data_monosubstituted_ddd38 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H50 B Cl P S4' _chemical_formula_weight 730.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 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 35.939(5) _cell_length_b 11.4367(17) _cell_length_c 22.415(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.668(2) _cell_angle_gamma 90.00 _cell_volume 8084(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6488 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64390 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 30.53 _reflns_number_total 12323 _reflns_number_gt 7448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker, 2008)' _computing_cell_refinement 'APEX II (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0982P)^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 12323 _refine_ls_number_parameters 466 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B B 0.07512(10) 0.9140(3) 0.20055(15) 0.0654(8) Uani 1 1 d . . . H0A H 0.0946 0.8576 0.2315 0.098 Uiso 1 1 calc R . . H0B H 0.0538 0.8744 0.1612 0.098 Uiso 1 1 calc R . . H0C H 0.0619 0.9560 0.2225 0.098 Uiso 1 1 calc R . . C1 C 0.14982(6) 1.08159(19) 0.24800(9) 0.0430(4) Uani 1 1 d . . . C2 C 0.16382(6) 1.04112(18) 0.31291(9) 0.0389(4) Uani 1 1 d . . . H2 H 0.1509 0.9803 0.3236 0.047 Uiso 1 1 calc R . . C3 C 0.20045(6) 1.10225(17) 0.36256(9) 0.0371(4) Uani 1 1 d . . . C4 C 0.22645(6) 1.08109(16) 0.43477(9) 0.0367(4) Uani 1 1 d . . . C5 C 0.22199(6) 0.99809(16) 0.47825(9) 0.0378(4) Uani 1 1 d . . . C6 C 0.18634(6) 0.92860(18) 0.47104(11) 0.0449(5) Uani 1 1 d . . . C7 C 0.14141(7) 0.94459(19) 0.43181(11) 0.0480(5) Uani 1 1 d . . . C8 C 0.11656(7) 1.0470(2) 0.40087(14) 0.0591(6) Uani 1 1 d . . . C9 C 0.12954(7) 1.1638(2) 0.40134(13) 0.0596(6) Uani 1 1 d . . . H9 H 0.1579 1.1858 0.4212 0.071 Uiso 1 1 calc R . . C10 C 0.09685(8) 1.2418(2) 0.37004(15) 0.0695(7) Uani 1 1 d . . . H10 H 0.1003 1.3213 0.3657 0.083 Uiso 1 1 calc R . . C11 C 0.07330(8) 1.0387(2) 0.37016(14) 0.0597(6) Uani 1 1 d . . . C12 C 0.05126(8) 0.9326(3) 0.36833(14) 0.0690(7) Uani 1 1 d . . . H12 H 0.0218 0.9287 0.3449 0.083 Uiso 1 1 calc R . . C13 C 0.07455(9) 0.8405(3) 0.40135(14) 0.0721(8) Uani 1 1 d . . . H13 H 0.0609 0.7722 0.4028 0.087 Uiso 1 1 calc R . . C14 C 0.11910(7) 0.84278(18) 0.43421(12) 0.0484(5) Uani 1 1 d . . . C15 C 0.19660(6) 0.82523(18) 0.51058(11) 0.0465(5) Uani 1 1 d . . . C16 C 0.23758(8) 0.79827(19) 0.56450(11) 0.0500(5) Uani 1 1 d . . . C17 C 0.26986(6) 0.87981(19) 0.58074(10) 0.0467(5) Uani 1 1 d . . . C18 C 0.26146(6) 0.97616(17) 0.53687(10) 0.0408(4) Uani 1 1 d . . . C19 C 0.26663(6) 1.13626(18) 0.46607(10) 0.0424(4) Uani 1 1 d . . . C20 C 0.27835(7) 1.2235(2) 0.43435(11) 0.0510(5) Uani 1 1 d . . . H20 H 0.3043 1.2614 0.4583 0.061 Uiso 1 1 calc R . . C21 C 0.25207(7) 1.25250(19) 0.36924(11) 0.0476(5) Uani 1 1 d . . . H21 H 0.2590 1.3128 0.3485 0.057 Uiso 1 1 calc R . . C22 C 0.21384(6) 1.19006(19) 0.33280(10) 0.0446(4) Uani 1 1 d . . . C23 C 0.24343(8) 0.6852(2) 0.60269(11) 0.0542(6) Uani 1 1 d . . . H23A H 0.2730 0.6626 0.6231 0.065 Uiso 1 1 calc R . . H23B H 0.2269 0.6248 0.5705 0.065 Uiso 1 1 calc R . . C24 C 0.23047(10) 0.6908(2) 0.65853(13) 0.0629(7) Uani 1 1 d . . . H24A H 0.2501 0.7407 0.6951 0.076 Uiso 1 1 calc R . . H24B H 0.2024 0.7252 0.6401 0.076 Uiso 1 1 calc R . . C25 C 0.23012(11) 0.5735(3) 0.68602(15) 0.0762(8) Uani 1 1 d . . . H25A H 0.2102 0.5245 0.6502 0.114 Uiso 1 1 calc R . . H25B H 0.2220 0.5802 0.7210 0.114 Uiso 1 1 calc R . . H25C H 0.2579 0.5397 0.7048 0.114 Uiso 1 1 calc R . . C26 C 0.31313(7) 0.8703(2) 0.64155(11) 0.0570(6) Uani 1 1 d . . . H26A H 0.3342 0.8909 0.6281 0.068 Uiso 1 1 calc R . . H26B H 0.3180 0.7897 0.6569 0.068 Uiso 1 1 calc R . . C27 C 0.31902(9) 0.9483(3) 0.70060(13) 0.0718(7) Uani 1 1 d . . . H27A H 0.3074 1.0251 0.6831 0.086 Uiso 1 1 calc R . . H27B H 0.3032 0.9157 0.7215 0.086 Uiso 1 1 calc R . . C28 C 0.36511(14) 0.9615(4) 0.75434(18) 0.1219(15) Uani 1 1 d . . . H28A H 0.3757 0.8875 0.7762 0.183 Uiso 1 1 calc R . . H28B H 0.3673 1.0180 0.7875 0.183 Uiso 1 1 calc R . . H28C H 0.3815 0.9872 0.7333 0.183 Uiso 1 1 calc R . . C29 C 0.12800(7) 0.9434(2) 0.12322(11) 0.0534(5) Uani 1 1 d . . . C30 C 0.14740(10) 0.8316(2) 0.16288(16) 0.0736(7) Uani 1 1 d . . . H30A H 0.1268 0.7915 0.1710 0.110 Uiso 1 1 calc R . . H30B H 0.1716 0.8507 0.2056 0.110 Uiso 1 1 calc R . . H30C H 0.1560 0.7822 0.1371 0.110 Uiso 1 1 calc R . . C31 C 0.09309(9) 0.9117(3) 0.05350(15) 0.0722(7) Uani 1 1 d . . . H31A H 0.0784 0.9813 0.0301 0.108 Uiso 1 1 calc R . . H31B H 0.0736 0.8594 0.0576 0.108 Uiso 1 1 calc R . . H31C H 0.1051 0.8742 0.0283 0.108 Uiso 1 1 calc R . . C32 C 0.16187(9) 1.0112(2) 0.11585(14) 0.0652(7) Uani 1 1 d . . . H32A H 0.1723 0.9648 0.0914 0.098 Uiso 1 1 calc R . . H32B H 0.1848 1.0294 0.1601 0.098 Uiso 1 1 calc R . . H32C H 0.1499 1.0824 0.0914 0.098 Uiso 1 1 calc R . . C33 C 0.07155(7) 1.1517(2) 0.12708(11) 0.0541(5) Uani 1 1 d . . . C34 C 0.02704(8) 1.1079(3) 0.07484(14) 0.0761(8) Uani 1 1 d . . . H34A H 0.0200 1.0397 0.0924 0.114 Uiso 1 1 calc R . . H34B H 0.0269 1.0886 0.0330 0.114 Uiso 1 1 calc R . . H34C H 0.0065 1.1682 0.0666 0.114 Uiso 1 1 calc R . . C35 C 0.08968(9) 1.2266(3) 0.09107(14) 0.0732(8) Uani 1 1 d . . . H35A H 0.0730 1.2962 0.0740 0.110 Uiso 1 1 calc R . . H35B H 0.0891 1.1833 0.0539 0.110 Uiso 1 1 calc R . . H35C H 0.1184 1.2474 0.1225 0.110 Uiso 1 1 calc R . . C36 C 0.06651(9) 1.2227(3) 0.18016(15) 0.0770(8) Uani 1 1 d . . . H36A H 0.0886 1.2804 0.1993 0.116 Uiso 1 1 calc R . . H36B H 0.0684 1.1717 0.2155 0.116 Uiso 1 1 calc R . . H36C H 0.0394 1.2608 0.1592 0.116 Uiso 1 1 calc R . . P P 0.105154(17) 1.02152(5) 0.17335(3) 0.04452(14) Uani 1 1 d . . . S1 S 0.180536(18) 1.19755(5) 0.24635(3) 0.05202(15) Uani 1 1 d . . . S2 S 0.299794(17) 1.07563(5) 0.54455(3) 0.04928(15) Uani 1 1 d . . . S3 S 0.152445(18) 0.73756(5) 0.48820(3) 0.05239(15) Uani 1 1 d . . . S4 S 0.048419(17) 1.17272(5) 0.33974(3) 0.05599(16) Uani 1 1 d . . . C1S C 0.02057(17) 0.6755(5) 0.2402(3) 0.0697(14) Uani 0.50 1 d PD . . C2S C 0.00613(19) 0.5858(4) 0.1829(2) 0.0642(13) Uani 0.50 1 d PD . . C3S C -0.0266(4) 0.5023(13) 0.1919(9) 0.072(3) Uani 0.50 1 d PD . . C4S C 0.0053(6) 0.4316(5) 0.2602(7) 0.074(3) Uani 0.50 1 d PD . . C5S C 0.0268(6) 0.5180(17) 0.3210(11) 0.114(7) Uani 0.50 1 d PD . . C6S C 0.06673(18) 0.5696(5) 0.3227(3) 0.0708(14) Uani 0.50 1 d PD . . C7S C -0.04820(16) 0.4247(5) -0.0510(2) 0.0631(13) Uani 0.50 1 d PD . . Cl2S Cl -0.07327(4) 0.44401(13) -0.00484(7) 0.0689(4) Uani 0.50 1 d PD . . Cl1S Cl 0.0000 0.5000 0.0000 0.0620(2) Uani 1 2 d SD . . 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 B 0.0586(16) 0.081(2) 0.0556(16) -0.0132(14) 0.0263(13) -0.0326(15) C1 0.0396(10) 0.0556(12) 0.0329(9) 0.0011(8) 0.0166(8) -0.0055(9) C2 0.0369(9) 0.0501(11) 0.0309(9) 0.0007(8) 0.0172(8) -0.0038(8) C3 0.0333(9) 0.0454(10) 0.0333(9) -0.0003(7) 0.0165(7) -0.0002(8) C4 0.0348(9) 0.0396(9) 0.0336(9) 0.0027(7) 0.0147(7) -0.0020(7) C5 0.0370(9) 0.0422(10) 0.0297(9) 0.0076(7) 0.0124(7) 0.0006(8) C6 0.0413(10) 0.0426(11) 0.0494(11) 0.0073(9) 0.0207(9) -0.0008(8) C7 0.0441(11) 0.0476(11) 0.0503(12) 0.0120(9) 0.0210(10) -0.0003(9) C8 0.0349(10) 0.0413(11) 0.0793(17) 0.0087(11) 0.0098(11) 0.0034(9) C9 0.0296(10) 0.0540(13) 0.0763(16) 0.0102(11) 0.0103(10) -0.0022(9) C10 0.0610(15) 0.0390(12) 0.098(2) 0.0171(12) 0.0295(15) 0.0118(11) C11 0.0465(12) 0.0602(14) 0.0677(16) 0.0054(12) 0.0237(12) 0.0006(11) C12 0.0451(13) 0.103(2) 0.0612(15) -0.0139(15) 0.0271(12) -0.0179(14) C13 0.0649(16) 0.093(2) 0.0657(17) -0.0070(15) 0.0371(14) -0.0291(16) C14 0.0405(10) 0.0419(11) 0.0607(13) 0.0074(9) 0.0224(10) -0.0019(8) C15 0.0391(10) 0.0449(11) 0.0492(11) 0.0082(9) 0.0161(9) 0.0061(8) C16 0.0703(14) 0.0498(12) 0.0400(11) 0.0010(9) 0.0345(11) 0.0106(10) C17 0.0430(10) 0.0527(12) 0.0383(10) -0.0168(9) 0.0147(9) 0.0022(9) C18 0.0390(10) 0.0457(10) 0.0347(9) 0.0033(8) 0.0151(8) -0.0003(8) C19 0.0367(9) 0.0477(11) 0.0352(9) 0.0033(8) 0.0112(8) -0.0003(8) C20 0.0421(11) 0.0622(13) 0.0505(12) -0.0092(10) 0.0236(10) -0.0163(10) C21 0.0439(11) 0.0522(12) 0.0456(11) 0.0048(9) 0.0208(9) -0.0100(9) C22 0.0420(10) 0.0555(12) 0.0354(10) 0.0010(8) 0.0178(8) -0.0070(9) C23 0.0740(15) 0.0506(12) 0.0462(12) 0.0054(9) 0.0353(11) 0.0155(11) C24 0.100(2) 0.0558(14) 0.0582(14) -0.0050(11) 0.0580(15) 0.0061(13) C25 0.104(2) 0.0748(18) 0.0750(18) 0.0058(14) 0.0633(18) 0.0039(16) C26 0.0482(12) 0.0680(15) 0.0442(12) -0.0025(10) 0.0136(10) 0.0033(11) C27 0.0695(17) 0.0780(18) 0.0539(15) -0.0188(13) 0.0184(13) -0.0055(14) C28 0.135(4) 0.136(3) 0.069(2) -0.052(2) 0.029(2) -0.035(3) C29 0.0541(13) 0.0654(14) 0.0422(11) -0.0040(10) 0.0244(10) -0.0030(11) C30 0.087(2) 0.0687(16) 0.0802(19) 0.0086(14) 0.0522(17) 0.0092(15) C31 0.0710(17) 0.0694(16) 0.0773(18) -0.0173(14) 0.0364(15) -0.0088(14) C32 0.0698(17) 0.0783(17) 0.0586(15) 0.0016(13) 0.0399(14) 0.0008(13) C33 0.0416(11) 0.0691(14) 0.0448(12) 0.0008(10) 0.0152(9) 0.0030(10) C34 0.0501(14) 0.096(2) 0.0584(15) -0.0044(14) 0.0068(12) 0.0049(14) C35 0.0663(16) 0.0819(18) 0.0553(15) 0.0176(13) 0.0163(13) 0.0151(14) C36 0.0645(16) 0.094(2) 0.0688(17) -0.0049(16) 0.0291(14) 0.0140(15) P 0.0391(3) 0.0600(3) 0.0320(3) -0.0015(2) 0.0151(2) -0.0083(2) S1 0.0497(3) 0.0658(4) 0.0352(3) 0.0064(2) 0.0161(2) -0.0151(2) S2 0.0410(3) 0.0592(3) 0.0372(3) 0.0131(2) 0.0104(2) 0.0009(2) S3 0.0483(3) 0.0451(3) 0.0608(3) 0.0095(2) 0.0237(3) -0.0050(2) S4 0.0403(3) 0.0473(3) 0.0680(4) 0.0086(3) 0.0160(3) 0.0074(2) C1S 0.066(3) 0.072(3) 0.054(3) -0.007(2) 0.014(2) -0.013(3) C2S 0.083(4) 0.053(3) 0.044(2) 0.003(2) 0.021(2) -0.015(3) C3S 0.076(6) 0.049(5) 0.090(9) -0.004(5) 0.039(7) -0.003(5) C4S 0.074(9) 0.062(3) 0.055(9) 0.009(3) 0.005(6) -0.003(4) C5S 0.134(12) 0.070(8) 0.079(7) -0.017(5) 0.004(7) -0.029(8) C6S 0.066(3) 0.079(4) 0.057(3) -0.012(3) 0.021(3) -0.019(3) C7S 0.063(3) 0.074(3) 0.042(2) -0.011(2) 0.017(2) -0.025(2) Cl2S 0.0708(8) 0.0820(9) 0.0620(7) -0.0137(6) 0.0382(7) -0.0225(7) Cl1S 0.0445(4) 0.0905(6) 0.0494(4) -0.0059(4) 0.0213(3) -0.0162(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B P 1.919(3) . ? B H0A 0.9600 . ? B H0B 0.9600 . ? B H0C 0.9600 . ? C1 C2 1.372(3) . ? C1 S1 1.737(2) . ? C1 P 1.809(2) . ? C2 C3 1.433(3) . ? C2 H2 0.9300 . ? C3 C22 1.412(3) . ? C3 C4 1.449(3) . ? C4 C19 1.415(3) . ? C4 C5 1.424(2) . ? C5 C18 1.419(3) . ? C5 C6 1.449(3) . ? C6 C15 1.416(3) . ? C6 C7 1.432(3) . ? C7 C14 1.429(3) . ? C7 C8 1.433(3) . ? C8 C11 1.368(3) . ? C8 C9 1.413(3) . ? C9 C10 1.370(3) . ? C9 H9 0.9300 . ? C10 S4 1.726(3) . ? C10 H10 0.9300 . ? C11 C12 1.439(4) . ? C11 S4 1.740(3) . ? C12 C13 1.328(4) . ? C12 H12 0.9300 . ? C13 C14 1.405(3) . ? C13 H13 0.9300 . ? C14 S3 1.720(2) . ? C15 C16 1.420(3) . ? C15 S3 1.735(2) . ? C16 C17 1.394(3) . ? C16 C23 1.508(3) . ? C17 C18 1.410(3) . ? C17 C26 1.501(3) . ? C18 S2 1.730(2) . ? C19 C20 1.402(3) . ? C19 S2 1.727(2) . ? C20 C21 1.345(3) . ? C20 H20 0.9300 . ? C21 C22 1.410(3) . ? C21 H21 0.9300 . ? C22 S1 1.723(2) . ? C23 C24 1.532(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.479(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.525(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.518(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C31 1.506(4) . ? C29 C32 1.517(3) . ? C29 C30 1.522(4) . ? C29 P 1.903(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C36 1.522(4) . ? C33 C35 1.521(4) . ? C33 C34 1.544(3) . ? C33 P 1.884(2) . ? 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 . ? C1S C2S 1.528(7) . ? C1S C1S 1.732(12) 2 ? C2S C5S 1.381(19) 2 ? C2S C3S 1.600(13) . ? C3S C5S 0.34(3) 2 ? C3S C4S 1.27(2) 2 ? C3S C6S 1.527(15) 2 ? C3S C4S 1.621(16) . ? C4S C4S 0.43(2) 2 ? C4S C3S 1.27(2) 2 ? C4S C5S 1.556(17) . ? C4S C5S 1.90(2) 2 ? C5S C3S 0.34(3) 2 ? C5S C6S 1.537(19) . ? C5S C2S 1.381(19) 2 ? C5S C4S 1.90(2) 2 ? C6S C3S 1.527(15) 2 ? C7S Cl2S 1.681(5) . ? C7S Cl1S 1.775(5) . ? Cl1S C7S 1.775(5) 5_565 ? 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 P B H0A 109.5 . . ? P B H0B 109.5 . . ? H0A B H0B 109.5 . . ? P B H0C 109.5 . . ? H0A B H0C 109.5 . . ? H0B B H0C 109.5 . . ? C2 C1 S1 111.51(15) . . ? C2 C1 P 124.34(16) . . ? S1 C1 P 124.15(11) . . ? C1 C2 C3 113.07(18) . . ? C1 C2 H2 123.5 . . ? C3 C2 H2 123.5 . . ? C22 C3 C4 117.59(16) . . ? C22 C3 C2 111.99(16) . . ? C4 C3 C2 130.21(17) . . ? C19 C4 C5 112.40(16) . . ? C19 C4 C3 115.91(16) . . ? C5 C4 C3 130.69(17) . . ? C18 C5 C4 111.16(17) . . ? C18 C5 C6 116.36(16) . . ? C4 C5 C6 132.30(17) . . ? C15 C6 C7 111.67(18) . . ? C15 C6 C5 115.91(18) . . ? C7 C6 C5 132.41(18) . . ? C14 C7 C6 111.13(18) . . ? C14 C7 C8 116.93(19) . . ? C6 C7 C8 131.2(2) . . ? C11 C8 C9 111.1(2) . . ? C11 C8 C7 118.7(2) . . ? C9 C8 C7 129.9(2) . . ? C10 C9 C8 114.4(2) . . ? C10 C9 H9 122.8 . . ? C8 C9 H9 122.8 . . ? C9 C10 S4 111.02(18) . . ? C9 C10 H10 124.5 . . ? S4 C10 H10 124.5 . . ? C8 C11 C12 123.3(2) . . ? C8 C11 S4 112.50(19) . . ? C12 C11 S4 124.0(2) . . ? C13 C12 C11 117.5(2) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? C12 C13 C14 122.2(3) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C7 120.9(2) . . ? C13 C14 S3 126.14(19) . . ? C7 C14 S3 112.48(15) . . ? C6 C15 C16 124.5(2) . . ? C6 C15 S3 111.96(15) . . ? C16 C15 S3 123.48(16) . . ? C17 C16 C15 118.06(19) . . ? C17 C16 C23 123.6(2) . . ? C15 C16 C23 118.3(2) . . ? C16 C17 C18 117.90(18) . . ? C16 C17 C26 123.9(2) . . ? C18 C17 C26 118.2(2) . . ? C17 C18 C5 124.65(18) . . ? C17 C18 S2 123.41(15) . . ? C5 C18 S2 111.74(14) . . ? C20 C19 C4 123.31(18) . . ? C20 C19 S2 125.00(16) . . ? C4 C19 S2 111.55(14) . . ? C21 C20 C19 120.01(19) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.06(19) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C3 C22 C21 123.02(18) . . ? C3 C22 S1 110.87(14) . . ? C21 C22 S1 125.76(16) . . ? C16 C23 C24 114.44(18) . . ? C16 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C16 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C23 111.7(2) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 C27 113.4(2) . . ? C17 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? C17 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 113.0(3) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C32 108.8(2) . . ? C31 C29 C30 108.9(2) . . ? C32 C29 C30 109.0(2) . . ? C31 C29 P 110.20(18) . . ? C32 C29 P 114.85(17) . . ? C30 C29 P 104.83(16) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 110.9(2) . . ? C36 C33 C34 107.3(2) . . ? C35 C33 C34 109.4(2) . . ? C36 C33 P 106.06(17) . . ? C35 C33 P 114.35(16) . . ? C34 C33 P 108.59(19) . . ? 