data_pbsulf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.50 H26 B O0.50 P S' _chemical_formula_weight 438.32 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.304(2) _cell_length_b 14.747(4) _cell_length_c 17.336(5) _cell_angle_alpha 86.360(8) _cell_angle_beta 81.222(8) _cell_angle_gamma 75.856(7) _cell_volume 2278.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9144 _exptl_absorpt_correction_T_max 0.9144 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17486 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9887 _reflns_number_gt 8695 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+1.1661P] 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 9887 _refine_ls_number_parameters 570 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P6 P 0.69773(4) 0.18107(3) 0.44435(2) 0.01212(9) Uani 1 1 d . . . P5 P 0.36292(4) 0.31158(3) -0.08037(2) 0.01238(9) Uani 1 1 d . . . S2 S 0.26806(5) 0.42778(3) -0.13176(2) 0.02041(10) Uani 1 1 d . . . S3 S 0.86319(4) 0.07354(3) 0.45756(2) 0.01962(10) Uani 1 1 d . . . C5 C 0.49373(17) 0.13557(10) -0.14848(8) 0.0128(3) Uani 1 1 d . . . C6 C 0.36300(17) 0.20722(10) -0.12994(8) 0.0126(3) Uani 1 1 d . . . C7 C 0.22588(17) 0.20051(11) -0.14916(9) 0.0157(3) Uani 1 1 d . . . H1 H 0.1392 0.2494 -0.1361 0.019 Uiso 1 1 calc R . . C8 C 0.67318(17) 0.22722(11) -0.09119(9) 0.0150(3) Uani 1 1 d . . . C9 C 0.26956(17) 0.29743(11) 0.01804(9) 0.0145(3) Uani 1 1 d . . . C10 C 0.52257(18) 0.06830(11) 0.40532(9) 0.0168(3) Uani 1 1 d . . . H2 H 0.5895 0.0186 0.4285 0.020 Uiso 1 1 calc R . . C11 C 0.60139(17) 0.23146(10) 0.53644(8) 0.0135(3) Uani 1 1 d . . . C12 C 0.89488(17) 0.29123(11) 0.38784(9) 0.0170(3) Uani 1 1 d . . . H3 H 0.9674 0.2451 0.4110 0.020 Uiso 1 1 calc R . . C13 C 0.33165(18) 0.44602(11) 0.25542(10) 0.0186(3) Uani 1 1 d . . . C14 C 0.47924(18) 0.20028(11) 0.57529(9) 0.0171(3) Uani 1 1 d . . . H4 H 0.4445 0.1541 0.5527 0.021 Uiso 1 1 calc R . . C15 C 0.54869(17) 0.15755(10) 0.39852(8) 0.0135(3) Uani 1 1 d . . . C16 C 0.64097(17) 0.34655(10) 0.35520(8) 0.0137(3) Uani 1 1 d . . . C17 C 0.75039(17) 0.27898(10) 0.38934(8) 0.0133(3) Uani 1 1 d . . . C18 C 0.87157(17) 0.03721(11) -0.22144(9) 0.0154(3) Uani 1 1 d . . . C19 C 0.47778(18) 0.05800(11) -0.18687(9) 0.0160(3) Uani 1 1 d . . . H5 H 0.5633 0.0083 -0.1998 0.019 Uiso 1 1 calc R . . C20 C 0.93245(18) 0.37110(12) 0.35243(10) 0.0193(3) Uani 1 1 d . . . H6 H 1.0306 0.3796 0.3516 0.023 Uiso 1 1 calc R . . C21 C 0.35173(17) 0.41774(10) 0.33272(9) 0.0144(3) Uani 1 1 d . . . C22 C 0.40801(19) 0.23647(11) 0.64696(9) 0.0200(3) Uani 1 1 d . . . H7 H 0.3253 0.2146 0.6734 0.024 Uiso 1 1 calc R . . B61 B 0.48095(19) 0.33246(12) 0.35173(9) 0.0138(3) Uani 1 1 d . . . C24 C 0.4358(2) 0.39648(13) 0.18722(10) 0.0254(4) Uani 1 1 d . . . H26 H 0.3785 0.3937 0.1448 0.038 Uiso 1 1 calc R . . H27 H 0.4834 0.3328 0.2038 0.038 Uiso 1 1 calc R . . H28 H 0.5129 0.4308 0.1689 0.038 Uiso 1 1 calc R . . C25 C 0.82688(19) 0.43848(12) 0.31832(10) 0.0198(3) Uani 1 1 d . . . H8 H 0.8530 0.4929 0.2938 0.024 Uiso 1 1 calc R . . C26 C 0.78979(16) 0.05441(10) -0.14654(9) 0.0136(3) Uani 1 1 d . . . C27 C 0.34146(18) 0.05168(11) -0.20639(9) 