C14 5.7(4) . . . . ? S3 C18 C19 C14 176.9(2) . . . . ? C15 C14 C19 O4 176.6(2) . . . . ? S2 C14 C19 O4 3.4(4) . . . . ? C15 C14 C19 C18 -4.3(4) . . . . ? S2 C14 C19 C18 -177.5(2) . . . . ? C17 C16 C20 C22 20.3(4) . . . . ? C15 C16 C20 C22 -159.7(3) . . . . ? C17 C16 C20 C23 141.3(3) . . . . ? C15 C16 C20 C23 -38.6(4) . . . . ? C17 C16 C20 C21 -99.9(3) . . . . ? C15 C16 C20 C21 80.1(3) . . . . ? O4 C24 C25 O5 101.1(3) . . . . ? O4 C24 C25 N3 -76.7(3) . . . . ? C32 C27 C28 O7 -178.1(2) . . . . ? S3 C27 C28 O7 -6.7(4) . . . . ? C32 C27 C28 C29 3.7(4) . . . . ? S3 C27 C28 C29 175.1(2) . . . . ? O7 C28 C29 C30 177.5(2) . . . . ? C27 C28 C29 C30 -4.2(4) . . . . ? O7 C28 C29 S4 5.2(4) . . . . ? C27 C28 C29 S4 -176.5(2) . . . . ? C28 C29 C30 C31 0.6(4) . . . . ? S4 C29 C30 C31 173.2(2) . . . . ? C29 C30 C31 C32 3.5(4) . . . . ? C29 C30 C31 C33 -177.9(3) . . . . ? C28 C27 C32 C31 0.5(4) . . . . ? S3 C27 C32 C31 -171.6(2) . . . . ? C30 C31 C32 C27 -4.0(4) . . . . ? C33 C31 C32 C27 177.3(2) . . . . ? C30 C31 C33 C36 20.8(5) . . . . ? C32 C31 C33 C36 -160.6(4) . . . . ? C30 C31 C33 C34 -102.5(4) . . . . ? C32 C31 C33 C34 76.2(4) . . . . ? C30 C31 C33 C35 137.4(4) . . . . ? C32 C31 C33 C35 -43.9(4) . . . . ? O7 C37 C38 O8 -99.2(3) . . . . ? O7 C37 C38 N5 79.9(3) . . . . ? C45 C40 C41 C42 -2.1(4) . . . . ? S4 C40 C41 C42 168.2(2) . . . . ? C40 C41 C42 C43 3.3(4) . . . . ? C40 C41 C42 C46 -173.5(3) . . . . ? C41 C42 C43 C44 -2.4(4) . . . . ? C46 C42 C43 C44 174.5(3) . . . . ? C42 C43 C44 C45 0.2(5) . . . . ? C42 C43 C44 S1 -171.7(2) . . . . ? C43 C44 C45 O10 -178.7(3) . . . . ? S1 C44 C45 O10 -7.3(4) . . . . ? C43 C44 C45 C40 1.0(4) . . . . ? S1 C44 C45 C40 172.4(2) . . . . ? C41 C40 C45 C44 -0.1(4) . . . . ? S4 C40 C45 C44 -169.4(2) . . . . ? C41 C40 C45 O10 179.6(3) . . . . ? S4 C40 C45 O10 10.3(4) . . . . ? C41 C42 C46 C47 92.5(4) . . . . ? C43 C42 C46 C47 -84.3(4) . . . . ? C41 C42 C46 C49 -145.1(3) . . . . ? C43 C42 C46 C49 38.2(4) . . . . ? C41 C42 C46 C48 -25.9(4) . . . . ? C43 C42 C46 C48 157.3(3) . . . . ? O10 C50 C51 O11 172.8(3) . . . . ? O10 C50 C51 N7 -7.6(4) . . . . ? O2 C12 N1 C13 -1.6(5) . . . . ? C11 C12 N1 C13 -179.4(3) . . . . ? O3 C13 N1 C12 172.8(3) . . . . ? N2 C13 N1 C12 -5.6(5) . . . . ? O5 C25 N3 C26 -13.0(5) . . . . ? C24 C25 N3 C26 164.7(3) . . . . ? O6 C26 N3 C25 -172.8(3) . . . . ? N4 C26 N3 C25 6.7(5) . . . . ? O8 C38 N5 C39 -0.1(6) . . . . ? C37 C38 N5 C39 -179.2(3) . . . . ? O9 C39 N5 C38 -179.3(3) . . . . ? N6 C39 N5 C38 0.3(5) . . . . ? O11 C51 N7 C52 0.6(5) . . . . ? C50 C51 N7 C52 -178.9(3) . . . . ? O12 C52 N7 C51 170.5(3) . . . . ? N8 C52 N7 C51 -11.4(4) . . . . ? C6 C1 O1 C11 83.2(3) . . . . ? C2 C1 O1 C11 -98.4(3) . . . . ? C12 C11 O1 C1 -177.4(3) . . . . ? C18 C19 O4 C24 105.1(3) . . . . ? C14 C19 O4 C24 -75.8(3) . . . . ? C25 C24 O4 C19 -79.0(3) . . . . ? C29 C28 O7 C37 -106.2(3) . . . . ? C27 C28 O7 C37 75.6(3) . . . . ? C38 C37 O7 C28 81.0(3) . . . . ? C44 C45 O10 C50 86.4(3) . . . . ? C40 C45 O10 C50 -93.4(3) . . . . ? C51 C50 O10 C45 -167.0(2) . . . . ? C1 C6 S1 C44 42.2(3) . . . . ? C5 C6 S1 C44 -146.0(2) . . . . ? C45 C44 S1 C6 54.2(3) . . . . ? C43 C44 S1 C6 -134.0(2) . . . . ? C3 C2 S2 C14 126.8(2) . . . . ? C1 C2 S2 C14 -62.5(3) . . . . ? C15 C14 S2 C2 144.4(2) . . . . ? C19 C14 S2 C2 -42.2(3) . . . . ? C17 C18 S3 C27 -122.6(2) . . . . ? C19 C18 S3 C27 66.0(3) . . . . ? C32 C27 S3 C18 -144.4(2) . . . . ? C28 C27 S3 C18 43.9(3) . . . . ? C45 C40 S4 C29 -36.4(3) . . . . ? C41 C40 S4 C29 153.9(2) . . . . ? C30 C29 S4 C40 123.1(2) . . . . ? C28 C29 S4 C40 -64.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O6 0.873(18) 2.38(3) 2.974(3) 125(3) 2 N2 H2B O12 0.864(18) 2.14(2) 2.978(3) 163(3) 2 N4 H4B O6 0.854(18) 2.094(19) 2.942(3) 172(3) 3 N6 H6A O5 0.88(4) 2.14(3) 2.976(4) 158(4) 4_566 N8 H8D O3 0.876(17) 2.155(19) 3.012(3) 166(3) 2_545 N1 H1A O1 0.853(17) 2.16(3) 2.607(3) 113(3) . N2 H2A O2 0.873(18) 2.08(3) 2.691(4) 126(3) . N3 H3A O12 0.844(17) 2.043(19) 2.862(3) 163(3) . N5 H5A O3 0.862(18) 2.14(2) 2.951(4) 158(3) . N6 H6B O8 0.88(4) 1.99(4) 2.675(5) 134(5) . N7 H7A O10 0.869(17) 2.27(3) 2.654(3) 107(2) . N8 H8E O11 0.852(18) 1.99(3) 2.663(4) 136(3) . C11 H11B S1 0.97 2.83 3.439(3) 121.8 . C24 H24A O12 0.97 2.44 3.082(4) 123.3 . C24 H24B S2 0.97 2.77 3.358(3) 119.8 . C32 H32 O6 0.93 2.57 3.479(3) 165.3 . C37 H37A S3 0.97 2.76 3.362(3) 121.0 . C37 H37B O3 0.97 2.43 3.130(4) 129.1 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.450 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.073 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.192 0.839 0.272 151 37 ' ' 2 0.192 0.161 0.728 151 38 ' ' 3 0.049 0.383 0.161 8 1 ' ' 4 0.308 0.661 0.772 151 37 ' ' 5 0.451 0.883 0.339 8 1 ' ' 6 0.692 0.339 0.228 151 38 ' ' 7 0.549 0.117 0.661 8 1 ' ' 8 0.951 0.617 0.839 8 1 ' ' _platon_squeeze_details ; During the refinement, except for the symmetry-disordered water O13 molecule being assigned, the other potential THF molecules are disordered and the refinement gave very unstable thermal factors. During the final refinement, the contribution of the solvent molecules to the crystal structure is treated by using the Platon/SQUEEZE procedure. Check using platon shows that there are 640.2 \%A^3^ volumes in the unit cell (approximately 152 electrons, i.e. ca. 4 THF molecules based on the solvents we have used and each host molecule was distributed one THF . So the suitable formula should be C~52~H~64~N~8~O~12~S~4~. 0.5(H~2~O).(C~4~ H~8~O). Some related items (i.e. D(calc), F000 & Mol.Wght ) have been added in the cif file. ; # start Validation Reply Form _vrf_CHEMW03_5 ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 2404.92 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 104.00 1249.14 H 1.01 130.00 131.04 N 14.01 16.00 224.11 O 16.00 25.00 399.97 S 32.07 8.00 256.53 Calculated formula weight 2260.80 RESPONSE: This is due to the serious disorders of the THF solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_DENSD01_5 ; PROBLEM: The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.95 <> 1.05 Crystal density given = 1.255 Calculated crystal density = 1.335 RESPONSE: This is due to the serious disorders of the THF solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_PLAT046_5 ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.34 The ratio of given/expected absorption coefficient lies outside the range 0.99 <> 1.01 Calculated value of mu = 0.228 Value of mu given = 0.223 RESPONSE: This is due to the serious disorders of the THF solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_ABSMU01_5 ; PROBLEM: The ratio of given/expected absorption coefficient lies outside the range 0.99 <> 1.01 Calculated value of mu = 0.228 Value of mu given = 0.223 RESPONSE: This is due to the serious disorders of the THF solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_PLAT605_5 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 149.00 A**3 RESPONSE: This is due to the highly disordered water solvent molecules which can not be modeled satisfactorily. So in the final refinement, the programe 'SQUEEZE' was used. The voids may accommodate ca. 4 THF molecules based on the solvents we have used and each host molecule was distributed one THF . ; #END data_4 _database_code_depnum_ccdc_archive 'CCDC 773844' #TrackingRef '- data 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H62 N6 O12 S4, 1.17 (CH3OH), 0.67 (CH2Cl2)' _chemical_formula_sum 'C52.84 H68.02 N6 O13.17 S4 Cl1.34' _chemical_formula_weight 1173.