# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Takayuki Kawashima' _publ_contact_author_email TAKAYUKI@CHEM.S.U-TOKYO.AC.JP _publ_section_title ; A novel ylide-stabilized carbene; formation and electron donating ability of amino(sulfur-ylide)carbene ; loop_ _publ_author_name 'Takayuki Kawashima' 'Junji Kobayashi' 'Shinya Nakafuji' 'Atsushi Yatabe' # Attachment 'CCDC-695652.cif' data_asycrhco _database_code_depnum_ccdc_archive 'CCDC 695652' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H27 Cl N O2 Rh S' _exptl_crystal_recrystallization_method Et2O/THF _chemical_melting_point 374 _exptl_crystal_description block _exptl_crystal_colour orange _diffrn_ambient_temperature 120(2) _chemical_formula_weight 591.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.903(5) _cell_length_b 11.130(5) _cell_length_c 13.844(7) _cell_angle_alpha 88.329(19) _cell_angle_beta 77.738(17) _cell_angle_gamma 66.558(14) _cell_volume 1365.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4640 _cell_measurement_theta_min 3.0402 _cell_measurement_theta_max 27.4835 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8523 _exptl_absorpt_correction_T_max 0.8523 _exptl_absorpt_process_details ; Jacobson, R. (1998) Private communication ; _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_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 8442 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4640 _reflns_number_gt 4172 _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^)+(0.0517P)^2^+2.7927P] 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 4640 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0995(4) 0.2147(4) 0.2786(3) 0.0177(8) Uani 1 1 d . . . Rh1 Rh 0.28882(3) 0.18311(3) 0.16910(2) 0.01783(14) Uani 1 1 d . . . Cl1 Cl 0.14794(10) 0.37466(9) 0.09484(7) 0.0183(2) Uani 1 1 d . . . C2 C 0.4558(5) 0.1559(4) 0.0606(3) 0.0240(9) Uani 1 1 d . . . O1 O 0.5481(4) 0.1432(3) -0.0070(2) 0.0361(8) Uani 1 1 d . . . C3 C 0.3918(5) 0.0340(5) 0.2246(3) 0.0334(11) Uani 1 1 d . . . O2 O 0.4579(5) -0.0599(4) 0.2585(3) 0.0614(12) Uani 1 1 d . . . N1 N 0.0782(4) 0.2409(3) 0.3790(2) 0.0205(7) Uani 1 1 d . . . C4 C -0.0663(5) 0.2587(4) 0.4295(3) 0.0247(10) Uani 1 1 d . . . H1 H -0.1052 0.2777 0.4987 0.030 Uiso 1 1 calc R . . C5 C -0.1426(5) 0.2441(4) 0.3625(3) 0.0253(10) Uani 1 1 d . . . H2 H -0.2441 0.2521 0.3752 0.030 Uiso 1 1 calc R . . C6 C -0.0385(5) 0.2145(4) 0.2702(3) 0.0214(9) Uani 1 1 d . . . S1 S -0.06429(11) 0.18406(10) 0.15526(7) 0.0188(2) Uani 1 1 d . . . C7 C 0.1833(4) 0.2610(4) 0.4276(3) 0.0191(9) Uani 1 1 d . . . C8 C 0.2577(5) 0.1665(4) 0.4856(3) 0.0232(9) Uani 1 1 d . . . C9 C 0.3547(5) 0.1914(5) 0.5347(3) 0.0305(11) Uani 1 1 d . . . H3 H 0.4068 0.1268 0.5752 0.037 Uiso 1 1 calc R . . C10 C 0.3776(5) 0.3059(4) 0.5265(3) 0.0262(10) Uani 1 1 d . . . C11 C 0.2985(5) 0.3994(4) 0.4663(3) 0.0226(9) Uani 1 1 d . . . H4 H 0.3138 0.4785 0.4587 0.027 Uiso 1 1 calc R . . C12 C 0.1991(5) 0.3812(4) 0.4175(3) 0.0210(9) Uani 1 1 d . . . C13 C 0.2384(6) 0.0378(4) 0.4975(3) 0.0309(11) Uani 1 1 d . . . H5 H 0.1323 0.0556 0.5259 0.046 Uiso 1 1 calc R . . H6 H 0.3012 -0.0159 0.5416 0.046 Uiso 1 1 calc R . . H7 H 0.2692 -0.0095 0.4326 0.046 Uiso 1 1 calc R . . C14 C 0.4793(6) 0.3326(5) 0.5817(4) 0.0358(12) Uani 1 1 d . . . H8 H 0.5672 0.2511 0.5834 0.054 Uiso 1 1 calc R . . H9 H 0.4240 0.3662 0.6495 0.054 Uiso 1 1 calc R . . H10 H 0.5128 0.3978 0.5481 0.054 Uiso 1 1 calc R . . C15 C 0.1076(5) 0.4864(4) 0.3613(3) 0.0221(9) Uani 1 1 d . . . H11 H 0.1394 0.5596 0.3587 0.033 Uiso 1 1 calc R . . H12 H 