0.0180(3) Uani 1 1 d . . . H9 H 0.3348 -0.0013 -0.2328 0.022 Uiso 1 1 calc R . . C28 C 0.5795(2) 0.33538(12) 0.64204(10) 0.0220(3) Uani 1 1 d . . . H10 H 0.6142 0.3813 0.6650 0.026 Uiso 1 1 calc R . . C29 C 0.7201(2) 0.37778(13) -0.01302(11) 0.0264(4) Uani 1 1 d . . . H29 H 0.7353 0.4280 0.0140 0.032 Uiso 1 1 calc R . . B60 B 0.65059(19) 0.13970(12) -0.12999(10) 0.0139(3) Uani 1 1 d . . . C31 C 0.21494(18) 0.12315(11) -0.18721(9) 0.0173(3) Uani 1 1 d . . . H11 H 0.1211 0.1190 -0.2001 0.021 Uiso 1 1 calc R . . C32 C 0.32811(18) 0.21279(11) 0.33684(9) 0.0175(3) Uani 1 1 d . . . H12 H 0.2609 0.2618 0.3131 0.021 Uiso 1 1 calc R . . C33 C 0.68289(18) 0.42620(11) 0.32004(9) 0.0174(3) Uani 1 1 d . . . H13 H 0.6113 0.4729 0.2968 0.021 Uiso 1 1 calc R . . C34 C 0.83849(18) -0.00432(11) -0.08348(9) 0.0170(3) Uani 1 1 d . . . C35 C 0.25397(18) 0.46650(11) 0.39444(10) 0.0180(3) Uani 1 1 d . . . C36 C 0.3222(2) 0.21751(11) 0.06274(9) 0.0206(3) Uani 1 1 d . . . H14 H 0.4070 0.1711 0.0419 0.025 Uiso 1 1 calc R . . C37 C 0.96725(19) -0.07607(11) -0.09595(10) 0.0202(3) Uani 1 1 d . . . H15 H 0.9998 -0.1147 -0.0529 0.024 Uiso 1 1 calc R . . C38 C 0.55439(17) 0.30390(11) -0.06717(9) 0.0149(3) Uani 1 1 d . . . C39 C 0.45138(17) 0.23249(10) 0.36374(8) 0.0136(3) Uani 1 1 d . . . C40 C 0.57849(19) 0.37768(12) -0.02867(11) 0.0229(4) Uani 1 1 d . . . H30 H 0.4967 0.4287 -0.0129 0.027 Uiso 1 1 calc R . . C41 C 0.07643(19) 0.35376(14) 0.12486(10) 0.0250(4) Uani 1 1 d . . . H48 H -0.0070 0.4006 0.1464 0.030 Uiso 1 1 calc R . . C42 C 0.1276(2) 0.27414(14) 0.16839(10) 0.0252(4) Uani 1 1 d . . . H49 H 0.0785 0.2659 0.2196 0.030 Uiso 1 1 calc R . . C43 C 1.04963(18) -0.09276(11) -0.16969(10) 0.0199(3) Uani 1 1 d . . . C44 C 0.39829(19) 0.05168(11) 0.37809(10) 0.0202(3) Uani 1 1 d . . . H16 H 0.3802 -0.0092 0.3830 0.024 Uiso 1 1 calc R . . C45 C 0.99931(18) -0.03638(11) -0.23197(10) 0.0183(3) Uani 1 1 d . . . H17 H 1.0530 -0.0481 -0.2829 0.022 Uiso 1 1 calc R . . C46 C 0.4573(2) 0.30446(12) 0.67999(9) 0.0216(3) Uani 1 1 d . . . H18 H 0.4073 0.3298 0.7286 0.026 Uiso 1 1 calc R . . C47 C 0.82618(19) 0.09987(12) -0.29061(10) 0.0216(3) Uani 1 1 d . . . H31 H 0.8692 0.1545 -0.2928 0.032 Uiso 1 1 calc R . . H32 H 0.7168 0.1205 -0.2849 0.032 Uiso 1 1 calc R . . H33 H 0.8632 0.0651 -0.3388 0.032 Uiso 1 1 calc R . . C48 C 0.14670(18) 0.36564(12) 0.04942(9) 0.0194(3) Uani 1 1 d . . . H19 H 0.1107 0.4203 0.0193 0.023 Uiso 1 1 calc R . . C49 C 0.83971(19) 0.30370(13) -0.03725(11) 0.0251(4) Uani 1 1 d . . . H34 H 0.9377 0.3034 -0.0276 0.030 Uiso 1 1 calc R . . C50 C 0.81554(18) 0.23015(12) -0.07554(10) 0.0209(3) Uani 1 1 d . . . H20 H 0.8984 0.1799 -0.0918 0.025 Uiso 1 1 calc R . . C51 C 0.2758(2) 0.43904(14) 0.47813(10) 0.0290(4) Uani 1 1 d . . . H35 H 0.3696 0.4518 0.4884 0.044 Uiso 1 1 calc R . . H36 H 0.2800 0.3722 0.4869 0.044 Uiso 1 1 calc R . . H37 H 0.1919 0.4754 0.5133 0.044 Uiso 1 1 calc R . . C52 C 0.30099(19) 0.12387(12) 0.34381(10) 0.0203(3) Uani 1 1 d . . . H21 H 0.2162 0.1126 0.3252 0.024 Uiso 1 1 calc R . . C53 C 0.65144(18) 0.29922(11) 0.57030(9) 0.0187(3) Uani 1 1 d . . . H22 H 0.7349 0.3207 0.5443 0.022 Uiso 1 1 