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.3779(12) _cell_length_b 20.3779(12) _cell_length_c 76.563(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 27534(4) _cell_formula_units_Z 18 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3518 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 17.84 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11131 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46006 _diffrn_reflns_av_R_equivalents 0.1200 _diffrn_reflns_av_sigmaI/netI 0.1373 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 90 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10797 _reflns_number_gt 4278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^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 10797 _refine_ls_number_parameters 763 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1431 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1634 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.820 _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 C1 C 0.8702(2) 0.7882(2) 0.08594(5) 0.0543(11) Uani 1 1 d . . . C2 C 0.9120(2) 0.7869(3) 0.10035(6) 0.0655(12) Uani 1 1 d . . . H2 H 0.9320 0.8277 0.1080 0.079 Uiso 1 1 calc R . . C3 C 0.9248(2) 0.7282(3) 0.10359(6) 0.0626(12) Uani 1 1 d . A . C4 C 0.8921(2) 0.6672(3) 0.09230(5) 0.0592(12) Uani 1 1 d . . . H4 H 0.8974 0.6253 0.0946 0.071 Uiso 1 1 calc R . . C5 C 0.8518(2) 0.6660(2) 0.07764(5) 0.0488(10) Uani 1 1 d . . . C6 C 0.8428(2) 0.7280(2) 0.07385(5) 0.0459(10) Uani 1 1 d . . . C7 C 0.9742(3) 0.7310(3) 0.11897(6) 0.0779(15) Uani 1 1 d D . . C8 C 0.9295(5) 0.6660(5) 0.13142(12) 0.117(3) Uani 0.73 1 d PD A 1 H8A H 0.9600 0.6714 0.1415 0.175 Uiso 0.73 1 calc PR A 1 H8B H 0.9155 0.6190 0.1257 0.175 Uiso 0.73 1 calc PR A 1 H8C H 0.8847 0.6665 0.1350 0.175 Uiso 0.73 1 calc PR A 1 C9 C 1.0448(4) 0.7319(6) 0.11192(10) 0.110(3) Uani 0.73 1 d PD A 1 H9A H 1.0312 0.6825 0.1076 0.165 Uiso 0.73 1 calc PR A 1 H9B H 1.0813 0.7456 0.1211 0.165 Uiso 0.73 1 calc PR A 1 H9C H 1.0662 0.7682 0.1026 0.165 Uiso 0.73 1 calc PR A 1 C10 C 1.0025(6) 0.8055(5) 0.12999(12) 0.114(3) Uani 0.73 1 d PD A 1 H10A H 0.9596 0.8070 0.1347 0.172 Uiso 0.73 1 calc PR A 1 H10B H 1.0310 0.8488 0.1226 0.172 Uiso 0.73 1 calc PR A 1 H10C H 1.0341 0.8062 0.1394 0.172 Uiso 0.73 1 calc PR A 1 C11 C 0.8369(3) 0.7898(2) 0.04766(5) 0.0672(13) Uani 1 1 d . . . H11A H 0.8818 0.8300 0.0532 0.081 Uiso 1 1 calc R . . H11B H 0.8013 0.8078 0.0461 0.081 Uiso 1 1 calc R . . C12 C 0.8581(3) 0.7746(3) 0.03026(6) 0.0778(14) Uani 1 1 d . . . C13 C 0.8754(3) 0.6822(4) 0.01256(6) 0.0794(15) Uani 1 1 d . . . C14 C 0.7242(2) 0.5445(2) 0.06112(5) 0.0497(10) Uani 1 1 d . . . C15 C 0.6944(2) 0.5261(2) 0.04420(5) 0.0530(11) Uani 1 1 d . . . H15 H 0.7274 0.5428 0.0347 0.064 Uiso 1 1 calc R . . C16 C 0.6168(2) 0.4836(2) 0.04110(5) 0.0522(11) Uani 1 1 d . . . C17 C 0.5700(2) 0.4620(2) 0.05565(5) 0.0561(11) Uani 1 1 d . . . H17 H 0.5178 0.4344 0.0540 0.067 Uiso 1 1 calc R . . C18 C 0.5974(2) 0.4797(2) 0.07255(5) 0.0520(11) Uani 1 1 d . . . C19 C 0.6754(2) 0.5188(2) 0.07550(5) 0.0502(10) Uani 1 1 d . . . C20 C 0.5859(2) 0.4582(2) 0.02259(5) 0.0616(12) Uani 1 1 d . . . C21 C 0.5050(3) 0.4449(3) 0.02107(6) 0.0860(15) Uani 1 1 d . . . H21A H 0.5034 0.4878 0.0257 0.129 Uiso 1 1 calc R . . H21B H 0.4709 0.4003 0.0275 0.129 Uiso 1 1 calc R . . H21C H 0.4901 0.4382 0.0090 0.129 Uiso 1 1 calc R . . C22 C 0.5837(3) 0.3832(3) 0.01915(7) 0.1067(19) Uani 1 1 d . . . H22A H 0.5677 0.3673 0.0074 0.160 Uiso 1 1 calc R . . H22B H 0.5487 0.3453 0.0271 0.160 Uiso 1 1 calc R . . H22C H 0.6333 0.3898 0.0209 0.160 Uiso 1 1 calc R . . C23 C 0.6365(3) 0.5153(3) 0.00899(6) 0.110(2) Uani 1 1 d . . . H23A H 0.6429 0.5642 0.0117 0.165 Uiso 1 1 calc R . . H23B H 0.6136 0.4997 -0.0023 0.165 Uiso 1 1 calc R . . H23C H 0.6850 0.5183 0.0090 0.165 Uiso 1 1 calc R . . C24 C 0.7201(3) 0.4713(3) 0.09778(6) 0.0904(16) Uani 1 1 d . . . H24A H 0.7620 0.4758 0.0908 0.108 Uiso 1 1 calc R . . H24B H 0.6762 0.4223 0.0952 0.108 Uiso 1 1 calc R . . C25 C 0.7391(4) 0.4736(4) 0.11629(9) 0.110(2) Uani 1 1 d . . . C26 C 0.7518(4) 0.5386(5) 0.14458(11) 0.139(3) Uani 1 1 d . . . C27 C 0.5479(2) 0.5161(2) 0.10388(5) 0.0509(11) Uani 1 1 d . . . C28 C 0.5385(2) 0.4997(2) 0.12181(5) 0.0605(12) Uani 1 1 d . . . H28 H 0.5321 0.4535 0.1256 0.073 Uiso 1 1 calc R . . C29 C 0.5381(2) 0.5487(3) 0.13401(5) 0.0640(12) Uani 1 1 d . B . C30 C 0.5494(2) 0.6169(3) 0.12792(6) 0.0715(14) Uani 1 1 d . . . H30 H 0.5499 0.6514 0.1359 0.086 Uiso 1 1 calc R . . C31 C 0.5601(2) 0.6369(2) 0.11058(6) 0.0616(12) Uani 1 1 d . . . C32 C 0.5596(2) 0.5861(2) 0.09836(5) 0.0557(11) Uani 1 1 d . . . C33 C 0.5216(3) 0.5271(3) 0.15328(6) 0.0955(18) Uani 1 1 d D . . C34 C 0.5845(6) 0.5916(7) 0.16379(19) 0.089(4) Uani 0.57 1 d PD B 1 H34A H 0.6320 0.5946 0.1613 0.134 Uiso 0.57 1 calc PR B 1 H34B H 0.5737 0.5823 0.1760 0.134 Uiso 0.57 1 calc PR B 1 H34C H 0.5872 0.6386 0.1607 0.134 Uiso 0.57 1 calc PR B 1 C35 C 0.4474(5) 0.5333(7) 0.15748(15) 0.120(4) Uani 0.57 1 d PD B 1 H35A H 0.4050 0.4950 0.1511 0.181 Uiso 0.57 1 calc PR B 1 H35B H 0.4563 0.5824 0.1541 0.181 Uiso 0.57 1 calc PR B 1 H35C H 0.4368 0.5263 0.1698 0.181 Uiso 0.57 1 calc PR B 1 C36 C 0.5034(8) 0.4494(5) 0.15771(17) 0.106(4) Uani 0.57 1 d PD B 1 H36A H 0.4615 0.4139 0.1507 0.159 Uiso 0.57 1 calc PR B 1 H36B H 0.4901 0.4400 0.1699 0.159 Uiso 0.57 1 calc PR B 1 H36C H 0.5466 0.4438 0.1554 0.159 Uiso 0.57 1 calc PR B 1 C37 C 0.4985(3) 0.5819(3) 0.07199(6) 0.0794(14) Uani 1 1 d . . . H37A H 0.4714 0.6028 0.0781 0.095 Uiso 1 1 calc R . . H37B H 0.4675 0.5271 0.0723 0.095 Uiso 1 1 calc R . . C38 C 0.5111(3) 0.6080(3) 0.05355(7) 0.0747(14) Uani 1 1 d . . . C39 C 0.6140(4) 0.6814(3) 0.03159(6) 0.0759(15) Uani 1 1 d . . . C40 C 0.6338(3) 0.7719(2) 0.08921(6) 0.0621(12) Uani 1 1 d . . . C41 C 0.6184(3) 0.8080(3) 0.07615(6) 0.0677(13) Uani 1 1 d . . . H41 H 0.5685 0.7962 0.0746 0.081 Uiso 1 1 calc R . . C42 C 0.6732(3) 0.8613(2) 0.06510(6) 0.0634(12) Uani 1 1 d . C . C43 C 0.7458(3) 0.8749(2) 0.06761(5) 0.0588(11) Uani 1 1 d . . . H43 H 0.7842 0.9095 0.0604 0.071 Uiso 1 1 calc R . . C44 C 0.7641(2) 0.8389(2) 0.08058(6) 0.0551(11) Uani 1 1 d . . . C45 C 0.7078(3) 0.7877(2) 0.09161(5) 0.0575(11) Uani 1 1 d . . . C46 C 0.6534(3) 0.9028(3) 0.05124(7) 0.0783(14) Uani 1 1 d D . . C47 C 0.6180(6) 0.9456(5) 0.06082(13) 0.088(3) Uani 0.62 1 d PD C 1 H47A H 0.6524 0.9781 0.0696 0.132 Uiso 0.62 1 calc PR C 1 H47B H 0.5710 0.9095 0.0662 0.132 Uiso 0.62 1 calc PR C 1 H47C H 0.6089 0.9755 0.0525 0.132 Uiso 0.62 1 calc PR C 1 C48 C 0.5965(7) 0.8479(7) 0.03827(15) 0.114(5) Uani 0.62 1 d PD C 1 H48A H 0.5543 0.8082 0.0444 0.171 Uiso 0.62 1 calc PR C 1 H48B H 0.6200 0.8264 0.0312 0.171 Uiso 0.62 1 calc PR C 1 H48C H 0.5791 0.8742 0.0309 0.171 Uiso 0.62 1 calc PR C 1 C49 C 0.7251(4) 0.9660(6) 0.04224(14) 0.106(3) Uani 0.62 1 d PD C 1 H49A H 0.7110 0.9928 0.0342 0.158 Uiso 0.62 1 calc PR C 1 H49B H 0.7502 0.9438 0.0361 0.158 Uiso 0.62 1 calc PR C 1 H49C H 0.7587 1.0005 0.0509 0.158 Uiso 0.62 1 calc PR C 1 C50 C 0.7511(3) 0.7926(3) 0.11996(6) 0.0955(17) Uani 1 1 d . . . H50A H 0.7131 0.8033 0.1246 0.115 Uiso 1 1 calc R . . H50B H 0.7962 0.8406 0.1174 0.115 Uiso 1 1 calc R . . C51 C 0.7697(4) 0.7511(5) 0.13351(8) 0.108(2) Uani 1 1 d . . . C8' C 0.9727(15) 0.6541(8) 0.1206(3) 0.117(8) Uani 0.27 1 d PD A 2 H8'1 H 0.9895 0.6501 0.1321 0.175 Uiso 0.27 1 calc PR A 2 H8'2 H 1.0057 0.6517 0.1120 0.175 Uiso 0.27 1 calc PR A 2 H8'3 H 0.9220 0.6132 0.1188 0.175 Uiso 0.27 1 calc PR A 2 C9' C 0.9432(15) 0.7428(18) 0.1364(2) 0.147(10) Uani 0.27 1 d PD A 2 H9'1 H 0.8915 0.7303 0.1348 0.220 Uiso 0.27 1 calc PR A 2 H9'2 H 0.9730 0.7948 0.1399 0.220 Uiso 0.27 1 calc PR A 2 H9'3 H 0.9459 0.7107 0.1452 0.220 Uiso 0.27 1 calc PR A 2 C10' C 1.0550(7) 0.7953(11) 0.1159(3) 0.102(7) Uani 0.27 1 d PD A 2 H10D H 1.0858 0.7995 0.1258 0.152 Uiso 0.27 1 calc PR A 2 H10E H 1.0549 0.8420 0.1144 0.152 Uiso 0.27 1 calc PR A 2 H10F H 1.0752 0.7848 0.1056 0.152 Uiso 0.27 1 calc PR A 2 C34' C 0.5490(9) 0.5898(11) 0.1667(3) 0.110(8) Uani 0.43 1 d PD B 2 H34D H 0.5484 0.5696 0.1780 0.164 Uiso 0.43 1 calc PR B 2 H34E H 0.5164 0.6111 0.1666 0.164 Uiso 0.43 1 calc PR B 2 H34F H 0.5998 0.6285 0.1639 0.164 Uiso 0.43 1 calc PR B 2 C35' C 0.4377(6) 0.4683(11) 0.1561(3) 0.181(9) Uani 0.43 1 d PD B 2 H35D H 0.4264 0.4216 0.1505 0.272 Uiso 0.43 1 calc PR B 2 H35E H 0.4067 0.4868 0.1511 0.272 Uiso 0.43 1 calc PR B 2 H35F H 0.4275 0.4599 0.1684 0.272 Uiso 0.43 1 calc PR B 2 C36' C 0.5640(8) 0.4810(8) 0.1581(2) 0.125(7) Uani 0.43 1 d PD B 2 H36D H 0.5509 0.4616 0.1697 0.188 Uiso 0.43 1 calc PR B 2 H36E H 0.6178 0.5142 0.1573 0.188 Uiso 0.43 1 calc PR B 2 H36F H 0.5487 0.4397 0.1500 0.188 Uiso 0.43 1 calc PR B 2 C47' C 0.6776(12) 0.9830(7) 0.0563(3) 0.151(8) Uani 0.38 1 d PD C 2 H47D H 0.7307 1.0096 0.0590 0.227 Uiso 0.38 1 calc PR C 2 H47E H 0.6494 0.9828 0.0664 0.227 Uiso 0.38 1 calc PR C 2 H47F