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 . . ? C1 P C33 105.03(10) . . ? C1 P C29 106.36(10) . . ? C33 P C29 112.96(11) . . ? C1 P B 109.55(11) . . ? C33 P B 111.83(13) . . ? C29 P B 110.77(13) . . ? C22 S1 C1 92.51(9) . . ? C19 S2 C18 92.01(9) . . ? C14 S3 C15 91.77(10) . . ? C10 S4 C11 90.97(11) . . ? C2S C1S C1S 103.1(4) . 2 ? C5S C2S C1S 111.4(11) 2 . ? C5S C2S C3S 9.9(13) 2 . ? C1S C2S C3S 105.5(7) . . ? C5S C3S C4S 145(6) 2 2 ? C5S C3S C6S 85(5) 2 2 ? C4S C3S C6S 128.8(17) 2 2 ? C5S C3S C4S 142(5) 2 . ? C4S C3S C4S 9.9(6) 2 . ? C6S C3S C4S 128.3(14) 2 . ? C5S C3S C2S 45(5) 2 . ? C4S C3S C2S 107.9(13) 2 . ? C6S C3S C2S 110.4(9) 2 . ? C4S C3S C2S 100.9(11) . . ? C4S C4S C3S 139.8(15) 2 2 ? C4S C4S C5S 138(3) 2 . ? C3S C4S C5S 7.1(13) 2 . ? C4S C4S C3S 30.3(12) 2 . ? C3S C4S C3S 110.3(13) 2 . ? C5S C4S C3S 109.9(6) . . ? C4S C4S C5S 33(2) 2 2 ? C3S C4S C5S 108.8(5) 2 2 ? C5S C4S C5S 109.1(15) . 2 ? C3S C4S C5S 6.2(9) . 2 ? C3S C5S C6S 82(5) 2 . ? C3S C5S C2S 125(6) 2 2 ? C6S C5S C2S 123.2(14) . 2 ? C3S C5S C4S 28(5) 2 . ? C6S C5S C4S 109.3(15) . . ? C2S C5S C4S 104.6(14) 2 . ? C3S C5S C4S 32(5) 2 2 ? C6S C5S C4S 110.6(15) . 2 ? C2S C5S C4S 97.2(12) 2 2 ? C4S C5S C4S 8.8(7) . 2 ? C5S C6S C3S 12.6(12) . 2 ? Cl2S C7S Cl1S 100.7(2) . . ? C7S Cl1S C7S 180.0(3) . 5_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.296 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.064 #===END data_disubstituted_zz3tri075 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H84 B2 P2 S4' _chemical_formula_weight 993.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 10.0104(14) _cell_length_b 13.3519(19) _cell_length_c 23.116(3) _cell_angle_alpha 82.239(3) _cell_angle_beta 89.817(3) _cell_angle_gamma 68.130(2) _cell_volume 2837.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6446 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40163 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 28.32 _reflns_number_total 14074 _reflns_number_gt 8672 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX II (Bruker, 2008)' _computing_cell_refinement 'APEX II (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0540P)^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 14074 _refine_ls_number_parameters 601 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0965 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.06757(17) 0.66506(13) 0.22161(7) 0.0424(4) Uani 1 1 d . . . C2 C 0.02590(16) 0.76873(12) 0.19286(6) 0.0393(4) Uani 1 1 d . . . H2 H 0.0895 0.8043 0.1851 0.047 Uiso 1 1 calc R . . C3 C -0.12453(16) 0.81817(12) 0.17557(6) 0.0370(3) Uani 1 1 d . . . C4 C -0.19958(16) 0.91744(12) 0.14027(6) 0.0383(3) Uani 1 1 d . . . C5 C -0.14991(16) 1.00161(12) 0.11427(7) 0.0393(4) Uani 1 1 d . . . C6 C -0.02714(16) 1.02241(12) 0.12855(6) 0.0378(3) Uani 1 1 d . . . C7 C 0.05640(16) 0.99906(12) 0.18309(7) 0.0377(3) Uani 1 1 d . . . C8 C 0.01773(16) 0.97746(12) 0.24096(7) 0.0377(3) Uani 1 1 d . . . C9 C -0.11776(17) 0.98270(12) 0.26321(7) 0.0416(4) Uani 1 1 d . . . H9 H -0.1985 0.9962 0.2391 0.050 Uiso 1 1 calc R . . C10 C -0.11913(16) 0.96646(13) 0.32243(7) 0.0429(4) Uani 1 1 d . . . C11 C 0.11951(17) 0.95855(13) 0.28732(7) 0.0428(4) Uani 1 1 d . . . C12 C 0.25358(17) 0.96724(14) 0.27745(8) 0.0491(4) Uani 1 1 d . . . H12 H 0.3211 0.9508 0.3083 0.059 Uiso 1 1 calc R . . C13 C 0.28402(17) 0.99995(13) 0.22215(8) 0.0472(4) Uani 1 1 d . . . H13 H 0.3702 1.0098 0.2154 0.057 Uiso 1 1 calc R . . C14 C 0.18382(17) 1.01853(12) 0.17558(7) 0.0420(4) Uani 1 1 d . . . C15 C 0.02513(17) 1.07801(12) 0.08422(7) 0.0430(4) Uani 1 1 d . . . C16 C -0.05264(18) 1.13190(13) 0.03019(7) 0.0451(4) Uani 1 1 d . . . C17 C -0.19000(18) 1.13138(13) 0.02227(7) 0.0448(4) Uani 1 1 d . . . C18 C -0.23342(17) 1.06307(13) 0.06424(7) 0.0443(4) Uani 1 1 d . . . C19 C -0.33680(17) 0.93325(13) 0.11658(7) 0.0457(4) Uani 1 1 d . . . C20 C -0.40745(18) 0.86240(15) 0.13518(8) 0.0527(4) Uani 1 1 d . . . H20 H -0.5013 0.8784 0.1214 0.063 Uiso 1 1 calc R . . C21 C -0.33872(18) 0.77057(15) 0.17333(8) 0.0541(5) Uani 1 1 d . . . H21 H -0.3862 0.7248 0.1873 0.065 Uiso 1 1 calc R . . C22 C -0.19442(17) 0.74550(13) 0.19151(7) 0.0431(4) Uani 1 1 d . . . C23 C 0.01584(19) 1.18992(14) -0.01308(7) 0.0537(4) Uani 1 1 d . . . H23A H -0.0234 1.1934 -0.0519 0.064 Uiso 1 1 calc R . . H23B H 0.1184 1.1470 -0.0120 0.064 Uiso 1 1 calc R . . C24 C -0.0051(2) 1.30565(15) -0.00300(8) 0.0630(5) Uani 1 1 d . . . H24A H -0.1048 1.3533 -0.0127 0.076 Uiso 1 1 calc R . . H24B H 0.0152 1.3055 0.0380 0.076 Uiso 1 1 calc R . . C25 C 0.0925(3) 1.3496(2) -0.03973(10) 0.0894(7) Uani 1 1 d . . . H25A H 0.1912 1.3080 -0.0268 0.134 Uiso 1 1 calc R . . H25B H 0.0692 1.4247 -0.0355 0.134 Uiso 1 1 calc R . . H25C H 0.0787 1.3438 -0.0800 0.134 Uiso 1 1 calc R . . C26 C -0.2936(2) 1.19824(15) -0.02817(7) 0.0573(5) Uani 1 1 d . . . H26A H -0.3445 1.1556 -0.0414 0.069 Uiso 1 1 calc R . . H26B H -0.2401 1.2159 -0.0604 0.069 Uiso 1 1 calc R . . C27 C -0.4028(2) 1.30370(19) -0.01107(9) 0.0853(7) Uani 1 1 d . . . H27A H -0.4419 1.2862 0.0257 0.102 Uiso 1 1 calc R . . H27B H -0.3526 1.3511 -0.0045 0.102 Uiso 1 1 calc R . . C28 C -0.5254(2) 1.3650(2) -0.05493(11) 0.0986(8) Uani 1 1 d . . . H28A H -0.4897 1.3926 -0.0896 0.148 Uiso 1 1 calc R . . H28B H -0.5945 1.4246 -0.0387 0.148 Uiso 1 1 calc R . . H28C H -0.5706 1.3170 -0.0646 0.148 Uiso 1 1 calc R . . C29 C 0.3026(2) 0.46681(14) 0.20225(8) 0.0609(5) Uani 1 1 d . . . H29 H 0.4081 0.4336 0.2061 0.073 Uiso 1 1 calc R . . C30 C 0.2666(3) 0.50676(16) 0.13636(8) 0.0751(6) Uani 1 1 d . . . H30A H 0.1629 0.5420 0.1296 0.090 Uiso 1 1 calc R . . H30B H 0.3084 0.5605 0.1238 0.090 Uiso 1 1 calc R . . C31 C 0.3220(2) 0.41577(17) 0.10047(8) 0.0666(5) Uani 1 1 d . . . H31A H 0.2887 0.4439 0.0600 0.080 Uiso 1 1 calc R . . H31B H 0.4265 0.3883 0.1023 0.080 Uiso 1 1 calc R . . C32 C 0.2763(3) 0.32804(17) 0.11979(9) 0.0788(6) Uani 1 1 d . . . H32A H 0.3210 0.2693 0.0970 0.095 Uiso 1 1 calc R . . H32B H 0.1727 0.3529 0.1130 0.095 Uiso 1 1 calc R . . C33 C 0.3149(2) 0.28507(15) 0.18408(8) 0.0663(5) Uani 1 1 d . . . H33A H 0.4189 0.2518 0.1903 0.080 Uiso 1 1 calc R . . H33B H 0.2758 0.2295 0.1960 0.080 Uiso 1 1 calc R . . C34 C 0.2546(2) 0.37798(15) 0.22164(8) 0.0624(5) Uani 1 1 d . . . H34A H 0.1501 0.4054 0.2190 0.075 Uiso 1 1 calc R . . H34B H 0.2864 0.3497 0.2622 0.075 Uiso 1 1 calc R . . C35 C 0.26235(19) 0.53100(13) 0.31964(7) 0.0499(4) Uani 1 1 d . . . H35 H 0.2065 0.4840 0.3251 0.060 Uiso 1 1 calc R . . C36 C 0.1971(2) 0.62470(16) 0.35528(8) 0.0660(5) Uani 1 1 d . . . H36A H 0.2471 0.6746 0.3483 0.079 Uiso 1 1 calc R . . H36B H 0.0965 0.6645 0.3427 0.079 Uiso 1 1 calc R . . C37 C 0.2083(2) 0.5824(2) 0.42056(9) 0.0809(7) Uani 1 1 d . . . H37A H 0.1692 0.6436 0.4421 0.097 Uiso 1 1 calc R . . H37B H 0.1512 0.5376 0.4280 0.097 Uiso 1 1 calc R . . C38 C 0.3612(3) 0.5167(2) 0.44173(9) 0.0868(7) Uani 1 1 d . . . H38A H 0.3640 0.4882 0.4828 0.104 Uiso 1 1 calc R . . H38B H 0.4163 0.5634 0.4379 0.104 Uiso 1 1 calc R . . C39 C 0.4282(3) 0.42396(19) 0.40762(10) 0.0960(8) Uani 1 1 d . . . H39A H 0.3796 0.3731 0.4151 0.115 Uiso 1 1 calc R . . H39B H 0.5286 0.3856 0.4208 0.115 Uiso 1 1 calc R . . C40 C 0.4193(2) 0.46267(17) 0.34182(9) 0.0740(6) Uani 1 1 d . . . H40A H 0.4573 0.3999 0.3213 0.089 Uiso 1 1 calc R . . H40B H 0.4778 0.5062 0.3336 0.089 Uiso 1 1 calc R . . C41 C -0.2914(2) 0.85457(14) 0.38613(8) 0.0587(5) Uani 1 1 d . . . H41 H -0.3787 0.8690 0.4082 0.070 Uiso 1 1 calc R . . C42 C -0.1694(2) 0.77310(14) 0.42630(8) 0.0585(5) Uani 1 1 d . . . H42A H -0.1584 0.8055 0.4602 0.070 Uiso 1 1 calc R . . H42B H -0.0802 0.7549 0.4061 0.070 Uiso 1 1 calc R . . C43 C -0.1979(2) 0.66831(15) 0.44638(8) 0.0635(5) Uani 1 1 d . . . H43A H -0.1154 0.6157 0.4700 0.076 Uiso 1 1 calc R . . H43B H -0.2810 0.6851 0.4703 0.076 Uiso 1 1 calc R . . C44 C -0.2247(2) 0.61989(16) 0.39515(9) 0.0686(6) Uani 1 1 d . . . H44A H -0.2499 0.5576 0.4090 0.082 Uiso 1 1 calc R . . H44B H -0.1370 0.5941 0.3742 0.082 Uiso 1 1 calc R . . C45 C -0.3447(2) 0.70132(14) 0.35373(9) 0.0657(5) Uani 1 1 d . . . H45A H -0.4349 0.7205 0.3732 0.079 Uiso 1 1 calc R . . H45B H -0.3543 0.6681 0.3200 0.079 Uiso 1 1 calc R . . C46 C -0.3153(2) 0.80444(15) 0.33344(9) 0.0662(5) Uani 1 1 d . . . H46A H -0.3965 0.8567 0.3090 0.079 Uiso 1 1 calc R . . H46B H -0.2306 0.7868 0.3104 0.079 Uiso 1 1 calc R . . C47 C -0.23961(18) 1.03318(14) 0.43081(7) 0.0500(4) Uani 1 1 d . . . H47 H -0.1437 0.9832 0.4467 0.060 Uiso 1 1 calc R . . C48 C -0.2364(2) 1.14632(15) 0.41862(8) 0.0615(5) Uani 1 1 d . . . H48A H -0.3285 1.1967 0.4006 0.074 Uiso 1 1 calc R . . H48B H -0.1626 1.1462 0.3913 0.074 Uiso 1 1 calc R . . C49 C -0.2053(2) 1.18548(18) 0.47511(9) 0.0748(6) Uani 1 1 d . . . H49A H -0.1088 1.1399 0.4908 0.090 Uiso 1 1 calc R . . H49B H -0.2100 1.2598 0.4661 0.090 Uiso 1 1 calc R . . C50 C -0.3126(2) 1.18048(18) 0.52013(9) 0.0744(6) Uani 1 1 d . . . H50A H -0.4079 1.2318 0.5060 0.089 Uiso 1 1 calc R . . H50B H -0.2876 1.2013 0.5560 0.089 Uiso 1 1 calc R . . C51 C -0.3146(2) 1.06729(18) 0.53260(8) 0.0697(6) Uani 1 1 d . . . H51A H -0.3866 1.0668 0.5607 0.084 Uiso 1 1 calc R . . H51B H -0.2215 1.0171 0.5498 0.084 Uiso 1 1 calc R . . C52 C -0.3482(2) 1.02907(18) 0.47739(8) 0.0638(5) Uani 1 1 d . . . H52A H -0.4449 1.0752 0.4621 0.077 Uiso 1 1 calc R . . H52B H -0.3445 0.9550 0.4866 0.077 Uiso 1 1 calc R . . B1 B 0.3754(2) 0.66456(19) 0.22422(11) 0.0685(7) Uani 1 1 d . . . H1A H 0.3610 0.6950 0.1836 0.103 Uiso 1 1 calc R . . H1B H 0.4745 0.6173 0.2325 0.103 Uiso 1 1 calc R . . H1C H 0.3510 0.7223 0.2477 0.103 Uiso 1 1 calc R . . B2 B -0.4497(2) 1.0871(2) 0.32034(11) 0.0769(7) Uani 1 1 d . . . H2A H -0.4426 1.1573 0.3115 0.115 Uiso 1 1 calc R . . H2B H -0.5318 1.0934 0.3433 0.115 Uiso 1 1 calc R . . H2C H -0.4604 1.0609 0.2846 0.115 Uiso 1 1 calc R . . P1 P 0.25425(5) 0.58232(3) 0.241951(19) 0.04463(11) Uani 1 1 d . . . P2 P -0.27825(5) 0.98677(4) 0.36357(2) 0.04870(12) Uani 1 1 d . . . S1 S -0.07668(5) 0.62257(4) 0.22950(2) 0.05073(12) Uani 1 1 d . . . S2 S -0.39381(5) 1.03951(4) 0.05766(2) 0.05482(13) Uani 1 1 d . . . S3 S 0.19350(5) 1.07811(4) 0.10448(2) 0.05104(12) Uani 1 1 d . . . S4 S 0.04910(5) 0.94126(4) 0.354450(18) 0.05026(12) Uani 1 1 d . . . C1S C 1.1309(3) 0.26902(15) 0.40484(10) 0.0847(7) Uani 1 1 d D . . H1S1 H 1.2045 0.2986 0.3980 0.127 Uiso 1 1 calc R . . H1S2 H 1.1675 0.2037 0.4327 0.127 Uiso 1 1 calc R . . H1S3 H 1.0488 0.3215 0.4198 0.127 Uiso 1 1 calc R . . C2S C 1.0866(3) 0.24251(18) 0.34794(10) 0.0975(8) Uani 1 1 d D . . H2S1 H 1.0833 0.1705 0.3576 0.117 Uiso 1 1 calc R . . H2S2 H 1.1679 0.2336 0.3234 0.117 Uiso 1 1 calc R . . C3S C 0.9537(3) 0.30749(18) 0.30766(10) 0.0941(8) Uani 1 1 d D . . H3S1 H 0.9652 0.3771 0.3020 0.113 Uiso 1 1 calc R . . H3S2 H 0.8810 0.3164 0.3365 0.113 Uiso 1 1 calc R . . C4S C 0.8567(3) 0.32449(16) 0.25209(9) 0.0885(8) Uani 1 1 d D . . H4S1 H 0.8851 0.2495 0.2452 0.106 Uiso 1 1 calc R . . H4S2 H 0.7640 0.3403 0.2695 0.106 Uiso 1 1 calc R . . C5S C 0.8065(2) 0.38360(16) 0.18963(9) 0.0715(6) Uani 1 1 d D . . H5S1 H 0.7280 0.4539 0.1881 0.086 Uiso 1 1 calc R . . H5S2 H 0.8842 0.3897 0.1661 0.086 Uiso 1 1 calc R . . C6S C 0.7586(2) 0.29326(14) 0.17683(8) 0.0721(6) Uani 1 1 d D . . H6S1 H 0.6990 0.3167 0.1413 0.108 Uiso 1 1 calc R . . H6S2 H 0.7047 0.2764 0.2085 0.108 Uiso 1 1 calc R . . H6S3 H 0.8417 0.2295 0.1726 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0454(9) 0.0441(9) 0.0432(9) -0.0076(7) 0.0026(7) -0.0227(8) C2 0.0427(9) 0.0390(9) 0.0401(9) -0.0079(7) 0.0001(7) -0.0190(7) C3 0.0387(8) 0.0426(9) 0.0350(8) -0.0094(7) 0.0039(7) -0.0199(7) C4 0.0369(8) 0.0412(9) 0.0387(8) -0.0121(7) 0.0007(7) -0.0145(7) C5 0.0383(8) 0.0397(9) 0.0391(9) -0.0096(7) 0.0005(7) -0.0125(7) C6 0.0384(8) 0.0374(8) 0.0381(8) -0.0069(7) 0.0001(7) -0.0142(7) C7 0.0347(8) 0.0353(8) 0.0434(9) -0.0077(7) 0.0002(7) -0.0130(7) C8 0.0357(8) 0.0373(9) 0.0413(9) -0.0078(7) -0.0023(7) -0.0144(7) C9 0.0419(9) 0.0448(9) 0.0393(9) -0.0086(7) -0.0044(7) -0.0169(7) C10 0.0392(9) 0.0515(10) 0.0397(9) -0.0101(7) -0.0020(7) -0.0176(8) C11 0.0402(9) 0.0476(10) 0.0415(9) -0.0089(7) -0.0018(7) -0.0165(7) C12 0.0376(9) 0.0597(11) 0.0499(10) -0.0108(8) -0.0066(8) -0.0170(8) C13 0.0355(9) 0.0539(10) 0.0583(11) -0.0123(8) -0.0018(8) -0.0221(8) C14 0.0411(9) 0.0390(9) 0.0474(9) -0.0069(7) 0.0017(7) -0.0166(7) C15 0.0450(9) 0.0401(9) 0.0439(9) -0.0096(7) 0.0021(7) -0.0149(7) C16 0.0531(10) 0.0399(9) 0.0397(9) -0.0069(7) 0.0054(8) -0.0140(8) C17 0.0515(10) 0.0427(9) 0.0344(9) -0.0094(7) -0.0008(7) -0.0099(8) C18 0.0434(9) 0.0449(9) 0.0437(9) -0.0119(7) -0.0042(7) -0.0135(8) C19 0.0398(9) 0.0513(10) 0.0449(9) -0.0121(8) -0.0049(7) -0.0141(8) C20 0.0398(9) 0.0634(12) 0.0630(12) -0.0173(10) -0.0001(8) -0.0259(9) C21 0.0451(10) 0.0655(12) 0.0645(12) -0.0160(10) 0.0074(9) -0.0331(9) C22 0.0430(9) 0.0484(10) 0.0450(9) -0.0132(7) 0.0066(7) -0.0230(8) C23 0.0608(11) 0.0577(11) 0.0390(9) -0.0053(8) 0.0089(8) -0.0187(9) C24 0.0772(13) 0.0615(12) 0.0550(12) -0.0043(9) 0.0068(10) -0.0329(11) C25 0.1043(18) 0.0941(17) 0.0880(17) -0.0033(14) 0.0195(14) -0.0613(15) C26 0.0650(12) 0.0624(12) 0.0378(9) -0.0006(8) -0.0079(8) -0.0186(10) C27 0.0660(14) 0.0893(17) 0.0670(14) 0.0059(12) -0.0001(11) 0.0034(12) C28 0.0719(15) 0.105(2) 0.0914(18) 0.0010(15) -0.0010(13) -0.0075(14) C29 0.0740(13) 0.0442(10) 0.0582(12) -0.0123(9) 0.0048(10) -0.0133(9) C30 0.1074(18) 0.0615(13) 0.0547(12) -0.0119(10) 0.0093(12) -0.0286(12) C31 0.0699(13) 0.0819(15) 0.0480(11) -0.0045(10) 0.0091(10) -0.0301(11) C32 0.1070(18) 0.0747(15) 0.0612(13) -0.0066(11) 0.0142(12) -0.0428(14) C33 0.0859(15) 0.0499(11) 0.0631(13) -0.0148(9) 0.0161(11) -0.0232(10) C34 0.0702(13) 0.0540(12) 0.0635(12) -0.0096(9) 0.0133(10) -0.0235(10) C35 0.0560(11) 0.0439(10) 0.0438(10) -0.0044(8) -0.0031(8) -0.0124(8) C36 0.0627(12) 0.0720(13) 0.0483(11) -0.0141(10) -0.0027(9) -0.0065(10) C37 0.0795(15) 0.1056(18) 0.0511(12) -0.0160(12) -0.0015(11) -0.0256(14) C38 0.0929(17) 0.1031(19) 0.0566(13) -0.0063(13) -0.0181(12) -0.0294(15) C39 0.1038(19) 0.0743(16) 0.0750(16) 0.0041(13) -0.0248(14) 0.0015(14) C40 0.0714(14) 0.0682(14) 0.0585(13) -0.0022(10) -0.0140(10) -0.0012(11) C41 0.0664(12) 0.0499(11) 0.0607(12) -0.0130(9) -0.0105(10) -0.0211(9) C42 0.0658(12) 0.0548(11) 0.0490(11) -0.0022(9) -0.0095(9) -0.0178(9) C43 0.0939(15) 0.0583(12) 0.0442(10) -0.0005(9) -0.0164(10) -0.0376(11) C44 0.0701(13) 0.0628(13) 0.0678(13) 0.0030(10) -0.0197(11) -0.0231(11) C45 0.0783(14) 0.0385(10) 0.0651(12) 0.0031(9) -0.0184(10) -0.0080(9) C46 