calc R . . C55 C 0.7487(2) 0.00809(13) -0.00301(10) 0.0240(4) Uani 1 1 d . . . H38 H 0.7923 -0.0425 0.0321 0.036 Uiso 1 1 calc R . . H39 H 0.6450 0.0064 -0.0058 0.036 Uiso 1 1 calc R . . H40 H 0.7506 0.0684 0.0170 0.036 Uiso 1 1 calc R . . C56 C 0.13845(18) 0.54204(11) 0.37774(11) 0.0232(4) Uani 1 1 d . . . H23 H 0.0721 0.5747 0.4196 0.028 Uiso 1 1 calc R . . C57 C 0.2150(2) 0.52196(12) 0.24129(11) 0.0252(4) Uani 1 1 d . . . H24 H 0.2017 0.5408 0.1889 0.030 Uiso 1 1 calc R . . C61 C 1.1895(2) -0.17119(13) -0.18137(12) 0.0297(4) Uani 1 1 d . . . H41 H 1.2343 -0.1719 -0.2364 0.045 Uiso 1 1 calc R . . H42 H 1.1636 -0.2311 -0.1666 0.045 Uiso 1 1 calc R . . H43 H 1.2614 -0.1614 -0.1487 0.045 Uiso 1 1 calc R . . C60 C 0.2507(2) 0.20594(13) 0.13753(10) 0.0260(4) Uani 1 1 d . . . H25 H 0.2860 0.1513 0.1678 0.031 Uiso 1 1 calc R . . C58 C 0.1182(2) 0.57055(12) 0.30164(12) 0.0264(4) Uani 1 1 d . . . C59 C -0.0051(3) 0.65328(15) 0.28423(17) 0.0452(6) Uani 1 1 d . . . H50 H 0.0362 0.7083 0.2712 0.068 Uiso 1 1 calc R . . H51 H -0.0821 0.6658 0.3302 0.068 Uiso 1 1 calc R . . H52 H -0.0498 0.6395 0.2400 0.068 Uiso 1 1 calc R . . O1 O 0.82827(19) 0.87756(12) 0.38656(11) 0.0490(4) Uani 1 1 d . . . C63 C 0.8867(3) 0.81617(19) 0.44663(15) 0.0488(6) Uani 1 1 d . . . H44 H 0.9963 0.7995 0.4358 0.073 Uiso 1 1 calc R . . H45 H 0.8491 0.7594 0.4488 0.073 Uiso 1 1 calc R . . H46 H 0.8550 0.8472 0.4968 0.073 Uiso 1 1 calc R . . H47 H 0.827(6) -0.038(4) 0.421(3) 0.18(2) Uiso 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 P6 0.01158(18) 0.01159(18) 0.01218(18) 0.00004(13) -0.00259(13) -0.00036(14) P5 0.01282(19) 0.01080(18) 0.01270(18) -0.00237(13) -0.00155(14) -0.00089(14) S2 0.0276(2) 0.01258(18) 0.01857(19) -0.00034(14) -0.00585(16) 0.00144(16) S3 0.0177(2) 0.01595(19) 0.0222(2) -0.00063(14) -0.00627(15) 0.00383(15) C5 0.0142(7) 0.0126(7) 0.0116(6) -0.0009(5) -0.0017(5) -0.0029(6) C6 0.0148(7) 0.0127(7) 0.0098(6) -0.0001(5) -0.0015(5) -0.0028(6) C7 0.0137(7) 0.0170(7) 0.0152(7) -0.0001(5) -0.0021(5) -0.0013(6) C8 0.0147(7) 0.0153(7) 0.0148(7) -0.0035(5) -0.0004(5) -0.0034(6) C9 0.0143(7) 0.0168(7) 0.0133(7) -0.0034(5) -0.0016(5) -0.0047(6) C10 0.0199(8) 0.0142(7) 0.0159(7) -0.0001(6) -0.0040(6) -0.0026(6) C11 0.0145(7) 0.0130(7) 0.0118(6) 0.0006(5) -0.0032(5) -0.0001(6) C12 0.0121(7) 0.0203(7) 0.0174(7) -0.0017(6) -0.0022(6) -0.0013(6) C13 0.0193(8) 0.0165(7) 0.0225(8) 0.0021(6) -0.0085(6) -0.0066(6) C14 0.0191(8) 0.0143(7) 0.0174(7) 0.0016(6) -0.0022(6) -0.0037(6) C15 0.0130(7) 0.0138(7) 0.0131(7) -0.0014(5) -0.0019(5) -0.0017(6) C16 0.0131(7) 0.0139(7) 0.0132(7) -0.0015(5) -0.0010(5) -0.0017(6) C17 0.0138(7) 0.0134(7) 0.0122(6) -0.0013(5) -0.0010(5) -0.0023(6) C18 0.0144(7) 0.0160(7) 0.0170(7) -0.0037(6) -0.0023(6) -0.0052(6) C19 0.0172(7) 0.0134(7) 0.0169(7) -0.0036(5) -0.0014(6) -0.0026(6) C20 0.0130(7) 0.0232(8) 0.0224(8) -0.0031(6) 0.0001(6) -0.0066(6) C21 0.0111(7) 0.0118(7) 0.0214(7) 0.0010(6) -0.0054(6) -0.0036(6) C22 0.0204(8) 0.0180(7) 0.0188(8) 0.0026(6) 0.0027(6) -0.0035(6) B61 0.0142(8) 0.0142(8) 0.0117(7) -0.0003(6) -0.0028(6) -0.0005(6) C24 0.0311(9) 0.0277(9) 0.0185(8) 0.0011(7) -0.0065(7) -0.0079(7) C25 