H 0.6680 1.0078 0.0468 0.227 Uiso 0.38 1 calc PR C 2 C48' C 0.5663(6) 0.8584(12) 0.0475(3) 0.137(9) Uani 0.38 1 d PD C 2 H48D H 0.5558 0.8794 0.0373 0.206 Uiso 0.38 1 calc PR C 2 H48E H 0.5396 0.8625 0.0573 0.206 Uiso 0.38 1 calc PR C 2 H48F H 0.5502 0.8060 0.0454 0.206 Uiso 0.38 1 calc PR C 2 C49' C 0.6906(11) 0.8993(12) 0.03378(16) 0.134(6) Uani 0.38 1 d PD C 2 H49D H 0.6662 0.8479 0.0297 0.201 Uiso 0.38 1 calc PR C 2 H49E H 0.7434 0.9172 0.0357 0.201 Uiso 0.38 1 calc PR C 2 H49F H 0.6850 0.9306 0.0252 0.201 Uiso 0.38 1 calc PR C 2 N1 N 0.85200(19) 0.7072(2) 0.02716(4) 0.0659(10) Uani 1 1 d . . . H1 H 0.8306 0.6741 0.0353 0.079 Uiso 1 1 calc R . . N2 N 0.9132(3) 0.7333(2) 0.00046(5) 0.1102(16) Uani 1 1 d . . . H2A H 0.9294 0.7211 -0.0086 0.132 Uiso 1 1 calc R . . H2B H 0.9217 0.7789 0.0017 0.132 Uiso 1 1 calc R . . N3 N 0.7311(2) 0.5233(3) 0.12625(7) 0.1101(16) Uani 1 1 d . . . H3 H 0.7121 0.5481 0.1214 0.132 Uiso 1 1 calc R . . N4 N 0.7703(4) 0.4920(4) 0.15303(7) 0.186(3) Uani 1 1 d . . . H4A H 0.7793 0.4973 0.1641 0.223 Uiso 1 1 calc R . . H4B H 0.7731 0.4571 0.1474 0.223 Uiso 1 1 calc R . . N5 N 0.5844(2) 0.6480(2) 0.04809(5) 0.0686(10) Uani 1 1 d . . . H5 H 0.6177 0.6538 0.0558 0.082 Uiso 1 1 calc R . . N6 N 0.5608(2) 0.6723(2) 0.02002(5) 0.0884(13) Uani 1 1 d . . . H6A H 0.5739 0.6934 0.0099 0.106 Uiso 1 1 calc R . . H6B H 0.5137 0.6454 0.0227 0.106 Uiso 1 1 calc R . . O1 O 0.80369(14) 0.72552(15) 0.05904(3) 0.0556(7) Uani 1 1 d . . . O2 O 0.8770(3) 0.8233(2) 0.01908(5) 0.1372(17) Uani 1 1 d . . . O3 O 0.8605(2) 0.6169(2) 0.01211(4) 0.1153(14) Uani 1 1 d . . . O4 O 0.70378(15) 0.53030(15) 0.09242(3) 0.0624(8) Uani 1 1 d . . . O5 O 0.7626(3) 0.4330(3) 0.12165(5) 0.1378(16) Uani 1 1 d . . . O6 O 0.7465(4) 0.5905(3) 0.15175(7) 0.171(2) Uani 1 1 d . . . O7 O 0.56860(16) 0.60449(15) 0.08074(3) 0.0619(8) Uani 1 1 d . . . O8 O 0.4576(2) 0.5935(2) 0.04430(5) 0.1232(15) Uani 1 1 d . . . O9 O 0.6805(2) 0.7169(2) 0.02949(4) 0.1072(13) Uani 1 1 d . . . O10 O 0.72400(17) 0.75085(16) 0.10454(4) 0.0735(9) Uani 1 1 d . . . O11 O 0.8068(3) 0.7831(3) 0.14638(6) 0.162(2) Uani 1 1 d . . . O12 O 0.7374(3) 0.6782(3) 0.13024(6) 0.1422(17) Uani 1 1 d . . . H12 H 0.7471 0.6572 0.1382 0.213 Uiso 1 1 calc R . . S1 S 0.86208(7) 0.87101(6) 0.084001(15) 0.0688(4) Uani 1 1 d . . . S2 S 0.82430(6) 0.59007(6) 0.062867(14) 0.0591(3) Uani 1 1 d . . . S3 S 0.53120(6) 0.44070(6) 0.089758(14) 0.0654(4) Uani 1 1 d . . . S4 S 0.56052(8) 0.72112(7) 0.104549(18) 0.0903(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(3) 0.056(3) 0.048(3) 0.004(2) -0.002(2) 0.024(2) C2 0.057(3) 0.070(3) 0.055(3) -0.004(2) -0.013(2) 0.020(3) C3 0.046(3) 0.071(3) 0.058(3) 0.005(3) -0.010(2) 0.019(3) C4 0.046(3) 0.068(3) 0.059(3) 0.012(3) -0.001(2) 0.024(2) C5 0.039(2) 0.057(3) 0.049(3) 0.007(2) 0.001(2) 0.023(2) C6 0.040(2) 0.057(3) 0.036(2) 0.001(2) -0.005(2) 0.021(2) C7 0.062(3) 0.086(4) 0.065(3) 0.009(3) -0.023(3) 0.022(3) C8 0.093(7) 0.132(9) 0.091(7) 0.046(7) -0.014(5) 0.031(6) C9 0.078(6) 0.147(8) 0.103(7) 0.012(7) -0.021(5) 0.054(7) C10 0.109(7) 0.126(8) 0.093(7) -0.015(6) -0.058(6) 0.047(6) C11 0.092(4) 0.071(3) 0.040(3) 0.001(2) -0.007(3) 0.041(3) C12 0.103(4) 0.069(4) 0.054(3) 0.008(3) 0.005(3) 0.038(3) C13 0.109(4) 0.097(4) 0.045(3) 0.005(3) 0.017(3) 0.061(4) C14 0.051(3) 0.050(3) 0.049(3) -0.002(2) 0.001(2) 0.026(2) C15 0.057(3) 0.057(3) 0.048(3) 0.004(2) 0.006(2) 0.031(2) C16 0.056(3) 0.045(3) 0.053(3) -0.001(2) -0.004(2) 0.023(2) C17 0.050(3) 0.053(3) 0.053(3) -0.002(2) 0.001(2) 0.017(2) C18 0.056(3) 0.048(3) 0.042(3) 0.000(2) 0.002(2) 0.018(2) C19 0.056(3) 0.047(3) 0.045(3) -0.002(2) -0.002(2) 0.024(2) C20 0.067(3) 0.071(3) 0.044(3) -0.011(2) -0.010(2) 0.032(3) C21 0.083(4) 0.113(4) 0.072(3) -0.023(3) -0.025(3) 0.057(3) C22 0.145(5) 0.109(4) 0.093(4) -0.050(3) -0.047(4) 0.084(4) C23 0.103(4) 0.139(5) 0.050(3) 0.005(3) -0.005(3) 0.032(4) C24 0.113(4) 0.108(4) 0.056(3) 0.014(3) -0.016(3) 0.060(4) C25 0.129(5) 0.145(6) 0.101(5) 0.026(5) -0.002(4) 0.104(5) C26 0.134(6) 0.194(9) 0.122(8) 0.029(7) 0.026(5) 0.107(6) C27 0.052(3) 0.049(3) 0.044(3) 0.000(2) 0.002(2) 0.020(2) C28 0.060(3) 0.052(3) 0.052(3) 0.010(2) -0.002(2) 0.014(2) C29 0.074(3) 0.055(3) 0.041(3) -0.001(3) 0.006(2) 0.016(3) C30 0.082(3) 0.061(3) 0.051(3) -0.004(3) 0.021(3) 0.020(3) C31 0.067(3) 0.057(3) 0.057(3) 0.002(2) 0.019(2) 0.028(2) C32 0.054(3) 0.057(3) 0.047(3) 0.015(2) 0.010(2) 0.021(2) C33 0.096(5) 0.096(5) 0.055(4) -0.001(3) -0.003(3) 0.018(4) C34 0.110(10) 0.106(9) 0.056(8) -0.008(7) -0.007(8) 0.057(8) C35 0.114(10) 0.129(10) 0.091(8) 0.027(9) 0.037(7) 0.040(9) C36 0.150(12) 0.078(8) 0.068(7) 0.029(6) 0.022(10) 0.041(9) C37 0.074(4) 0.099(4) 0.060(3) 0.020(3) 0.002(3) 0.039(3) C38 0.080(4) 0.074(3) 0.067(4) 0.011(3) -0.008(3) 0.035(3) C39 0.104(5) 0.066(3) 0.047(3) 0.012(3) -0.013(4) 0.034(3) C40 0.076(3) 0.049(3) 0.067(3) 0.001(2) 0.006(3) 0.036(3) C41 0.068(3) 0.062(3) 0.083(4) -0.006(3) -0.001(3) 0.040(3) C42 0.065(3) 0.052(3) 0.071(3) 0.002(3) 0.006(3) 0.028(3) C43 0.072(3) 0.048(3) 0.057(3) 0.006(2) 0.008(3) 0.030(3) C44 0.062(3) 0.046(3) 0.054(3) -0.006(2) 0.004(2) 0.024(2) C45 0.081(4) 0.051(3) 0.051(3) 0.004(2) 0.003(3) 0.041(3) C46 0.092(4) 0.076(4) 0.080(4) 0.006(3) -0.009(3) 0.051(4) C47 0.106(8) 0.077(7) 0.104(8) 0.012(6) -0.001(7) 0.063(6) C48 0.151(12) 0.106(8) 0.083(10) -0.010(7) -0.040(9) 0.063(10) C49 0.115(8) 0.095(8) 0.112(9) 0.048(7) 0.001(7) 0.057(7) C50 0.139(5) 0.125(5) 0.049(3) 0.015(3) 0.008(3) 0.087(4) C51 0.129(6) 0.140(6) 0.067(4) 0.007(5) 0.026(4) 0.076(5) C8' 0.12(2) 0.13(2) 0.10(2) 0.006(18) -0.046(17) 0.07(2) C9' 0.15(3) 0.16(3) 0.14(3) 0.00(2) -0.01(2) 0.08(3) C10' 0.079(16) 0.12(2) 0.100(19) 0.013(17) -0.019(14) 0.041(16) C34' 0.122(17) 0.127(14) 0.087(13) -0.030(11) 0.003(14) 0.067(13) C35' 0.17(2) 0.18(2) 0.138(18) 0.015(19) 0.011(15) 0.048(19) C36' 0.159(17) 0.111(14) 0.068(10) 0.023(11) 0.007(14) 0.038(13) C47' 0.18(2) 0.126(19) 0.16(2) 0.000(16) -0.01(2) 0.082(18) C48' 0.138(18) 0.15(2) 0.13(2) 0.033(17) -0.025(16) 0.077(16) C49' 0.147(19) 0.143(18) 0.112(15) 0.028(14) -0.013(14) 0.073(16) N1 0.081(3) 0.063(3) 0.052(2) 0.005(2) 0.015(2) 0.035(2) N2 0.158(4) 0.087(3) 0.062(3) 0.010(3) 0.047(3) 0.044(3) N3 0.100(4) 0.172(5) 0.077(4) -0.006(4) -0.016(3) 0.082(4) N4 0.250(7) 0.318(9) 0.105(4) 0.050(5) 0.010(4) 0.228(7) N5 0.086(3) 0.069(3) 0.048(2) 0.005(2) -0.009(2) 0.038(2) N6 0.103(3) 0.088(3) 0.048(2) 0.012(2) -0.016(2) 0.029(3) O1 0.0619(18) 0.0657(19) 0.0383(16) -0.0001(15) -0.0100(14) 0.0313(16) O2 0.244(5) 0.108(3) 0.071(3) 0.021(2) 0.035(3) 0.097(3) O3 0.192(4) 0.095(3) 0.075(3) 0.015(2) 0.058(3) 0.085(3) O4 0.0641(19) 0.073(2) 0.0453(18) -0.0113(16) -0.0062(15) 0.0307(17) O5 0.171(4) 0.184(4) 0.103(3) 0.032(3) 0.005(3) 0.122(4) O6 0.261(7) 0.212(6) 0.115(4) 0.016(4) 0.009(4) 0.174(5) O7 0.067(2) 0.070(2) 0.0469(18) 0.0128(15) 0.0068(16) 0.0329(16) O8 0.089(3) 0.163(4) 0.089(3) 0.034(3) -0.024(2) 0.041(3) O9 0.093(3) 0.133(3) 0.069(2) 0.034(2) -0.002(2) 0.037(3) O10 0.098(2) 0.077(2) 0.058(2) 0.0055(18) 0.0055(18) 0.053(2) O11 0.218(5) 0.240(6) 0.082(3) -0.029(4) -0.032(3) 0.154(5) O12 0.152(4) 0.122(4) 0.142(4) 0.048(3) -0.002(3) 0.061(3) S1 0.0736(8) 0.0582(7) 0.0660(8) -0.0084(6) -0.0070(6) 0.0266(7) S2 0.0518(7) 0.0651(7) 0.0623(7) -0.0048(6) 0.0012(6) 0.0305(6) S3 0.0686(8) 0.0515(7) 0.0582(7) -0.0022(6) 0.0135(6) 0.0165(6) S4 0.1023(11) 0.0717(9) 0.1074(11) 0.0214(8) 0.0468(9) 0.0514(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.403(5) . ? C1 C6 1.411(5) . ? C1 S1 1.782(4) . ? C2 C3 1.368(6) . ? C2 H2 0.9300 . ? C3 C4 1.381(6) . ? C3 C7 1.531(6) . ? C4 C5 1.384(5) . ? C4 H4 0.9300 . ? C5 C6 1.395(5) . ? C5 S2 1.766(4) . ? C6 O1 1.373(4) . ? C7 C8 1.512(6) . ? C7 C10' 1.524(9) . ? C7 C9 1.527(7) . ? C7 C9' 1.543(9) . ? C7 C8' 1.558(9) . ? C7 C10 1.573(7) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.431(4) . ? C11 C12 1.480(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.218(5) . ? C12 N1 1.337(5) . ? C13 O3 1.210(5) . ? C13 N2 1.316(6) . ? C13 N1 1.406(5) . ? C14 C19 1.397(5) . ? C14 C15 1.400(5) . ? C14 S2 1.775(4) . ? C15 C16 1.392(5) . ? C15 H15 0.9300 . ? C16 C17 1.387(5) . ? C16 C20 1.532(5) . ? C17 C18 1.384(5) . ? C17 H17 