0.0834(14) 0.0607(12) 0.0669(13) -0.0157(10) -0.0149(11) -0.0388(11) C47 0.0440(9) 0.0608(11) 0.0443(10) -0.0157(8) 0.0037(8) -0.0160(8) C48 0.0667(12) 0.0590(12) 0.0607(12) -0.0163(9) 0.0049(10) -0.0233(10) C49 0.0807(15) 0.0734(14) 0.0739(14) -0.0250(11) -0.0061(12) -0.0281(12) C50 0.0761(14) 0.0799(15) 0.0538(12) -0.0278(11) -0.0077(11) -0.0078(12) C51 0.0629(12) 0.0979(17) 0.0467(11) -0.0207(11) 0.0075(9) -0.0249(12) C52 0.0577(11) 0.0862(15) 0.0522(11) -0.0217(10) 0.0141(9) -0.0285(11) B1 0.0497(13) 0.0673(15) 0.0875(18) 0.0034(13) 0.0058(12) -0.0257(12) B2 0.0461(13) 0.111(2) 0.0675(16) -0.0136(15) -0.0099(11) -0.0224(14) P1 0.0457(2) 0.0397(2) 0.0460(3) -0.00517(19) 0.00262(19) -0.0136(2) P2 0.0406(2) 0.0629(3) 0.0436(3) -0.0133(2) 0.00216(19) -0.0187(2) S1 0.0537(3) 0.0467(3) 0.0582(3) -0.0045(2) 0.0059(2) -0.0272(2) S2 0.0430(2) 0.0623(3) 0.0550(3) -0.0048(2) -0.0139(2) -0.0161(2) S3 0.0475(2) 0.0565(3) 0.0533(3) -0.0037(2) 0.0056(2) -0.0256(2) S4 0.0428(2) 0.0680(3) 0.0390(2) -0.0089(2) -0.00449(18) -0.0192(2) C1S 0.0969(17) 0.0394(11) 0.1017(18) -0.0041(11) -0.0035(14) -0.0093(11) C2S 0.136(2) 0.0627(14) 0.0811(17) -0.0212(12) -0.0138(16) -0.0191(15) C3S 0.1019(19) 0.0639(15) 0.0824(17) 0.0020(12) 0.0011(15) 0.0036(13) C4S 0.119(2) 0.0483(12) 0.0737(15) -0.0287(11) 0.0014(14) 0.0039(12) C5S 0.0796(14) 0.0641(13) 0.0774(15) -0.0193(11) -0.0145(11) -0.0311(11) C6S 0.1110(17) 0.0360(10) 0.0488(11) 0.0050(8) -0.0184(11) -0.0077(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.362(2) . ? C1 S1 1.7381(16) . ? C1 P1 1.8058(16) . ? C2 C3 1.434(2) . ? C2 H2 0.9300 . ? C3 C4 1.399(2) . ? C3 C22 1.405(2) . ? C4 C19 1.410(2) . ? C4 C5 1.450(2) . ? C5 C18 1.396(2) . ? C5 C6 1.407(2) . ? C6 C15 1.398(2) . ? C6 C7 1.447(2) . ? C7 C14 1.399(2) . ? C7 C8 1.414(2) . ? C8 C11 1.412(2) . ? C8 C9 1.430(2) . ? C9 C10 1.358(2) . ? C9 H9 0.9300 . ? C10 S4 1.7365(16) . ? C10 P2 1.8037(16) . ? C11 C12 1.405(2) . ? C11 S4 1.7249(17) . ? C12 C13 1.365(2) . ? C12 H12 0.9300 . ? C13 C14 1.406(2) . ? C13 H13 0.9300 . ? C14 S3 1.7455(17) . ? C15 C16 1.425(2) . ? C15 S3 1.7513(16) . ? C16 C17 1.390(2) . ? C16 C23 1.501(2) . ? C17 C18 1.420(2) . ? C17 C26 1.507(2) . ? C18 S2 1.7580(17) . ? C19 C20 1.402(2) . ? C19 S2 1.7531(17) . ? C20 C21 1.356(2) . ? C20 H20 0.9300 . ? C21 C22 1.407(2) . ? C21 H21 0.9300 . ? C22 S1 1.7408(17) . ? C23 C24 1.530(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.519(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.528(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.496(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.455(2) . ? C29 C30 1.541(3) . ? C29 P1 1.8107(18) . ? C29 H29 0.9800 . ? C30 C31 1.496(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.428(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.515(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.545(2) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.529(2) . ? C35 C40 1.541(2) . ? C35 P1 1.8245(17) . ? C35 H35 0.9800 . ? C36 C37 1.527(3) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.497(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.499(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.531(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.511(2) . ? C41 C46 1.527(2) . ? C41 P2 1.8245(18) . ? C41 H41 0.9800 . ? C42 C43 1.542(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.493(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.514(2) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.526(2) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.511(2) . ? C47 C52 1.538(2) . ? C47 P2 1.8416(16) . ? C47 H47 0.9800 . ? C48 C49 1.544(3) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.506(3) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.507(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.519(2) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? B1 P1 1.926(2) . ? B1 H1A 0.9600 . ? B1 H1B 0.9600 . ? B1 H1C 0.9600 . ? B2 P2 1.917(2) . ? B2 H2A 0.9600 . ? B2 H2B 0.9600 . ? B2 H2C 0.9600 . ? C1S C2S 1.516(3) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C2S C3S 1.523(3) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.553(3) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S C5S 1.537(2) . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? C5S C6S 1.517(2) . ? C5S H5S1 0.9700 . ? C5S H5S2 0.9700 . ? C6S H6S1 0.9600 . ? C6S H6S2 0.9600 . ? C6S H6S3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 S1 111.63(12) . . ? C2 C1 P1 122.01(12) . . ? S1 C1 P1 126.14(9) . . ? C1 C2 C3 114.14(14) . . ? C1 C2 H2 122.9 . . ? C3 C2 H2 122.9 . . ? C4 C3 C22 119.28(14) . . ? C4 C3 C2 129.10(14) . . ? C22 C3 C2 111.01(14) . . ? C3 C4 C19 117.30(14) . . ? C3 C4 C5 130.08(14) . . ? C19 C4 C5 111.54(14) . . ? C18 C5 C6 117.43(14) . . ? C18 C5 C4 112.10(13) . . ? C6 C5 C4 130.19(14) . . ? C15 C6 C5 117.10(14) . . ? C15 C6 C7 111.65(13) . . ? C5 C6 C7 131.22(14) . . ? C14 C7 C8 117.59(14) . . ? C14 C7 C6 111.93(14) . . ? C8 C7 C6 129.64(14) . . ? C11 C8 C7 118.58(14) . . ? C11 C8 C9 110.44(14) . . ? C7 C8 C9 130.59(14) . . ? C10 C9 C8 114.62(14) . . ? C10 C9 H9 122.7 . . ? C8 C9 H9 122.7 . . ? C9 C10 S4 111.19(12) . . ? C9 C10 P2 125.08(12) . . ? S4 C10 P2 123.20(9) . . ? C12 C11 C8 121.62(15) . . ? C12 C11 S4 126.28(12) . . ? C8 C11 S4 111.65(12) . . ? C13 C12 C11 119.48(15) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 119.35(15) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C7 C14 C13 122.42(15) . . ? C7 C14 S3 112.13(12) . . ? C13 C14 S3 125.23(12) . . ? C6 C15 C16 123.77(15) . . ? C6 C15 S3 111.85(12) . . ? C16 C15 S3 124.33(13) . . ? C17 C16 C15 117.57(15) . . ? C17 C16 C23 124.36(15) . . ? C15 C16 C23 118.00(15) . . ? C16 C17 C18 117.53(14) . . ? C16 C17 C26 123.76(16) . . ? C18 C17 C26 118.71(15) . . ? C5 C18 C17 123.96(15) . . ? C5 C18 S2 111.65(12) . . ? C17 C18 S2 124.30(12) . . ? C20 C19 C4 121.94(15) . . ? C20 C19 S2 125.80(13) . . ? C4 C19 S2 111.89(12) . . ? C21 C20 C19 119.91(16) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.00(16) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C21 C22 C3 121.61(15) . . ? C21 C22 S1 126.69(13) . . ? C3 C22 S1 111.49(11) . . ? C16 C23 C24 115.02(14) . . ? C16 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C16 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C23 111.80(17) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 C27 111.70(15) . . ? C17 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? C17 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 115.06(19) . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C26 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 110.91(17) . . ? C34 C29 P1 119.63(14) . . ? C30 C29 P1 109.99(13) . . ? C34 C29 H29 105.0 . . ? C30 C29 H29 105.0 . . ? P1 C29 H29 105.0 . . ? C31 C30 C29 112.37(16) . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? C32 C31 C30 112.68(18) . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? C30 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 C33 112.17(18) . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 110.84(16) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C29 C34 C33 111.20(16) . . ? C29 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C29 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C40 109.95(15) . . ? C36 C35 P1 110.95(12) . . ? C40 C35 P1 110.51(13) . . ? C36 C35 H35 108.5 . . ? C40 C35 H35 108.5 . . ? P1 C35 H35 108.5 . . ? C37 C36 C35 111.14(16) . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 111.51(18) . . ? C38 C37 H37A 109.3 . . ? C36 C37 H37A 109.3 . . ? C38 C37 H37B 109.3 . . ? C36 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 111.18(19) . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38B 109.4 . . ? C39 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C38 C39 C40 112.18(18) . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39B 109.2 . . ? C40 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C39 C40 C35 110.94(18) . . ? C39 C40 H40A 109.5 . . ? C35 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C46 110.66(15) . . ? C42 C41 P2 115.75(13) . . ? C46 C41 P2 111.30(13) . . ? C42 C41 H41 106.1 . . ? C46 C41 H41 106.1 . . ? P2 C41 H41 106.1 . . ? C41 C42 C43 111.15(15) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C42 110.98(15) . . ? C44 C43 H43A 109.4 . . ? C42 C43 H43A 109.4 . . ? C44 C43 H43B 109.4 . . ? C42 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C43 C44 C45 112.03(17) . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44B 109.2 . . ? C45 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 111.60(17) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C41 110.13(17) . . ? C45 C46 H46A 109.6 . . ? C41 C46 H46A 109.6 . . ? C45 C46 H46B 109.6 . . ? C41 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C48 C47 C52 110.41(15) . . ? C48 C47 P2 111.70(12) . . ? C52 C47 P2 111.44(12) . . ? C48 C47 H47 107.7 . . ? C52 C47 H47 107.7 . . ? P2 C47 H47 107.7 . . ? C47 C48 C49 111.62(16) . . ? C47 C48 H48A 109.3 . . ? C49 C48 H48A 109.3 . . ? C47 C48 H48B 109.3 . . ? C49 C48 H48B 109.3 . . ? H48A C48 H48B 108.0 . . ? C50 C49 C48 110.94(17) . . ? C50 C49 H49A 109.5 . . ? C48 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 108.0 . . ? C49 C50 C51 110.93(17) . . ? C49 C50 H50A 109.5 . . ? C51 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 108.0 . . ? C50 C51 C52 111.61(17) . . ? C50 C51 H51A 109.3 . . ? C52 C51 H51A 109.3 . . ? C50 C51 H51B 109.3 . . ? C52 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? C51 C52 C47 110.78(16) . . ? C51 C52 H52A 109.5 . . ? C47 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? H1A B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? P2 B2 H2A 109.5 . . ? P2 B2 H2B 109.5 . . ? H2A B2 H2B 109.5 . . ? P2 B2 H2C 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? C1 P1 C29 106.68(8) . . ? C1 P1 C35 106.61(8) . . ? C29 P1 C35 107.78(8) . . ? C1 P1 B1 111.16(9) . . ? C29 P1 B1 111.60(10) . . ? C35 P1 B1 112.68(10) . . ? C10 P2 C41 108.61(9) . . ? C10 P2 C47 104.49(7) . . ? C41 P2 C47 106.35(8) . . ? C10 P2 B2 112.32(9) . . ? C41 P2 B2 111.25(10) . . ? C47 P2 B2 113.40(10) . . ? C1 S1 C22 91.67(8) . . ? C19 S2 C18 91.28(8) . . ? C14 S3 C15 91.21(8) . . ? C11 S4 C10 91.99(7) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S C2S C3S 128.5(2) . . ? C1S C2S H2S1 105.2 . . ? C3S C2S H2S1 105.2 . . ? C1S C2S H2S2 105.2 . . ? C3S C2S H2S2 105.2 . . ? H2S1 C2S H2S2 105.9 . . ? C2S C3S C4S 152.0(2) . . ? C2S C3S H3S1 98.6 . . ? C4S C3S H3S1 98.6 . . ? C2S C3S H3S2 98.6 . . ? C4S C3S H3S2 98.6 . . ? H3S1 C3S H3S2 103.8 . . ? C5S C4S C3S 147.8(2) . . ? C5S C4S H4S1 99.8 . . ? C3S C4S H4S1 99.8 . . ? C5S C4S H4S2 99.8 . . ? C3S C4S H4S2 99.8 . . ? H4S1 C4S H4S2 104.1 . . ? C6S C5S C4S 90.18(15) . . ? C6S C5S H5S1 113.6 . . ? C4S C5S H5S1 113.6 . . ? C6S C5S H5S2 113.6 . . ? C4S C5S H5S2 113.6 . . ? H5S1 C5S H5S2 110.9 . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.384 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.035 #===END data_enantiomerP_ddd46b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H62 B2 P2 S4' _chemical_formula_weight 802.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.9438(16) _cell_length_b 17.258(3) _cell_length_c 27.890(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.592(3) _cell_angle_gamma 90.00 _cell_volume 4732.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 1 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5937 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'software Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47173 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.1123 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 0.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16657 _reflns_number_gt 8536 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX II (Bruker, 2008)' _computing_cell_refinement 'APEX II (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.1723P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(13) _refine_ls_number_reflns 16657 _refine_ls_number_parameters 937 _refine_ls_number_restraints 245 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.3288 _refine_ls_wR_factor_gt 0.2783 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.007 _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 C1A C 0.8056(8) 0.3782(6) 0.0933(3) 0.085(2) Uani 1 1 d . . . C2A C 0.8189(9) 0.4577(5) 0.1088(3) 0.080(2) Uani 1 1 d . . . H2A H 0.9014 0.4839 0.1144 0.096 Uiso 1 1 calc R . . C3A C 0.6918(9) 0.4917(5) 0.1147(3) 0.078(2) Uani 1 1 d . . . C4A C 0.6653(8) 0.5666(6) 0.1331(3) 0.084(2) Uani 1 1 d . . . C5A C 0.7570(8) 0.6302(5) 0.1462(3) 0.076(2) Uani 1 1 d . . . C6A C 0.8912(8) 0.6461(5) 0.1365(3) 0.077(2) Uani 1 1 d . . . C7A C 0.9548(8) 0.6253(5) 0.0963(4) 0.081(2) Uani 1 1 d . . . C8A C 0.9016(9) 0.5979(5) 0.0490(4) 0.087(3) Uani 1 1 d . . . C9A C 0.7636(10) 0.5894(5) 0.0266(4) 0.085(2) Uani 1 1 d . . . H9A H 0.6906 0.5977 0.0433 0.102 Uiso 1 1 calc R . . C10A C 0.7458(8) 0.5677(5) -0.0227(4) 0.082(3) Uani 1 1 d . . . C11A C 0.9899(9) 0.5828(5) 0.0151(4) 0.088(3) Uani 1 1 d . . . C12A C 1.1319(11) 0.5930(6) 0.0241(5) 0.103(3) Uani 1 1 d . . . H12A H 1.1878 0.5781 0.0018 0.124 Uiso 1 1 calc R . . C13A C 1.1829(10) 0.6265(6) 0.0680(5) 0.106(4) Uani 1 1 d . . . H13A H 1.2748 0.6387 0.0752 0.128 Uiso 1 1 calc R . . C14A C 1.0942(9) 0.6420(5) 0.1016(4) 0.092(3) Uani 1 1 d . . . C15A C 0.9726(9) 0.6936(5) 0.1663(4) 0.086(3) Uani 1 1 d . . . C16A C 0.9308(11) 0.7341(6) 0.2056(4) 0.096(3) Uani 1 1 d . . . C17A C 0.7887(10) 0.7336(6) 0.2088(3) 0.087(2) Uani 1 1 d . . . C18A C 0.7083(8) 0.6778(5) 0.1800(3) 0.072(2) Uani 1 1 d . . . C19A C 0.5353(9) 0.5792(5) 0.1469(3) 0.079(2) Uani 1 1 d . . . C20A C 0.4360(8) 0.5231(7) 0.1356(4) 0.096(3) Uani 1 1 d . . . H20A H 0.3502 0.5338 0.1435 0.115 Uiso 1 1 calc R . . C21A C 0.4520(10) 0.4557(7) 0.1148(4) 0.095(3) Uani 1 1 d . . . H21A H 0.3805 0.4211 0.1068 0.114 Uiso 1 1 calc R . . C22A C 0.5846(7) 0.4398(5) 0.1054(3) 0.077(2) Uani 1 1 d . . . C23A C 1.0315(13) 0.7862(7) 0.2374(5) 0.126(4) Uani 1 1 d . . . H23A H 1.0028 0.7912 0.2690 0.152 Uiso 1 1 calc R . . H23B H 1.1202 0.7617 0.2420 0.152 Uiso 1 1 calc R . . C24A C 0.7232(11) 0.7833(6) 0.2436(4) 0.104(3) Uani 1 1 d . . . H24A H 0.7927 0.8012 0.2693 0.124 Uiso 1 1 calc R . . H24B H 0.6591 0.7520 0.2582 0.124 Uiso 1 1 calc R . . C25A C 1.0440(17) 0.8684(9) 0.2157(7) 0.165(6) Uani 1 1 d . . . H25A H 0.9637 0.8984 0.2194 0.198 Uiso 1 1 calc R . . H25B H 1.0483 0.8639 0.1813 0.198 