0.0193(8) 0.0184(8) 0.0227(8) 0.0006(6) -0.0002(6) -0.0083(6) C26 0.0114(7) 0.0126(7) 0.0173(7) -0.0032(5) -0.0027(5) -0.0032(5) C27 0.0211(8) 0.0174(7) 0.0174(7) -0.0044(6) -0.0030(6) -0.0070(6) C28 0.0270(9) 0.0207(8) 0.0190(8) -0.0050(6) -0.0028(6) -0.0063(7) C29 0.0239(9) 0.0236(9) 0.0351(10) -0.0137(7) -0.0019(7) -0.0104(7) B60 0.0147(8) 0.0140(8) 0.0121(7) -0.0016(6) -0.0005(6) -0.0026(6) C31 0.0161(7) 0.0216(8) 0.0164(7) 0.0000(6) -0.0042(6) -0.0075(6) C32 0.0169(7) 0.0168(7) 0.0188(7) 0.0008(6) -0.0062(6) -0.0022(6) C33 0.0174(8) 0.0146(7) 0.0192(7) 0.0015(6) -0.0034(6) -0.0022(6) C34 0.0165(7) 0.0171(7) 0.0173(7) -0.0017(6) -0.0029(6) -0.0033(6) C35 0.0140(7) 0.0151(7) 0.0255(8) -0.0012(6) -0.0024(6) -0.0047(6) C36 0.0255(8) 0.0178(7) 0.0169(7) -0.0021(6) -0.0011(6) -0.0028(7) C37 0.0187(8) 0.0182(8) 0.0235(8) 0.0015(6) -0.0070(6) -0.0017(6) C38 0.0139(7) 0.0148(7) 0.0162(7) -0.0033(5) -0.0008(5) -0.0036(6) C39 0.0137(7) 0.0134(7) 0.0129(6) -0.0004(5) -0.0015(5) -0.0021(6) C40 0.0191(8) 0.0176(8) 0.0324(9) -0.0104(7) -0.0010(7) -0.0042(6) C41 0.0157(8) 0.0364(10) 0.0202(8) -0.0099(7) 0.0025(6) -0.0023(7) C42 0.0247(9) 0.0374(10) 0.0157(7) -0.0061(7) 0.0022(6) -0.0135(8) C43 0.0136(7) 0.0153(7) 0.0303(9) -0.0041(6) -0.0029(6) -0.0016(6) C44 0.0261(9) 0.0151(7) 0.0214(8) -0.0018(6) -0.0048(6) -0.0078(7) C45 0.0149(7) 0.0188(7) 0.0210(8) -0.0068(6) 0.0015(6) -0.0047(6) C46 0.0263(9) 0.0198(8) 0.0148(7) -0.0018(6) 0.0009(6) -0.0004(7) C47 0.0221(8) 0.0235(8) 0.0177(7) 0.0000(6) -0.0018(6) -0.0036(7) C48 0.0146(7) 0.0236(8) 0.0186(7) -0.0050(6) -0.0028(6) -0.0005(6) C49 0.0154(8) 0.0293(9) 0.0334(9) -0.0116(7) -0.0032(7) -0.0084(7) C50 0.0142(7) 0.0226(8) 0.0261(8) -0.0086(6) -0.0020(6) -0.0032(6) C51 0.0299(10) 0.0297(9) 0.0221(9) -0.0019(7) 0.0019(7) -0.0002(8) C52 0.0209(8) 0.0207(8) 0.0228(8) -0.0027(6) -0.0083(6) -0.0077(7) C53 0.0180(8) 0.0204(8) 0.0181(7) -0.0022(6) -0.0008(6) -0.0059(6) C55 0.0264(9) 0.0258(9) 0.0168(8) 0.0015(6) -0.0005(6) -0.0023(7) C56 0.0135(7) 0.0158(8) 0.0401(10) -0.0061(7) -0.0030(7) -0.0022(6) C57 0.0270(9) 0.0192(8) 0.0328(9) 0.0056(7) -0.0183(7) -0.0052(7) C61 0.0173(8) 0.0234(9) 0.0433(11) -0.0044(8) -0.0020(7) 0.0042(7) C60 0.0373(10) 0.0228(8) 0.0184(8) 0.0005(6) -0.0028(7) -0.0090(8) C58 0.0189(8) 0.0144(7) 0.0489(11) 0.0014(7) -0.0171(8) -0.0026(7) C59 0.0346(11) 0.0237(10) 0.0767(17) 0.0005(10) -0.0290(11) 0.0066(9) O1 0.0474(10) 0.0448(9) 0.0565(11) 0.0008(8) -0.0156(8) -0.0098(8) C63 0.0501(14) 0.0521(14) 0.0444(13) -0.0018(11) -0.0121(11) -0.0092(12) _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 P6 C17 1.8062(16) . ? P6 C15 1.8111(16) . ? P6 C11 1.8147(15) . ? P6 S3 1.9507(6) . ? P5 C38 1.8058(16) . ? P5 C6 1.8094(16) . ? P5 C9 1.8165(16) . ? P5 S2 1.9535(6) . ? C5 C19 1.408(2) . ? C5 C6 1.412(2) . ? C5 B60 1.557(2) . ? C6 C7 1.394(2) . ? C7 C31 1.386(2) . ? C7 H1 0.9500 . ? C8 C50 1.403(2) . ? C8 C38 1.408(2) . ? C8 B60 1.565(2) . ? C9 C48 1.390(2) . ? C9 C36 1.395(2) . ? C10 C15 1.390(2) . ? C10 C44 1.393(2) . ? C10 H2 0.9500 . ? C11 C14 1.392(2) . ? C11 C53 1.395(2) . ? C12 C20 1.389(2) . ? C12 C17 1.396(2) . ? C12 H3 0.9500 . ? C13 C57 1.394(2) . ? C13 C21 1.404(2) . ? C13 C24 1.511(2) . ? C14 C22 1.388(2) . ? C14 H4 0.9500 . ? C15 C39 1.413(2) . ? C16 C33 1.401(2) . ? C16 C17 1.412(2) . ? C16 B61 1.563(2) . ? C18 C45 1.397(2) . ? C18 C26 1.405(2) . ? C18 C47 1.514(2) . ? C19 C27 1.387(2) . ? C19 H5 0.9500 . ? C20 C25 1.388(2) . ? C20 H6 0.9500 . ? C21 C35 1.404(2) . ? C21 B61 1.570(2) . ? C22 C46 1.386(2) . ? C22 H7 0.9500 . ? B61 C39 1.560(2) . ? C24 H26 0.9800 . ? C24 H27 0.9800 . ? C24 H28 0.9800 . ? C25 C33 1.391(2) . ? C25 H8 0.9500 . ? C26 C34 1.411(2) . ? C26 B60 1.574(2) . ? C27 C31 1.388(2) . ? C27 H9 0.9500 . ? C28 C46 1.386(3) . ? C28 C53 1.391(2) . ? C28 H10 0.9500 . ? C29 C40 1.385(2) . ? C29 C49 1.389(2) . ? C29 H29 0.9500 . ? C31 H11 0.9500 . ? C32 C52 1.389(2) . ? C32 C39 1.400(2) . ? C32 H12 0.9500 . ? C33 H13 0.9500 . ? C34 C37 1.390(2) . ? C34 C55 1.510(2) . ? C35 C56 1.396(2) . ? C35 C51 1.512(2) . ? C36 C60 1.384(2) . ? C36 H14 0.9500 . ? C37 C43 1.390(2) . ? C37 H15 0.9500 . ? C38 C40 1.392(2) . ? C40 H30 0.9500 . ? C41 C42 1.378(3) . ? C41 C48 1.391(2) . ? C41 H48 0.9500 . ? C42 C60 1.388(3) . ? C42 H49 0.9500 . ? C43 C45 1.388(2) . ? C43 C61 1.512(2) . ? C44 C52 1.385(2) . ? C44 H16 0.9500 . ? C45 H17 0.9500 . ? C46 H18 0.9500 . ? C47 H31 0.9800 . ? C47 H32 0.9800 . ? C47 H33 0.9800 . ? C48 H19 0.9500 . ? C49 C50 1.387(2) . ? C49 H34 0.9500 . ? C50 H20 0.9500 . ? C51 H35 0.9800 . ? C51 H36 0.9800 . ? C51 H37 0.9800 . ? C52 H21 0.9500 . ? C53 H22 0.9500 . ? C55 H38 0.9800 . ? C55 H39 0.9800 . ? C55 H40 0.9800 . ? C56 C58 1.385(3) . ? C56 H23 0.9500 . ? C57 C58 1.382(3) . ? C57 H24 0.9500 . ? C61 H41 0.9800 . ? C61 H42 0.9800 . ? C61 H43 0.9800 . ? C60 H25 0.9500 . ? C58 C59 1.507(2) . ? C59 H50 0.9800 . ? C59 H51 0.9800 . ? C59 H52 0.9800 . ? O1 C63 1.419(3) . ? C63 H44 0.9800 . ? C63 H45 0.9800 . ? C63 H46 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 P6 C15 105.29(7) . . ? C17 P6 C11 103.49(7) . . ? C15 P6 C11 103.39(7) . . ? C17 P6 S3 115.02(5) . . ? C15 P6 S3 115.48(5) . . ? C11 P6 S3 112.80(5) . . ? C38 P5 C6 106.74(7) . . ? C38 P5 C9 103.79(7) . . ? C6 P5 C9 105.18(7) . . ? C38 P5 S2 114.11(6) . . ? C6 P5 S2 113.87(5) . . ? C9 P5 S2 112.25(5) . . ? C19 C5 C6 116.65(14) . . ? C19 C5 B60 119.84(13) . . ? C6 C5 B60 123.50(13) . . ? C7 C6 C5 121.02(13) . . ? C7 C6 P5 116.43(11) . . ? C5 C6 P5 122.56(11) . . ? C31 C7 C6 120.57(14) . . ? C31 C7 H1 119.7 . . ? C6 C7 H1 119.7 . . ? C50 C8 C38 116.73(14) . . ? C50 C8 B60 120.22(13) . . ? C38 C8 B60 122.98(14) . . ? C48 C9 C36 119.67(15) . . ? C48 C9 P5 120.67(12) . . ? C36 C9 P5 119.67(12) . . ? C15 C10 C44 120.02(14) . . ? C15 C10 H2 120.0 . . ? C44 C10 H2 120.0 . . ? C14 C11 C53 119.34(14) . . ? C14 C11 P6 119.98(12) . . ? C53 C11 P6 120.65(12) . . ? C20 C12 C17 119.83(14) . . ? C20 C12 H3 120.1 . . ? C17 C12 H3 120.1 . . ? C57 C13 C21 119.48(16) . . ? C57 C13 C24 119.38(15) . . ? C21 C13 C24 121.14(14) . . ? C22 C14 C11 120.24(15) . . ? C22 C14 H4 119.9 . . ? C11 C14 H4 119.9 . . ? C10 C15 C39 121.11(14) . . ? C10 C15 P6 119.36(11) . . ? C39 C15 P6 119.18(12) . . ? C33 C16 C17 117.51(14) . . ? C33 C16 B61 120.04(13) . . ? C17 C16 B61 