0.9300 . ? C18 C19 1.395(5) . ? C18 S3 1.765(4) . ? C19 O4 1.390(4) . ? C20 C23 1.518(6) . ? C20 C22 1.531(6) . ? C20 C21 1.534(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O4 1.457(5) . ? C24 C25 1.464(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O5 1.216(6) . ? C25 N3 1.341(7) . ? C26 O6 1.243(8) . ? C26 N4 1.348(8) . ? C26 N3 1.454(8) . ? C27 C32 1.388(5) . ? C27 C28 1.403(5) . ? C27 S3 1.767(4) . ? C28 C29 1.371(5) . ? C28 H28 0.9300 . ? C29 C30 1.373(6) . ? C29 C33 1.528(6) . ? C30 C31 1.373(5) . ? C30 H30 0.9300 . ? C31 C32 1.392(5) . ? C31 S4 1.774(4) . ? C32 O7 1.387(4) . ? C33 C36 1.473(7) . ? C33 C34' 1.510(9) . ? C33 C34 1.527(8) . ? C33 C35' 1.535(9) . ? C33 C36' 1.604(9) . ? C33 C35 1.612(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 O7 1.429(5) . ? C37 C38 1.486(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O8 1.206(5) . ? C38 N5 1.360(5) . ? C39 O9 1.185(6) . ? C39 N6 1.339(6) . ? C39 N5 1.419(6) . ? C40 C41 1.367(5) . ? C40 C45 1.388(6) . ? C40 S4 1.770(4) . ? C41 C42 1.388(6) . ? C41 H41 0.9300 . ? C42 C43 1.376(5) . ? C42 C46 1.533(6) . ? C43 C44 1.391(5) . ? C43 H43 0.9300 . ? C44 C45 1.387(5) . ? C44 S1 1.782(4) . ? C45 O10 1.379(5) . ? C46 C47' 1.502(9) . ? C46 C48 1.512(8) . ? C46 C49 1.544(7) . ? C46 C49' 1.556(9) . ? C46 C48' 1.563(9) . ? C46 C47 1.564(7) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 O10 1.397(5) . ? C50 C51 1.503(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O11 1.215(7) . ? C51 O12 1.313(7) . ? C8' H8'1 0.9600 . ? C8' H8'2 0.9600 . ? C8' H8'3 0.9600 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C34' H34D 0.9600 . ? C34' H34E 0.9600 . ? C34' H34F 0.9600 . ? C35' H35D 0.9600 . ? C35' H35E 0.9600 . ? C35' H35F 0.9600 . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? C47' H47D 0.9600 . ? C47' H47E 0.9600 . ? C47' H47F 0.9600 . ? C48' H48D 0.9600 . ? C48' H48E 0.9600 . ? C48' H48F 0.9600 . ? C49' H49D 0.9600 . ? C49' H49E 0.9600 . ? C49' H49F 0.9600 . ? N1 H1 0.8600 . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 H3 0.8600 . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 H5 0.8600 . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O12 H12 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.6(4) . . ? C2 C1 S1 115.4(3) . . ? C6 C1 S1 125.9(3) . . ? C3 C2 C1 122.9(4) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 117.1(4) . . ? C2 C3 C7 121.0(4) . . ? C4 C3 C7 121.8(4) . . ? C3 C4 C5 122.6(4) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C4 C5 C6 119.9(4) . . ? C4 C5 S2 117.4(3) . . ? C6 C5 S2 122.1(3) . . ? O1 C6 C5 118.4(4) . . ? O1 C6 C1 122.9(4) . . ? C5 C6 C1 118.5(4) . . ? C8 C7 C10' 140.1(9) . . ? C8 C7 C9 112.6(6) . . ? C10' C7 C9 47.9(9) . . ? C8 C7 C3 110.8(4) . . ? C10' C7 C3 108.8(9) . . ? C9 C7 C3 109.0(5) . . ? C8 C7 C9' 58.5(10) . . ? C10' C7 C9' 110.4(11) . . ? C9 C7 C9' 139.4(11) . . ? C3 C7 C9' 110.9(11) . . ? C8 C7 C8' 50.7(9) . . ? C10' C7 C8' 110.2(10) . . ? C9 C7 C8' 65.5(10) . . ? C3 C7 C8' 110.1(8) . . ? C9' C7 C8' 106.4(10) . . ? C8 C7 C10 106.0(6) . . ? C10' C7 C10 62.4(9) . . ? C9 C7 C10 106.9(5) . . ? C3 C7 C10 111.5(5) . . ? C9' C7 C10 50.8(10) . . ? C8' C7 C10 137.8(9) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? O1 C11 C12 114.2(4) . . ? O1 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? O1 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O2 C12 N1 122.7(5) . . ? O2 C12 C11 118.0(5) . . ? N1 C12 C11 119.2(4) . . ? O3 C13 N2 125.1(5) . . ? O3 C13 N1 118.5(5) . . ? N2 C13 N1 116.4(5) . . ? C19 C14 C15 119.8(4) . . ? C19 C14 S2 123.5(3) . . ? C15 C14 S2 116.2(3) . . ? C16 C15 C14 122.0(4) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C17 C16 C15 116.6(4) . . ? C17 C16 C20 122.3(4) . . ? C15 C16 C20 121.0(4) . . ? C18 C17 C16 122.9(4) . . ? C18 C17 H17 118.5 . . ? C16 C17 H17 118.5 . . ? C17 C18 C19 119.8(4) . . ? C17 C18 S3 117.5(3) . . ? C19 C18 S3 122.2(3) . . ? O4 C19 C18 120.4(4) . . ? O4 C19 C14 120.9(4) . . ? C18 C19 C14 118.7(4) . . ? C23 C20 C22 108.5(4) . . ? C23 C20 C16 111.6(4) . . ? C22 C20 C16 107.4(4) . . ? C23 C20 C21 110.0(4) . . ? C22 C20 C21 108.5(4) . . ? C16 C20 C21 110.7(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 C25 114.3(5) . . ? O4 C24 H24A 108.7 . . ? C25 C24 H24A 108.7 . . ? O4 C24 H24B 108.7 . . ? C25 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N3 124.1(6) . . ? O5 C25 C24 119.5(7) . . ? N3 C25 C24 116.4(5) . . ? O6 C26 N4 124.1(8) . . ? O6 C26 N3 118.0(8) . . ? N4 C26 N3 117.7(8) . . ? C32 C27 C28 118.4(4) . . ? C32 C27 S3 124.5(3) . . ? C28 C27 S3 116.6(3) . . ? C29 C28 C27 122.9(4) . . ? C29 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C28 C29 C30 116.6(4) . . ? C28 C29 C33 121.9(4) . . ? C30 C29 C33 121.4(4) . . ? C29 C30 C31 123.4(4) . . ? C29 C30 H30 118.3 . . ? C31 C30 H30 118.3 . . ? C30 C31 C32 119.2(4) . . ? C30 C31 S4 117.5(3) . . ? C32 C31 S4 122.7(3) . . ? O7 C32 C27 120.4(4) . . ? O7 C32 C31 120.1(4) . . ? C27 C32 C31 119.5(4) . . ? C36 C33 C34' 122.7(13) . . ? C36 C33 C34 117.1(9) . . ? C36 C33 C29 115.6(6) . . ? C34' C33 C29 118.5(11) . . ? C34 C33 C29 107.0(7) . . ? C36 C33 C35' 63.0(8) . . ? C34' C33 C35' 111.2(10) . . ? C34 C33 C35' 136.5(10) . . ? C29 C33 C35' 110.9(8) . . ? C34' C33 C36' 105.1(10) . . ? C34 C33 C36' 85.3(9) . . ? C29 C33 C36' 106.5(8) . . ? C35' C33 C36' 103.1(9) . . ? C36 C33 C35 107.2(7) . . ? C34' C33 C35 76.3(8) . . ? C34 C33 C35 104.1(7) . . ? C29 C33 C35 104.5(6) . . ? C35' C33 C35 46.4(8) . . ? C36' C33 C35 143.2(8) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? O7 C37 C38 111.4(4) . . ? O7 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? O7 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? O8 C38 N5 123.6(5) . . ? O8 C38 C37 119.8(5) . . ? N5 C38 C37 116.6(5) . . ? O9 C39 N6 126.4(5) . . ? O9 C39 N5 119.8(5) . . ? N6 C39 N5 113.7(5) . . ? C41 C40 C45 119.1(4) . . ? C41 C40 S4 116.6(4) . . ? C45 C40 S4 123.3(4) . . ? C40 C41 C42 123.8(4) . . ? C40 C41 H41 118.1 . . ? C42 C41 H41 118.1 . . ? C43 C42 C41 115.8(4) . . ? C43 C42 C46 122.6(4) . . ? C41 C42 C46 121.6(4) . . ? C42 C43 C44 122.5(4) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 119.5(4) . . ? C45 C44 S1 122.8(4) . . ? C43 C44 S1 117.2(3) . . ? O10 C45 C44 120.9(4) . . ? O10 C45 C40 119.8(4) . . ? C44 C45 C40 119.3(4) . . ? C47' C46 C48 133.6(11) . . ? C47' C46 C42 112.8(9) . . ? C48 C46 C42 111.2(7) . . ? C47' C46 C49 63.3(8) . . ? C48 C46 C49 112.3(7) . . ? C42 C46 C49 111.6(5) . . ? C47' C46 C49' 111.8(9) . . ? C48 C46 C49' 67.2(7) . . ? C42 C46 C49' 107.5(7) . . ? C49 C46 C49' 51.4(7) . . ? C47' C46 C48' 109.8(10) . . ? C42 C46 C48' 110.1(10) . . ? C49 C46 C48' 136.6(10) . . ? C49' C46 C48' 104.6(9) . . ? C48 C46 C47 108.9(7) . . ? C42 C46 C47 107.8(5) . . ? C49 C46 C47 104.7(6) . . ? C49' C46 C47 143.1(8) . . ? C48' C46 C47 72.8(8) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? O10 C50 C51 112.0(5) . . ? O10 C50 H50A 109.2 . . ? C51 C50 H50A 109.2 . . ? O10 C50 H50B 109.2 . . ? C51 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? O11 C51 O12 126.0(7) . . ? O11 C51 C50 121.5(7) . . ? O12 C51 C50 112.4(6) . . ? C7 C8' H8'1 109.5 . . ? C7 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7 C9' H9'1 109.5 . . ? C7 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C7 C10' H10D 109.5 . . ? C7 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C33 C34' H34D 109.5 . . ? C33 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C33 C35' H35D 109.5 . . ? C33 C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C33 C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C33 C36' H36D 109.5 . . ? C33 C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C33 C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C46 C47' H47D 109.5 . . ? C46 C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? C46 C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? C46 C48' H48D 109.5 . . ? C46 C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C46 C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? C46 C49' H49D 109.5 . . ? C46 C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? C46 C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? C12 N1 C13 129.7(4) . . ? C12 