Uiso 1 1 calc R . . C26A C 0.6482(15) 0.8540(8) 0.2186(5) 0.129(4) Uani 1 1 d . . . H26A H 0.7119 0.8853 0.2038 0.155 Uiso 1 1 calc R . . H26B H 0.5778 0.8363 0.1930 0.155 Uiso 1 1 calc R . . C27A C 1.165(3) 0.9093(12) 0.2392(9) 0.241(11) Uani 1 1 d . . . H27A H 1.1696 0.9595 0.2247 0.362 Uiso 1 1 calc R . . H27B H 1.2447 0.8801 0.2353 0.362 Uiso 1 1 calc R . . H27C H 1.1598 0.9153 0.2731 0.362 Uiso 1 1 calc R . . C28A C 0.585(2) 0.9029(11) 0.2539(6) 0.185(7) Uani 1 1 d . . . H28A H 0.5344 0.9446 0.2368 0.277 Uiso 1 1 calc R . . H28B H 0.6547 0.9238 0.2778 0.277 Uiso 1 1 calc R . . H28C H 0.5243 0.8716 0.2696 0.277 Uiso 1 1 calc R . . C29A C 0.957(2) 0.3285(16) 0.0184(6) 0.219(9) Uani 1 1 d DU . . H29A H 0.8897 0.2920 0.0030 0.262 Uiso 1 1 calc R . . H29B H 0.9243 0.3797 0.0082 0.262 Uiso 1 1 calc R . . C30A C 1.070(2) 0.3166(18) -0.0019(7) 0.242(9) Uani 1 1 d DU . . H30A H 1.0989 0.2639 0.0060 0.291 Uiso 1 1 calc R . . H30B H 1.1396 0.3502 0.0150 0.291 Uiso 1 1 calc R . . C31A C 1.074(3) 0.3260(14) -0.0509(6) 0.240(10) Uani 1 1 d DU . . H31A H 1.1172 0.2797 -0.0612 0.288 Uiso 1 1 calc R . . H31B H 0.9805 0.3246 -0.0667 0.288 Uiso 1 1 calc R . . C32A C 1.133(4) 0.3868(16) -0.0712(10) 0.281(14) Uani 1 1 d DU . . H32A H 1.1401 0.3750 -0.1044 0.421 Uiso 1 1 calc R . . H32B H 1.2227 0.3957 -0.0537 0.421 Uiso 1 1 calc R . . H32C H 1.0789 0.4324 -0.0699 0.421 Uiso 1 1 calc R . . C33A C 0.9102(14) 0.2254(6) 0.0988(5) 0.134(4) Uani 1 1 d DU . . H33A H 0.8230 0.2123 0.0801 0.161 Uiso 1 1 calc R . . H33B H 0.9780 0.1918 0.0881 0.161 Uiso 1 1 calc R . . C34A C 0.9042(17) 0.2090(8) 0.1502(6) 0.160(5) Uani 1 1 d DU . . H34A H 0.8293 0.2370 0.1607 0.192 Uiso 1 1 calc R . . H34B H 0.9880 0.2251 0.1700 0.192 Uiso 1 1 calc R . . C35A C 0.884(3) 0.1227(10) 0.1552(9) 0.234(9) Uani 1 1 d DU . . H35A H 0.7991 0.1075 0.1356 0.281 Uiso 1 1 calc R . . H35B H 0.9572 0.0953 0.1431 0.281 Uiso 1 1 calc R . . C36A C 0.881(3) 0.1011(17) 0.2052(10) 0.325(16) Uani 1 1 d DU . . H36A H 0.8782 0.0457 0.2078 0.488 Uiso 1 1 calc R . . H36B H 0.8020 0.1230 0.2160 0.488 Uiso 1 1 calc R . . H36C H 0.9614 0.1203 0.2251 0.488 Uiso 1 1 calc R . . C37A C 0.591(2) 0.4540(16) -0.0802(10) 0.233(11) Uani 1 1 d DU . . H37A H 0.5194 0.4485 -0.1077 0.279 Uiso 1 1 calc R . . H37B H 0.6766 0.4463 -0.0923 0.279 Uiso 1 1 calc R . . C38A C 0.577(4) 0.3952(17) -0.0492(13) 0.285(13) Uani 1 1 d DU . . H38A H 0.4941 0.4023 -0.0353 0.342 Uiso 1 1 calc R . . H38B H 0.6531 0.3954 -0.0230 0.342 Uiso 1 1 calc R . . C39A C 0.572(4) 0.3245(18) -0.0736(13) 0.297(13) Uani 1 1 d DU . . H39A H 0.5327 0.3336 -0.1071 0.356 Uiso 1 1 calc R . . H39B H 0.6650 0.3072 -0.0737 0.356 Uiso 1 1 calc R . . C40A C 0.503(3) 0.2663(17) -0.0565(11) 0.272(13) Uani 1 1 d DU . . H40A H 0.4703 0.2315 -0.0825 0.408 Uiso 1 1 calc R . . H40B H 0.4275 0.2870 -0.0429 0.408 Uiso 1 1 calc R . . H40C H 0.5622 0.2387 -0.0319 0.408 Uiso 1 1 calc R . . C41A C 0.604(2) 0.5973(17) -0.1144(6) 0.243(11) Uani 1 1 d DU . . H41A H 0.7005 0.5966 -0.1157 0.292 Uiso 1 1 calc R . . H41B H 0.5637 0.5610 -0.1390 0.292 Uiso 1 1 calc R . . C42A C 0.563(3) 0.6658(16) -0.1319(9) 0.281(11) Uani 1 1 d DU . . H42A H 0.6082 0.7032 -0.1089 0.337 Uiso 1 1 calc R . . H42B H 0.4671 0.6687 -0.1291 0.337 Uiso 1 1 calc R . . C43A C 0.574(3) 0.696(2) -0.1781(9) 0.304(13) Uani 1 1 d DU . . H43A H 0.6708 0.7035 -0.1784 0.365 Uiso 1 1 calc R . . H43B H 0.5469 0.6540 -0.2008 0.365 Uiso 1 1 calc R . . C44A C 0.514(5) 0.759(2) -0.1981(15) 0.41(2) Uani 1 1 d DU . . H44A H 0.5667 0.7805 -0.2209 0.609 Uiso 1 1 calc R . . H44B H 0.5055 0.7966 -0.1732 0.609 Uiso 1 1 calc R . . H44C H 0.4246 0.7460 -0.2145 0.609 Uiso 1 1 calc R . . B1A B 1.1145(12) 0.3625(9) 0.1206(6) 0.131(5) Uani 1 1 d . . . H1A1 H 1.1276 0.4149 0.1107 0.196 Uiso 1 1 calc R . . H1A2 H 1.1896 0.3312 0.1142 0.196 Uiso 1 1 calc R . . H1A3 H 1.1092 0.3614 0.1547 0.196 Uiso 1 1 calc R . . B2A B 0.4324(13) 0.5819(12) -0.0347(7) 0.151(7) Uani 1 1 d . . . H2A1 H 0.4343 0.5595 -0.0031 0.226 Uiso 1 1 calc R . . H2A2 H 0.3530 0.5642 -0.0557 0.226 Uiso 1 1 calc R . . H2A3 H 0.4300 0.6373 -0.0323 0.226 Uiso 1 1 calc R . . P1A P 0.9497(3) 0.32276(16) 0.08536(12) 0.1003(8) Uani 1 1 d . . . P2A P 0.5881(3) 0.5518(2) -0.06018(11) 0.1104(9) Uani 1 1 d . . . S1A S 0.6386(2) 0.35080(15) 0.08686(10) 0.0950(7) Uani 1 1 d . . . S2A S 0.5365(2) 0.66213(15) 0.18283(9) 0.0937(7) Uani 1 1 d . . . S3A S 1.1425(3) 0.69494(16) 0.15611(12) 0.1083(9) Uani 1 1 d . . . S4A S 0.9016(3) 0.55623(16) -0.04148(11) 0.1020(8) Uani 1 1 d . . . C1B C 0.7566(8) 0.7400(5) 0.5186(4) 0.093(3) Uani 1 1 d . . . C2B C 0.7320(9) 0.7194(5) 0.4696(4) 0.078(2) Uani 1 1 d . . . H2B H 0.6448 0.7130 0.4526 0.094 Uiso 1 1 calc R . . C3B C 0.8489(9) 0.7091(5) 0.4483(4) 0.090(3) Uani 1 1 d . . . C4B C 0.8643(10) 0.6808(5) 0.4009(5) 0.096(3) Uani 1 1 d . . . C5B C 0.7610(10) 0.6566(5) 0.3618(4) 0.090(3) Uani 1 1 d . . . C6B C 0.6210(11) 0.6735(5) 0.3518(3) 0.091(3) Uani 1 1 d . . . C7B C 0.5390(9) 0.7425(5) 0.3632(3) 0.085(2) Uani 1 1 d . . . C8B C 0.5868(9) 0.8151(5) 0.3815(3) 0.078(2) Uani 1 1 d . . . C9B C 0.7185(10) 0.8472(5) 0.3872(3) 0.082(2) Uani 1 1 d . . . H9B H 0.7953 0.8191 0.3824 0.098 Uiso 1 1 calc R . . C10B C 0.7226(8) 0.9258(6) 0.4007(3) 0.084(2) Uani 1 1 d . . . C11B C 0.4895(9) 0.8681(6) 0.3891(3) 0.089(3) Uani 1 1 d . . . C12B C 0.3450(9) 0.8553(7) 0.3798(4) 0.095(3) Uani 1 1 d . . . H12B H 0.2828 0.8917 0.3878 0.114 Uiso 1 1 calc R . . C13B C 0.3066(10) 0.7882(9) 0.3592(4) 0.107(3) Uani 1 1 d . . . H13B H 0.2141 0.7785 0.3508 0.128 Uiso 1 1 calc R . . C14B C 0.3969(11) 0.7325(7) 0.3495(3) 0.095(3) Uani 1 1 d . . . C15B C 0.5370(12) 0.6242(6) 0.3189(3) 0.099(3) Uani 1 1 d . . . C16B C 0.5891(18) 0.5644(7) 0.2939(4) 0.118(4) Uani 1 1 d . . . C17B C 0.7257(18) 0.5602(6) 0.2939(4) 0.121(4) Uani 1 1 d . . . C18B C 0.8123(12) 0.6056(6) 0.3300(4) 0.107(3) Uani 1 1 d . . . C19B C 0.9938(14) 0.6592(7) 0.3923(6) 0.130(5) Uani 1 1 d . . . C20B C 1.1111(14) 0.6758(8) 0.4276(9) 0.150(7) Uani 1 1 d . . . H20B H 1.1976 0.6639 0.4209 0.180 Uiso 1 1 calc R . . C21B C 1.0962(12) 0.7078(8) 0.4690(7) 0.130(5) Uani 1 1 d . . . H21B H 1.1727 0.7204 0.4910 0.156 Uiso 1 1 calc R . . C22B C 0.9653(11) 0.7232(6) 0.4806(5) 0.106(3) Uani 1 1 d . . . C23B C 0.485(2) 0.5115(8) 0.2626(4) 0.158(6) Uani 1 1 d . . . H23C H 0.4090 0.5426 0.2472 0.190 Uiso 1 1 calc R . . H23D H 0.5273 0.4875 0.2372 0.190 Uiso 1 1 calc R . . C24B C 0.792(2) 0.5086(9) 0.2599(6) 0.175(7) Uani 1 1 d . . . H24C H 0.8785 0.5311 0.2550 0.210 Uiso 1 1 calc R . . H24D H 0.7345 0.5065 0.2286 0.210 Uiso 1 1 calc R . . C25B C 0.431(2) 0.4475(9) 0.2940(5) 0.186(8) Uani 1 1 d . . . H25C H 0.5038 0.4119 0.3057 0.223 Uiso 1 1 calc R . . H25D H 0.3988 0.4709 0.3218 0.223 Uiso 1 1 calc R . . C26B C 0.815(2) 0.4294(9) 0.2788(6) 0.190(8) Uani 1 1 d . . . H26C H 0.7297 0.4064 0.2840 0.228 Uiso 1 1 calc R . . H26D H 0.8751 0.4307 0.3097 0.228 Uiso 1 1 calc R . . C27B C 0.317(3) 0.4043(14) 0.2646(8) 0.295(17) Uani 1 1 d . . . H27D H 0.2883 0.3628 0.2836 0.442 Uiso 1 1 calc R . . H27E H 0.3478 0.3833 0.2362 0.442 Uiso 1 1 calc R . . H27F H 0.2424 0.4388 0.2551 0.442 Uiso 1 1 calc R . . C28B C 0.882(3) 0.3793(12) 0.2414(10) 0.272(14) Uani 1 1 d . . . H28D H 0.8952 0.3273 0.2534 0.409 Uiso 1 1 calc R . . H28E H 0.9680 0.4013 0.2373 0.409 Uiso 1 1 calc R . . H28F H 0.8230 0.3788 0.2108 0.409 Uiso 1 1 calc R . . C29B C 0.640(2) 0.8660(11) 0.5696(8) 0.202(8) Uani 1 1 d DU . . H29C H 0.5691 0.8769 0.5889 0.243 Uiso 1 1 calc R . . H29D H 0.7260 0.8750 0.5905 0.243 Uiso 1 1 calc R . . C30B C 0.631(3) 0.9215(9) 0.5343(10) 0.234(9) Uani 1 1 d DU . . H30C H 0.5413 0.9189 0.5149 0.281 Uiso 1 1 calc R . . H30D H 0.6978 0.9116 0.5132 0.281 Uiso 1 1 calc R . . C31B C 0.651(3) 0.9970(12) 0.5546(13) 0.280(12) Uani 1 1 d DU . . H31C H 0.7071 0.9918 0.5861 0.336 Uiso 1 1 calc R . . H31D H 0.7037 1.0264 0.5342 0.336 Uiso 1 1 calc R . . C32B C 0.540(3) 1.0403(14) 0.5607(8) 0.235(10) Uani 1 1 d DU . . H32D H 0.5684 1.0925 0.5689 0.352 Uiso 1 1 calc R . . H32E H 0.4980 1.0186 0.5864 0.352 Uiso 1 1 calc R . . H32F H 0.4770 1.0403 0.5312 0.352 Uiso 1 1 calc R . . C33B C 0.690(2) 0.7248(11) 0.6158(6) 0.175(6) Uani 1 1 d DU . . H33C H 0.7823 0.7429 0.6252 0.210 Uiso 1 1 calc R . . H33D H 0.6350 0.7488 0.6377 0.210 Uiso 1 1 calc R . . C34B C 0.690(2) 0.6415(11) 0.6248(7) 0.213(8) Uani 1 1 d DU . . H34C H 0.7623 0.6210 0.6089 0.255 Uiso 1 1 calc R . . H34D H 0.6057 0.6227 0.6062 0.255 Uiso 1 1 calc R . . C35B C 0.702(2) 0.5988(14) 0.6732(8) 0.234(9) Uani 1 1 d DU . . H35C H 0.6220 0.6068 0.6887 0.281 Uiso 1 1 calc R . . H35D H 0.7150 0.5436 0.6690 0.281 Uiso 1 1 calc R . . C36B C 0.819(3) 0.6331(18) 0.7007(9) 0.263(12) Uani 1 1 d DU . . H36D H 0.8329 0.6115 0.7327 0.395 Uiso 1 1 calc R . . H36E H 0.8058 0.6880 0.7025 0.395 Uiso 1 1 calc R . . H36F H 0.8971 0.6228 0.6852 0.395 Uiso 1 1 calc R . . C37B C 0.9459(18) 0.9818(14) 0.4720(6) 0.228(10) Uani 1 1 d DU . . H37C H 0.8952 1.0210 0.4867 0.273 Uiso 1 1 calc R . . H37D H 0.9189 0.9324 0.4843 0.273 Uiso 1 1 calc R . . C38B C 1.077(2) 0.992(2) 0.4923(9) 0.287(11) Uani 1 1 d DU . . H38C H 1.1064 1.0421 0.4824 0.345 Uiso 1 1 calc R . . H38D H 1.1314 0.9533 0.4785 0.345 Uiso 1 1 calc R . . C39B C 1.110(3) 0.9874(14) 0.5421(8) 0.281(12) Uani 1 1 d DU . . H39C H 1.1628 1.0328 0.5532 0.337 Uiso 1 1 calc R . . H39D H 1.0260 0.9897 0.5559 0.337 Uiso 1 1 calc R . . C40B C 1.180(2) 0.924(2) 0.5601(12) 0.302(14) Uani 1 1 d DU . . H40D H 1.1934 0.9252 0.5949 0.452 Uiso 1 1 calc R . . H40E H 1.2670 0.9225 0.5489 0.452 Uiso 1 1 calc R . . H40F H 1.1298 0.8778 0.5491 0.452 Uiso 1 1 calc R . . C41B C 0.8238(15) 1.0789(8) 0.3948(6) 0.140(4) Uani 1 1 d DU . . H41C H 0.7543 1.0904 0.4148 0.168 Uiso 1 1 calc R . . H41D H 0.9015 1.1114 0.4063 0.168 Uiso 1 1 calc R . . C42B C 0.774(2) 1.1012(12) 0.3475(7) 0.204(7) Uani 1 1 d DU . . H42C H 0.7037 1.0641 0.3355 0.245 Uiso 1 1 calc R . . H42D H 0.8476 1.0933 0.3288 0.245 Uiso 1 1 calc R . . C43B C 0.720(3) 1.1753(13) 0.3346(13) 0.284(12) Uani 1 1 d DU . . H43C H 0.6759 1.1740 0.3011 0.341 Uiso 1 1 calc R . . H43D H 0.6504 1.1873 0.3546 0.341 Uiso 1 1 calc R . . C44B C 0.813(4) 1.231(2) 0.3397(15) 0.348(19) Uani 1 1 d DU . . H44D H 0.7686 1.2806 0.3329 0.522 Uiso 1 1 calc R . . H44E H 0.8762 1.2229 0.3175 0.522 Uiso 1 1 calc R . . H44F H 0.8598 1.2313 0.3723 0.522 Uiso 1 1 calc R . . B1B B 0.4550(15) 0.7313(11) 0.5326(6) 0.132(5) Uani 1 1 d . . . H1B1 H 0.3960 0.7441 0.5557 0.198 Uiso 1 1 calc R . . H1B2 H 0.4528 0.6764 0.5271 0.198 Uiso 1 1 calc R . . H1B3 H 0.4250 0.7577 0.5026 0.198 Uiso 1 1 calc R . . B2B B 0.9969(16) 0.9445(9) 0.3672(7) 0.143(6) Uani 1 1 d . . . H2B1 H 1.0198 0.8919 0.3761 0.215 Uiso 1 1 calc R . . H2B2 H 1.0777 0.9757 0.3720 0.215 Uiso 1 1 calc R . . H2B3 H 0.9569 0.9465 0.3337 0.215 Uiso 1 1 calc R . . P1B P 0.6321(3) 0.7617(2) 0.55660(11) 0.1122(9) Uani 1 1 d . . . P2B P 0.8734(3) 0.98230(16) 0.40550(12) 0.1039(9) Uani 1 1 d . . . S1B S 0.9312(3) 0.75060(18) 0.53700(12) 0.1160(10) Uani 1 1 d . . . S2B S 0.9875(4) 0.60279(19) 0.33987(16) 0.1424(13) Uani 1 1 d . . . S3B S 0.3645(3) 0.6471(2) 0.31533(10) 0.1192(10) Uani 1 1 d . . . S4B S 0.5624(3) 0.95903(16) 0.40585(11) 0.0995(8) 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 C1A 0.039(4) 0.111(7) 0.103(6) 0.020(5) 0.007(4) -0.012(4) C2A 0.073(5) 0.065(5) 0.102(6) 0.014(4) 0.013(4) -0.002(4) C3A 0.062(5) 0.077(5) 0.091(5) 0.022(4) 0.001(4) 0.002(4) C4A 0.051(5) 0.089(6) 0.113(6) 0.025(5) 0.021(4) 0.009(4) C5A 0.047(4) 0.077(5) 0.103(6) 0.017(4) 0.007(4) -0.005(4) C6A 0.042(4) 0.066(5) 0.122(7) 0.012(5) 0.012(4) 0.000(4) C7A 0.053(5) 0.052(4) 0.137(8) 0.018(5) 0.007(5) -0.005(4) C8A 0.052(5) 0.062(5) 0.154(9) 0.028(5) 0.035(6) 0.004(4) C9A 0.083(7) 0.061(5) 0.114(7) 0.022(5) 0.025(5) 0.007(4) C10A 0.050(5) 0.066(5) 0.134(8) 0.035(5) 0.028(5) 0.015(4) C11A 0.062(5) 0.079(6) 0.129(7) 0.025(5) 0.035(5) 0.014(4) C12A 0.084(7) 0.073(6) 0.163(10) 0.027(7) 0.053(7) 0.016(5) C13A 0.058(6) 0.088(7) 0.182(11) 0.037(7) 0.046(7) 0.004(5) C14A 0.056(5) 0.066(5) 0.153(8) 0.037(5) 0.010(5) 0.001(4) C15A 0.057(5) 0.068(5) 0.132(7) 0.010(5) 0.009(5) 0.001(4) C16A 0.088(7) 0.074(6) 0.119(7) 0.010(5) -0.007(6) -0.010(5) C17A 0.080(6) 0.086(6) 0.094(6) 0.016(5) 0.008(5) 0.011(5) C18A 0.055(4) 0.078(5) 0.080(5) 0.010(4) 0.004(4) 0.003(4) C19A 0.066(5) 0.089(6) 0.082(5) 0.010(4) 0.009(4) 0.012(5) C20A 0.041(5) 0.130(9) 0.118(7) 0.035(7) 0.014(4) 0.001(5) C21A 0.069(6) 0.104(8) 0.113(7) 0.017(6) 0.017(5) -0.008(5) C22A 0.042(4) 0.097(6) 0.091(5) 0.009(4) 0.011(4) -0.013(4) C23A 0.099(9) 0.108(9) 0.160(10) 0.010(7) -0.022(7) -0.011(7) C24A 0.094(7) 0.095(7) 0.115(7) 0.007(6) -0.005(6) -0.004(6) C25A 0.145(13) 0.108(10) 0.227(16) -0.004(10) -0.024(11) -0.037(9) C26A 0.139(11) 0.119(9) 0.129(9) 0.013(8) 0.020(8) 0.026(8) C27A 0.28(3) 0.140(16) 0.29(3) -0.017(15) -0.02(2) -0.055(17) C28A 0.23(2) 0.173(16) 0.153(12) -0.034(11) 0.025(12) 0.068(14) C29A 0.172(15) 0.34(3) 0.147(12) -0.084(14) 0.021(9) 0.065(16) C30A 0.205(17) 0.37(3) 0.167(11) -0.042(15) 0.070(12) -0.041(18) C31A 0.29(2) 0.28(2) 0.168(12) -0.090(14) 0.087(13) -0.124(18) C32A 0.40(4) 0.22(3) 0.24(2) -0.002(19) 0.09(2) -0.05(2) C33A 0.124(9) 0.073(6) 0.207(11) -0.006(7) 0.030(9) 0.003(6) C34A 0.150(11) 0.118(8) 0.219(12) 0.024(9) 0.054(11) 0.012(9) C35A 0.26(2) 0.138(10) 0.31(2) 0.071(14) 0.080(18) -0.003(13) C36A 0.38(4) 0.24(3) 0.36(3) 0.18(2) 0.08(3) 0.06(3) C37A 0.135(14) 0.25(2) 0.30(3) -0.138(19) -0.038(16) 0.046(17) C38A 0.24(2) 0.26(2) 0.36(3) -0.134(19) 0.03(2) 0.00(2) C39A 0.30(3) 0.26(2) 0.34(3) -0.14(2) 0.08(2) -0.04(2) C40A 0.30(4) 0.22(2) 0.32(3) -0.09(2) 0.11(2) 0.04(2) C41A 0.193(17) 0.40(3) 0.140(12) 0.121(15) 0.025(11) 0.063(19) C42A 0.29(2) 0.35(3) 0.240(18) 0.108(17) 0.149(17) 0.07(2) C43A 0.29(2) 0.40(3) 0.240(19) 0.185(19) 0.080(19) 0.09(2) C44A 0.49(5) 0.39(5) 0.37(4) 0.18(3) 0.20(4) 0.20(4) B1A 0.056(7) 0.120(10) 0.206(15) -0.048(10) -0.011(8) 0.001(7) B2A 0.057(7) 0.201(18) 0.202(16) 0.080(14) 0.042(8) 0.041(9) P1A 0.0665(15) 0.0896(17) 0.144(2) -0.0176(15) 0.0130(14) -0.0028(12) P2A 0.0820(18) 0.144(3) 0.1069(19) 0.0069(17) 0.0200(14) 0.0214(17) S1A 0.0618(13) 0.0942(17) 0.1271(18) -0.0062(13) 0.0085(12) -0.0228(12) S2A 0.0716(14) 0.0981(17) 0.1150(17) 0.0161(13) 0.0254(12) 0.0110(12) S3A 0.0589(14) 0.0921(17) 0.170(3) 0.0215(17) 0.0045(14) -0.0074(12) S4A 0.0830(16) 0.0952(17) 0.139(2) 0.0200(15) 0.0549(15) 0.0145(13) C1B 0.049(5) 0.068(5) 0.158(9) 0.042(6) 0.001(5) -0.002(4) C2B 0.060(5) 0.067(5) 0.105(7) 0.019(4) 0.003(4) -0.004(4) C3B 0.059(6) 