0.0008 0.5173 0.3942 0.033 Uiso 1 1 calc R . . H13 H 0.1223 0.4519 0.2938 0.033 Uiso 1 1 calc R . . C16 C -0.0963(5) 0.0360(4) 0.1654(3) 0.0189(9) Uani 1 1 d . . . C17 C -0.0611(5) -0.0426(4) 0.2407(3) 0.0279(10) Uani 1 1 d . . . H14 H -0.0211 -0.0188 0.2900 0.033 Uiso 1 1 calc R . . C18 C -0.0837(5) -0.1590(4) 0.2454(3) 0.0291(10) Uani 1 1 d . . . H15 H -0.0576 -0.2146 0.2978 0.035 Uiso 1 1 calc R . . C19 C -0.1440(5) -0.1945(4) 0.1745(3) 0.0252(10) Uani 1 1 d . . . C20 C -0.1764(5) -0.1114(4) 0.0964(3) 0.0240(9) Uani 1 1 d . . . H16 H -0.2155 -0.1346 0.0463 0.029 Uiso 1 1 calc R . . C21 C -0.1530(5) 0.0021(4) 0.0910(3) 0.0227(9) Uani 1 1 d . . . H17 H -0.1748 0.0569 0.0375 0.027 Uiso 1 1 calc R . . C22 C -0.1767(6) -0.3144(4) 0.1806(4) 0.0365(12) Uani 1 1 d . . . H18 H -0.1427 -0.3628 0.2371 0.055 Uiso 1 1 calc R . . H19 H -0.1235 -0.3702 0.1195 0.055 Uiso 1 1 calc R . . H20 H -0.2855 -0.2890 0.1891 0.055 Uiso 1 1 calc R . . C23 C -0.2458(5) 0.3047(4) 0.1506(3) 0.0203(9) Uani 1 1 d . . . C24 C -0.2473(5) 0.4119(4) 0.0960(3) 0.0281(10) Uani 1 1 d . . . H21 H -0.1556 0.4152 0.0606 0.034 Uiso 1 1 calc R . . C25 C -0.3850(5) 0.5143(5) 0.0941(4) 0.0320(11) Uani 1 1 d . . . H22 H -0.3871 0.5871 0.0560 0.038 Uiso 1 1 calc R . . C26 C -0.5209(5) 0.5114(4) 0.1475(3) 0.0278(10) Uani 1 1 d . . . C27 C -0.5152(5) 0.4007(4) 0.1999(3) 0.0250(10) Uani 1 1 d . . . H23 H -0.6061 0.3956 0.2350 0.030 Uiso 1 1 calc R . . C28 C -0.3797(5) 0.2998(4) 0.2009(3) 0.0261(10) Uani 1 1 d . . . H24 H -0.3775 0.2253 0.2368 0.031 Uiso 1 1 calc R . . C29 C -0.6702(5) 0.6245(5) 0.1477(4) 0.0420(13) Uani 1 1 d . . . H25 H -0.7498 0.5914 0.1556 0.063 Uiso 1 1 calc R . . H26 H -0.6638 0.6671 0.0849 0.063 Uiso 1 1 calc R . . H27 H -0.6938 0.6881 0.2027 0.063 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 0.018(2) 0.018(2) 0.019(2) -0.0041(16) -0.0045(16) -0.0081(17) Rh1 0.0154(2) 0.0216(2) 0.0170(2) -0.00038(14) -0.00241(14) -0.00837(15) Cl1 0.0162(5) 0.0187(5) 0.0196(5) 0.0052(4) -0.0024(4) -0.0076(4) C2 0.027(2) 0.020(2) 0.028(2) 0.0021(18) -0.010(2) -0.0108(19) O1 0.0266(17) 0.042(2) 0.0301(18) -0.0035(15) 0.0087(15) -0.0111(15) C3 0.026(2) 0.042(3) 0.023(2) 0.001(2) 0.0031(19) -0.007(2) O2 0.048(2) 0.059(3) 0.043(2) 0.017(2) 0.0038(19) 0.006(2) N1 0.0241(18) 0.0257(18) 0.0161(17) -0.0002(14) -0.0020(14) -0.0155(16) C4 0.026(2) 0.035(2) 0.014(2) -0.0023(17) 0.0022(17) -0.017(2) C5 0.019(2) 0.037(3) 0.022(2) -0.0054(19) 0.0016(17) -0.016(2) C6 0.019(2) 0.029(2) 0.019(2) -0.0075(17) -0.0028(16) -0.0121(18) S1 0.0168(5) 0.0243(5) 0.0182(5) -0.0014(4) -0.0032(4) -0.0114(4) C7 0.017(2) 0.027(2) 0.0148(19) -0.0008(16) -0.0050(15) -0.0096(18) C8 0.031(2) 0.024(2) 0.019(2) 0.0060(17) -0.0067(17) -0.0157(19) C9 0.033(3) 0.040(3) 0.022(2) 0.003(2) -0.0105(19) -0.017(2) C10 0.025(2) 0.037(3) 0.023(2) -0.0026(19) -0.0068(18) -0.018(2) C11 0.031(2) 0.019(2) 0.021(2) 0.0039(17) -0.0023(18) -0.0157(19) C12 0.023(2) 0.023(2) 0.018(2) -0.0049(16) 0.0017(16) -0.0126(18) C13 0.042(3) 0.029(2) 0.032(2) 0.0057(19) -0.013(2) -0.022(2) C14 0.038(3) 0.045(3) 0.034(3) 0.004(2) -0.019(2) -0.020(2) C15 0.026(2) 0.019(2) 0.022(2) 0.0069(17) -0.0081(17) -0.0088(18) C16 0.020(2) 0.0164(19) 0.019(2) 0.0017(16) -0.0026(16) -0.0080(17) C17 0.029(2) 0.031(2) 0.025(2) -0.0091(19) -0.0056(19) -0.013(2) C18 0.038(3) 0.022(2) 0.026(2) 0.0040(18) -0.010(2) -0.008(2) C19 0.022(2) 0.020(2) 0.031(2) -0.0034(18) -0.0019(18) -0.0074(18) C20 0.024(2) 0.027(2) 0.025(2) -0.0050(18) -0.0048(18) -0.0147(19) C21 0.020(2) 0.028(2) 0.019(2) 0.0006(17) -0.0055(17) -0.0078(18) C22 