N1 H1 115.2 . . ? C13 N1 H1 115.2 . . ? C13 N2 H2A 120.0 . . ? C13 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C25 N3 C26 125.3(6) . . ? C25 N3 H3 117.3 . . ? C26 N3 H3 117.3 . . ? C26 N4 H4A 120.0 . . ? C26 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C38 N5 C39 129.6(4) . . ? C38 N5 H5 115.2 . . ? C39 N5 H5 115.2 . . ? C39 N6 H6A 120.0 . . ? C39 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C6 O1 C11 118.0(3) . . ? C19 O4 C24 111.8(3) . . ? C32 O7 C37 113.2(3) . . ? C45 O10 C50 113.8(3) . . ? C51 O12 H12 109.5 . . ? C44 S1 C1 106.38(19) . . ? C5 S2 C14 106.55(18) . . ? C18 S3 C27 107.07(19) . . ? C40 S4 C31 109.4(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C50 H50B S1 0.97 2.81 3.411(5) 121.0 . C34 H34A O6 0.96 2.49 3.440(13) 172.8 . C11 H11B O9 0.97 2.56 3.092(6) 114.7 . C11 H11A S1 0.97 2.60 3.146(4) 115.9 . O12 H12 O6 0.82 1.71 2.505(6) 163.2 . N6 H6B O8 0.86 1.99 2.661(5) 134.4 . N6 H6A O3 0.86 2.03 2.887(5) 171.6 11_565 N5 H5 O7 0.86 2.16 2.618(4) 113.1 . N4 H4B O5 0.86 2.02 2.656(7) 130.6 . N4 H4A O11 0.86 2.27 3.053(8) 151.1 13_665 N3 H3 O12 0.86 2.53 3.109(8) 125.8 . N3 H3 O4 0.86 2.24 2.667(5) 110.6 . N2 H2B O2 0.86 2.06 2.699(5) 130.5 . N2 H2A O9 0.86 2.07 2.928(5) 174.0 12_655 N1 H1 O1 0.86 2.30 2.727(4) 111.2 . N1 H1 S2 0.86 2.68 3.484(4) 156.3 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.308 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.046 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 223 56 ' ' 2 0.000 0.000 0.142 118 39 ' ' 3 0.000 0.000 0.274 48 8 ' ' 4 0.000 0.000 0.500 872 146 ' ' 5 0.000 0.000 0.726 48 12 ' ' 6 0.000 0.000 0.858 118 29 ' ' 7 0.333 0.667 0.167 872 146 ' ' 8 0.333 0.667 0.667 221 55 ' ' 9 0.333 0.667 0.808 118 39 ' ' 10 0.333 0.667 0.525 118 29 ' ' 11 0.333 0.667 0.393 50 12 ' ' 12 0.333 0.667 0.941 48 8 ' ' 13 0.667 0.333 0.833 872 146 ' ' 14 0.667 0.333 0.333 221 55 ' ' 15 0.667 0.333 0.475 118 39 ' ' 16 0.667 0.333 0.192 118 30 ' ' 17 0.667 0.333 0.059 48 12 ' ' 18 0.667 0.333 0.607 50 8 ' ' _platon_squeeze_details ; During the refinement, the potential methanol and dichloromethane molecules are seriously disordered. During the final refinement, the contribution of the solvent molecules to the crystal structure is treated by using the Platon/SQUEEZE procedure. Check using platon shows that there are 4446.0 \%A^3^ volumes in the unit cell (approximately 871 electrons, i.e. ca. 21 methanol and 12 CH~2~Cl~2~ molecules based on the solvents we have used and each host molecule was distributed 1.17 methanol and 0.67 CH~2~Cl~2~ molecules). So the suitable formula should be C~51~ H~62~ N~6~ O~12~ S~4.(MeOH)~1.17~.(CH~2~Cl~2~)~0.67~. Some related items (i.e. D(calc), F000 & Mol.Wght ) have been added in the cif file. ; # start Validation Reply Form _vrf_ABSMU01_4 ; PROBLEM: The ratio of given/expected absorption coefficient lies outside the range 0.90 <> 1.10 Calculated value of mu = 0.277 Value of mu given = 0.213 RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_CHEMW01_4 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.95 <> 1.05 Calculated formula weight = 1079.3239 Formula weight given = 1163.7800 RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_CHEMW03_4 ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 >From the CIF: _cell_formula_units_Z 18 >From the CIF: _chemical_formula_weight 1163.78 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 51.00 612.56 H 1.01 62.00 62.50 N 14.01 6.00 84.04 O 16.00 12.00 191.99 S 32.07 4.00 128.26 Calculated formula weight 1079.35 RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_DENSD01_4 ; PROBLEM: The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.95 <> 1.05 Crystal density given = 1.172 Calculated crystal density = 1.263 RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_PLAT046_4 ; PROBLEM: Reported Z, MW and D(calc) are Inconsistent .... 1.26 RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_PLAT068_4 ; PROBLEM: Reported F000 Differs from Calcd (or Missing)... ? RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. But in the cif file some related items were added, i.e. the Z, formual weight, F000, D(calc). ; _vrf_PLAT605_4 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 893.00 A**3 RESPONSE: RESPONSE: This is due to the serious disorders of the methanol and dichloromethane solvents, attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON were used to treated this. The voids may accommodate ca. 21 methanol and 12 CH~2~Cl~2~ molecules based on the solvents we have used and each host molecule was distributed 1.17 methanol and 0.67 CH~2~Cl~2~ molecules. ; # Attachment '- 5 (acetone).cif' data_t _database_code_depnum_ccdc_archive 'CCDC 784335' #TrackingRef '- 5 (acetone).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H71 N8 O13.50 S4' _chemical_formula_weight 1188.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.8193(10) _cell_length_b 25.0193(18) _cell_length_c 16.0602(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.2550(10) _cell_angle_gamma 90.00 _cell_volume 5953.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8187 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.65 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2516 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9557 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43783 _diffrn_reflns_av_R_equivalents 0.1189 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11689 _reflns_number_gt 8904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+2.8101P] 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 11689 _refine_ls_number_parameters 744 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.39589(18) 0.18095(11) 0.72961(17) 0.0199(6) Uani 1 1 d . . . C2 C 0.42136(19) 0.16643(11) 0.65006(17) 0.0214(6) Uani 1 1 d . . . C3 C 0.45875(19) 0.11656(11) 0.63494(17) 0.0233(6) Uani 1 1 d . . . H3 H 0.4771 0.1080 0.5802 0.028 Uiso 1 1 calc R . . C4 C 0.46991(19) 0.07885(11) 0.69817(17) 0.0212(6) Uani 1 1 d . . . C5 C 0.43804(19) 0.09271(11) 0.77612(17) 0.0214(6) Uani 1 1 d . . . H5 H 0.4412 0.0670 0.8195 0.026 Uiso 1 1 calc R . . C6 C 0.40155(18) 0.14294(11) 0.79319(17) 0.0199(6) Uani 1 1 d . . . C7 C 0.5151(2) 0.02439(11) 0.68270(18) 0.0238(6) Uani 1 1 d . . . C8 C 0.5711(4) 0.02432(18) 0.6066(3) 0.095(2) Uani 1 1 d . . . H8A H 0.6057 -0.0090 0.6043 0.142 Uiso 1 1 calc R . . H8B H 0.6126 0.0548 0.6086 0.142 Uiso 1 1 calc R . . H8C H 0.5317 0.0271 0.5570 0.142 Uiso 1 1 calc R . . C9 C 0.5808(4) 0.0115(2) 0.7547(3) 0.092(2) Uani 1 1 d . . . H9A H 0.5470 0.0061 0.8058 0.137 Uiso 1 1 calc R . . H9B H 0.6232 0.0412 0.7627 0.137 Uiso 1 1 calc R . . H9C H 0.6143 -0.0212 0.7419 0.137 Uiso 1 1 calc R . . C10 C 0.4448(3) -0.01816(16) 0.6790(5) 0.099(2) Uani 1 1 d . . . H10A H 0.4079 -0.0139 0.6280 0.148 Uiso 1 1 calc R . . H10B H 0.4063 -0.0152 0.7276 0.148 Uiso 1 1 calc R . . H10C H 0.4740 -0.0533 0.6789 0.148 Uiso 1 1 calc R . . C11 C 0.4252(2) 0.26613(12) 0.78796(19) 0.0297(7) Uani 1 1 d . . . H11A H 0.4573 0.2454 0.8320 0.036 Uiso 1 1 calc R . . H11B H 0.3916 0.2953 0.8151 0.036 Uiso 1 1 calc R . . C12 C 0.4934(2) 0.28983(13) 0.7290(2) 0.0332(7) Uani 1 1 d . . . C13 C 0.5088(3) 0.36003(16) 0.6207(2) 0.0464(10) Uani 1 1 d . . . C14 C 0.27793(19) 0.19464(11) 0.90112(16) 0.0198(6) Uani 1 1 d . . . C15 C 0.19442(19) 0.17417(11) 0.87527(16) 0.0204(6) Uani 1 1 d . . . C16 C 0.11786(19) 0.20608(11) 0.88310(16) 0.0205(6) Uani 1 1 d . . . C17 C 0.12512(19) 0.25635(11) 0.91996(17) 0.0233(6) Uani 1 1 d . . . H17 H 0.0727 0.2780 0.9240 0.028 Uiso 1 1 calc R . . C18 C 0.20712(19) 0.27575(11) 0.95108(17) 0.0214(6) Uani 1 1 d . . . C19 C 0.28299(19) 0.24461(11) 0.93912(16) 0.0209(6) Uani 1 1 d . . . H19 H 0.3402 0.2577 0.9574 0.025 Uiso 1 1 calc R . . C20 C 0.2116(2) 0.32940(12) 0.99731(18) 0.0255(7) Uani 1 1 d . . . C21 C 0.1475(2) 0.37004(12) 0.9550(2) 0.0339(8) Uani 1 1 d . . . H21A H 0.1605 0.3722 0.8956 0.051 Uiso 1 1 calc R . . H21B H 0.1562 0.4052 0.9807 0.051 Uiso 1 1 calc R . . H21C H 0.0848 0.3585 0.9618 0.051 Uiso 1 1 calc R . . C22 C 0.1817(3) 0.31932(14) 1.0870(2) 0.0414(9) Uani 1 1 d . . . H22A H 0.1204 0.3046 1.0861 0.062 Uiso 1 1 calc R . . H22B H 0.1826 0.3531 1.1180 