0.071(5) 0.136(8) 0.031(5) 0.008(6) 0.003(4) C4B 0.073(6) 0.071(6) 0.152(9) 0.016(6) 0.046(6) 0.008(5) C5B 0.087(7) 0.058(5) 0.133(8) 0.011(5) 0.039(6) -0.006(5) C6B 0.106(8) 0.077(6) 0.095(6) 0.002(5) 0.032(5) -0.001(5) C7B 0.080(6) 0.080(6) 0.097(6) 0.005(5) 0.022(5) -0.005(5) C8B 0.076(6) 0.081(6) 0.078(5) 0.008(4) 0.015(4) -0.004(5) C9B 0.086(6) 0.065(5) 0.096(6) 0.016(4) 0.018(5) 0.016(4) C10B 0.053(5) 0.097(7) 0.104(6) 0.014(5) 0.015(4) 0.005(4) C11B 0.061(5) 0.094(6) 0.115(6) 0.021(5) 0.020(5) 0.007(5) C12B 0.055(5) 0.111(8) 0.117(7) 0.025(6) 0.007(5) 0.010(5) C13B 0.048(5) 0.140(10) 0.125(8) 0.028(7) -0.009(5) -0.001(6) C14B 0.096(8) 0.111(7) 0.077(5) 0.019(5) 0.008(5) -0.026(6) C15B 0.120(8) 0.101(7) 0.081(5) -0.019(5) 0.036(5) -0.025(6) C16B 0.188(14) 0.095(8) 0.080(6) 0.009(6) 0.043(8) -0.025(8) C17B 0.181(14) 0.075(6) 0.122(9) 0.003(6) 0.070(9) 0.011(8) C18B 0.122(9) 0.080(6) 0.132(8) -0.002(6) 0.063(7) -0.011(6) C19B 0.108(10) 0.088(7) 0.209(13) 0.041(8) 0.076(9) 0.030(7) C20B 0.074(9) 0.091(9) 0.30(2) 0.055(11) 0.059(12) 0.018(7) C21B 0.056(7) 0.107(10) 0.227(16) 0.034(10) 0.019(8) 0.005(6) C22B 0.079(7) 0.072(6) 0.163(10) 0.033(6) 0.005(7) 0.001(5) C23B 0.28(2) 0.104(8) 0.098(7) -0.013(6) 0.055(9) -0.074(11) C24B 0.29(2) 0.104(10) 0.152(12) 0.006(9) 0.084(13) 0.023(12) C25B 0.32(2) 0.126(11) 0.108(8) -0.012(8) 0.011(11) -0.102(14) C26B 0.32(3) 0.120(12) 0.137(11) -0.020(9) 0.069(13) 0.050(13) C27B 0.52(5) 0.19(2) 0.183(17) -0.038(14) 0.08(2) -0.20(3) C28B 0.42(4) 0.119(14) 0.31(3) -0.023(17) 0.15(3) 0.016(19) C29B 0.184(16) 0.147(11) 0.30(2) -0.054(12) 0.099(16) -0.019(13) C30B 0.222(18) 0.104(10) 0.37(3) -0.033(11) 0.016(18) -0.023(12) C31B 0.29(2) 0.124(10) 0.41(3) -0.084(14) 0.02(2) 0.005(14) C32B 0.29(3) 0.175(18) 0.22(2) -0.030(15) -0.010(19) 0.040(16) C33B 0.188(15) 0.197(13) 0.135(10) 0.034(10) 0.009(9) -0.013(13) C34B 0.233(18) 0.174(13) 0.213(14) 0.032(12) -0.028(13) 0.000(15) C35B 0.24(2) 0.188(17) 0.254(19) 0.069(14) -0.042(15) 0.021(15) C36B 0.29(3) 0.26(3) 0.213(18) -0.006(19) -0.026(17) 0.01(2) C37B 0.156(12) 0.34(2) 0.197(14) -0.174(16) 0.054(10) -0.106(15) C38B 0.188(15) 0.36(3) 0.296(19) -0.15(2) -0.034(17) -0.006(18) C39B 0.25(2) 0.28(2) 0.290(19) -0.19(2) -0.044(16) 0.051(17) C40B 0.130(16) 0.37(4) 0.39(3) -0.11(3) -0.021(19) 0.07(2) C41B 0.122(10) 0.098(8) 0.205(11) 0.001(8) 0.040(9) 0.030(7) C42B 0.196(16) 0.189(14) 0.219(14) 0.037(13) 0.006(13) 0.083(13) C43B 0.37(3) 0.179(18) 0.29(2) 0.084(19) 0.02(2) 0.064(17) C44B 0.46(5) 0.20(2) 0.37(4) 0.03(3) 0.02(4) 0.01(2) B1B 0.100(10) 0.165(15) 0.132(11) 0.048(10) 0.018(8) -0.008(9) B2B 0.101(10) 0.102(10) 0.243(19) -0.018(11) 0.077(11) -0.005(8) P1B 0.099(2) 0.123(2) 0.1124(19) 0.0080(17) 0.0081(15) -0.0187(17) P2B 0.0768(17) 0.0822(17) 0.156(2) -0.0097(15) 0.0279(16) 0.0000(13) S1B 0.0773(17) 0.1040(19) 0.155(3) 0.0284(18) -0.0200(16) -0.0148(14) S2B 0.137(3) 0.100(2) 0.210(4) 0.018(2) 0.093(3) 0.023(2) S3B 0.116(2) 0.134(2) 0.1053(18) 0.0059(16) 0.0086(15) -0.0425(19) S4B 0.0726(15) 0.0932(17) 0.136(2) -0.0060(14) 0.0268(14) 0.0197(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1A C2A 1.439(13) . ? C1A S1A 1.710(8) . ? C1A P1A 1.763(10) . ? C2A C3A 1.426(12) . ? C2A H2A 0.9300 . ? C3A C22A 1.387(12) . ? C3A C4A 1.429(13) . ? C4A C5A 1.439(13) . ? C4A C19A 1.419(11) . ? C5A C6A 1.428(11) . ? C5A C18A 1.389(12) . ? C6A C15A 1.348(13) . ? C6A C7A 1.412(13) . ? C7A C14A 1.402(12) . ? C7A C8A 1.427(14) . ? C8A C11A 1.408(12) . ? C8A C9A 1.428(13) . ? C9A C10A 1.410(13) . ? C9A H9A 0.9300 . ? C10A S4A 1.720(8) . ? C10A P2A 1.771(10) . ? C11A C12A 1.408(14) . ? C11A S4A 1.749(11) . ? C12A C13A 1.380(16) . ? C12A H12A 0.9300 . ? C13A C14A 1.406(15) . ? C13A H13A 0.9300 . ? C14A S3A 1.777(12) . ? C15A C16A 1.414(14) . ? C15A S3A 1.755(9) . ? C16A C17A 1.429(13) . ? C16A C23A 1.526(15) . ? C17A C18A 1.422(13) . ? C17A C24A 1.514(14) . ? C18A S2A 1.744(8) . ? C19A C20A 1.386(14) . ? C19A S2A 1.746(10) . ? C20A C21A 1.320(15) . ? C20A H20A 0.9300 . ? C21A C22A 1.409(12) . ? C21A H21A 0.9300 . ? C22A S1A 1.731(10) . ? C23A C25A 1.556(19) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A C26A 1.541(16) . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? C25A C27A 1.46(2) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C26A C28A 1.506(18) . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A C30A 1.347(15) . ? C29A P1A 1.882(18) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A C31A 1.383(15) . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C31A C32A 1.366(16) . ? C31A H31A 0.9700 . ? C31A H31B 0.9700 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C33A C34A 1.471(14) . ? C33A P1A 1.777(12) . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C34A C35A 1.511(15) . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C35A C36A 1.450(17) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C37A C38A 1.355(19) . ? C37A P2A 1.78(2) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C38A C39A 1.395(19) . ? C38A H38A 0.9700 . ? C38A H38B 0.9700 . ? C39A C40A 1.344(19) . ? C39A H39A 0.9700 . ? C39A H39B 0.9700 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.318(17) . ? C41A P2A 1.730(17) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A C43A 1.408(16) . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C43A C44A 1.331(18) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C44A H44A 0.9600 . ? C44A H44B 0.9600 . ? C44A H44C 0.9600 . ? B1A P1A 1.909(12) . ? B1A H1A1 0.9600 . ? B1A H1A2 0.9600 . ? B1A H1A3 0.9600 . ? B2A P2A 1.870(13) . ? B2A H2A1 0.9600 . ? B2A H2A2 0.9600 . ? B2A H2A3 0.9600 . ? C1B C2B 1.397(14) . ? C1B S1B 1.745(9) . ? C1B P1B 1.787(11) . ? C2B C3B 1.394(13) . ? C2B H2B 0.9300 . ? C3B C22B 1.379(14) . ? C3B C4B 1.438(15) . ? C4B C19B 1.395(14) . ? C4B C5B 1.443(16) . ? C5B C6B 1.409(14) . ? C5B C18B 1.398(14) . ? C6B C7B 1.504(14) . ? C6B C15B 1.428(14) . ? C7B C14B 1.418(13) . ? C7B C8B 1.408(13) . ? C8B C11B 1.370(12) . ? C8B C9B 1.408(12) . ? C9B C10B 1.407(13) . ? C9B H9B 0.9300 . ? C10B S4B 1.719(8) . ? C10B P2B 1.777(9) . ? C11B C12B 1.439(13) . ? C11B S4B 1.763(11) . ? C12B C13B 1.324(16) . ? C12B H12B 0.9300 . ? C13B C14B 1.370(16) . ? C13B H13B 0.9300 . ? C14B S3B 1.759(12) . ? C15B C16B 1.386(16) . ? C15B S3B 1.749(12) . ? C16B C17B 1.360(18) . ? C16B C23B 1.551(18) . ? C17B C18B 1.453(18) . ? C17B C24B 1.524(18) . ? C18B S2B 1.723(13) . ? C19B C20B 1.44(2) . ? C19B S2B 1.751(17) . ? C20B C21B 1.31(2) . ? C20B H20B 0.9300 . ? C21B C22B 1.413(17) . ? C21B H21B 0.9300 . ? C22B S1B 1.723(14) . ? C23B C25B 1.554(17) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B C26B 1.47(2) . ? C24B H24C 0.9700 . ? C24B H24D 0.9700 . ? C25B C27B 1.49(3) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26B C28B 1.57(2) . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B C30B 1.365(17) . ? C29B P1B 1.836(19) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30B C31B 1.423(16) . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? C31B C32B 1.362(16) . ? C31B H31C 0.9700 . ? C31B H31D 0.9700 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33B C34B 1.459(16) . ? C33B P1B 1.782(15) . ? C33B H33C 0.9700 . ? C33B H33D 0.9700 . ? C34B C35B 1.527(16) . ? C34B H34C 0.9700 . ? C34B H34D 0.9700 . ? C35B C36B 1.422(17) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C36B H36D 0.9600 . ? C36B H36E 0.9600 . ? C36B H36F 0.9600 . ? C37B C38B 1.356(16) . ? C37B P2B 1.887(19) . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C38B C39B 1.378(18) . ? C38B H38C 0.9700 . ? C38B H38D 0.9700 . ? C39B C40B 1.361(18) . ? C39B H39C 0.9700 . ? C39B H39D 0.9700 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.392(15) . ? C41B P2B 1.752(13) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.414(17) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.331(19) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B H44D 0.9600 . ? C44B H44E 0.9600 . ? C44B H44F 0.9600 . ? B1B P1B 1.863(15) . ? B1B H1B1 0.9600 . ? B1B H1B2 0.9600 . ? B1B H1B3 0.9600 . ? B2B P2B 1.863(14) . ? B2B H2B1 0.9600 . ? B2B H2B2 0.9600 . ? B2B H2B3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A C1A S1A 109.8(7) . . ? C2A C1A P1A 121.0(6) . . ? S1A C1A P1A 129.2(6) . . ? C1A C2A C3A 112.6(8) . . ? C1A C2A H2A 123.7 . . ? C3A C2A H2A 123.7 . . ? C22A C3A C2A 112.4(8) . . ? C22A C3A C4A 118.3(8) . . ? C2A C3A C4A 128.9(8) . . ? C5A C4A C19A 112.5(9) . . ? C5A C4A C3A 129.6(8) . . ? C19A C4A C3A 117.4(8) . . ? C4A C5A C6A 132.3(9) . . ? C4A C5A C18A 110.6(7) . . ? C6A C5A C18A 116.4(8) . . ? C15A C6A C5A 119.4(9) . . ? C15A C6A C7A 110.2(8) . . ? C5A C6A C7A 130.1(8) . . ? C14A C7A C6A 114.7(9) . . ? C14A C7A C8A 112.9(9) . . ? C6A C7A C8A 132.0(7) . . ? C11A C8A C9A 109.9(10) . . ? C11A C8A C7A 120.0(8) . . ? C9A C8A C7A 129.7(8) . . ? C10A C9A C8A 115.3(8) . . ? C10A C9A H9A 122.4 . . ? C8A C9A H9A 122.4 . . ? C9A C10A S4A 109.9(7) . . ? C9A C10A P2A 126.0(6) . . ? S4A C10A P2A 124.1(7) . . ? C8A C11A C12A 124.5(10) . . ? C8A C11A S4A 112.1(7) . . ? C12A C11A S4A 123.2(8) . . ? C13A C12A C11A 115.9(10) . . ? C13A C12A H12A 122.0 . . ? C11A C12A H12A 122.0 . . ? C12A C13A C14A 119.1(10) . . ? C12A C13A H13A 120.4 . . ? C14A C13A H13A 120.4 . . ? C7A C14A C13A 126.9(11) . . ? C7A C14A S3A 109.4(8) . . ? C13A C14A S3A 123.5(8) . . ? C6A C15A C16A 124.1(8) . . ? C6A C15A S3A 114.3(8) . . ? C16A C15A S3A 121.4(8) . . ? C17A C16A C15A 116.9(8) . . ? C17A C16A C23A 122.4(11) . . ? C15A C16A C23A 119.9(10) . . ? C16A C17A C18A 116.6(8) . . ? C16A C17A C24A 124.1(9) . . ? C18A C17A C24A 119.1(9) . . ? C17A C18A C5A 124.1(8) . . ? C17A C18A S2A 123.4(7) . . ? C5A C18A S2A 112.5(6) . . ? C4A C19A C20A 118.6(9) . . ? C4A C19A S2A 110.7(7) . . ? C20A C19A S2A 130.3(8) . . ? C21A C20A C19A 125.9(9) . . ? C21A C20A H20A 117.0 . . ? C19A C20A H20A 117.0 . . ? C20A C21A C22A 115.6(9) . . ? C20A C21A H21A 122.2 . . ? C22A C21A H21A 122.2 . . ? C3A C22A C21A 123.5(9) . . ? C3A C22A S1A 111.5(6) . . ? C21A C22A S1A 124.7(7) . . ? C25A C23A C16A 113.2(10) . . ? C25A C23A H23A 108.9 . . ? C16A C23A H23A 108.9 . . ? C25A C23A H23B 108.9 . . ? C16A C23A H23B 108.9 . . ? H23A C23A H23B 107.8 . . ? C17A C24A C26A 112.6(9) . . ? C17A C24A H24A 109.1 . . ? C26A C24A H24A 109.1 . . ? C17A C24A H24B 109.1 . . ? C26A C24A H24B 109.1 . . ? H24A C24A H24B 107.8 . . ? C23A C25A C27A 111.9(14) . . ? C23A C25A H25A 109.2 . . ? C27A C25A H25A 109.2 . . ? C23A C25A H25B 109.2 . . ? C27A C25A H25B 109.2 . . ? H25A C25A H25B 107.9 . . ? C28A C26A C24A 111.7(11) . . ? C28A C26A H26A 109.3 . . ? C24A C26A H26A 109.3 . . ? C28A C26A H26B 109.3 . . ? C24A C26A H26B 109.3 . . ? H26A C26A H26B 107.9 . . ? C25A C27A H27A 109.5 . . ? C25A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C26A C28A H28A 109.5 . . ? C26A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C26A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C30A C29A P1A 124.6(15) . . ? C30A C29A H29A 106.2 . . ? P1A C29A H29A 106.2 . . ? C30A C29A H29B 106.2 . . ? P1A C29A H29B 106.2 . . ? H29A C29A H29B 106.4 . . ? C29A C30A C31A 123(2) . . ? C29A C30A H30A 106.5 . . ? C31A C30A H30A 106.5 . . ? C29A C30A H30B 106.5 . . ? C31A C30A H30B 106.5 . . ? H30A C30A H30B 106.5 . . ? C32A C31A C30A 125(2) . . ? C32A C31A H31A 106.0 . . ? C30A C31A H31A 106.0 . . ? C32A C31A H31B 106.0 . . ? C30A C31A H31B 106.0 . . ? H31A C31A H31B 106.3 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C34A C33A P1A 115.5(10) . . ? C34A C33A H33A 108.4 . . ? P1A C33A H33A 108.4 . . ? C34A C33A H33B 108.4 . . ? P1A C33A H33B 108.4 . . ? H33A C33A H33B 107.5 . . ? C33A C34A C35A 107.8(15) . . ? C33A C34A H34A 110.1 . . ? C35A C34A H34A 110.1 . . ? C33A C34A H34B 110.1 . . ? C35A C34A H34B 110.1 . . ? H34A C34A H34B 108.5 . . ? C36A C35A C34A 111(2) . . ? C36A C35A H35A 109.4 . . ? C34A C35A H35A 109.4 . . ? C36A C35A H35B 109.4 . . ? C34A C35A H35B 109.4 . . ? H35A C35A H35B 108.0 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C38A C37A P2A 120(2) . . ? C38A C37A H37A 107.3 . . ? P2A C37A H37A 107.3 . . ? C38A C37A H37B 107.3 . . ? P2A C37A H37B 107.3 . . ? H37A C37A H37B 106.9 . . ? C37A C38A C39A 110(3) . . ? C37A C38A H38A 109.7 . . ? C39A C38A H38A 109.6 . . ? C37A C38A H38B 109.7 . . ? C39A C38A H38B 109.7 . . ? H38A C38A H38B 108.2 . . ? C40A C39A C38A 118(3) . . ? C40A C39A H39A 107.9 . . ? C38A C39A H39A 107.9 . . ? C40A C39A H39B 107.9 . . ? C38A C39A H39B 107.9 . . ? H39A C39A H39B 107.2 . . ? C39A C40A H40A 109.5 . . ? C39A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C39A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? C42A C41A P2A 131.9(19) . . ? C42A C41A H41A 104.3 . . ? P2A C41A H41A 104.3 . . ? C42A C41A H41B 104.3 . . ? P2A C41A H41B 104.3 . . ? H41A C41A H41B 105.6 . . ? C41A C42A C43A 127(3) . . ? C41A C42A H42A 105.5 . . ? C43A C42A H42A 105.5 . . ? C41A C42A H42B 105.5 . . ? C43A C42A H42B 105.5 . . ? H42A C42A H42B 106.0 . . ? C44A C43A C42A 126(3) . . ? C44A C43A H43A 105.7 . . ? C42A C43A H43A 105.7 . . ? C44A C43A H43B 105.7 . . ? C42A C43A H43B 105.7 . . ? H43A C43A H43B 106.2 . . ? C43A C44A H44A 109.5 . . ? C43A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C43A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? P1A B1A H1A1 109.5 . . ? P1A B1A H1A2 109.5 . . ? H1A1 B1A H1A2 109.5 . . ? P1A B1A H1A3 109.5 . . ? H1A1 B1A H1A3 109.5 . . ? H1A2 B1A H1A3 109.5 . . ? P2A B2A H2A1 109.5 . . ? P2A B2A H2A2 109.5 . . ? H2A1 B2A H2A2 109.5 . . ? P2A B2A H2A3 109.5 . . ? H2A1 B2A H2A3 109.5 . . ? H2A2 B2A H2A3 109.5 . . ? C33A P1A C1A 106.1(5) . . ? C33A P1A B1A 115.5(7) . . ? C1A P1A B1A 113.1(5) . . ? C33A P1A C29A 107.5(10) . . ? C1A P1A C29A 104.4(7) . . ? B1A P1A C29A 109.6(9) . . ? C41A P2A C37A 98.5(14) . . ? C41A P2A C10A 105.0(9) . . ? C37A P2A C10A 106.1(8) . . ? C41A P2A B2A 113.1(9) . . ? C37A P2A B2A 115.8(11) . . ? C10A P2A B2A 116.3(7) . . ? C1A S1A C22A 93.6(4) . . ? C19A S2A C18A 91.3(4) . . ? C15A S3A C14A 89.3(5) . . ? C10A S4A C11A 92.8(5) . . ? C2B C1B S1B 109.6(7) . . ? C2B C1B P1B 126.7(7) . . ? S1B C1B P1B 123.4(7) . . ? C3B C2B C1B 114.5(8) . . ? C3B C2B H2B 122.8 . . ? C1B C2B H2B 122.8 . . ? C22B C3B C2B 111.7(11) . . ? C22B C3B C4B 117.8(10) . . ? C2B C3B C4B 130.2(9) . . ? C19B C4B C5B 111.4(11) . . ? C19B C4B C3B 118.4(12) . . ? C5B C4B C3B 129.1(8) . . ? C6B C5B C18B 116.6(10) . . ? C6B C5B C4B 131.3(9) . . ? C18B C5B C4B 112.0(10) . . ? C5B C6B C7B 132.3(9) . . ? C5B C6B C15B 118.0(9) . . ? C7B C6B C15B 109.0(9) . . ? C14B C7B C8B 118.4(9) . . ? C14B C7B C6B 