0.045(3) 0.023(2) 0.043(3) -0.004(2) -0.007(2) -0.016(2) C23 0.019(2) 0.023(2) 0.022(2) -0.0014(17) -0.0041(17) -0.0122(18) C24 0.027(2) 0.033(2) 0.033(2) 0.009(2) -0.0075(19) -0.021(2) C25 0.031(3) 0.029(2) 0.042(3) 0.016(2) -0.012(2) -0.017(2) C26 0.030(2) 0.022(2) 0.035(3) 0.0061(19) -0.011(2) -0.012(2) C27 0.019(2) 0.028(2) 0.030(2) -0.0003(18) -0.0032(18) -0.0118(19) C28 0.024(2) 0.029(2) 0.028(2) -0.0027(18) -0.0007(18) -0.015(2) C29 0.028(3) 0.034(3) 0.061(4) 0.007(2) -0.011(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.382(5) . ? C1 C6 1.397(6) . ? C1 Rh1 2.058(4) . ? Rh1 C3 1.816(5) . ? Rh1 C2 1.912(5) . ? Rh1 Cl1 2.3799(13) . ? C2 O1 1.128(5) . ? C3 O2 1.139(6) . ? N1 C4 1.390(5) . ? N1 C7 1.443(5) . ? C4 C5 1.364(6) . ? C4 H1 0.9500 . ? C5 C6 1.414(6) . ? C5 H2 0.9500 . ? C6 S1 1.727(4) . ? S1 C23 1.778(4) . ? S1 C16 1.794(4) . ? C7 C8 1.371(6) . ? C7 C12 1.407(6) . ? C8 C9 1.401(6) . ? C8 C13 1.519(6) . ? C9 C10 1.377(6) . ? C9 H3 0.9500 . ? C10 C11 1.404(6) . ? C10 C14 1.504(6) . ? C11 C12 1.384(6) . ? C11 H4 0.9500 . ? C12 C15 1.483(6) . ? C13 H5 0.9800 . ? C13 H6 0.9800 . ? C13 H7 0.9800 . ? C14 H8 0.9800 . ? C14 H9 0.9800 . ? C14 H10 0.9800 . ? C15 H11 0.9800 . ? C15 H12 0.9800 . ? C15 H13 0.9800 . ? C16 C17 1.353(6) . ? C16 C21 1.398(6) . ? C17 C18 1.397(6) . ? C17 H14 0.9500 . ? C18 C19 1.391(6) . ? C18 H15 0.9500 . ? C19 C20 1.407(6) . ? C19 C22 1.490(6) . ? C20 C21 1.370(6) . ? C20 H16 0.9500 . ? C21 H17 0.9500 . ? C22 H18 0.9800 . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? C23 C28 1.381(6) . ? C23 C24 1.391(6) . ? C24 C25 1.392(6) . ? C24 H21 0.9500 . ? C25 C26 1.403(6) . ? C25 H22 0.9500 . ? C26 C27 1.400(6) . ? C26 C29 1.512(6) . ? C27 C28 1.368(6) . ? C27 H23 0.9500 . ? C28 H24 0.9500 . ? C29 H25 0.9800 . ? C29 H26 0.9800 . ? C29 H27 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 N1 C1 C6 102.9(3) . . ? N1 C1 Rh1 128.3(3) . . ? C6 C1 Rh1 128.7(3) . . ? C3 Rh1 C2 92.81(19) . . ? C3 Rh1 C1 89.87(18) . . ? C2 Rh1 C1 175.88(16) . . ? C3 Rh1 Cl1 177.80(17) . . ? C2 Rh1 Cl1 87.96(13) . . ? C1 Rh1 Cl1 89.24(12) . . ? O1 C2 Rh1 175.8(4) . . ? O2 C3 Rh1 179.1(4) . . ? C1 N1 C4 111.7(3) . . ? C1 N1 C7 126.1(3) . . ? C4 N1 C7 122.0(3) . . ? C5 C4 N1 108.3(4) . . ? C5 C4 H1 125.9 . . ? N1 C4 H1 125.9 . . ? C4 C5 C6 105.3(4) . . ? C4 C5 H2 127.4 . . ? C6 C5 H2 127.4 . . ? C1 C6 C5 111.8(4) . . ? C1 C6 S1 119.6(3) . . ? C5 C6 S1 128.6(3) . . ? C6 S1 C23 104.4(2) . . ? C6 S1 C16 105.0(2) . . ? C23 S1 C16 102.36(19) . . ? C8 C7 C12 122.6(4) . . ? C8 C7 N1 119.3(4) . . ? C12 C7 N1 118.0(4) . . ? C7 C8 C9 117.8(4) . . ? C7 C8 C13 122.3(4) . . ? C9 C8 C13 119.9(4) . . ? C10 C9 C8 122.6(4) . . ? C10 C9 H3 118.7 . . ? C8 C9 H3 118.7 . . ? C9 C10 C11 117.2(4) . . ? C9 C10 C14 122.0(4) . . ? C11 C10 C14 120.8(4) . . ? C12 C11 C10 122.7(4) . . ? C12 C11 H4 118.7 . . ? C10 C11 H4 118.7 . . ? C11 C12 C7 117.0(4) . . ? C11 C12 C15 121.4(4) . . ? C7 C12 C15 121.5(4) . . ? C8 C13 H5 109.5 . . ? C8 C13 H6 109.5 . . ? H5 C13 H6 109.5 . . ? C8 C13 H7 109.5 . . ? H5 C13 H7 109.5 . . ? H6 C13 H7 109.5 . . ? C10 C14 H8 109.5 . . ? C10 C14 H9 109.5 . . ? H8 C14 H9 109.5 . . ? C10 C14 H10 109.5 . . ? H8 C14 H10 109.5 . . ? H9 C14 H10 109.5 . . ? C12 C15 H11 109.5 . . ? C12 C15 H12 109.5 . . ? H11 C15 H12 109.5 . . ? C12 C15 H13 109.5 . . ? H11 C15 H13 109.5 . . ? H12 C15 H13 109.5 . . ? C17 C16 C21 121.3(4) . . ? C17 C16 S1 120.9(3) . . ? C21 C16 S1 117.8(3) . . ? C16 C17 C18 119.7(4) . . ? C16 C17 H14 120.1 . . ? C18 C17 H14 120.1 . . ? C17 C18 C19 