0.062 Uiso 1 1 calc R . . H22C H 0.2231 0.2939 1.1142 0.062 Uiso 1 1 calc R . . C23 C 0.3067(2) 0.35280(13) 0.9984(2) 0.0421(9) Uani 1 1 d . . . H23A H 0.3465 0.3305 1.0333 0.063 Uiso 1 1 calc R . . H23B H 0.3052 0.3891 1.0211 0.063 Uiso 1 1 calc R . . H23C H 0.3292 0.3538 0.9415 0.063 Uiso 1 1 calc R . . C24 C 0.15120(19) 0.08497(11) 0.90010(18) 0.0238(6) Uani 1 1 d . . . H24A H 0.1285 0.0532 0.8694 0.029 Uiso 1 1 calc R . . H24B H 0.1002 0.1012 0.9299 0.029 Uiso 1 1 calc R . . C25 C 0.2247(2) 0.06855(12) 0.96191(19) 0.0269(7) Uani 1 1 d . . . C26 C 0.3707(2) 0.01851(11) 0.96275(18) 0.0244(6) Uani 1 1 d . . . C27 C 0.01401(19) 0.14889(11) 0.76227(18) 0.0230(6) Uani 1 1 d . . . C28 C 0.04280(19) 0.17320(11) 0.68974(19) 0.0240(6) Uani 1 1 d . . . C29 C 0.03649(19) 0.14557(12) 0.61480(18) 0.0245(6) Uani 1 1 d . . . C30 C 0.00276(19) 0.09326(11) 0.61369(18) 0.0240(6) Uani 1 1 d . . . H30 H 0.0002 0.0743 0.5625 0.029 Uiso 1 1 calc R . . C31 C -0.02698(19) 0.06833(11) 0.68533(18) 0.0230(6) Uani 1 1 d . . . C32 C -0.02165(19) 0.09754(11) 0.75942(18) 0.0236(6) Uani 1 1 d . . . H32 H -0.0430 0.0819 0.8092 0.028 Uiso 1 1 calc R . . C33 C -0.0691(2) 0.01248(12) 0.68524(19) 0.0281(7) Uani 1 1 d . . . C34 C -0.0314(3) -0.02111(14) 0.7582(2) 0.0444(9) Uani 1 1 d . . . H34A H 0.0345 -0.0230 0.7551 0.067 Uiso 1 1 calc R . . H34B H -0.0567 -0.0573 0.7550 0.067 Uiso 1 1 calc R . . H34C H -0.0480 -0.0045 0.8109 0.067 Uiso 1 1 calc R . . C35 C -0.0500(3) -0.01802(13) 0.6043(2) 0.0416(9) Uani 1 1 d . . . H35A H -0.0793 0.0004 0.5572 0.062 Uiso 1 1 calc R . . H35B H -0.0739 -0.0544 0.6083 0.062 Uiso 1 1 calc R . . H35C H 0.0153 -0.0195 0.5960 0.062 Uiso 1 1 calc R . . C36 C -0.1712(2) 0.01855(14) 0.6931(3) 0.0447(9) Uani 1 1 d . . . H36A H -0.1845 0.0353 0.7466 0.067 Uiso 1 1 calc R . . H36B H -0.1998 -0.0168 0.6901 0.067 Uiso 1 1 calc R . . H36C H -0.1948 0.0410 0.6476 0.067 Uiso 1 1 calc R . . C37 C 0.0176(2) 0.26585(12) 0.6737(2) 0.0357(8) Uani 1 1 d . . . H37A H -0.0300 0.2667 0.7159 0.043 Uiso 1 1 calc R . . H37B H -0.0115 0.2591 0.6186 0.043 Uiso 1 1 calc R . . C38 C 0.0658(2) 0.31875(12) 0.67237(19) 0.0302(7) Uani 1 1 d . . . C39 C 0.2112(2) 0.36244(12) 0.71169(18) 0.0281(7) Uani 1 1 d . . . C40 C 0.1498(2) 0.21726(12) 0.52235(18) 0.0248(6) Uani 1 1 d . . . C41 C 0.2335(2) 0.19945(11) 0.55227(17) 0.0223(6) Uani 1 1 d . . . C42 C 0.30813(19) 0.23263(11) 0.54631(17) 0.0219(6) Uani 1 1 d . . . C43 C 0.2984(2) 0.28346(12) 0.51048(17) 0.0239(6) Uani 1 1 d . . . H43 H 0.3493 0.3064 0.5087 0.029 Uiso 1 1 calc R . . C44 C 0.2159(2) 0.30123(11) 0.47745(17) 0.0242(6) Uani 1 1 d . . . C45 C 0.1421(2) 0.26757(12) 0.48534(17) 0.0253(7) Uani 1 1 d . . . H45 H 0.0847 0.2791 0.4650 0.030 Uiso 1 1 calc R . . C46 C 0.2085(2) 0.35412(12) 0.42863(19) 0.0295(7) Uani 1 1 d . . . C47 C 0.2802(3) 0.39453(14) 0.4573(3) 0.0493(10) Uani 1 1 d . . . H47A H 0.2723 0.4279 0.4259 0.074 Uiso 1 1 calc R . . H47B H 0.3404 0.3799 0.4474 0.074 Uiso 1 1 calc R . . H47C H 0.2739 0.4017 0.5168 0.074 Uiso 1 1 calc R . . C48 C 0.2228(4) 0.34190(16) 0.3367(2) 0.0632(13) Uani 1 1 d . . . H48A H 0.1764 0.3168 0.3168 0.095 Uiso 1 1 calc R . . H48B H 0.2826 0.3260 0.3300 0.095 Uiso 1 1 calc R . . H48C H 0.2184 0.3751 0.3044 0.095 Uiso 1 1 calc R . . C49 C 0.1165(2) 0.38006(14) 0.4400(3) 0.0472(10) Uani 1 1 d . . . H49A H 0.1158 0.4154 0.4137 0.071 Uiso 1 1 calc R . . H49B H 0.1050 0.3838 0.4996 0.071 Uiso 1 1 calc R . . H49C H 0.0696 0.3576 0.4140 0.071 Uiso 1 1 calc R . . C50 C 0.2562(2) 0.10822(12) 0.52554(19) 0.0314(7) Uani 1 1 d . . . H50A H 0.3183 0.1118 0.5048 0.038 Uiso 1 1 calc R . . H50B H 0.2137 0.1133 0.4778 0.038 Uiso 1 1 calc R . . C51 C 0.2439(2) 0.05325(12) 0.56094(18) 0.0265(7) Uani 1 1 d . . . C52 C 0.21753(19) 0.00335(11) 0.69168(19) 0.0239(6) Uani 1 1 d . . . C53 C 0.7917(5) 0.2983(3) 0.8170(4) 0.118(2) Uani 1 1 d . . . H53A H 0.8363 0.2864 0.8590 0.177 Uiso 1 1 calc R . . H53B H 0.7955 0.2757 0.7674 0.177 Uiso 1 1 calc R . . H53C H 0.7310 0.2957 0.8397 0.177 Uiso 1 1 calc R . . C54 C 0.8094(9) 0.3518(3) 0.7953(4) 0.181(5) Uani 1 1 d . . . C55 C 0.8063(5) 0.3694(3) 0.7114(4) 0.121(2) Uani 1 1 d . . . H55A H 0.7529 0.3919 0.7020 0.181 Uiso 1 1 calc R . . H55B H 0.8030 0.3384 0.6742 0.181 Uiso 1 1 calc R . . H55C H 0.8607 0.3901 0.6999 0.181 Uiso 1 1 calc R . . N1 N 0.46262(19) 0.33120(11) 0.68198(16) 0.0346(6) Uani 1 1 d . . . H1 H 0.4068 0.3414 0.6908 0.041 Uiso 1 1 calc R . . N2 N 0.5927(2) 0.34465(15) 0.6076(2) 0.0650(10) Uani 1 1 d . . . H2A H 0.6253 0.3615 0.5708 0.078 Uiso 1 1 calc R . . H2B H 0.6159 0.3176 0.6358 0.078 Uiso 1 1 calc R . . N3 N 0.28575(16) 0.03320(9) 0.93037(15) 0.0249(5) Uani 1 1 d . . . H3A H 0.2693 0.0176 0.8833 0.030 Uiso 1 1 calc R . . N4 N 0.39402(19) 0.03689(11) 1.03734(16) 0.0359(7) Uani 1 1 d . . . H4A H 0.4469 0.0286 1.0597 0.043 Uiso 1 1 calc R . . H4B H 0.3566 0.0574 1.0646 0.043 Uiso 1 1 calc R . . N5 N 0.15239(18) 0.31858(10) 0.70347(16) 0.0313(6) Uani 1 1 d . . . H5A H 0.1737 0.2875 0.7203 0.038 Uiso 1 1 calc R . . N6 N 0.1845(2) 0.40773(10) 0.67736(17) 0.0365(7) Uani 1 1 d . . . H6A H 0.2193 0.4362 0.6808 0.044 Uiso 1 1 calc R . . H6B H 0.1320 0.4095 0.6509 0.044 Uiso 1 1 calc R . . N7 N 0.23055(17) 0.04975(9) 0.64494(15) 0.0250(6) Uani 1 1 d . . . H7 H 0.2302 0.0801 0.6726 0.030 Uiso 1 1 calc R . . N8 N 0.20445(18) -0.04180(10) 0.64914(16) 0.0316(6) Uani 1 1 d . . . H8D H 0.1952 -0.0720 0.6758 0.038 Uiso 1 1 calc R . . H8E H 0.2050 -0.0415 0.5944 0.038 Uiso 1 1 calc R . . O1 O 0.36263(13) 0.23181(7) 0.74389(12) 0.0242(4) Uani 1 1 d . . . O2 O 0.56928(17) 0.27149(11) 0.72589(19) 0.0560(7) Uani 1 1 d . . . O3 O 0.4696(2) 0.39697(13) 0.58525(18) 0.0704(9) Uani 1 1 d . . . O4 O 0.18792(13) 0.12316(7) 0.84250(12) 0.0230(4) Uani 1 1 d . . . O5 O 0.23027(16) 0.08713(10) 1.03184(13) 0.0390(6) Uani 1 1 d . . . O6 O 0.41773(15) -0.01030(8) 0.91968(13) 0.0319(5) Uani 1 1 d . . . O7 O 0.08029(14) 0.22401(8) 0.69294(13) 0.0277(5) Uani 1 1 d . . . O8 O 0.02666(17) 0.35796(9) 0.64594(16) 0.0460(6) Uani 1 1 d . . . O9 O 0.28346(15) 0.35621(8) 0.74980(14) 0.0355(5) Uani 1 1 d . . . O10 O 0.24075(14) 0.14857(7) 0.58663(12) 0.0250(5) Uani 1 1 d . . . O11 O 0.24683(18) 0.01476(9) 0.51493(14) 0.0425(6) Uani 1 1 d . . . O12 O 0.21771(15) 0.00610(8) 0.76768(13) 0.0316(5) Uani 1 1 d . . . O13 O 0.8774(7) 0.3689(4) 0.8412(4) 0.263(5) Uani 1 1 d . . . O14 O 0.4554(7) 0.4956(5) 0.4911(8) 0.162(5) Uani 0.50 1 d P . . H14A H 0.4296 0.5167 0.4597 0.243 Uiso 0.50 1 d PR . . H14B H 0.4179 0.4738 0.5065 0.243 Uiso 0.50 1 d PR . . S1 S 0.42124(5) 0.21296(3) 0.56611(5) 0.02603(19) Uani 1 1 d . . . S2 S 0.37883(5) 0.15615(3) 0.89927(4) 0.02093(17) Uani 1 1 d . . . S3 S 0.00653(5) 0.18475(3) 0.85754(5) 0.02596(19) Uani 1 1 d . . . S4 S 0.05364(5) 0.17493(3) 0.51531(5) 0.0303(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0158(14) 0.0173(14) 0.0266(15) -0.0006(11) -0.0012(11) 0.0012(11) C2 0.0171(15) 0.0229(15) 0.0242(14) 0.0052(11) 0.0004(11) 0.0003(12) C3 0.0207(16) 0.0273(16) 0.0219(14) -0.0015(11) 0.0021(11) 0.0007(12) C4 0.0192(15) 0.0205(15) 0.0238(14) -0.0020(11) -0.0001(11) -0.0011(12) C5 0.0215(15) 0.0189(14) 0.0237(14) 0.0024(11) -0.0005(11) 0.0038(12) C6 0.0142(14) 0.0219(15) 0.0235(14) 0.0001(11) -0.0007(11) 0.0007(11) C7 0.0240(16) 0.0202(15) 0.0273(15) -0.0031(11) 0.0033(12) 0.0043(12) C8 0.158(6) 0.048(3) 0.082(3) 0.022(2) 0.070(4) 0.056(3) C9 0.103(4) 0.090(4) 0.079(3) -0.038(3) -0.040(3) 0.076(3) C10 0.041(3) 0.028(2) 0.228(7) -0.032(3) 0.021(3) -0.003(2) C11 0.0363(19) 0.0198(15) 0.0330(17) -0.0046(12) 0.0020(14) -0.0021(13) C12 0.0283(19) 0.0294(18) 0.0418(19) -0.0053(14) 0.0015(14) -0.0047(14) C13 0.055(3) 0.050(2) 0.0338(19) 0.0018(17) -0.0067(18) -0.026(2) C14 0.0176(15) 0.0226(15) 0.0192(14) -0.0010(11) -0.0006(11) 0.0012(11) C15 0.0245(16) 0.0201(14) 0.0166(13) -0.0030(10) 0.0008(11) 0.0017(12) C16 0.0178(15) 0.0232(15) 0.0205(14) -0.0016(11) 0.0007(11) -0.0003(12) C17 0.0186(15) 0.0235(15) 0.0279(15) -0.0040(12) 0.0028(12) 0.0032(12) C18 0.0203(15) 0.0202(15) 0.0238(14) -0.0046(11) 0.0025(11) 0.0001(12) C19 0.0201(15) 0.0233(15) 0.0192(14) -0.0019(11) 0.0010(11) -0.0002(12) C20 0.0239(16) 0.0230(15) 0.0296(16) -0.0082(12) 0.0016(12) 0.0011(12) C21 