113.3(9) . . ? C8B C7B C6B 128.0(9) . . ? C11B C8B C9B 112.8(8) . . ? C11B C8B C7B 116.2(9) . . ? C9B C8B C7B 130.4(9) . . ? C10B C9B C8B 113.4(8) . . ? C10B C9B H9B 123.3 . . ? C8B C9B H9B 123.3 . . ? C9B C10B S4B 110.8(7) . . ? C9B C10B P2B 122.7(7) . . ? S4B C10B P2B 126.3(6) . . ? C8B C11B C12B 125.4(10) . . ? C8B C11B S4B 111.3(7) . . ? C12B C11B S4B 123.0(8) . . ? C13B C12B C11B 115.3(10) . . ? C13B C12B H12B 122.4 . . ? C11B C12B H12B 122.4 . . ? C12B C13B C14B 123.0(9) . . ? C12B C13B H13B 118.5 . . ? C14B C13B H13B 118.5 . . ? C13B C14B C7B 121.1(10) . . ? C13B C14B S3B 128.5(9) . . ? C7B C14B S3B 110.1(9) . . ? C6B C15B C16B 122.7(11) . . ? C6B C15B S3B 112.1(8) . . ? C16B C15B S3B 125.2(10) . . ? C17B C16B C15B 119.2(11) . . ? C17B C16B C23B 123.6(13) . . ? C15B C16B C23B 116.9(15) . . ? C16B C17B C18B 117.4(10) . . ? C16B C17B C24B 123.9(15) . . ? C18B C17B C24B 118.7(15) . . ? C5B C18B C17B 123.0(11) . . ? C5B C18B S2B 111.9(9) . . ? C17B C18B S2B 125.1(9) . . ? C20B C19B C4B 120.4(14) . . ? C20B C19B S2B 127.3(11) . . ? C4B C19B S2B 111.9(12) . . ? C21B C20B C19B 120.0(13) . . ? C21B C20B H20B 120.0 . . ? C19B C20B H20B 120.0 . . ? C20B C21B C22B 120.8(14) . . ? C20B C21B H21B 119.6 . . ? C22B C21B H21B 119.6 . . ? C3B C22B C21B 121.9(13) . . ? C3B C22B S1B 112.6(9) . . ? C21B C22B S1B 125.1(11) . . ? C25B C23B C16B 111.1(10) . . ? C25B C23B H23C 109.4 . . ? C16B C23B H23C 109.4 . . ? C25B C23B H23D 109.4 . . ? C16B C23B H23D 109.4 . . ? H23C C23B H23D 108.0 . . ? C17B C24B C26B 112.3(12) . . ? C17B C24B H24C 109.1 . . ? C26B C24B H24C 109.1 . . ? C17B C24B H24D 109.1 . . ? C26B C24B H24D 109.1 . . ? H24C C24B H24D 107.9 . . ? C27B C25B C23B 110.1(13) . . ? C27B C25B H25C 109.6 . . ? C23B C25B H25C 109.6 . . ? C27B C25B H25D 109.6 . . ? C23B C25B H25D 109.6 . . ? H25C C25B H25D 108.2 . . ? C24B C26B C28B 109.3(15) . . ? C24B C26B H26C 109.8 . . ? C28B C26B H26C 109.8 . . ? C24B C26B H26D 109.8 . . ? C28B C26B H26D 109.8 . . ? H26C C26B H26D 108.3 . . ? C25B C27B H27D 109.5 . . ? C25B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C25B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C26B C28B H28D 109.5 . . ? C26B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C26B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C30B C29B P1B 123.3(16) . . ? C30B C29B H29C 106.5 . . ? P1B C29B H29C 106.5 . . ? C30B C29B H29D 106.5 . . ? P1B C29B H29D 106.5 . . ? H29C C29B H29D 106.5 . . ? C29B C30B C31B 111(2) . . ? C29B C30B H30C 109.3 . . ? C31B C30B H30C 109.3 . . ? C29B C30B H30D 109.3 . . ? C31B C30B H30D 109.3 . . ? H30C C30B H30D 108.0 . . ? C32B C31B C30B 119(2) . . ? C32B C31B H31C 107.6 . . ? C30B C31B H31C 107.6 . . ? C32B C31B H31D 107.6 . . ? C30B C31B H31D 107.6 . . ? H31C C31B H31D 107.1 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C34B C33B P1B 120.2(14) . . ? C34B C33B H33C 107.3 . . ? P1B C33B H33C 107.3 . . ? C34B C33B H33D 107.3 . . ? P1B C33B H33D 107.3 . . ? H33C C33B H33D 106.9 . . ? C33B C34B C35B 128.7(19) . . ? C33B C34B H34C 105.1 . . ? C35B C34B H34C 105.1 . . ? C33B C34B H34D 105.1 . . ? C35B C34B H34D 105.1 . . ? H34C C34B H34D 105.9 . . ? C36B C35B C34B 103.1(19) . . ? C36B C35B H35C 111.1 . . ? C34B C35B H35C 111.1 . . ? C36B C35B H35D 111.1 . . ? C34B C35B H35D 111.1 . . ? H35C C35B H35D 109.1 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C38B C37B P2B 127.8(17) . . ? C38B C37B H37C 105.3 . . ? P2B C37B H37C 105.3 . . ? C38B C37B H37D 105.3 . . ? P2B C37B H37D 105.3 . . ? H37C C37B H37D 106.0 . . ? C37B C38B C39B 119(3) . . ? C37B C38B H38C 107.6 . . ? C39B C38B H38C 107.6 . . ? C37B C38B H38D 107.6 . . ? C39B C38B H38D 107.6 . . ? H38C C38B H38D 107.1 . . ? C40B C39B C38B 116(2) . . ? C40B C39B H39C 108.2 . . ? C38B C39B H39C 108.2 . . ? C40B C39B H39D 108.2 . . ? C38B C39B H39D 108.2 . . ? H39C C39B H39D 107.3 . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C42B C41B P2B 118.4(12) . . ? C42B C41B H41C 107.7 . . ? P2B C41B H41C 107.7 . . ? C42B C41B H41D 107.7 . . ? P2B C41B H41D 107.7 . . ? H41C C41B H41D 107.1 . . ? C41B C42B C43B 124(2) . . ? C41B C42B H42C 106.3 . . ? C43B C42B H42C 106.3 . . ? C41B C42B H42D 106.3 . . ? C43B C42B H42D 106.3 . . ? H42C C42B H42D 106.4 . . ? C44B C43B C42B 113(3) . . ? C44B C43B H43C 108.9 . . ? C42B C43B H43C 108.9 . . ? C44B C43B H43D 108.9 . . ? C42B C43B H43D 108.9 . . ? H43C C43B H43D 107.7 . . ? C43B C44B H44D 109.5 . . ? C43B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C43B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? P1B B1B H1B1 109.5 . . ? P1B B1B H1B2 109.5 . . ? H1B1 B1B H1B2 109.5 . . ? P1B B1B H1B3 109.5 . . ? H1B1 B1B H1B3 109.5 . . ? H1B2 B1B H1B3 109.5 . . ? P2B B2B H2B1 109.5 . . ? P2B B2B H2B2 109.5 . . ? H2B1 B2B H2B2 109.5 . . ? P2B B2B H2B3 109.5 . . ? H2B1 B2B H2B3 109.5 . . ? H2B2 B2B H2B3 109.5 . . ? C1B P1B C33B 108.6(7) . . ? C1B P1B C29B 108.0(7) . . ? C33B P1B C29B 99.8(10) . . ? C1B P1B B1B 115.4(7) . . ? C33B P1B B1B 112.8(8) . . ? C29B P1B B1B 111.1(10) . . ? C41B P2B C10B 107.2(6) . . ? C41B P2B B2B 115.4(8) . . ? C10B P2B B2B 112.7(6) . . ? C41B P2B C37B 103.2(9) . . ? C10B P2B C37B 105.4(7) . . ? B2B P2B C37B 112.0(9) . . ? C1B S1B C22B 91.4(6) . . ? C18B S2B C19B 91.5(6) . . ? C15B S3B C14B 93.4(5) . . ? C11B S4B C10B 91.7(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.427 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.071 #===END data_enantiomerM_ddd46a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H62 B2 P2 S4' _chemical_formula_weight 802.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.9470(16) _cell_length_b 17.253(3) _cell_length_c 27.870(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.649(3) _cell_angle_gamma 90.00 _cell_volume 4728.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 1 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.297 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6352 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'software Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX II' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61229 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 0.74 _diffrn_reflns_theta_max 27.00 _reflns_number_total 20658 _reflns_number_gt 11544 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX II (Bruker, 2008)' _computing_cell_refinement 'APEX II (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.1328P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(7) _refine_ls_number_reflns 20658 _refine_ls_number_parameters 937 _refine_ls_number_restraints 245 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.1935(4) 0.6184(3) 0.90605(16) 0.0818(11) Uani 1 1 d . . . C2A C 0.1805(4) 0.5435(2) 0.89157(16) 0.0789(10) Uani 1 1 d . . . H2A H 0.0975 0.5177 0.8862 0.095 Uiso 1 1 calc R . . C3A C 0.3084(4) 0.5073(2) 0.88523(16) 0.0782(10) Uani 1 1 d . . . C4A C 0.3333(4) 0.4330(3) 0.86750(16) 0.0771(10) Uani 1 1 d . . . C5A C 0.2410(4) 0.3706(2) 0.85288(17) 0.0804(11) Uani 1 1 d . . . C6A C 0.1092(4) 0.3543(2) 0.86383(19) 0.0845(12) Uani 1 1 d . . . C7A C 0.0435(4) 0.3763(2) 0.9048(2) 0.0846(12) Uani 1 1 d . . . C8A C 0.0998(4) 0.4027(2) 0.95202(19) 0.0808(12) Uani 1 1 d . . . C9A C 0.2380(4) 0.4098(2) 0.97414(19) 0.0809(11) Uani 1 1 d . . . H9A H 0.3111 0.4003 0.9578 0.097 Uiso 1 1 calc R . . C10A C 0.2527(4) 0.4318(3) 1.02150(19) 0.0857(12) Uani 1 1 d . . . C11A C 0.0104(5) 0.4179(3) 0.9859(2) 0.0917(14) Uani 1 1 d . . . C12A C -0.1299(5) 0.4056(3) 0.9757(3) 0.1043(16) Uani 1 1 d . . . H12A H -0.1862 0.4190 0.9982 0.125 Uiso 1 1 calc R . . C13A C -0.1821(5) 0.3740(3) 0.9327(3) 0.1100(19) Uani 1 1 d . . . H13A H -0.2745 0.3631 0.9260 0.132 Uiso 1 1 calc R . . C14A C -0.0959(4) 0.3572(3) 0.8972(2) 0.0941(14) Uani 1 1 d . . . C15A C 0.0255(5) 0.3074(3) 0.8313(2) 0.0937(13) Uani 1 1 d . . . C16A C 0.0692(5) 0.2647(3) 0.7941(2) 0.0996(14) Uani 1 1 d . . . C17A C 0.2106(5) 0.2665(3) 0.79055(19) 0.0941(13) Uani 1 1 d . . . C18A C 0.2909(4) 0.3207(3) 0.82019(17) 0.0850(12) Uani 1 1 d . . . C19A C 0.4621(4) 0.4215(3) 0.85345(16) 0.0820(11) Uani 1 1 d . . . C20A C 0.5669(4) 0.4738(3) 0.86342(19) 0.0939(13) Uani 1 1 d . . . H20A H 0.6517 0.4620 0.8552 0.113 Uiso 1 1 calc R . . C21A C 0.5478(4) 0.5425(4) 0.88515(18) 0.0947(14) Uani 1 1 d . . . H21A H 0.6198 0.5767 0.8935 0.114 Uiso 1 1 calc R . . C22A C 0.4152(4) 0.5608(3) 0.89479(16) 0.0840(11) Uani 1 1 d . . . C23A C -0.0298(6) 0.2152(4) 0.7625(2) 0.1195(19) Uani 1 1 d . . . H23A H -0.1177 0.2408 0.7576 0.143 Uiso 1 1 calc R . . H23B H -0.0002 0.2098 0.7311 0.143 Uiso 1 1 calc R . . C24A C 0.2771(6) 0.2171(3) 0.7560(2) 0.1074(16) Uani 1 1 d . . . H24A H 0.3421 0.2483 0.7418 0.129 Uiso 1 1 calc R . . H24B H 0.2083 0.1996 0.7298 0.129 Uiso 1 1 calc R . . C25A C -0.0460(8) 0.1331(4) 0.7841(3) 0.150(3) Uani 1 1 d . . . H25A H -0.0530 0.1384 0.8183 0.181 Uiso 1 1 calc R . . H25B H 0.0351 0.1031 0.7816 0.181 Uiso 1 1 calc R . . C26A C 0.3499(7) 0.1467(4) 0.7808(2) 0.1221(18) Uani 1 1 d . . . H26A H 0.4197 0.1642 0.8067 0.147 Uiso 1 1 calc R . . H26B H 0.2852 0.1158 0.7954 0.147 Uiso 1 1 calc R . . C27A C -0.1650(12) 0.0906(7) 0.7601(5) 0.215(5) Uani 1 1 d . . . H27A H -0.1682 0.0404 0.7748 0.322 Uiso 1 1 calc R . . H27B H -0.1586 0.0846 0.7263 0.322 Uiso 1 1 calc R . . H27C H -0.2461 0.1188 0.7636 0.322 Uiso 1 1 calc R . . C28A C 0.4148(10) 0.0965(6) 0.7460(3) 0.178(4) Uani 1 1 d . . . H28A H 0.4646 0.0552 0.7636 0.267 Uiso 1 1 calc R . . H28B H 0.4756 0.1274 0.7303 0.267 Uiso 1 1 calc R . . H28C H 0.3452 0.0752 0.7220 0.267 Uiso 1 1 calc R . . C29A C 0.0472(9) 0.6778(9) 0.9806(3) 0.209(5) Uani 1 1 d DU . . H29A H 0.1024 0.6339 0.9932 0.250 Uiso 1 1 calc R . . H29B H 0.0976 0.7236 0.9928 0.250 Uiso 1 1 calc R . . C30A C -0.0593(13) 0.6759(13) 1.0030(4) 0.277(7) Uani 1 1 d DU . . H30A H -0.1123 0.6325 0.9884 0.333 Uiso 1 1 calc R . . H30B H -0.1106 0.7218 0.9915 0.333 Uiso 1 1 calc R . . C31A C -0.0723(16) 0.6716(9) 1.0519(4) 0.246(6) Uani 1 1 d DU . . H31A H 0.0197 0.6716 1.0693 0.295 Uiso 1 1 calc R . . H31B H -0.1125 0.7204 1.0596 0.295 Uiso 1 1 calc R . . C32A C -0.1391(19) 0.6165(11) 1.0729(6) 0.289(8) Uani 1 1 d DU . . H32A H -0.1432 0.6307 1.1060 0.433 Uiso 1 1 calc R . . H32B H -0.0922 0.5680 1.0722 0.433 Uiso 1 1 calc R . . H32C H -0.2297 0.6114 1.0556 0.433 Uiso 1 1 calc R . . C33A C 0.0926(7) 0.7749(4) 0.9011(3) 0.1289(19) Uani 1 1 d DU . . H33A H 0.0262 0.8091 0.9121 0.155 Uiso 1 1 calc R . . H33B H 0.1804 0.7873 0.9196 0.155 Uiso 1 1 calc R . . C34A C 0.0978(9) 0.7918(4) 0.8505(3) 0.153(2) Uani 1 1 d DU . . H34A H 0.0156 0.7731 0.8307 0.184 Uiso 1 1 calc R . . H34B H 0.1747 0.7652 0.8402 0.184 Uiso 1 1 calc R . . C35A C 0.1117(16) 0.8799(6) 0.8432(4) 0.218(5) Uani 1 1 d DU . . H35A H 0.0340 0.9059 0.8531 0.261 Uiso 1 1 calc R . . H35B H 0.1927 0.8983 0.8637 0.261 Uiso 1 1 calc R . . C36A C 0.120(2) 0.8993(12) 0.7951(6) 0.331(11) Uani 1 1 d DU . . H36A H 0.1225 0.9547 0.7920 0.496 Uiso 1 1 calc R . . H36B H 0.0415 0.8794 0.7744 0.496 Uiso 1 1 calc R . . H36C H 0.2006 0.8772 0.7859 0.496 Uiso 1 1 calc R . . C37A C 0.4101(12) 0.5437(8) 1.0795(5) 0.214(5) Uani 1 1 d DU . . H37A H 0.3257 0.5507 1.0925 0.256 Uiso 1 1 calc R . . H37B H 0.4828 0.5486 1.1067 0.256 Uiso 1 1 calc R . . C38A C 0.421(2) 0.6040(8) 1.0509(7) 0.268(7) Uani 1 1 d DU . . H38A H 0.3388 0.6073 1.0275 0.322 Uiso 1 1 calc R . . H38B H 0.4959 0.5943 1.0330 0.322 Uiso 1 1 calc R . . C39A C 0.443(2) 0.6758(9) 1.0738(7) 0.294(8) Uani 1 1 d DU . . H39A H 0.3556 0.6925 1.0818 0.353 Uiso 1 1 calc R . . H39B H 0.5011 0.6666 1.1044 0.353 Uiso 1 1 calc R . . C40A C 0.4931(18) 0.7338(8) 1.0538(6) 0.258(7) Uani 1 1 d DU . . H40A H 0.5272 0.7711 1.0782 0.388 Uiso 1 1 calc R . . H40B H 0.4237 0.7574 1.0307 0.388 Uiso 1 1 calc R . . H40C H 0.5660 0.7164 1.0375 0.388 Uiso 1 1 calc R . . C41A C 0.3989(11) 0.4084(7) 1.1172(3) 0.184(4) Uani 1 1 d DU . . H41A H 0.4583 0.4385 1.1410 0.221 Uiso 1 1 calc R . . H41B H 0.3067 0.4178 1.1232 0.221 Uiso 1 1 calc R . . C42A C 0.4254(16) 0.3352(7) 1.1269(5) 0.244(6) Uani 1 1 d DU . . H42A H 0.5159 0.3251 1.1194 0.293 Uiso 1 1 calc R . . H42B H 0.3628 0.3051 1.1042 0.293 Uiso 1 1 calc R . . C43A C 0.4203(19) 0.3019(13) 1.1769(6) 0.302(9) Uani 1 1 d DU . . H43A H 0.4295 0.3462 1.1986 0.362 Uiso 1 1 calc R . . H43B H 0.3278 0.2835 1.1760 0.362 Uiso 1 1 calc R . . C44A C 0.496(3) 0.2490(18) 1.1993(8) 0.425(17) Uani 1 1 d DU . . H44A H 0.4501 0.2264 1.2239 0.638 Uiso 1 1 calc R . . H44B H 0.5802 0.2714 1.2140 0.638 Uiso 1 1 calc R . . H44C H 0.5130 0.2097 1.1766 0.638 Uiso 1 1 calc R . . B1A B -0.1143(6) 0.6386(5) 0.8789(4) 0.140(3) Uani 1 1 d . . . H1A1 H -0.1282 0.5861 0.8886 0.211 Uiso 1 1 calc R . . H1A2 H -0.1082 0.6399 0.8449 0.211 Uiso 1 1 calc R . . H1A3 H -0.1893 0.6701 0.8852 0.211 Uiso 1 1 calc R . . B2A B 0.5664(7) 0.4155(7) 1.0315(3) 0.139(3) Uani 1 1 d . . . H2A1 H 0.5618 0.4387 0.9999 0.208 Uiso 1 1 calc R . . H2A2 H 0.5659 0.3601 1.0284 0.208 Uiso 1 1 calc R . . H2A3 H 0.6485 0.4317 1.0516 0.208 Uiso 1 1 calc R . . P1A P 0.05105(13) 0.67776(8) 0.91497(6) 0.1023(4) Uani 1 1 d . . . P2A P 0.41181(16) 0.44798(11) 1.06053(6) 0.1142(5) Uani 1 1 d . . . S1A S 0.36169(12) 0.64927(8) 0.91308(5) 0.0988(4) Uani 1 1 d . . . S2A S 0.46333(12) 0.33831(8) 0.81719(5) 0.0952(3) Uani 1 1 d . . . S3A S -0.14229(12) 0.30551(8) 0.84412(7) 0.1116(5) Uani 1 1 d . . . S4A S 0.09813(14) 0.44379(8) 1.04168(6) 0.1041(4) Uani 1 1 d . . . C1B C 0.2419(5) 0.2593(3) 0.4827(2) 0.0940(14) Uani 1 1 d . . . C2B C 0.2688(4) 0.2810(3) 0.53002(19) 0.0850(12) Uani 1 1 d . . . H2B H 0.3566 0.2880 0.5464 0.102 Uiso 1 1 calc R . . C3B C 0.1517(4) 0.2918(3) 0.5521(2) 0.0929(14) Uani 1 1 d . . . C4B C 0.1382(5) 0.3203(3) 0.5991(3) 0.1029(16) Uani 1 1 d . . . C5B C 0.2429(6) 0.3430(3) 0.6389(2) 0.0974(14) Uani 1 1 d . . . C6B C 0.3819(5) 0.3253(3) 0.64876(18) 0.0931(13) Uani 1 1 d . . . C7B C 0.4595(5) 0.2580(3) 0.63614(17) 0.0852(11) Uani 1 1 d . . . C8B C 0.4142(4) 0.1844(3) 0.61880(16) 0.0807(10) Uani 1 1 d . . . C9B C 0.2812(4) 0.1514(2) 0.61295(16) 0.0810(11) Uani 1 1 d . . . H9B H 0.2042 0.1793 0.6175 0.097 Uiso 1 1 calc R . . C10B C 0.2779(4) 0.0766(3) 0.60037(18) 0.0862(11) Uani 1 1 d . . . C11B C 0.5106(4) 0.1303(3) 0.61097(17) 0.0901(12) Uani 1 1 d . . . C12B C 0.6517(5) 0.1448(4) 0.6202(2) 0.1071(17) Uani 1 1 d . . . H12B H 0.7138 0.1084 0.6123 0.128 Uiso 1 1 calc R . . C13B C 0.6939(6) 0.2132(4) 0.6410(2) 0.1084(17) Uani 1 1 d . . . H13B H 0.7864 0.2231 0.6491 0.130 Uiso 1 1 calc R . . C14B C 0.5999(5) 0.2686(3) 0.65032(18) 0.0970(14) Uani 1 1 d . . . C15B C 0.4680(7) 0.3756(3) 