120.9(4) . . ? C17 C18 H15 119.6 . . ? C19 C18 H15 119.6 . . ? C18 C19 C20 117.7(4) . . ? C18 C19 C22 122.0(4) . . ? C20 C19 C22 120.3(4) . . ? C21 C20 C19 121.6(4) . . ? C21 C20 H16 119.2 . . ? C19 C20 H16 119.2 . . ? C20 C21 C16 118.9(4) . . ? C20 C21 H17 120.6 . . ? C16 C21 H17 120.6 . . ? C19 C22 H18 109.5 . . ? C19 C22 H19 109.5 . . ? H18 C22 H19 109.5 . . ? C19 C22 H20 109.5 . . ? H18 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C28 C23 C24 120.2(4) . . ? C28 C23 S1 124.1(3) . . ? C24 C23 S1 115.7(3) . . ? C25 C24 C23 119.0(4) . . ? C25 C24 H21 120.5 . . ? C23 C24 H21 120.5 . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H22 119.5 . . ? C26 C25 H22 119.5 . . ? C27 C26 C25 118.4(4) . . ? C27 C26 C29 120.7(4) . . ? C25 C26 C29 121.0(4) . . ? C28 C27 C26 120.4(4) . . ? C28 C27 H23 119.8 . . ? C26 C27 H23 119.8 . . ? C23 C28 C27 121.0(4) . . ? C23 C28 H24 119.5 . . ? C27 C28 H24 119.5 . . ? C26 C29 H25 109.5 . . ? C26 C29 H26 109.5 . . ? H25 C29 H26 109.5 . . ? C26 C29 H27 109.5 . . ? H25 C29 H27 109.5 . . ? H26 C29 H27 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 N1 C1 Rh1 C3 65.1(4) . . . . ? C6 C1 Rh1 C3 -114.6(4) . . . . ? N1 C1 Rh1 C2 -164(2) . . . . ? C6 C1 Rh1 C2 16(2) . . . . ? N1 C1 Rh1 Cl1 -116.9(3) . . . . ? C6 C1 Rh1 Cl1 63.4(4) . . . . ? C3 Rh1 C2 O1 146(5) . . . . ? C1 Rh1 C2 O1 16(7) . . . . ? Cl1 Rh1 C2 O1 -32(5) . . . . ? C2 Rh1 C3 O2 -3(36) . . . . ? C1 Rh1 C3 O2 174(100) . . . . ? Cl1 Rh1 C3 O2 108(35) . . . . ? C6 C1 N1 C4 -1.2(4) . . . . ? Rh1 C1 N1 C4 179.0(3) . . . . ? C6 C1 N1 C7 -175.4(4) . . . . ? Rh1 C1 N1 C7 4.8(6) . . . . ? C1 N1 C4 C5 0.1(5) . . . . ? C7 N1 C4 C5 174.6(4) . . . . ? N1 C4 C5 C6 1.1(5) . . . . ? N1 C1 C6 C5 1.9(5) . . . . ? Rh1 C1 C6 C5 -178.3(3) . . . . ? N1 C1 C6 S1 -179.6(3) . . . . ? Rh1 C1 C6 S1 0.2(5) . . . . ? C4 C5 C6 C1 -1.9(5) . . . . ? C4 C5 C6 S1 179.7(4) . . . . ? C1 C6 S1 C23 -135.3(3) . . . . ? C5 C6 S1 C23 43.0(5) . . . . ? C1 C6 S1 C16 117.4(4) . . . . ? C5 C6 S1 C16 -64.3(4) . . . . ? C1 N1 C7 C8 -108.6(5) . . . . ? C4 N1 C7 C8 77.8(5) . . . . ? C1 N1 C7 C12 74.7(5) . . . . ? C4 N1 C7 C12 -98.9(5) . . . . ? C12 C7 C8 C9 -1.2(6) . . . . ? N1 C7 C8 C9 -177.7(4) . . . . ? C12 C7 C8 C13 179.1(4) . . . . ? N1 C7 C8 C13 2.6(6) . . . . ? C7 C8 C9 C10 -0.1(7) . . . . ? C13 C8 C9 C10 179.6(4) . . . . ? C8 C9 C10 C11 0.2(7) . . . . ? C8 C9 C10 C14 178.5(4) . . . . ? C9 C10 C11 C12 1.0(6) . . . . ? C14 C10 C11 C12 -177.3(4) . . . . ? C10 C11 C12 C7 -2.2(6) . . . . ? C10 C11 C12 C15 174.8(4) . . . . ? C8 C7 C12 C11 2.3(6) . . . . ? N1 C7 C12 C11 178.8(3) . . . . ? C8 C7 C12 C15 -174.7(4) . . . . ? N1 C7 C12 C15 1.9(5) . . . . ? C6 S1 C16 C17 -16.1(4) . . . . ? C23 S1 C16 C17 -124.9(4) . . . . ? C6 S1 C16 C21 166.5(3) . . . . ? C23 S1 C16 C21 57.7(4) . . . . ? C21 C16 C17 C18 -1.1(6) . . . . ? S1 C16 C17 C18 -178.4(3) . . . . ? C16 C17 C18 C19 -0.8(7) . . . . ? C17 C18 C19 C20 2.0(6) . . . . ? C17 C18 C19 C22 -176.8(4) . . . . ? C18 C19 C20 C21 -1.4(6) . . . . ? C22 C19 C20 C21 177.5(4) . . . . ? C19 C20 C21 C16 -0.4(6) . . . . ? C17 C16 C21 C20 1.7(6) . . . . ? S1 C16 C21 C20 179.1(3) . . . . ? C6 S1 C23 C28 -75.1(4) . . . . ? C16 S1 C23 C28 34.1(4) . . . . ? C6 S1 C23 C24 101.6(4) . . . . ? C16 S1 C23 C24 -149.2(3) . . . . ? C28 C23 C24 C25 0.8(7) . . . . ? S1 C23 C24 C25 -176.0(3) . . . . ? C23 C24 C25 C26 1.1(7) . . . . ? C24 C25 C26 C27 -2.4(7) . . . . ? C24 C25 C26 C29 178.2(5) . . . . ? C25 C26 C27 C28 1.8(7) . . . . ? C29 C26 C27 C28 -178.8(4) . . . . ? C24 C23 C28 C27 -1.4(6) . . . . ? S1 C23 C28 C27 175.2(3) . . . . ? C26 C27 C28 C23 0.