122.36(14) . . ? C12 C17 C16 121.06(14) . . ? C12 C17 P6 119.19(11) . . ? C16 C17 P6 119.45(12) . . ? C45 C18 C26 119.83(14) . . ? C45 C18 C47 119.41(14) . . ? C26 C18 C47 120.72(14) . . ? C27 C19 C5 122.26(14) . . ? C27 C19 H5 118.9 . . ? C5 C19 H5 118.9 . . ? C25 C20 C12 120.19(15) . . ? C25 C20 H6 119.9 . . ? C12 C20 H6 119.9 . . ? C35 C21 C13 119.38(14) . . ? C35 C21 B61 119.17(14) . . ? C13 C21 B61 121.45(14) . . ? C46 C22 C14 120.19(16) . . ? C46 C22 H7 119.9 . . ? C14 C22 H7 119.9 . . ? C39 B61 C16 119.79(13) . . ? C39 B61 C21 119.88(14) . . ? C16 B61 C21 120.28(14) . . ? C13 C24 H26 109.5 . . ? C13 C24 H27 109.5 . . ? H26 C24 H27 109.5 . . ? C13 C24 H28 109.5 . . ? H26 C24 H28 109.5 . . ? H27 C24 H28 109.5 . . ? C20 C25 C33 119.87(15) . . ? C20 C25 H8 120.1 . . ? C33 C25 H8 120.1 . . ? C18 C26 C34 118.75(14) . . ? C18 C26 B60 122.27(13) . . ? C34 C26 B60 118.92(13) . . ? C19 C27 C31 119.72(14) . . ? C19 C27 H9 120.1 . . ? C31 C27 H9 120.1 . . ? C46 C28 C53 120.07(16) . . ? C46 C28 H10 120.0 . . ? C53 C28 H10 120.0 . . ? C40 C29 C49 119.31(15) . . ? C40 C29 H29 120.3 . . ? C49 C29 H29 120.3 . . ? C5 B60 C8 120.96(13) . . ? C5 B60 C26 121.06(13) . . ? C8 B60 C26 117.93(13) . . ? C7 C31 C27 119.78(15) . . ? C7 C31 H11 120.1 . . ? C27 C31 H11 120.1 . . ? C52 C32 C39 122.07(14) . . ? C52 C32 H12 119.0 . . ? C39 C32 H12 119.0 . . ? C25 C33 C16 121.54(14) . . ? C25 C33 H13 119.2 . . ? C16 C33 H13 119.2 . . ? C37 C34 C26 119.83(14) . . ? C37 C34 C55 119.70(15) . . ? C26 C34 C55 120.43(14) . . ? C56 C35 C21 119.32(16) . . ? C56 C35 C51 120.29(15) . . ? C21 C35 C51 120.37(14) . . ? C60 C36 C9 119.94(15) . . ? C60 C36 H14 120.0 . . ? C9 C36 H14 120.0 . . ? C43 C37 C34 121.70(15) . . ? C43 C37 H15 119.1 . . ? C34 C37 H15 119.1 . . ? C40 C38 C8 120.93(15) . . ? C40 C38 P5 115.88(12) . . ? C8 C38 P5 123.16(12) . . ? C32 C39 C15 117.10(14) . . ? C32 C39 B61 120.30(13) . . ? C15 C39 B61 122.55(14) . . ? C29 C40 C38 120.92(15) . . ? C29 C40 H30 119.5 . . ? C38 C40 H30 119.5 . . ? C42 C41 C48 120.14(16) . . ? C42 C41 H48 119.9 . . ? C48 C41 H48 119.9 . . ? C41 C42 C60 120.17(16) . . ? C41 C42 H49 119.9 . . ? C60 C42 H49 119.9 . . ? C45 C43 C37 118.33(14) . . ? C45 C43 C61 121.20(16) . . ? C37 C43 C61 120.47(16) . . ? C52 C44 C10 120.09(15) . . ? C52 C44 H16 120.0 . . ? C10 C44 H16 120.0 . . ? C43 C45 C18 121.53(15) . . ? C43 C45 H17 119.2 . . ? C18 C45 H17 119.2 . . ? C28 C46 C22 119.97(15) . . ? C28 C46 H18 120.0 . . ? C22 C46 H18 120.0 . . ? C18 C47 H31 109.5 . . ? C18 C47 H32 109.5 . . ? H31 C47 H32 109.5 . . ? C18 C47 H33 109.5 . . ? H31 C47 H33 109.5 . . ? H32 C47 H33 109.5 . . ? C9 C48 C41 119.97(16) . . ? C9 C48 H19 120.0 . . ? C41 C48 H19 120.0 . . ? C50 C49 C29 119.72(16) . . ? C50 C49 H34 120.1 . . ? C29 C49 H34 120.1 . . ? C49 C50 C8 122.38(15) . . ? C49 C50 H20 118.8 . . ? C8 C50 H20 118.8 . . ? C35 C51 H35 109.5 . . ? C35 C51 H36 109.5 . . ? H35 C51 H36 109.5 . . ? C35 C51 H37 109.5 . . ? H35 C51 H37 109.5 . . ? H36 C51 H37 109.5 . . ? C44 C52 C32 119.62(15) . . ? C44 C52 H21 120.2 . . ? C32 C52 H21 120.2 . . ? C28 C53 C11 120.19(16) . . ? C28 C53 H22 119.9 . . ? C11 C53 H22 119.9 . . ? C34 