0.0360(19) 0.0211(16) 0.0449(19) -0.0042(13) 0.0041(15) 0.0040(14) C22 0.057(2) 0.0338(19) 0.0334(19) -0.0111(14) 0.0005(17) 0.0023(17) C23 0.0311(19) 0.0272(18) 0.068(2) -0.0198(16) -0.0031(17) -0.0024(15) C24 0.0205(16) 0.0189(15) 0.0321(16) -0.0019(12) 0.0012(12) -0.0017(12) C25 0.0242(17) 0.0235(16) 0.0333(17) 0.0016(12) 0.0054(13) 0.0005(13) C26 0.0273(17) 0.0183(14) 0.0276(15) 0.0036(12) 0.0005(12) 0.0038(12) C27 0.0152(15) 0.0237(15) 0.0299(15) -0.0026(12) -0.0035(12) -0.0002(12) C28 0.0157(15) 0.0188(15) 0.0372(17) 0.0007(12) -0.0052(12) -0.0040(11) C29 0.0160(15) 0.0252(16) 0.0321(16) 0.0043(12) -0.0023(12) 0.0001(12) C30 0.0199(15) 0.0219(15) 0.0299(16) -0.0017(12) -0.0046(12) -0.0020(12) C31 0.0178(15) 0.0213(15) 0.0296(15) 0.0011(12) -0.0057(12) -0.0016(12) C32 0.0172(15) 0.0252(16) 0.0283(15) 0.0009(12) 0.0001(12) -0.0045(12) C33 0.0272(17) 0.0231(16) 0.0337(17) 0.0004(12) -0.0039(13) -0.0073(13) C34 0.055(2) 0.0286(18) 0.049(2) 0.0053(15) -0.0093(18) -0.0093(17) C35 0.046(2) 0.0300(18) 0.049(2) -0.0073(15) 0.0037(17) -0.0120(16) C36 0.033(2) 0.037(2) 0.064(2) 0.0000(17) 0.0046(17) -0.0132(16) C37 0.0270(18) 0.0266(17) 0.053(2) 0.0006(15) -0.0015(15) 0.0005(14) C38 0.0350(19) 0.0221(16) 0.0334(17) -0.0024(13) -0.0019(14) 0.0004(14) C39 0.0345(19) 0.0193(15) 0.0306(16) -0.0033(12) 0.0038(14) -0.0013(13) C40 0.0237(16) 0.0263(16) 0.0243(15) 0.0029(12) -0.0007(12) -0.0050(13) C41 0.0257(16) 0.0215(15) 0.0198(14) 0.0023(11) -0.0006(12) 0.0000(12) C42 0.0198(15) 0.0266(16) 0.0193(14) 0.0009(11) 0.0001(11) 0.0015(12) C43 0.0226(16) 0.0241(15) 0.0250(15) 0.0038(12) -0.0003(12) -0.0035(12) C44 0.0254(16) 0.0227(15) 0.0244(15) 0.0038(12) 0.0000(12) 0.0015(12) C45 0.0214(16) 0.0298(17) 0.0246(15) 0.0042(12) -0.0021(12) 0.0001(13) C46 0.0302(18) 0.0289(17) 0.0292(16) 0.0099(13) -0.0021(13) -0.0005(14) C47 0.041(2) 0.0312(19) 0.075(3) 0.0238(18) -0.0083(19) -0.0082(16) C48 0.114(4) 0.042(2) 0.034(2) 0.0153(17) 0.008(2) 0.004(2) C49 0.034(2) 0.038(2) 0.069(3) 0.0245(18) -0.0025(18) 0.0052(16) C50 0.0367(19) 0.0291(17) 0.0281(16) 0.0005(13) -0.0037(14) -0.0030(14) C51 0.0237(16) 0.0262(16) 0.0294(16) -0.0002(13) -0.0032(12) 0.0015(13) C52 0.0188(15) 0.0207(15) 0.0319(17) -0.0028(12) -0.0028(12) 0.0042(12) C53 0.160(7) 0.107(5) 0.089(4) 0.028(4) 0.020(4) -0.034(5) C54 0.382(16) 0.117(6) 0.044(3) 0.005(3) -0.002(6) -0.126(8) C55 0.135(6) 0.119(6) 0.107(5) 0.045(4) -0.024(4) -0.013(5) N1 0.0325(16) 0.0321(15) 0.0393(16) 0.0045(12) 0.0041(12) -0.0098(12) N2 0.049(2) 0.082(3) 0.065(2) 0.014(2) 0.0226(18) -0.021(2) N3 0.0245(14) 0.0229(13) 0.0272(13) -0.0034(10) -0.0034(10) 0.0064(11) N4 0.0359(16) 0.0451(17) 0.0264(14) -0.0056(12) -0.0056(12) 0.0160(13) N5 0.0343(16) 0.0159(13) 0.0434(16) 0.0037(11) -0.0036(12) -0.0018(11) N6 0.0450(18) 0.0224(14) 0.0417(16) 0.0051(11) -0.0099(13) -0.0090(12) N7 0.0286(14) 0.0163(12) 0.0301(13) -0.0028(10) -0.0022(11) 0.0004(10) N8 0.0419(17) 0.0191(13) 0.0335(14) -0.0015(11) -0.0028(12) -0.0024(12) O1 0.0216(11) 0.0190(10) 0.0320(11) 0.0017(8) 0.0015(9) 0.0033(8) O2 0.0302(15) 0.0572(18) 0.081(2) 0.0121(15) 0.0123(13) 0.0064(13) O3 0.081(2) 0.074(2) 0.0551(18) 0.0325(16) -0.0176(16) -0.0260(18) O4 0.0242(11) 0.0187(10) 0.0259(10) -0.0055(8) -0.0019(8) 0.0024(8) O5 0.0360(14) 0.0542(15) 0.0269(12) -0.0106(11) 0.0026(10) 0.0146(12) O6 0.0299(12) 0.0304(12) 0.0353(12) -0.0064(9) -0.0033(10) 0.0102(10) O7 0.0234(11) 0.0194(11) 0.0402(12) 0.0007(9) -0.0043(9) -0.0051(9) O8 0.0446(15) 0.0256(12) 0.0671(17) 0.0058(11) -0.0134(13) 0.0032(11) O9 0.0308(13) 0.0238(11) 0.0515(14) -0.0039(10) -0.0070(11) 0.0012(10) O10 0.0295(12) 0.0187(10) 0.0268(11) 0.0049(8) -0.0018(9) -0.0010(9) O11 0.0667(18) 0.0265(12) 0.0342(13) -0.0065(10) -0.0004(12) 0.0015(12) O12 0.0427(14) 0.0230(11) 0.0291(12) -0.0008(9) -0.0006(10) 0.0047(10) O13 0.371(12) 0.319(11) 0.098(5) 0.029(6) 0.009(6) -0.196(10) O14 0.168(12) 0.137(8) 0.179(11) 0.078(8) -0.041(10) -0.032(10) S1 0.0203(4) 0.0308(4) 0.0271(4) 0.0103(3) 0.0025(3) 0.0029(3) S2 0.0183(4) 0.0239(4) 0.0206(3) -0.0013(3) -0.0003(3) 0.0047(3) S3 0.0165(4) 0.0298(4) 0.0316(4) -0.0076(3) 0.0000(3) 0.0001(3) S4 0.0278(4) 0.0342(4) 0.0287(4) 0.0072(3) -0.0074(3) -0.0110(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.386(3) . ? C1 C2 1.389(4) . ? C1 C6 1.396(4) . ? C2 C3 1.389(4) . ? C2 S1 1.781(3) . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 C7 1.541(4) . ? C5 C6 1.397(4) . ? C5 H5 0.9500 . ? C6 S2 1.775(3) . ? C7 C10 1.489(5) . ? C7 C8 1.492(5) . ? C7 C9 1.530(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O1 1.438(3) . ? C11 C12 1.521(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O2 1.217(4) . ? C12 N1 1.354(4) . ? C13 O3 1.225(5) . ? C13 N2 1.323(5) . ? C13 N1 1.410(4) . ? C14 C19 1.393(4) . ? C14 C15 1.394(4) . ? C14 S2 1.779(3) . ? C15 O4 1.383(3) . ? C15 C16 1.395(4) . ? C16 C17 1.393(4) . ? C16 S3 1.774(3) . ? C17 C18 1.391(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 C20 1.535(4) . ? C19 H19 0.9500 . ? C20 C23 1.526(4) . ? C20 C22 1.538(4) . ? C20 C21 1.539(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O4 1.445(3) . ? C24 C25 1.515(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O5 1.217(4) . ? C25 N3 1.370(4) . ? C26 O6 1.227(4) . ? C26 N4 1.322(4) . ? C26 N3 1.401(4) . ? C27 C28 1.389(4) . ? C27 C32 1.390(4) . ? C27 S3 1.779(3) . ? C28 O7 1.388(3) . ? C28 C29 1.389(4) . ? C29 C30 1.401(4) . ? C29 S4 1.782(3) . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 C32 1.397(4) . ? C31 C33 1.530(4) . ? C32 H32 0.9500 . ? C33 C36 1.529(5) . ? C33 C34 1.537(4) . ? C33 C35 1.538(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O7 1.429(4) . ? C37 C38 1.504(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O8 1.212(4) . ? C38 N5 1.366(4) . ? C39 O9 1.232(4) . ? C39 N6 1.317(4) . ? C39 N5 1.406(4) . ? C40 C41 1.394(4) . ? C40 C45 1.395(4) . ? C40 S4 1.777(3) . ? C41 C42 1.388(4) . ? C41 O10 1.390(3) . ? C42 C43 1.402(4) . ? C42 S1 1.769(3) . ? C43 C44 1.394(4) . ? C43 H43 0.9500 . ? C44 C45 1.388(4) . ? C44 C46 1.541(4) . ? C45 H45 0.9500 . ? C46 C49 1.524(5) . ? C46 C48 1.526(5) . ? C46 C47 1.530(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 O10 1.430(4) . ? C50 C51 1.501(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O11 1.215(4) . ? C51 N7 1.370(4) . ? C52 O12 1.223(3) . ? C52 N8 1.332(4) . ? C52 N7 1.398(4) . ? C53 C54 1.408(8) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 O13 1.308(11) . ? C54 C55 1.418(8) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? N5 H5A 0.8800 . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? N7 H7 0.8800 . ? N8 H8D 0.8800 . ? N8 H8E 0.8800 . ? O14 O14 1.36(2) 3_666 ? O14 H14A 0.8199 . ? O14 H14B 0.8200 . ? 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 O1 C1 C2 119.8(2) . . ? O1 C1 C6 121.4(2) . . ? C2 C1 C6 118.8(2) . . ? C1 C2 C3 120.9(2) . . ? C1 C2 S1 122.0(2) . . ? C3 C2 S1 116.7(2) . . ? C2 C3 C4 121.5(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 116.7(3) . . ? C5 C4 C7 121.5(2) . . ? C3 C4 C7 121.8(2) . . ? C4 C5 C6 122.7(3) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C1 C6 C5 119.1(3) . . ? C1 C6 S2 124.4(2) . . ? C5 C6 S2 116.0(2) . . ? C10 C7 C8 111.5(4) . . ? C10 C7 C9 108.2(4) . . ? C8 C7 C9 105.2(4) . . ? C10 C7 C4 109.4(3) . . ? C8 C7 C4 112.6(3) . . ? C9 C7 C4 109.