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.948 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.107 # Attachment 'CCDC-695653.cif' data_s+isomer _database_code_depnum_ccdc_archive 'CCDC 695653' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 B N O S' _chemical_properties_physical hygroscopic _exptl_crystal_recrystallization_method THF/Methanol _chemical_melting_point 408 _exptl_crystal_description Block _exptl_crystal_colour Colorless _diffrn_ambient_temperature 120(2) _chemical_formula_weight 749.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_int_tables_number 61 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.673(5) _cell_length_b 23.053(7) _cell_length_c 19.701(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8481(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7364 _cell_measurement_theta_min 3.0402 _cell_measurement_theta_max 27.4835 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9773 _exptl_absorpt_correction_T_max 0.9773 _exptl_absorpt_process_details ; Jacobson, R. (1998) Private communication ; _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_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 52084 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7364 _reflns_number_gt 5971 _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^)+(0.0674P)^2^+4.3119P] 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 7364 _refine_ls_number_parameters 512 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.09166(10) 0.14153(8) 0.55828(10) 0.0210(4) Uani 1 1 d . . . H1 H 0.1040 0.1744 0.5317 0.025 Uiso 1 1 calc R . . N1 N 0.06717(9) 0.09000(7) 0.53470(8) 0.0223(4) Uani 1 1 d . . . C2 C 0.05535(11) 0.05307(9) 0.58862(10) 0.0252(5) Uani 1 1 d . . . H2 H 0.0382 0.0144 0.5853 0.030 Uiso 1 1 calc R . . C3 C 0.07216(11) 0.08084(9) 0.64722(10) 0.0251(5) Uani 1 1 d . . . H3 H 0.0691 0.0658 0.6920 0.030 Uiso 1 1 calc R . . C4 C 0.09531(10) 0.13734(8) 0.62759(10) 0.0211(4) Uani 1 1 d . . . S1 S 0.12278(2) 0.19695(2) 0.67415(2) 0.02032(14) Uani 1 1 d . . . C5 C 0.19991(10) 0.17389(9) 0.72063(10) 0.0225(4) Uani 1 1 d . . . C6 C 0.24133(11) 0.12837(9) 0.69748(11) 0.0262(5) Uani 1 1 d . . . H4 H 0.2270 0.1063 0.6591 0.031 Uiso 1 1 calc R . . C7 C 0.30452(11) 0.11561(10) 0.73176(11) 0.0293(5) Uani 1 1 d . . . H5 H 0.3337 0.0845 0.7163 0.035 Uiso 1 1 calc R . . C8 C 0.32581(11) 0.14748(10) 0.78825(11) 0.0290(5) Uani 1 1 d . . . C9 C 0.28324(11) 0.19372(9) 0.80927(11) 0.0290(5) Uani 1 1 d . . . H6 H 0.2974 0.2162 0.8473 0.035 Uiso 1 1 calc R . . C10 C 0.22049(11) 0.20731(9) 0.77538(10) 0.0254(5) Uani 1 1 d . . . H7 H 0.1920 0.2392 0.7896 0.031 Uiso 1 1 calc R . . C11 C 0.39232(12) 0.13144(11) 0.82713(13) 0.0391(6) Uani 1 1 d . . . H8 H 0.3791 0.1081 0.8668 0.059 Uiso 1 1 calc R . . H9 H 0.4168 0.1668 0.8421 0.059 Uiso 1 1 calc R . . H10 H 0.4243 0.1089 0.7978 0.059 Uiso 1 1 calc R . . C12 C 0.05534(10) 0.20824(9) 0.73658(10) 0.0213(4) Uani 1 1 d . . . C13 C 0.01136(11) 0.25559(9) 0.72474(10) 0.0252(5) Uani 1 1 d . . . H11 H 0.0205 0.2811 0.6879 0.030 Uiso 1 1 calc R . . C14 C -0.04644(11) 0.26495(9) 0.76785(11) 0.0281(5) Uani 1 1 d . . . H12 H -0.0770 0.2972 0.7602 0.034 Uiso 1 1 calc R . . C15 C -0.06016(10) 0.22791(10) 0.82187(10) 0.0273(5) Uani 1 1 d . . . C16 C -0.01440(11) 0.18115(10) 0.83255(10) 0.0289(5) Uani 1 1 d . . . H13 H -0.0232 0.1557 0.8695 0.035 Uiso 1 1 calc R . . C17 C 0.04379(11) 0.17088(9) 0.79051(10) 0.0251(5) Uani 1 1 d . . . H14 H 0.0749 0.1390 0.7985 0.030 Uiso 1 1 calc R . . C18 C -0.12380(11) 0.23740(11) 0.86717(12) 0.0377(6) Uani 1 1 d . . . H15 H -0.1437 0.2761 0.8589 0.057 Uiso 1 1 calc R . . H16 H -0.1089 0.2343 0.9147 0.057 Uiso 1 1 calc R . . H17 H -0.1603 0.2080 0.8574 0.057 Uiso 1 1 calc R . . C19 C 0.05968(11) 0.07641(8) 0.46368(10) 0.0237(5) Uani 1 1 d . . . C20 C 0.11282(11) 0.04316(9) 0.43268(11) 0.0271(5) Uani 1 1 d . . . C21 C 0.10656(13) 0.03351(10) 0.36344(11) 0.0343(5) Uani 1 1 d . . . H18 H 0.1425 0.0114 0.3411 0.041 Uiso 1 1 calc R . . C22 C 0.04965(14) 0.05499(10) 0.32574(11) 0.0371(6) Uani 1 1 d . . . C23 C -0.00216(13) 0.08707(10) 0.35881(12) 0.0373(6) Uani 1 1 d . . . H19 H -0.0414 0.1018 0.3334 0.045 Uiso 1 1 calc R . . C24 C 0.00128(12) 0.09861(9) 0.42834(11) 0.0300(5) Uani 1 1 d . . . C25 C 0.17490(13) 0.01960(11) 0.47215(12) 0.0389(6) Uani 1 1 d . . . H20 H 0.1937 0.0498 0.5022 0.058 Uiso 1 1 calc R . . H21 H 0.2125 0.0071 0.4407 0.058 Uiso 1 1 calc R . . H22 H 0.1591 -0.0136 0.4994 0.058 Uiso 1 1 calc R . . C26 C 0.04471(18) 0.04221(14) 0.25085(13) 0.0622(9) Uani 1 1 d . . . H23 H 0.0311 0.0015 0.2442 0.093 Uiso 1 1 calc R . . H24 H 0.0913 0.0493 0.2295 0.093 Uiso 1 1 calc R . . H25 H 0.0086 0.0674 0.2302 0.093 Uiso 1 1 calc R . . C27 C -0.05535(13) 0.13378(11) 0.46337(15) 0.0460(7) Uani 1 1 d . . . H26 H -0.0655 0.1168 0.5080 0.069 Uiso 1 1 calc R . . H27 H -0.0991 0.1338 0.4359 0.069 Uiso 1 1 calc R . . H28 H -0.0384 0.1737 0.4691 0.069 Uiso 1 1 calc R . . B1 B 0.12962(12) 0.34411(10) 0.52584(11) 0.0210(5) Uani 1 1 d . . . C28 C 0.16251(10) 0.28307(8) 0.49580(10) 0.0206(4) Uani 1 1 d . . . C29 C 0.13292(11) 0.25732(9) 0.43735(10) 0.0232(4) Uani 1 1 d . . . H29 H 0.0942 0.2765 0.4155 0.028 Uiso 1 1 calc R . . C30 C 0.15732(11) 0.20543(9) 0.41004(10) 0.0262(5) Uani 1 1 d . . . H30 H 0.1345 0.1892 0.3714 0.031 Uiso 1 1 calc R . . C31 C 0.21529(11) 0.17743(9) 0.43956(12) 0.0301(5) Uani 1 1 d . . . H31 H 0.2329 0.1422 0.4210 0.036 Uiso 1 1 calc R . . C32 C 0.24687(12) 0.20149(9) 0.49611(12) 0.0315(5) Uani 1 1 d . . . H32 H 0.2870 0.1830 0.5163 0.038 Uiso 1 1 calc R . . C33 C 0.22039(10) 0.25288(9) 0.52396(11) 0.0258(5) Uani 1 1 d . . . H33 H 0.2425 0.2680 0.5636 0.031 Uiso 1 1 calc R . . C34 C 0.04770(10) 0.33404(8) 0.55548(10) 0.0206(4) Uani 1 1 d . . . C35 C 0.01494(11) 0.37744(9) 0.59516(11) 0.0256(5) Uani 1 1 d . . . H34 H 0.0419 0.4110 0.6066 0.031 Uiso 1 1 calc R . . C36 C -0.05485(11) 0.37328(10) 0.61823(11) 0.0298(5) Uani 1 1 d . . . H35 H -0.0747 0.4038 0.6446 0.036 Uiso 1 1 calc R . . C37 C -0.09583(11) 0.32514(9) 0.60317(11) 0.0295(5) Uani 1 1 d . . . H36 H -0.1436 0.3219 0.6194 0.035 Uiso 1 1 calc R . . C38 C -0.06604(11) 0.28173(9) 0.56401(11) 0.0279(5) Uani 1 1 d . . . H37 H -0.0936 0.2485 0.5527 0.033 Uiso 1 1 calc R . . C39 C 0.00412(10) 0.28647(9) 0.54097(10) 0.0230(4) Uani 1 1 d . . . H38 H 0.0232 0.2559 0.5141 0.028 Uiso 1 1 calc R . . C40 C 0.18089(10) 0.36937(9) 0.58737(10) 0.0228(4) Uani 1 1 d . . . C41 C 0.23523(12) 0.40974(11) 0.57767(12) 0.0392(6) Uani 1 1 d . . . H39 H 0.2423 0.4249 0.5334 0.047 Uiso 1 1 calc R . . C42 C 0.27976(14) 0.42904(13) 0.62961(13) 0.0480(7) Uani 1 1 d . . . H40 H 0.3164 0.4564 0.6200 0.058 Uiso 1 1 calc R . . C43 C 0.27115(13) 0.40894(11) 0.69456(12) 0.0414(6) Uani 1 1 d . . . H41 H 0.3009 0.4225 0.7304 0.050 Uiso 1 1 calc R . . C44 C 0.21821(13) 0.36854(11) 0.70653(12) 0.0389(6) Uani 1 1 d . . . H42 H 0.2115 0.3536 0.7510 0.047 Uiso 1 1 calc R . . C45 C 0.17492(12) 0.34978(10) 0.65419(11) 0.0324(5) Uani 1 1 d . . . H43 H 0.1390 0.3219 0.6642 0.039 Uiso 1 1 calc R . . C46 C 0.12607(10) 