C55 H38 109.5 . . ? C34 C55 H39 109.5 . . ? H38 C55 H39 109.5 . . ? C34 C55 H40 109.5 . . ? H38 C55 H40 109.5 . . ? H39 C55 H40 109.5 . . ? C58 C56 C35 121.64(16) . . ? C58 C56 H23 119.2 . . ? C35 C56 H23 119.2 . . ? C58 C57 C13 121.61(17) . . ? C58 C57 H24 119.2 . . ? C13 C57 H24 119.2 . . ? C43 C61 H41 109.5 . . ? C43 C61 H42 109.5 . . ? H41 C61 H42 109.5 . . ? C43 C61 H43 109.5 . . ? H41 C61 H43 109.5 . . ? H42 C61 H43 109.5 . . ? C36 C60 C42 120.10(17) . . ? C36 C60 H25 119.9 . . ? C42 C60 H25 119.9 . . ? C57 C58 C56 118.58(15) . . ? C57 C58 C59 120.19(19) . . ? C56 C58 C59 121.23(19) . . ? C58 C59 H50 109.5 . . ? C58 C59 H51 109.5 . . ? H50 C59 H51 109.5 . . ? C58 C59 H52 109.5 . . ? H50 C59 H52 109.5 . . ? H51 C59 H52 109.5 . . ? O1 C63 H44 109.5 . . ? O1 C63 H45 109.5 . . ? H44 C63 H45 109.5 . . ? O1 C63 H46 109.5 . . ? H44 C63 H46 109.5 . . ? H45 C63 H46 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C19 C5 C6 C7 -0.1(2) . . . . ? B60 C5 C6 C7 178.84(14) . . . . ? C19 C5 C6 P5 179.76(11) . . . . ? B60 C5 C6 P5 -1.3(2) . . . . ? C38 P5 C6 C7 -177.35(11) . . . . ? C9 P5 C6 C7 72.80(13) . . . . ? S2 P5 C6 C7 -50.51(13) . . . . ? C38 P5 C6 C5 2.81(14) . . . . ? C9 P5 C6 C5 -107.04(13) . . . . ? S2 P5 C6 C5 129.65(11) . . . . ? C5 C6 C7 C31 -0.2(2) . . . . ? P5 C6 C7 C31 179.99(12) . . . . ? C38 P5 C9 C48 122.68(13) . . . . ? C6 P5 C9 C48 -125.37(13) . . . . ? S2 P5 C9 C48 -1.03(15) . . . . ? C38 P5 C9 C36 -56.98(15) . . . . ? C6 P5 C9 C36 54.98(15) . . . . ? S2 P5 C9 C36 179.31(12) . . . . ? C17 P6 C11 C14 144.31(12) . . . . ? C15 P6 C11 C14 34.68(14) . . . . ? S3 P6 C11 C14 -90.75(12) . . . . ? C17 P6 C11 C53 -37.85(14) . . . . ? C15 P6 C11 C53 -147.48(13) . . . . ? S3 P6 C11 C53 87.09(13) . . . . ? C53 C11 C14 C22 0.1(2) . . . . ? P6 C11 C14 C22 177.97(12) . . . . ? C44 C10 C15 C39 -0.4(2) . . . . ? C44 C10 C15 P6 172.78(12) . . . . ? C17 P6 C15 C10 155.15(12) . . . . ? C11 P6 C15 C10 -96.57(13) . . . . ? S3 P6 C15 C10 27.12(14) . . . . ? C17 P6 C15 C39 -31.51(13) . . . . ? C11 P6 C15 C39 76.77(13) . . . . ? S3 P6 C15 C39 -159.54(10) . . . . ? C20 C12 C17 C16 0.1(2) . . . . ? C20 C12 C17 P6 -173.56(12) . . . . ? C33 C16 C17 C12 -0.1(2) . . . . ? B61 C16 C17 C12 176.50(13) . . . . ? C33 C16 C17 P6 173.54(11) . . . . ? B61 C16 C17 P6 -9.82(19) . . . . ? C15 P6 C17 C12 -154.55(12) . . . . ? C11 P6 C17 C12 97.25(13) . . . . ? S3 P6 C17 C12 -26.24(13) . . . . ? C15 P6 C17 C16 31.66(13) . . . . ? C11 P6 C17 C16 -76.54(13) . . . . ? S3 P6 C17 C16 159.97(10) . . . . ? C6 C5 C19 C27 0.5(2) . . . . ? B60 C5 C19 C27 -178.47(15) . . . . ? C17 C12 C20 C25 -0.2(2) . . . . ? C57 C13 C21 C35 0.0(2) . . . . ? C24 C13 C21 C35 179.03(15) . . . . ? C57 C13 C21 B61 179.76(15) . . . . ? C24 C13 C21 B61 -1.2(2) . . . . ? C11 C14 C22 C46 0.5(2) . . . . ? C33 C16 B61 C39 158.75(14) . . . . ? C17 C16 B61 C39 -17.8(2) . . . . ? C33 C16 B61 C21 -18.7(2) . . . . ? C17 C16 B61 C21 164.78(14) . . . . ? C35 C21 B61 C39 87.94(18) . . . . ? C13 C21 B61 C39 -91.86(18) . . . . ? C35 C21 B61 C16 -94.65(18) . . . . ? C13 C21 B61 C16 85.56(19) . . . . ? C12 C20 C25 C33 0.4(2) . . . . ? C45 C18 C26 C34 -0.7(2) . . . . ? C47 