0.6802(2) 0.1130(18) Uani 1 1 d . . . C16B C 0.4119(9) 0.4364(4) 0.7061(2) 0.123(2) Uani 1 1 d . . . C17B C 0.2774(11) 0.4399(4) 0.7055(2) 0.132(3) Uani 1 1 d . . . C18B C 0.1928(7) 0.3935(3) 0.6711(2) 0.1156(19) Uani 1 1 d . . . C19B C 0.0101(6) 0.3411(3) 0.6083(3) 0.126(2) Uani 1 1 d . . . C20B C -0.1088(6) 0.3250(4) 0.5746(4) 0.134(3) Uani 1 1 d . . . H20B H -0.1941 0.3365 0.5827 0.160 Uiso 1 1 calc R . . C21B C -0.0989(6) 0.2942(4) 0.5324(4) 0.130(2) Uani 1 1 d . . . H21B H -0.1769 0.2838 0.5105 0.156 Uiso 1 1 calc R . . C22B C 0.0314(5) 0.2768(3) 0.5201(2) 0.1061(17) Uani 1 1 d . . . C23B C 0.5130(11) 0.4893(5) 0.7365(2) 0.160(3) Uani 1 1 d . . . H23C H 0.5879 0.4583 0.7526 0.192 Uiso 1 1 calc R . . H23D H 0.4689 0.5135 0.7614 0.192 Uiso 1 1 calc R . . C24B C 0.2113(12) 0.4922(5) 0.7402(3) 0.170(4) Uani 1 1 d . . . H24C H 0.2707 0.4951 0.7711 0.204 Uiso 1 1 calc R . . H24D H 0.1262 0.4691 0.7459 0.204 Uiso 1 1 calc R . . C25B C 0.5703(12) 0.5536(5) 0.7061(3) 0.182(4) Uani 1 1 d . . . H25C H 0.6048 0.5299 0.6788 0.218 Uiso 1 1 calc R . . H25D H 0.4973 0.5886 0.6933 0.218 Uiso 1 1 calc R . . C26B C 0.1843(14) 0.5725(5) 0.7208(3) 0.194(4) Uani 1 1 d . . . H26C H 0.1223 0.5707 0.6904 0.233 Uiso 1 1 calc R . . H26D H 0.2685 0.5963 0.7148 0.233 Uiso 1 1 calc R . . C27B C 0.679(2) 0.5978(8) 0.7346(4) 0.323(12) Uani 1 1 d . . . H27D H 0.7066 0.6391 0.7152 0.484 Uiso 1 1 calc R . . H27E H 0.7550 0.5643 0.7447 0.484 Uiso 1 1 calc R . . H27F H 0.6468 0.6190 0.7626 0.484 Uiso 1 1 calc R . . C28B C 0.1211(18) 0.6204(7) 0.7585(5) 0.262(8) Uani 1 1 d . . . H28D H 0.1071 0.6727 0.7472 0.393 Uiso 1 1 calc R . . H28E H 0.1813 0.6202 0.7888 0.393 Uiso 1 1 calc R . . H28F H 0.0354 0.5980 0.7630 0.393 Uiso 1 1 calc R . . C29B C 0.3532(13) 0.1349(7) 0.4288(5) 0.198(4) Uani 1 1 d DU . . H29C H 0.2631 0.1265 0.4107 0.238 Uiso 1 1 calc R . . H29D H 0.4177 0.1236 0.4068 0.238 Uiso 1 1 calc R . . C30B C 0.3724(14) 0.0808(6) 0.4650(5) 0.211(5) Uani 1 1 d DU . . H30C H 0.3069 0.0901 0.4868 0.253 Uiso 1 1 calc R . . H30D H 0.4624 0.0879 0.4833 0.253 Uiso 1 1 calc R . . C31B C 0.3590(17) 0.0000(7) 0.4482(8) 0.282(7) Uani 1 1 d DU . . H31C H 0.3205 -0.0289 0.4727 0.338 Uiso 1 1 calc R . . H31D H 0.2917 -0.0005 0.4192 0.338 Uiso 1 1 calc R . . C32B C 0.4661(14) -0.0407(8) 0.4381(5) 0.232(6) Uani 1 1 d DU . . H32D H 0.4389 -0.0933 0.4306 0.348 Uiso 1 1 calc R . . H32E H 0.5367 -0.0401 0.4656 0.348 Uiso 1 1 calc R . . H32F H 0.4994 -0.0179 0.4107 0.348 Uiso 1 1 calc R . . C33B C 0.3091(10) 0.2729(6) 0.3847(3) 0.166(3) Uani 1 1 d DU . . H33C H 0.3634 0.2493 0.3625 0.199 Uiso 1 1 calc R . . H33D H 0.2162 0.2553 0.3754 0.199 Uiso 1 1 calc R . . C34B C 0.3117(13) 0.3569(6) 0.3779(4) 0.207(4) Uani 1 1 d DU . . H34C H 0.3982 0.3748 0.3950 0.248 Uiso 1 1 calc R . . H34D H 0.2420 0.3782 0.3949 0.248 Uiso 1 1 calc R . . C35B C 0.2924(14) 0.3971(10) 0.3258(5) 0.242(6) Uani 1 1 d DU . . H35C H 0.2881 0.4529 0.3295 0.290 Uiso 1 1 calc R . . H35D H 0.3698 0.3852 0.3096 0.290 Uiso 1 1 calc R . . C36B C 0.175(2) 0.3712(11) 0.2980(5) 0.306(9) Uani 1 1 d DU . . H36D H 0.1648 0.3957 0.2667 0.459 Uiso 1 1 calc R . . H36E H 0.0985 0.3837 0.3138 0.459 Uiso 1 1 calc R . . H36F H 0.1800 0.3160 0.2940 0.459 Uiso 1 1 calc R . . C37B C 0.0566(9) 0.0211(9) 0.5285(4) 0.215(6) Uani 1 1 d DU . . H37C H 0.0731 0.0735 0.5182 0.258 Uiso 1 1 calc R . . H37D H 0.1157 -0.0121 0.5127 0.258 Uiso 1 1 calc R . . C38B C -0.0705(12) 0.0039(11) 0.5070(6) 0.280(7) Uani 1 1 d DU . . H38C H -0.1299 0.0349 0.5240 0.336 Uiso 1 1 calc R . . H38D H -0.0851 -0.0495 0.5159 0.336 Uiso 1 1 calc R . . C39B C -0.1248(16) 0.0094(8) 0.4584(5) 0.250(7) Uani 1 1 d DU . . H39C H -0.0537 -0.0058 0.4400 0.300 Uiso 1 1 calc R . . H39D H -0.1956 -0.0295 0.4523 0.300 Uiso 1 1 calc R . . C40B C -0.1772(17) 0.0751(9) 0.4391(7) 0.277(8) Uani 1 1 d DU . . H40D H -0.1886 0.0715 0.4043 0.416 Uiso 1 1 calc R . . H40E H -0.1169 0.1173 0.4496 0.416 Uiso 1 1 calc R . . H40F H -0.2638 0.0841 0.4493 0.416 Uiso 1 1 calc R . . C41B C 0.1790(8) -0.0793(4) 0.6057(4) 0.147(2) Uani 1 1 d DU . . H41C H 0.1031 -0.1127 0.5934 0.176 Uiso 1 1 calc R . . H41D H 0.2514 -0.0903 0.5869 0.176 Uiso 1 1 calc R . . C42B C 0.2235(12) -0.0999(7) 0.6529(4) 0.205(4) Uani 1 1 d DU . . H42C H 0.1491 -0.0902 0.6709 0.246 Uiso 1 1 calc R . . H42D H 0.2957 -0.0641 0.6652 0.246 Uiso 1 1 calc R . . C43B C 0.275(2) -0.1796(8) 0.6658(9) 0.298(9) Uani 1 1 d DU . . H43C H 0.3343 -0.1967 0.6433 0.358 Uiso 1 1 calc R . . H43D H 0.3257 -0.1800 0.6983 0.358 Uiso 1 1 calc R . . C44B C 0.170(3) -0.2252(15) 0.6634(12) 0.419(18) Uani 1 1 d DU . . H44D H 0.2003 -0.2777 0.6690 0.629 Uiso 1 1 calc R . . H44E H 0.1166 -0.2214 0.6317 0.629 Uiso 1 1 calc R . . H44F H 0.1155 -0.2103 0.6875 0.629 Uiso 1 1 calc R . . B1B B 0.5468(7) 0.2704(7) 0.4696(3) 0.133(3) Uani 1 1 d . . . H1B1 H 0.6081 0.2582 0.4472 0.199 Uiso 1 1 calc R . . H1B2 H 0.5752 0.2439 0.4997 0.199 Uiso 1 1 calc R . . H1B3 H 0.5475 0.3253 0.4752 0.199 Uiso 1 1 calc R . . B2B B 0.0008(8) 0.0581(5) 0.6323(4) 0.148(3) Uani 1 1 d . . . H2B1 H -0.0210 0.1107 0.6229 0.222 Uiso 1 1 calc R . . H2B2 H 0.0400 0.0566 0.6659 0.222 Uiso 1 1 calc R . . H2B3 H -0.0806 0.0273 0.6274 0.222 Uiso 1 1 calc R . . P1B P 0.36779(18) 0.23832(11) 0.44327(6) 0.1143(5) Uani 1 1 d . . . P2B P 0.12689(14) 0.01789(8) 0.59408(7) 0.1064(4) Uani 1 1 d . . . S1B S 0.06872(15) 0.24952(9) 0.46321(7) 0.1185(5) Uani 1 1 d . . . S2B S 0.0139(2) 0.39746(10) 0.66069(9) 0.1475(7) Uani 1 1 d . . . S3B S 0.63765(18) 0.35197(11) 0.68435(5) 0.1207(5) Uani 1 1 d . . . S4B S 0.43794(13) 0.04127(8) 0.59424(6) 0.1017(4) 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 C1A 0.062(2) 0.076(3) 0.107(3) 0.006(2) 0.011(2) -0.0101(18) C2A 0.057(2) 0.067(2) 0.111(3) 0.010(2) 0.0110(19) -0.0042(17) C3A 0.052(2) 0.078(3) 0.105(3) 0.020(2) 0.0129(19) -0.0026(17) C4A 0.057(2) 0.082(3) 0.095(3) 0.024(2) 0.0178(18) 0.0028(18) C5A 0.056(2) 0.076(2) 0.109(3) 0.022(2) 0.012(2) 0.0063(18) C6A 0.063(2) 0.065(2) 0.126(3) 0.021(2) 0.016(2) 0.0015(18) C7A 0.059(2) 0.060(2) 0.137(4) 0.023(2) 0.024(2) 0.0021(17) C8A 0.061(2) 0.063(2) 0.125(4) 0.024(2) 0.034(2) 0.0066(17) C9A 0.063(2) 0.067(2) 0.119(3) 0.023(2) 0.034(2) 0.0085(17) C10A 0.075(3) 0.073(2) 0.117(4) 0.021(2) 0.040(2) 0.013(2) C11A 0.070(2) 0.074(3) 0.139(4) 0.030(2) 0.043(3) 0.014(2) C12A 0.067(3) 0.095(3) 0.159(5) 0.025(4) 0.043(3) 0.005(2) C13A 0.053(2) 0.090(3) 0.194(6) 0.053(4) 0.039(3) 0.007(2) C14A 0.057(2) 0.076(3) 0.150(4) 0.024(3) 0.020(2) 0.0002(19) C15A 0.068(3) 0.081(3) 0.129(4) 0.019(3) 0.007(3) -0.006(2) C16A 0.088(3) 0.080(3) 0.126(4) 0.019(3) 0.002(3) -0.003(2) C17A 0.089(3) 0.086(3) 0.107(3) 0.020(3) 0.013(3) 0.011(2) C18A 0.071(2) 0.080(3) 0.104(3) 0.019(2) 0.017(2) 0.003(2) C19A 0.060(2) 0.090(3) 0.096(3) 0.027(2) 0.0142(19) 0.004(2) C20A 0.057(2) 0.115(4) 0.111(3) 0.022(3) 0.020(2) 0.003(2) C21A 0.056(2) 0.117(4) 0.109(3) 0.019(3) 0.009(2) -0.014(2) C22A 0.055(2) 0.096(3) 0.101(3) 0.015(2) 0.0117(19) -0.011(2) C23A 0.099(4) 0.107(4) 0.143(4) 0.004(3) -0.016(3) -0.012(3) C24A 0.107(4) 0.098(3) 0.114(4) 0.008(3) 0.005(3) 0.006(3) C25A 0.119(5) 0.109(5) 0.211(7) 0.000(5) -0.015(5) -0.019(4) C26A 0.128(5) 0.109(4) 0.128(4) 0.009(3) 0.014(4) 0.025(4) C27A 0.201(10) 0.173(9) 0.263(12) -0.033(8) 0.012(9) -0.067(8) C28A 0.198(9) 0.180(8) 0.159(6) -0.014(6) 0.036(6) 0.084(7) C29A 0.119(6) 0.344(16) 0.163(7) -0.104(8) 0.023(5) 0.023(7) C30A 0.198(10) 0.47(2) 0.175(7) -0.048(11) 0.057(7) -0.119(13) C31A 0.295(14) 0.275(14) 0.187(8) -0.111(9) 0.103(8) -0.124(11) C32A 0.34(2) 0.276(19) 0.269(14) -0.009(14) 0.095(14) -0.093(16) C33A 0.106(4) 0.093(4) 0.189(6) -0.017(4) 0.028(4) 0.002(3) C34A 0.162(7) 0.121(5) 0.182(6) -0.013(5) 0.042(6) 0.001(5) C35A 0.275(13) 0.151(7) 0.230(10) 0.046(7) 0.047(10) -0.007(8) C36A 0.40(2) 0.30(2) 0.304(15) 0.168(17) 0.080(17) 0.086(18) C37A 0.139(7) 0.198(8) 0.285(14) -0.113(9) -0.028(8) 0.010(8) C38A 0.252(13) 0.185(9) 0.374(19) -0.099(10) 0.068(13) -0.020(11) C39A 0.36(2) 0.217(11) 0.319(18) -0.088(11) 0.103(15) -0.085(14) C40A 0.34(2) 0.152(8) 0.310(16) -0.064(10) 0.129(14) 0.002(10) C41A 0.168(7) 0.232(9) 0.153(6) 0.051(7) 0.027(5) 0.039(8) C42A 0.321(14) 0.163(8) 0.293(11) 0.057(8) 0.191(11) 0.011(9) C43A 0.293(17) 0.344(19) 0.269(14) 0.158(14) 0.043(13) 0.016(15) C44A 0.46(3) 0.50(4) 0.36(2) 0.19(2) 0.21(2) 0.23(3) B1A 0.060(3) 0.120(5) 0.231(9) -0.052(6) -0.008(4) 0.003(3) B2A 0.072(4) 0.209(9) 0.138(5) 0.032(6) 0.024(3) 0.027(5) P1A 0.0692(7) 0.0889(8) 0.1480(12) -0.0195(8) 0.0137(7) -0.0049(6) P2A 0.0862(8) 0.1463(13) 0.1137(10) 0.0078(9) 0.0269(7) 0.0225(8) S1A 0.0659(6) 0.0933(8) 0.1356(10) -0.0060(7) 0.0104(6) -0.0206(5) S2A 0.0743(7) 0.0984(8) 0.1171(9) 0.0157(7) 0.0285(6) 0.0111(6) S3A 0.0631(6) 0.0954(8) 0.1736(13) 0.0169(9) 0.0093(7) -0.0076(6) S4A 0.0884(8) 0.0964(8) 0.1391(10) 0.0186(7) 0.0547(7) 0.0147(6) C1B 0.074(3) 0.078(3) 0.124(4) 0.027(3) 0.000(2) -0.001(2) C2B 0.067(2) 0.074(2) 0.111(3) 0.017(2) 0.004(2) -0.0084(19) C3B 0.062(2) 0.073(3) 0.142(4) 0.026(3) 0.012(3) 0.0021(19) C4B 0.089(3) 0.069(3) 0.161(5) 0.024(3) 0.052(3) 0.011(2) C5B 0.101(4) 0.072(3) 0.128(4) 0.009(3) 0.045(3) -0.007(2) C6B 0.103(4) 0.078(3) 0.103(3) 0.009(2) 0.032(3) -0.011(2) C7B 0.084(3) 0.081(3) 0.093(3) 0.005(2) 0.021(2) -0.003(2) C8B 0.073(2) 0.082(3) 0.088(3) 0.008(2) 0.017(2) 0.005(2) C9B 0.065(2) 0.076(3) 0.107(3) 0.018(2) 0.030(2) 0.0114(19) C10B 0.074(3) 0.072(3) 0.115(3) 0.008(2) 0.020(2) 0.013(2) C11B 0.069(3) 0.099(3) 0.104(3) 0.013(3) 0.018(2) 0.016(2) C12B 0.065(3) 0.135(5) 0.121(4) 0.024(4) 0.015(2) 0.018(3) C13B 0.071(3) 0.129(5) 0.121(4) 0.027(4) 0.003(3) -0.011(3) C14B 0.078(3) 0.116(4) 0.097(3) 0.018(3) 0.013(2) -0.015(3) C15B 0.151(5) 0.095(3) 0.099(3) -0.004(3) 0.041(3) -0.032(4) C16B 0.181(7) 0.097(4) 0.103(4) 0.001(3) 0.055(4) -0.035(4) C17B 0.205(8) 0.082(3) 0.128(5) -0.001(3) 0.081(5) 0.003(4) C18B 0.140(5) 0.079(3) 0.142(5) 0.001(3) 0.070(4) 0.000(3) C19B 0.097(4) 0.080(3) 0.213(7) 0.035(4) 0.066(4) 0.025(3) C20B 0.080(4) 0.093(4) 0.237(8) 0.045(5) 0.054(5) 0.023(3) C21B 0.071(3) 0.104(4) 0.213(8) 0.046(5) 0.018(4) 0.003(3) C22B 0.072(3) 0.079(3) 0.165(5) 0.038(3) 0.012(3) -0.004(2) C23B 0.260(10) 0.122(5) 0.109(4) -0.015(4) 0.061(5) -0.080(6) C24B 0.260(11) 0.102(4) 0.166(6) 0.005(4) 0.093(7) 0.017(6) C25B 0.289(12) 0.128(6) 0.129(5) 0.001(4) 0.031(6) -0.092(7) C26B 0.308(14) 0.126(6) 0.165(7) 0.008(5) 0.089(8) 0.047(7) C27B 0.55(3) 0.232(14) 0.180(9) -0.014(8) 0.037(13) -0.256(18) C28B 0.43(2) 0.133(7) 0.254(12) 0.002(8) 0.167(14) 0.079(11) C29B 0.205(10) 0.173(8) 0.234(11) -0.054(7) 0.089(9) -0.036(8) C30B 0.213(10) 0.146(7) 0.271(13) -0.047(7) 0.029(10) -0.016(8) C31B 0.292(15) 0.143(7) 0.401(19) -0.094(9) 0.024(14) 0.040(9) C32B 0.252(13) 0.200(11) 0.233(12) -0.033(9) 0.003(10) 0.048(9) C33B 0.172(7) 0.188(7) 0.134(5) 0.004(5) 0.008(5) 0.002(6) C34B 0.214(10) 0.169(7) 0.218(9) 0.042(7) -0.033(8) 0.009(8) C35B 0.229(12) 0.236(12) 0.243(11) 0.065(10) -0.019(9) 0.054(10) C36B 0.39(2) 0.272(18) 0.220(12) -0.023(13) -0.057(13) 0.048(17) C37B 0.126(6) 0.327(15) 0.193(8) -0.116(9) 0.033(5) -0.055(8) C38B 0.179(9) 0.323(17) 0.304(13) -0.059(12) -0.081(10) 0.038(11) C39B 0.241(13) 0.199(11) 0.277(12) -0.069(10) -0.073(10) 0.044(10) C40B 0.247(15) 0.191(11) 0.361(19) -0.020(12) -0.062(13) -0.027(11) C41B 0.142(6) 0.080(3) 0.229(7) -0.006(4) 0.062(5) 0.004(4) C42B 0.202(10) 0.177(8) 0.229(9) 0.033(8) 0.010(8) 0.074(7) C43B 0.38(2) 0.187(12) 0.332(17) 0.073(13) 0.065(18) 0.070(13) C44B 0.54(4) 0.240(18) 0.45(3) 0.10(3) -0.02(3) -0.06(2) B1B 0.094(4) 0.181(8) 0.123(5) 0.004(5) 0.015(4) -0.017(5) B2B 0.100(5) 0.126(6) 0.232(10) -0.015(6) 0.071(6) 0.006(4) P1B 0.1052(10) 0.1246(11) 0.1105(10) 0.0013(8) 0.0079(8) -0.0199(9) P2B 0.0794(8) 0.0835(8) 0.1598(13) -0.0094(8) 0.0294(8) 0.0002(6) S1B 0.0825(8) 0.1058(9) 0.1549(13) 0.0268(9) -0.0219(8) -0.0142(7) S2B 0.1465(15) 0.0997(10) 0.2185(19) 0.0213(12) 0.1001(14) 0.0294(10) S3B 0.1226(11) 0.1303(11) 0.1070(9) 0.0018(8) 0.0103(8) -0.0419(10) S4B 0.0760(7) 0.0912(8) 0.1411(10) -0.0034(7) 0.0265(7) 0.0184(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1A C2A 1.354(6) . ? C1A S1A 1.739(4) . ? C1A P1A 1.795(5) . ? C2A C3A 1.453(6) . ? C2A H2A 0.9300 . ? C3A C22A 1.402(6) . ? C3A C4A 1.410(7) . ? C4A C5A 1.434(6) . ? C4A C19A 1.409(6) . ? C5A C6A 1.418(6) . ? C5A C18A 1.397(7) . ? C6A C15A 1.394(7) . ? C6A C7A 1.450(7) . ? C7A C14A 1.410(6) . ? C7A C8A 1.425(7) . ? C8A C11A 1.416(6) . ? C8A C9A 1.424(6) . ? C9A C10A 1.360(7) . ? C9A H9A 0.9300 . ? C10A S4A 1.727(4) . ? C10A P2A 1.803(5) . ? C11A C12A 1.398(7) . ? C11A S4A 1.723(6) . ? C12A C13A 1.349(9) . ? C12A H12A 0.9300 . ? C13A C14A 1.433(8) . ? C13A H13A 0.9300 . ? C14A S3A 1.729(6) . ? C15A C16A 1.393(8) . ? C15A S3A 1.759(5) . ? C16A C17A 1.425(7) . ? C16A C23A 1.488(8) . ? C17A C18A 1.412(7) . ? C17A C24A 1.512(8) . ? C18A S2A 1.757(5) . ? C19A C20A 1.376(7) . ? C19A S2A 1.756(5) . ? C20A C21A 1.356(8) . ? C20A H20A 0.9300 . ? C21A C22A 1.421(6) . ? C21A H21A 0.9300 . ? C22A S1A 1.718(5) . ? C23A C25A 1.557(10) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A C26A 1.526(8) . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? C25A C27A 1.466(12) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C26A C28A 1.515(10) . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A C30A 1.309(10) . ? C29A P1A 1.835(9) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A C31A 1.389(11) . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? C31A C32A 1.344(12) . ? C31A H31A 0.9700 . ? C31A H31B 0.9700 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C33A C34A 1.450(9) . ? C33A P1A 1.782(7) . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C34A C35A 1.543(11) . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C35A C36A 1.394(12) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C36A H36A 0.9600 . ? C36A H36B 0.9600 . ? C36A H36C 0.9600 . ? C37A C38A 1.326(14) . ? C37A P2A 1.734(12) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C38A C39A 1.395(13) . ? C38A H38A 0.9700 . ? C38A H38B 0.9700 . ? C39A C40A 1.284(13) . ? C39A H39A 0.9700 . ? C39A H39B 0.9700 . ? C40A H40A 0.9600 . ? C40A H40B 0.9600 . ? C40A H40C 0.9600 . ? C41A C42A 1.310(12) . ? C41A P2A 1.743(9) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A C43A 1.515(13) . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C43A C44A 1.281(14) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C44A H44A 0.9600 . ? C44A H44B 0.9600 . ? C44A H44C 0.9600 . ? B1A P1A 1.917(6) . ? B1A H1A1 0.9600 . ? B1A H1A2 0.9600 . ? B1A H1A3 0.9600 . ? B2A P2A 1.926(7) . ? B2A H2A1 0.9600 . ? B2A H2A2 0.9600 . ? B2A H2A3 0.9600 . ? C1B C2B 1.359(7) . ? C1B S1B 1.734(5) . ? C1B P1B 1.822(6) . ? C2B C3B 1.409(7) . ? C2B H2B 0.9300 . ? C3B C22B 1.404(8) . ? C3B C4B 1.425(8) . ? C4B C19B 1.384(7) . ? C4B C5B 1.458(9) . ? C5B C6B 1.402(8) . ? C5B C18B 1.395(8) . ? C6B C7B 1.465(7) . ? C6B C15B 1.424(8) . ? C7B C14B 1.406(7) . ? C7B C8B 1.409(7) . ? C8B C11B 1.379(6) . ? C8B C9B 1.427(6) . ? C9B C10B 1.336(7) . ? C9B H9B 0.9300 . ? C10B S4B 1.737(4) . ? C10B P2B 1.798(5) . ? C11B C12B 1.411(7) . ? C11B S4B 1.731(6) . ? C12B C13B 1.353(9) . ? C12B H12B 0.9300 . ? C13B C14B 1.388(9) . ? C13B H13B 0.9300 . ? C14B S3B 1.733(6) . ? C15B C16B 1.433(9) . ? C15B S3B 1.723(7) . ? C16B C17B 1.337(11) . ? C16B C23B 1.518(10) . ? C17B C18B 1.423(10) . ? C17B C24B 1.541(10) . ? C18B S2B 1.760(7) . ? C19B C20B 1.422(11) . ? C19B S2B 1.751(8) . ? C20B C21B 1.308(11) . ? C20B H20B 0.9300 . ? C21B C22B 1.421(9) . ? C21B H21B 0.9300 . ? C22B S1B 1.748(7) . ? C23B C25B 1.556(10) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B C26B 1.497(12) . ? C24B H24C 0.9700 . ? C24B H24D 0.9700 . ? C25B C27B 1.456(15) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26B C28B 1.543(13) . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B C30B 1.366(12) . ? C29B P1B 1.831(12) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30B C31B 1.470(11) . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? C31B C32B 1.341(12) . ? C31B H31C 0.9700 . ? C31B H31D 0.9700 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33B C34B 1.461(11) . ? C33B P1B 1.755(9) . ? C33B H33C 0.9700 . ? C33B H33D 0.9700 . ? C34B C35B 1.595(12) . ? C34B H34C 0.9700 . ? C34B H34D 0.9700 . ? C35B C36B 1.374(13) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C36B H36D 0.9600 . ? C36B H36E 0.9600 . ? C36B H36F 0.9600 . ? C37B C38B 1.348(10) . ? C37B P2B 1.858(10) . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C38B C39B 1.385(13) . ? C38B H38C 0.9700 . ? C38B H38D 0.9700 . ? C39B C40B 1.327(13) . ? C39B H39C 0.9700 . ? C39B H39D 0.9700 . ? C40B H40D 0.9600 . ? C40B H40E 0.9600 . ? C40B H40F 0.9600 . ? C41B C42B 1.370(10) . ? C41B P2B 1.770(7) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.492(13) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B C44B 1.301(16) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B H44D 0.9600 . ? C44B H44E 0.9600 . ? C44B H44F 0.9600 . ? B1B P1B 1.904(8) . ? B1B H1B1 0.9600 . ? B1B H1B2 0.9600 . ? B1B H1B3 0.9600 . ? B2B P2B 1.895(8) . ? B2B H2B1 0.9600 . ? B2B H2B2 0.9600 . ? B2B H2B3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A C1A S1A 111.9(3) . . ? C2A C1A P1A 122.9(3) . . ? S1A C1A P1A 125.1(3) . . ? C1A C2A C3A 113.6(4) . . ? C1A C2A H2A 123.2 . . ? C3A C2A H2A 123.2 . . ? C22A C3A C2A 110.2(4) . . ? C22A C3A C4A 119.9(4) . . ? C2A C3A C4A 129.6(4) . . ? C5A C4A C19A 112.7(4) . . ? C5A C4A C3A 130.1(4) . . ? C19A C4A C3A 116.1(4) . . ? C4A C5A C6A 131.4(4) . . ? C4A C5A C18A 111.9(4) . . ? C6A C5A C18A 116.6(4) . . ? C15A C6A C5A 117.2(5) . . ? C15A C6A C7A 111.6(4) . . ? C5A C6A C7A 131.2(4) . . ? C14A C7A C6A 111.7(5) . . ? C14A C7A C8A 117.1(4) . . ? C6A C7A C8A 130.5(4) . . ? C11A C8A C9A 110.9(5) . . ? C11A C8A C7A 118.4(4) . . ? C9A C8A C7A 130.3(4) . . ? C10A C9A C8A 113.6(4) . . ? C10A C9A H9A 123.2 . . ? C8A C9A H9A 123.2 . . ? C9A C10A S4A 112.2(4) . . ? C9A C10A P2A 125.8(3) . . ? S4A C10A P2A 121.9(3) . . ? C8A C11A C12A 123.0(6) . . ? C8A C11A S4A 111.5(4) . . ? C12A C11A S4A 125.3(4) . . ? C13A C12A C11A 118.7(5) . . ? C13A C12A H12A 120.6 . . ? C11A C12A H12A 120.6 . . ? C12A C13A C14A 120.4(5) . . ? C12A C13A H13A 119.8 . . ? C14A C13A H13A 119.8 . . ? C7A C14A C13A 121.7(5) . . ? C7A C14A S3A 112.3(4) . . ? C13A C14A S3A 125.8(4) . . ? C6A C15A C16A 124.6(4) . . ? C6A C15A S3A 111.8(4) . . ? C16A C15A S3A 123.6(4) . . ? C17A C16A C15A 117.5(5) . . ? C17A C16A C23A 123.0(6) . . ? C15A C16A C23A 119.3(5) . . ? C16A C17A C18A 116.8(5) . . ? C16A C17A C24A 124.2(5) . . ? C18A C17A C24A 118.9(5) . . ? C17A C18A C5A 124.3(4) . . ? C17A C18A S2A 123.8(4) . . ? C5A C18A S2A 111.7(4) . . ? C4A C19A C20A 123.0(5) . . ? C4A C19A S2A 111.1(3) . . ? C20A C19A S2A 125.6(4) . . ? C21A C20A C19A 120.7(4) . . ? C21A C20A H20A 119.7 . . ? C19A C20A H20A 119.7 . . ? C20A C21A C22A 118.4(4) . . ? C20A C21A H21A 120.8 . . ? C22A C21A H21A 120.8 . . ? C3A C22A C21A 121.0(5) . . ? C3A C22A S1A 112.5(3) . . ? C21A C22A S1A 126.3(4) . . ? C25A C23A C16A 113.1(5) . . ? C25A C23A H23A 109.0 . . ? C16A C23A H23A 109.0 . . ? C25A C23A H23B 109.0 . . ? C16A C23A H23B 109.0 . . ? H23A C23A H23B 107.8 . . ? C17A C24A C26A 112.5(5) . . ? C17A C24A H24A 109.1 . . ? C26A C24A H24A 109.1 . . ? C17A C24A H24B 109.1 . . ? C26A C24A H24B 109.1 . . ? H24A C24A H24B 107.8 . . ? C23A C25A C27A 113.7(7) . . ? C23A C25A H25A 108.8 . . ? C27A C25A H25A 108.8 . . ? C23A C25A H25B 108.8 . . ? C27A C25A H25B 108.8 . . ? H25A C25A H25B 107.7 . . ? C28A C26A C24A 112.5(6) . . ? C28A C26A H26A 109.1 . . ? C24A C26A H26A 109.1 . . ? C28A C26A H26B 109.1 . . ? C24A C26A H26B 109.1 . . ? H26A C26A H26B 107.8 . . ? C25A C27A H27A 109.5 . . ? C25A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C26A C28A H28A 109.5 . . ? C26A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C26A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C30A C29A P1A 128.0(8) . . ? C30A C29A H29A 105.3 . . ? P1A C29A H29A 105.3 . . ? C30A C29A H29B 105.3 . . ? P1A C29A H29B 105.3 . . ? H29A C29A H29B 106.0 . . ? C29A C30A C31A 132.1(13) . . ? C29A C30A H30A 104.2 . . ? C31A C30A H30A 104.2 . . ? C29A C30A H30B 104.2 . . ? C31A C30A H30B 104.2 . . ? H30A C30A H30B 105.5 . . ? C32A C31A C30A 126.2(13) . . ? C32A C31A H31A 105.8 . . ? C30A C31A H31A 105.8 . . ? C32A C31A H31B 105.8 . . ? C30A C31A H31B 105.8 . . ? H31A C31A H31B 106.2 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C34A C33A P1A 116.3(5) . . ? C34A C33A H33A 108.2 . . ? P1A C33A H33A 108.2 . . ? C34A C33A H33B 108.2 . . ? P1A C33A H33B 108.2 . . ? H33A C33A H33B 107.4 . . ? C33A C34A C35A 110.1(8) . . ? C33A C34A H34A 109.6 . . ? C35A C34A H34A 109.6 . . ? C33A C34A H34B 109.6 . . ? C35A C34A H34B 109.6 . . ? H34A C34A H34B 108.2 . . ? C36A C35A C34A 112.5(13) . . ? C36A C35A H35A 109.1 . . ? C34A C35A H35A 109.1 . . ? C36A C35A H35B 109.1 . . ? C34A C35A H35B 109.1 . . ? H35A C35A H35B 107.8 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C38A C37A P2A 124.0(12) . . ? C38A C37A H37A 106.3 . . ? P2A C37A H37A 106.3 . . ? C38A C37A H37B 106.3 . . ? P2A C37A H37B 106.3 . . ? H37A C37A H37B 106.4 . . ? C37A C38A C39A 116.3(17) . . ? C37A C38A H38A 108.2 . . ? C39A C38A H38A 108.2 . . ? C37A C38A H38B 108.2 . . ? C39A C38A H38B 108.2 . . ? H38A C38A H38B 107.4 . . ? C40A C39A C38A 122.4(18) . . ? C40A C39A H39A 106.7 . . ? C38A C39A H39A 106.7 . . ? C40A C39A H39B 106.7 . . ? C38A C39A H39B 106.7 . . ? H39A C39A H39B 106.6 . . ? C39A C40A H40A 109.5 . . ? C39A C40A H40B 109.5 . . ? H40A C40A H40B 109.5 . . ? C39A C40A H40C 109.5 . . ? H40A C40A H40C 109.5 . . ? H40B C40A H40C 109.5 . . ? C42A C41A P2A 121.7(10) . . ? C42A C41A H41A 106.9 . . ? P2A C41A H41A 106.9 . . ? C42A C41A H41B 106.9 . . ? P2A C41A H41B 106.9 . . ? H41A C41A H41B 106.7 . . ? C41A C42A C43A 121.5(14) . . ? C41A C42A H42A 107.0 . . ? C43A C42A H42A 107.0 . . ? C41A C42A H42B 107.0 . . ? C43A C42A H42B 107.0 . . ? H42A C42A H42B 106.7 . . ? C44A C43A C42A 128(2) . . ? C44A C43A H43A 105.2 . . ? C42A C43A H43A 105.2 . . ? C44A C43A H43B 105.2 . . ? C42A C43A H43B 105.2 . . ? H43A C43A H43B 106.0 . . ? C43A C44A H44A 109.5 . . ? C43A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C43A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? P1A B1A H1A1 109.5 . . ? P1A B1A H1A2 109.5 . . ? H1A1 B1A H1A2 109.5 . . ? P1A B1A H1A3 109.5 . . ? H1A1 B1A H1A3 109.5 . . ? H1A2 B1A H1A3 109.5 . . ? P2A B2A H2A1 109.5 . . ? P2A B2A H2A2 109.5 . . ? H2A1 B2A H2A2 109.5 . . ? P2A B2A H2A3 109.5 . . ? H2A1 B2A H2A3 109.5 . . ? H2A2 B2A H2A3 109.5 . . ? C33A P1A C1A 107.0(3) . . ? C33A P1A B1A 115.2(4) . . ? C1A P1A B1A 111.0(3) . . ? C33A P1A C29A 104.9(5) . . ? C1A P1A C29A 105.9(4) . . ? B1A P1A C29A 112.2(5) . . ? C41A P2A C37A 95.2(7) . . ? C41A P2A C10A 108.0(4) . . ? C37A P2A C10A 106.5(4) . . ? C41A P2A B2A 116.1(4) . . ? C37A P2A B2A 116.8(6) . . ? C10A P2A B2A 112.7(3) . . ? C1A S1A C22A 91.7(2) . . ? C19A S2A C18A 91.3(2) . . ? C15A S3A C14A 91.5(2) . . ? C10A S4A C11A 91.7(2) . . ? C2B C1B S1B 111.8(4) . . ? C2B C1B P1B 125.9(4) . . ? S1B C1B P1B 122.2(3) . . ? C3B C2B C1B 113.9(4) . . ? C3B C2B H2B 123.1 . . ? C1B C2B H2B 123.1 . . ? C22B C3B C2B 112.4(5) . . ? C22B C3B C4B 117.2(5) . . ? C2B C3B C4B 130.2(5) . . ? C19B C4B C5B 111.2(6) . . ? C19B C4B C3B 118.4(6) . . ? C5B C4B C3B 129.6(4) . . ? C6B C5B C18B 116.6(6) . . ? C6B C5B C4B 131.4(5) . . ? C18B C5B C4B 111.9(5) . . ? C5B C6B C7B 131.7(5) . . ? C5B C6B C15B 118.1(5) . . ? C7B C6B C15B 110.0(5) . . ? C14B C7B C8B 117.8(4) . . ? C14B C7B C6B 111.5(5) . . ? C8B C7B C6B 130.1(4) . . ? C11B C8B C9B 111.5(4) . . ? C11B C8B C7B 118.1(4) . . ? C9B C8B C7B 130.0(4) . . ? C10B C9B C8B 113.7(4) . . ? C10B C9B H9B 123.1 . . ? C8B C9B H9B 123.1 . . ? C9B C10B S4B 112.2(3) . . ? C9B C10B P2B 123.9(3) . . ? S4B C10B P2B 123.9(3) . . ? C8B C11B C12B 123.2(5) . . ? C8B C11B S4B 111.8(3) . . ? C12B C11B S4B 124.8(4) . . ? C13B C12B C11B 117.9(5) . . ? C13B C12B H12B 121.0 . . ? C11B C12B H12B 121.0 . . ? C12B C13B C14B 120.4(5) . . ? C12B C13B H13B 119.8 . . ? C14B C13B H13B 119.8 . . ? C13B C14B C7B 121.8(5) . . ? C13B C14B S3B 125.3(4) . . ? C7B C14B S3B 112.7(4) . . ? C6B C15B C16B 120.9(6) . . ? C6B C15B S3B 112.9(4) . . ? C16B C15B S3B 126.2(5) . . ? C17B C16B C15B 119.4(6) . . ? C17B C16B C23B 123.9(7) . . ? C15B C16B C23B 116.5(8) . . ? C16B C17B C18B 118.2(5) . . ? C16B C17B C24B 122.6(8) . . ? C18B C17B C24B 119.2(9) . . ? C5B C18B C17B 123.5(6) . . ? C5B C18B S2B 111.6(5) . . ? C17B C18B S2B 124.8(5) . . ? C20B C19B C4B 121.7(7) . . ? C20B C19B S2B 124.7(5) . . ? C4B C19B S2B 113.2(6) . . ? C21B C20B C19B 120.3(6) . . ? C21B C20B H20B 119.9 . . ? C19B C20B H20B 119.9 . . ? C20B C21B C22B 119.9(7) . . ? C20B C21B H21B 120.1 . . ? C22B C21B H21B 120.1 . . ? C3B C22B C21B 121.9(7) . . ? C3B C22B S1B 110.4(4) . . ? C21B C22B S1B 127.0(5) . . ? C16B C23B C25B 113.0(6) . . ? C16B C23B H23C 109.0 . . ? C25B C23B H23C 109.0 . . ? C16B C23B H23D 109.0 . . ? C25B C23B H23D 109.0 . . ? H23C C23B H23D 107.8 . . ? C17B C24B C26B 112.7(7) . . ? C17B C24B H24C 109.1 . . ? C26B C24B H24C 109.1 . . ? C17B C24B H24D 109.1 . . ? C26B C24B H24D 109.1 . . ? H24C C24B H24D 107.8 . . ? C27B C25B C23B 112.3(7) . . ? C27B C25B H25C 109.2 . . ? C23B C25B H25C 109.2 . . ? C27B C25B H25D 109.2 . . ? C23B C25B H25D 109.2 . . ? H25C C25B H25D 107.9 . . ? C24B C26B C28B 108.5(8) . . ? C24B C26B H26C 110.0 . . ? C28B C26B H26C 110.0 . . ? C24B C26B H26D 110.0 . . ? C28B C26B H26D 110.0 . . ? H26C C26B H26D 108.4 . . ? C25B C27B H27D 109.5 . . ? C25B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C25B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C26B C28B H28D 109.5 . . ? C26B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C26B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C30B C29B P1B 120.4(9) . . ? C30B C29B H29C 107.2 . . ? P1B C29B H29C 107.2 . . ? C30B C29B H29D 107.2 . . ? P1B C29B H29D 107.2 . . ? H29C C29B H29D 106.9 . . ? C29B C30B C31B 114.7(13) . . ? C29B C30B H30C 108.6 . . ? C31B C30B H30C 108.6 . . ? C29B C30B H30D 108.6 . . ? C31B C30B H30D 108.6 . . ? H30C C30B H30D 107.6 . . ? C32B C31B C30B 121.8(15) . . ? C32B C31B H31C 106.9 . . ? C30B C31B H31C 106.9 . . ? C32B C31B H31D 106.9 . . ? C30B C31B H31D 106.9 . . ? H31C C31B H31D 106.7 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C34B C33B P1B 116.6(7) . . ? C34B C33B H33C 108.1 . . ? P1B C33B H33C 108.1 . . ? C34B C33B H33D 108.1 . . ? P1B C33B H33D 108.1 . . ? H33C C33B H33D 107.3 . . ? C33B C34B C35B 123.1(11) . . ? C33B C34B H34C 106.5 . . ? C35B C34B H34C 106.5 . . ? C33B C34B H34D 106.5 . . ? C35B C34B H34D 106.5 . . ? H34C C34B H34D 106.5 . . ? C36B C35B C34B 110.3(13) . . ? C36B C35B H35C 109.6 . . ? C34B C35B H35C 109.6 . . ? C36B C35B H35D 109.6 . . ? C34B C35B H35D 109.6 . . ? H35C C35B H35D 108.1 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C38B C37B P2B 128.2(10) . . ? C38B C37B H37C 105.2 . . ? P2B C37B H37C 105.2 . . ? C38B C37B H37D 105.2 . . ? P2B C37B H37D 105.2 . . ? H37C C37B H37D 106.0 . . ? C37B C38B C39B 128.3(16) . . ? C37B C38B H38C 105.2 . . ? C39B C38B H38C 105.2 . . ? C37B C38B H38D 105.2 . . ? C39B C38B H38D 105.2 . . ? H38C C38B H38D 105.9 . . ? C40B C39B C38B 121.8(16) . . ? C40B C39B H39C 106.9 . . ? C38B C39B H39C 106.9 . . ? C40B C39B H39D 106.9 . . ? C38B C39B H39D 106.9 . . ? H39C C39B H39D 106.7 . . ? C39B C40B H40D 109.5 . . ? C39B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C39B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C42B C41B P2B 117.6(7) . . ? C42B C41B H41C 107.9 . . ? P2B C41B H41C 107.9 . . ? C42B C41B H41D 107.9 . . ? P2B C41B H41D 107.9 . . ? H41C C41B H41D 107.2 . . ? C41B C42B C43B 121.3(14) . . ? C41B C42B H42C 107.0 . . ? C43B C42B H42C 107.0 . . ? C41B C42B H42D 107.0 . . ? C43B C42B H42D 107.0 . . ? H42C C42B H42D 106.7 . . ? C44B C43B C42B 108(2) . . ? C44B C43B H43C 110.2 . . ? C42B C43B H43C 110.2 . . ? C44B C43B H43D 110.2 . . ? C42B C43B H43D 110.2 . . ? H43C C43B H43D 108.5 . . ? C43B C44B H44D 109.5 . . ? C43B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C43B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? P1B B1B H1B1 109.5 . . ? P1B B1B H1B2 109.5 . . ? H1B1 B1B H1B2 109.5 . . ? P1B B1B H1B3 109.5 . . ? H1B1 B1B H1B3 109.5 . . ? H1B2 B1B H1B3 109.5 . . ? P2B B2B H2B1 109.5 . . ? P2B B2B H2B2 109.5 . . ? H2B1 B2B H2B2 109.5 . . ? P2B B2B H2B3 109.5 . . ? H2B1 B2B H2B3 109.5 . . ? H2B2 B2B H2B3 109.5 . . ? C1B P1B C33B 109.3(4) . . ? C1B P1B C29B 106.7(4) . . ? C33B P1B C29B 97.0(6) . . ? C1B P1B B1B 113.4(3) . . ? C33B P1B B1B 114.9(4) . . ? C29B P1B B1B 114.0(6) . . ? C41B P2B C10B 107.4(3) . . ? C41B P2B B2B 116.4(4) . . ? C10B P2B B2B 110.7(3) . . ? C41B P2B C37B 105.3(6) . . ? C10B P2B C37B 105.3(4) . . ? B2B P2B C37B 111.1(5) . . ? C1B S1B C22B 91.5(3) . . ? C18B S2B C19B 90.6(3) . . ? C15B S3B C14B 91.7(3) . . ? C11B S4B C10B 90.8(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.256 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.042