0.39056(8) 0.46196(10) 0.0208(4) Uani 1 1 d . . . C47 C 0.18429(11) 0.39721(9) 0.41753(10) 0.0246(5) Uani 1 1 d . . . H44 H 0.2257 0.3740 0.4246 0.030 Uiso 1 1 calc R . . C48 C 0.18406(11) 0.43595(9) 0.36399(10) 0.0276(5) Uani 1 1 d . . . H45 H 0.2251 0.4393 0.3357 0.033 Uiso 1 1 calc R . . C49 C 0.12423(12) 0.47003(9) 0.35130(11) 0.0316(5) Uani 1 1 d . . . H46 H 0.1238 0.4968 0.3146 0.038 Uiso 1 1 calc R . . C50 C 0.06549(13) 0.46430(10) 0.39298(12) 0.0340(5) Uani 1 1 d . . . H47 H 0.0238 0.4868 0.3846 0.041 Uiso 1 1 calc R . . C51 C 0.06683(11) 0.42564(9) 0.44728(11) 0.0271(5) Uani 1 1 d . . . H48 H 0.0258 0.4230 0.4756 0.033 Uiso 1 1 calc R . . C52 C 0.36360(17) 0.44747(16) 0.0499(2) 0.0707(9) Uani 1 1 d . . . H49 H 0.3901 0.4704 0.0165 0.106 Uiso 1 1 calc R . . H50 H 0.3142 0.4421 0.0343 0.106 Uiso 1 1 calc R . . H51 H 0.3866 0.4095 0.0553 0.106 Uiso 1 1 calc R . . O1 O 0.3633(3) 0.47664(16) 0.11241(17) 0.1440(15) Uani 1 1 d . . . H52 H 0.3515 0.5114 0.1063 0.216 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 0.0217(10) 0.0189(10) 0.0223(10) -0.0007(8) -0.0003(8) 0.0002(8) N1 0.0269(9) 0.0196(9) 0.0205(9) -0.0015(7) -0.0027(7) 0.0006(7) C2 0.0301(11) 0.0202(10) 0.0253(11) 0.0025(8) 0.0005(9) -0.0040(8) C3 0.0283(11) 0.0256(11) 0.0214(10) 0.0031(8) 0.0017(9) -0.0031(9) C4 0.0213(10) 0.0222(10) 0.0197(10) -0.0027(8) -0.0012(8) -0.0001(8) S1 0.0202(3) 0.0227(3) 0.0180(3) -0.00229(19) 0.00153(19) -0.00169(19) C5 0.0195(10) 0.0277(11) 0.0202(10) 0.0016(8) 0.0021(8) -0.0036(8) C6 0.0229(11) 0.0314(11) 0.0242(11) -0.0022(9) 0.0035(9) -0.0013(9) C7 0.0219(11) 0.0329(12) 0.0330(12) 0.0042(10) 0.0055(9) 0.0018(9) C8 0.0211(11) 0.0352(12) 0.0305(12) 0.0087(10) -0.0002(9) -0.0063(9) C9 0.0278(12) 0.0327(12) 0.0265(11) 0.0004(9) -0.0030(9) -0.0094(9) C10 0.0229(11) 0.0284(11) 0.0250(11) -0.0016(9) 0.0015(9) -0.0029(9) C11 0.0287(12) 0.0452(14) 0.0433(14) 0.0112(12) -0.0083(10) -0.0038(10) C12 0.0185(10) 0.0261(10) 0.0194(10) -0.0049(8) -0.0009(8) -0.0028(8) C13 0.0259(11) 0.0245(11) 0.0252(11) -0.0027(9) 0.0008(9) -0.0021(9) C14 0.0230(11) 0.0308(12) 0.0307(12) -0.0073(9) 0.0004(9) 0.0026(9) C15 0.0193(11) 0.0394(13) 0.0231(11) -0.0105(9) -0.0001(8) -0.0042(9) C16 0.0249(11) 0.0413(13) 0.0206(11) 0.0014(9) 0.0017(9) -0.0063(10) C17 0.0227(11) 0.0314(12) 0.0212(10) 0.0004(9) -0.0016(8) -0.0006(9) C18 0.0273(12) 0.0544(16) 0.0316(13) -0.0132(11) 0.0059(10) -0.0048(11) C19 0.0339(12) 0.0172(10) 0.0200(10) -0.0003(8) -0.0051(9) -0.0037(9) C20 0.0327(12) 0.0238(11) 0.0247(11) -0.0008(9) 0.0010(9) -0.0017(9) C21 0.0475(14) 0.0304(12) 0.0251(12) -0.0038(10) 0.0053(10) -0.0076(10) C22 0.0564(16) 0.0329(13) 0.0220(11) 0.0061(10) -0.0055(11) -0.0191(11) C23 0.0491(15) 0.0277(12) 0.0351(13) 0.0095(10) -0.0195(11) -0.0107(11) C24 0.0361(12) 0.0182(10) 0.0356(12) 0.0033(9) -0.0115(10) -0.0038(9) C25 0.0372(13) 0.0433(14) 0.0363(13) -0.0042(11) -0.0019(10) 0.0114(11) C26 0.091(2) 0.073(2) 0.0228(13) 0.0050(13) -0.0083(14) -0.0342(18) C27 0.0411(15) 0.0360(14) 0.0609(17) -0.0090(12) -0.0203(13) 0.0116(11) B1 0.0212(12) 0.0199(11) 0.0219(11) -0.0015(9) -0.0003(9) -0.0014(9) C28 0.0194(10) 0.0212(10) 0.0213(10) 0.0035(8) 0.0036(8) -0.0026(8) C29 0.0258(11) 0.0236(10) 0.0203(10) 0.0025(8) 0.0007(8) 0.0005(8) C30 0.0328(12) 0.0253(11) 0.0206(10) -0.0011(8) 0.0047(9) -0.0044(9) C31 0.0282(12) 0.0234(11) 0.0388(13) -0.0042(9) 0.0126(10) 0.0014(9) C32 0.0212(11) 0.0296(11) 0.0439(14) -0.0025(10) -0.0001(10) 0.0055(9) C33 0.0201(10) 0.0278(11) 0.0297(11) -0.0009(9) -0.0023(9) -0.0001(9) C34 0.0225(10) 0.0202(10) 