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 110.9(2) . . ? O1 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? O2 C12 N1 124.5(3) . . ? O2 C12 C11 120.4(3) . . ? N1 C12 C11 115.1(3) . . ? O3 C13 N2 125.7(4) . . ? O3 C13 N1 118.6(4) . . ? N2 C13 N1 115.7(4) . . ? C19 C14 C15 119.9(3) . . ? C19 C14 S2 117.1(2) . . ? C15 C14 S2 122.5(2) . . ? O4 C15 C14 120.4(2) . . ? O4 C15 C16 120.8(2) . . ? C14 C15 C16 118.8(2) . . ? C17 C16 C15 120.0(3) . . ? C17 C16 S3 115.6(2) . . ? C15 C16 S3 124.1(2) . . ? C18 C17 C16 121.8(3) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 117.3(2) . . ? C19 C18 C20 122.2(3) . . ? C17 C18 C20 120.5(3) . . ? C18 C19 C14 122.0(3) . . ? C18 C19 H19 119.0 . . ? C14 C19 H19 119.0 . . ? C23 C20 C18 111.8(2) . . ? C23 C20 C22 109.7(3) . . ? C18 C20 C22 107.4(2) . . ? C23 C20 C21 108.2(3) . . ? C18 C20 C21 110.2(2) . . ? C22 C20 C21 109.5(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O4 C24 C25 108.9(2) . . ? O4 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O4 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? O5 C25 N3 123.8(3) . . ? O5 C25 C24 122.3(3) . . ? N3 C25 C24 113.8(3) . . ? O6 C26 N4 125.1(3) . . ? O6 C26 N3 117.5(3) . . ? N4 C26 N3 117.4(3) . . ? C28 C27 C32 120.0(3) . . ? C28 C27 S3 121.8(2) . . ? C32 C27 S3 117.6(2) . . ? O7 C28 C27 120.0(3) . . ? O7 C28 C29 120.5(3) . . ? C27 C28 C29 119.5(3) . . ? C28 C29 C30 119.5(3) . . ? C28 C29 S4 124.3(2) . . ? C30 C29 S4 115.6(2) . . ? C31 C30 C29 121.9(3) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 117.2(3) . . ? C30 C31 C33 123.1(3) . . ? C32 C31 C33 119.6(3) . . ? C27 C32 C31 121.7(3) . . ? C27 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C36 C33 C31 108.3(3) . . ? C36 C33 C34 109.6(3) . . ? C31 C33 C34 110.9(2) . . ? C36 C33 C35 108.6(3) . . ? C31 C33 C35 111.8(3) . . ? C34 C33 C35 107.6(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O7 C37 C38 110.0(3) . . ? O7 C37 H37A 109.7 . . ? C38 C37 H37A 109.7 . . ? O7 C37 H37B 109.7 . . ? C38 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? O8 C38 N5 124.7(3) . . ? O8 C38 C37 119.6(3) . . ? N5 C38 C37 115.7(3) . . ? O9 C39 N6 124.5(3) . . ? O9 C39 N5 118.6(3) . . ? N6 C39 N5 116.9(3) . . ? C41 C40 C45 119.9(3) . . ? C41 C40 S4 122.5(2) . . ? C45 C40 S4 116.9(2) . . ? C42 C41 O10 121.4(3) . . ? C42 C41 C40 119.3(3) . . ? O10 C41 C40 119.3(3) . . ? C41 C42 C43 119.7(3) . . ? C41 C42 S1 125.0(2) . . ? C43 C42 S1 114.5(2) . . ? C44 C43 C42 121.8(3) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C45 C44 C43 117.2(3) . . ? C45 C44 C46 121.4(3) . . ? C43 C44 C46 121.3(3) . . ? C44 C45 C40 122.0(3) . . ? C44 C45 H45 119.0 . . ? C40 C45 H45 119.0 . . ? C49 C46 C48 110.1(3) . . ? C49 C46 C47 107.4(3) . . ? C48 C46 C47 108.2(3) . . ? C49 C46 C44 111.0(3) . . ? C48 C46 C44 108.1(3) . . ? C47 C46 C44 111.9(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O10 C50 C51 111.4(2) . . ? O10 C50 H50A 109.4 . . ? C51 C50 H50A 109.4 . . ? O10 C50 H50B 109.4 . . ? C51 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O11 C51 N7 123.8(3) . . ? O11 C51 C50 119.3(3) . . ? N7 C51 C50 116.9(3) . . ? O12 C52 N8 123.8(3) . . ? O12 C52 N7 119.5(3) . . ? N8 C52 N7 116.7(3) . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O13 C54 C53 108.4(9) . . ? O13 C54 C55 116.3(8) . . ? C53 C54 C55 121.9(6) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C12 N1 C13 128.2(3) . . ? C12 N1 H1 115.9 . . ? C13 N1 H1 115.9 . . ? C13 N2 H2A 120.0 . . ? C13 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C25 N3 C26 128.9(3) . . ? C25 N3 H3A 115.6 . . ? C26 N3 H3A 115.6 . . ? C26 N4 H4A 120.0 . . ? C26 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C38 N5 C39 127.4(3) . . ? C38 N5 H5A 116.3 . . ? C39 N5 H5A 116.3 . . ? C39 N6 H6A 120.0 . . ? C39 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C51 N7 C52 127.3(2) . . ? C51 N7 H7 116.3 . . ? C52 N7 H7 116.3 . . ? C52 N8 H8D 120.0 . . ? C52 N8 H8E 120.0 . . ? H8D N8 H8E 120.0 . . ? C1 O1 C11 113.7(2) . . ? C15 O4 C24 113.0(2) . . ? C28 O7 C37 113.9(2) . . ? C41 O10 C50 112.7(2) . . ? O14 O14 H14A 117.5 3_666 . ? O14 O14 H14B 134.7 3_666 . ? H14A O14 H14B 107.7 . . ? C42 S1 C2 107.65(13) . . ? C6 S2 C14 107.10(13) . . ? C16 S3 C27 106.00(13) . . ? C40 S4 C29 108.58(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 177.0(3) . . . . ? C6 C1 C2 C3 -5.2(4) . . . . ? O1 C1 C2 S1 5.1(4) . . . . ? C6 C1 C2 S1 -177.1(2) . . . . ? C1 C2 C3 C4 1.7(4) . . . . ? S1 C2 C3 C4 174.0(2) . . . . ? C2 C3 C4 C5 2.8(4) . . . . ? C2 C3 C4 C7 -177.3(3) . . . . ? C3 C4 C5 C6 -4.0(4) . . . . ? C7 C4 C5 C6 176.2(3) . . . . ? O1 C1 C6 C5 -178.2(2) . . . . ? C2 C1 C6 C5 4.1(4) . . . . ? O1 C1 C6 S2 -6.6(4) . . . . ? C2 C1 C6 S2 175.7(2) . . . . ? C4 C5 C6 C1 0.5(4) . . . . ? C4 C5 C6 S2 -171.7(2) . . . . ? C5 C4 C7 C10 74.8(4) . . . . ? C3 C4 C7 C10 -105.0(4) . . . . ? C5 C4 C7 C8 -160.5(4) . . . . ? C3 C4 C7 C8 19.6(5) . . . . ? C5 C4 C7 C9 -43.7(4) . . . . ? C3 C4 C7 C9 136.5(4) . . . . ? O1 C11 C12 O2 -101.5(4) . . . . ? O1 C11 C12 N1 78.1(3) . . . . ? C19 C14 C15 O4 -175.7(2) . . . . ? S2 C14 C15 O4 -3.5(4) . . . . ? C19 C14 C15 C16 4.3(4) . . . . ? S2 C14 C15 C16 176.5(2) . . . . ? O4 C15 C16 C17 176.9(2) . . . . ? C14 C15 C16 C17 -3.1(4) . . . . ? O4 C15 C16 S3 3.0(4) . . . . ? C14 C15 C16 S3 -177.0(2) . . . . ? C15 C16 C17 C18 -1.2(4) . . . . ? S3 C16 C17 C18 173.2(2) . . . . ? C16 C17 C18 C19 4.2(4) . . . . ? C16 C17 C18 C20 -175.3(3) . . . . ? C17 C18 C19 C14 -3.0(4) . . . . ? C20 C18 C19 C14 176.5(3) . . . . ? C15 C14 C19 C18 -1.2(4) . . . . ? S2 C14 C19 C18 -173.8(2) . . . . ? C19 C18 C20 C23 21.2(4) . . . . ? C17 C18 C20 C23 -159.4(3) . . . . ? C19 C18 C20 C22 -99.2(3) . . . . ? C17 C18 C20 C22 80.2(3) . . . . ? C19 C18 C20 C21 141.5(3) . . . . ? C17 C18 C20 C21 -39.0(4) . . . . ? O4 C24 C25 O5 100.6(3) . . . . ? O4 C24 C25 N3 -76.5(3) . . . . ? C32 C27 C28 O7 -178.5(3) . . . . ? S3 C27 C28 O7 10.4(4) . . . . ? C32 C27 C28 C29 -0.7(4) . . . . ? S3 C27 C28 C29 -171.8(2) . . . . ? O7 C28 C29 C30 176.7(3) . . . . ? C27 C28 C29 C30 -1.2(4) . . . . ? O7 C28 C29 S4 -12.5(4) . . . . ? C27 C28 C29 S4 169.6(2) . . . . ? C28 C29 C30 C31 1.7(4) . . . . ? S4 C29 C30 C31 -169.9(2) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C29 C30 C31 C33 176.4(3) . . . . ? C28 C27 C32 C31 2.1(4) . . . . ? S3 C27 C32 C31 173.6(2) . . . . ? C30 C31 C32 C27 -1.6(4) . . . . ? C33 C31 C32 C27 -178.5(3) . . . . ? C30 C31 C33 C36 -103.5(3) . . . . ? C32 C31 C33 C36 73.2(3) . . . . ? C30 C31 C33 C34 136.3(3) . . . . ? C32 C31 C33 C34 -47.1(4) . . . . ? C30 C31 C33 C35 16.1(4) . . . . ? C32 C31 C33 C35 -167.2(3) . . . . ? O7 C37 C38 O8 169.8(3) . . . . ? O7 C37 C38 N5 -11.3(4) . . . . ? C45 C40 C41 C42 1.3(4) . . . . ? S4 C40 C41 C42 172.0(2) . . . . ? C45 C40 C41 O10 -178.0(3) . . . . ? S4 C40 C41 O10 -7.3(4) . . . . ? O10 C41 C42 C43 179.3(3) . . . . ? C40 C41 C42 C43 0.1(4) . . . . ? O10 C41 C42 S1 9.5(4) . . . . ? C40 C41 C42 S1 -169.8(2) . . . . ? C41 C42 C43 C44 -2.5(4) . . . . ? S1 C42 C43 C44 168.4(2) . . . . ? C42 C43 C44 C45 3.3(4) . . . . ? C42 C43 C44 C46 -172.3(3) . . . . ? C43 C44 C45 C40 -1.9(4) . . . . ? C46 C44 C45 C40 173.7(3) . . . . ? C41 C40 C45 C44 -0.3(4) . . . . ? S4 C40 C45 C44 -171.5(2) . . . . ? C45 C44 C46 C49 35.7(4) . . . . ? C43 C44 C46 C49 -148.8(3) . . . . ? C45 C44 C46 C48 -85.1(4) . . . . ? C43 C44 C46 C48 90.3(4) . . . . ? C45 C44 C46 C47 155.8(3) . . . . ? C43 C44 C46 C47 -28.8(4) . . . . ? O10 C50 C51 O11 173.6(3) . . . . ? O10 C50 C51 N7 -7.0(4) . . . . ? O2 C12 N1 C13 1.5(5) . . . . ? C11 C12 N1 C13 -178.1(3) . . . . ? O3 C13 N1 C12 -179.1(3) . . . . ? N2 C13 N1 C12 -0.1(5) . . . . ? O5 C25 N3 C26 -11.8(5) . . . . ? C24 C25 N3 C26 165.3(3) . . . . ? O6 C26 N3 C25 -173.2(3) . . . . ? N4 C26 N3 C25 6.6(5) . . . . ? O8 C38 N5 C39 0.7(5) . . . . ? C37 C38 N5 C39 -178.1(3) . . . . ? O9 C39 N5 C38 171.8(3) . . . . ? N6 C39 N5 C38 -8.3(5) . . . . ? O11 C51 N7 C52 -0.7(5) . . . . ? C50 C51 N7 C52 180.0(3) . . . . ? O12 C52 N7 C51 171.0(3) . . . . ? N8 C52 N7 C51 -9.8(4) . . . . ? C2 C1 O1 C11 -106.4(3) . . . . ? C6 C1 O1 C11 75.9(3) . . . . ? C12 C11 O1 C1 81.1(3) . . . . ? C14 C15 O4 C24 104.5(3) . . . . ? C16 C15 O4 C24 -75.5(3) . . . . ? C25 C24 O4 C15 -78.8(3) . . . . ? C27 C28 O7 C37 -96.5(3) . . . . ? C29 C28 O7 C37 85.6(3) . . . . ? C38 C37 O7 C28 -175.7(3) . . . . ? C42 C41 O10 C50 -92.5(3) . . . . ? C40 C41 O10 C50 86.8(3) . . . . ? C51 C50 O10 C41 -167.7(2) . . . . ? C41 C42 S1 C2 -36.2(3) . . . . ? C43 C42 S1 C2 153.5(2) . . . . ? C1 C2 S1 C42 -64.9(3) . . . . ? C3 C2 S1 C42 122.9(2) . . . . ? C1 C6 S2 C14 44.8(3) . . . . ? C5 C6 S2 C14 -143.4(2) . . . . ? C19 C14 S2 C6 -121.5(2) . . . . ? C15 C14 S2 C6 66.1(3) . . . . ? C17 C16 S3 C27 143.4(2) . . . . ? C15 C16 S3 C27 -42.5(3) . . . . ? C28 C27 S3 C16 -62.0(3) . . . . ? C32 C27 S3 C16 126.7(2) . . . . ? C41 C40 S4 C29 54.1(3) . . . . ? C45 C40 S4 C29 -135.0(2) . . . . ? C28 C29 S4 C40 43.3(3) . . . . ? C30 C29 S4 C40 -145.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.930 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.083