C18 C26 C34 -178.35(15) . . . . ? C45 C18 C26 B60 176.33(14) . . . . ? C47 C18 C26 B60 -1.4(2) . . . . ? C5 C19 C27 C31 -0.7(2) . . . . ? C19 C5 B60 C8 176.91(14) . . . . ? C6 C5 B60 C8 -2.0(2) . . . . ? C19 C5 B60 C26 -5.6(2) . . . . ? C6 C5 B60 C26 175.48(14) . . . . ? C50 C8 B60 C5 -179.44(15) . . . . ? C38 C8 B60 C5 3.5(2) . . . . ? C50 C8 B60 C26 3.0(2) . . . . ? C38 C8 B60 C26 -174.03(14) . . . . ? C18 C26 B60 C5 80.4(2) . . . . ? C34 C26 B60 C5 -102.66(17) . . . . ? C18 C26 B60 C8 -102.12(17) . . . . ? C34 C26 B60 C8 74.87(19) . . . . ? C6 C7 C31 C27 0.0(2) . . . . ? C19 C27 C31 C7 0.4(2) . . . . ? C20 C25 C33 C16 -0.4(2) . . . . ? C17 C16 C33 C25 0.3(2) . . . . ? B61 C16 C33 C25 -176.44(14) . . . . ? C18 C26 C34 C37 1.5(2) . . . . ? B60 C26 C34 C37 -175.55(15) . . . . ? C18 C26 C34 C55 -176.31(15) . . . . ? B60 C26 C34 C55 6.6(2) . . . . ? C13 C21 C35 C56 0.1(2) . . . . ? B61 C21 C35 C56 -179.65(15) . . . . ? C13 C21 C35 C51 -178.35(16) . . . . ? B61 C21 C35 C51 1.8(2) . . . . ? C48 C9 C36 C60 0.9(3) . . . . ? P5 C9 C36 C60 -179.44(13) . . . . ? C26 C34 C37 C43 -0.8(3) . . . . ? C55 C34 C37 C43 177.06(16) . . . . ? C50 C8 C38 C40 -1.1(2) . . . . ? B60 C8 C38 C40 176.10(15) . . . . ? C50 C8 C38 P5 -178.67(12) . . . . ? B60 C8 C38 P5 -1.5(2) . . . . ? C6 P5 C38 C40 -179.12(13) . . . . ? C9 P5 C38 C40 -68.31(14) . . . . ? S2 P5 C38 C40 54.18(14) . . . . ? C6 P5 C38 C8 -1.39(15) . . . . ? C9 P5 C38 C8 109.42(14) . . . . ? S2 P5 C38 C8 -128.09(13) . . . . ? C52 C32 C39 C15 0.2(2) . . . . ? C52 C32 C39 B61 177.58(14) . . . . ? C10 C15 C39 C32 0.2(2) . . . . ? P6 C15 C39 C32 -173.06(11) . . . . ? C10 C15 C39 B61 -177.19(14) . . . . ? P6 C15 C39 B61 9.6(2) . . . . ? C16 B61 C39 C32 -159.38(14) . . . . ? C21 B61 C39 C32 18.0(2) . . . . ? C16 B61 C39 C15 17.9(2) . . . . ? C21 B61 C39 C15 -164.69(14) . . . . ? C49 C29 C40 C38 1.0(3) . . . . ? C8 C38 C40 C29 0.1(3) . . . . ? P5 C38 C40 C29 177.88(15) . . . . ? C48 C41 C42 C60 0.8(3) . . . . ? C34 C37 C43 C45 -0.8(2) . . . . ? C34 C37 C43 C61 179.81(16) . . . . ? C15 C10 C44 C52 0.4(2) . . . . ? C37 C43 C45 C18 1.7(2) . . . . ? C61 C43 C45 C18 -178.91(16) . . . . ? C26 C18 C45 C43 -1.0(2) . . . . ? C47 C18 C45 C43 176.72(15) . . . . ? C53 C28 C46 C22 0.9(3) . . . . ? C14 C22 C46 C28 -1.0(2) . . . . ? C36 C9 C48 C41 -0.3(2) . . . . ? P5 C9 C48 C41 180.00(13) . . . . ? C42 C41 C48 C9 -0.5(3) . . . . ? C40 C29 C49 C50 -1.0(3) . . . . ? C29 C49 C50 C8 0.0(3) . . . . ? C38 C8 C50 C49 1.0(3) . . . . ? B60 C8 C50 C49 -176.24(16) . . . . ? C10 C44 C52 C32 0.0(3) . . . . ? C39 C32 C52 C44 -0.2(3) . . . . ? C46 C28 C53 C11 -0.3(2) . . . . ? C14 C11 C53 C28 -0.2(2) . . . . ? P6 C11 C53 C28 -178.08(12) . . . . ? C21 C35 C56 C58 -0.4(3) . . . . ? C51 C35 C56 C58 178.13(17) . . . . ? C21 C13 C57 C58 0.1(3) . . . . ? C24 C13 C57 C58 -178.94(16) . . . . ? C9 C36 C60 C42 -0.6(3) . . . . ? C41 C42 C60 C36 -0.3(3) . . . . ? C13 C57 C58 C56 -0.3(3) . . . . ? C13 C57 C58 C59 179.01(17) . . . . ? C35 C56 C58 C57 0.5(3) . . . . ? C35 C56 C58 C59 -178.88(17) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.454 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.060