0.0190(10) 0.0015(8) -0.0027(8) 0.0011(8) C35 0.0263(11) 0.0212(10) 0.0294(11) -0.0026(9) 0.0020(9) -0.0021(8) C36 0.0269(12) 0.0291(12) 0.0333(12) -0.0028(10) 0.0045(9) 0.0056(9) C37 0.0189(11) 0.0338(12) 0.0359(12) 0.0025(10) 0.0034(9) 0.0006(9) C38 0.0243(11) 0.0265(11) 0.0328(12) 0.0010(9) -0.0008(9) -0.0056(9) C39 0.0245(11) 0.0210(10) 0.0235(10) -0.0001(8) -0.0006(8) 0.0006(8) C40 0.0209(10) 0.0221(10) 0.0254(11) -0.0033(8) 0.0000(8) 0.0018(8) C41 0.0377(14) 0.0537(15) 0.0263(12) 0.0024(11) -0.0012(10) -0.0219(12) C42 0.0403(14) 0.0683(18) 0.0355(14) -0.0010(13) -0.0044(11) -0.0279(13) C43 0.0404(14) 0.0521(16) 0.0317(13) -0.0066(11) -0.0115(11) -0.0131(12) C44 0.0465(15) 0.0441(14) 0.0260(12) 0.0036(10) -0.0059(10) -0.0088(12) C45 0.0365(13) 0.0314(12) 0.0295(12) 0.0015(10) -0.0048(10) -0.0112(10) C46 0.0237(10) 0.0178(10) 0.0210(10) -0.0041(8) -0.0022(8) -0.0024(8) C47 0.0254(11) 0.0233(10) 0.0251(11) -0.0023(8) -0.0007(8) 0.0022(8) C48 0.0323(12) 0.0266(11) 0.0240(11) -0.0023(9) 0.0041(9) -0.0043(9) C49 0.0449(14) 0.0245(11) 0.0253(11) 0.0043(9) 0.0015(10) 0.0005(10) C50 0.0388(13) 0.0280(12) 0.0351(13) 0.0061(10) -0.0001(10) 0.0086(10) C51 0.0257(11) 0.0246(11) 0.0312(12) 0.0002(9) 0.0019(9) 0.0029(9) C52 0.0530(19) 0.075(2) 0.084(3) 0.014(2) -0.0080(17) -0.0029(17) O1 0.220(4) 0.118(3) 0.095(2) 0.050(2) 0.032(2) 0.069(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.355(2) . ? C1 C4 1.371(3) . ? C1 H1 0.9500 . ? N1 C2 1.379(3) . ? N1 C19 1.441(3) . ? C2 C3 1.357(3) . ? C2 H2 0.9500 . ? C3 C4 1.426(3) . ? C3 H3 0.9500 . ? C4 S1 1.730(2) . ? S1 C12 1.780(2) . ? S1 C5 1.788(2) . ? C5 C10 1.380(3) . ? C5 C6 1.381(3) . ? C6 C7 1.391(3) . ? C6 H4 0.9500 . ? C7 C8 1.392(3) . ? C7 H5 0.9500 . ? C8 C9 1.393(3) . ? C8 C11 1.505(3) . ? C9 C10 1.384(3) . ? C9 H6 0.9500 . ? C10 H7 0.9500 . ? C11 H8 0.9800 . ? C11 H9 0.9800 . ? C11 H10 0.9800 . ? C12 C17 1.385(3) . ? C12 C13 1.386(3) . ? C13 C14 1.390(3) . ? C13 H11 0.9500 . ? C14 C15 1.388(3) . ? C14 H12 0.9500 . ? C15 C16 1.391(3) . ? C15 C18 1.502(3) . ? C16 C17 1.387(3) . ? C16 H13 0.9500 . ? C17 H14 0.9500 . ? C18 H15 0.9800 . ? C18 H16 0.9800 . ? C18 H17 0.9800 . ? C19 C24 1.391(3) . ? C19 C20 1.395(3) . ? C20 C21 1.387(3) . ? C20 C25 1.498(3) . ? C21 C22 1.388(3) . ? C21 H18 0.9500 . ? C22 C23 1.381(4) . ? C22 C26 1.507(3) . ? C23 C24 1.397(3) . ? C23 H19 0.9500 . ? C24 C27 1.501(3) . ? C25 H20 0.9800 . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C26 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C27 H26 0.9800 . ? C27 H27 0.9800 . ? C27 H28 0.9800 . ? B1 C28 1.645(3) . ? B1 C40 1.651(3) . ? B1 C46 1.654(3) . ? B1 C34 1.654(3) . ? C28 C33 1.400(3) . ? C28 C29 1.409(3) . ? C29 C30 1.389(3) . ? C29 H29 0.9500 . ? C30 C31 1.388(3) . ? C30 H30 0.9500 . ? C31 C32 1.377(3) . ? C31 H31 0.9500 . ? C32 C33 1.396(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.395(3) . ? C34 C35 1.409(3) . ? C35 C36 1.384(3) . ? C35 H34 0.9500 . ? C36 C37 1.380(3) . ? C36 H35 0.9500 . ? C37 C38 1.381(3) . ? C37 H36 0.9500 . ? C38 C39 1.391(3) . ? C38 H37 0.9500 . ? C39 H38 0.9500 . ? C40 C41 1.390(3) . ? C40 C45 1.396(3) . ? C41 C42 1.392(3) . ? C41 H39 0.9500 . ? C42 C43 1.370(3) . ? C42 H40 0.9500 . ? C43 C44 1.379(3) . ? C43 H41 0.9500 . ? C44 C45 1.380(3) . ? C44 H42 0.9500 . ? C45 H43 0.9500 . ? C46 C51 1.401(3) . ? C46 C47 1.404(3) . ? C47 C48 1.382(3) . ? C47 H44 0.9500 . ? C48 C49 1.389(3) . ? C48 H45 0.9500 . ? C49 C50 1.376(3) . ? C49 H46 0.9500 . ? C50 C51 1.393(3) . ? C50 H47 0.9500 . ? C51 H48 0.9500 . ? C52 O1 1.403(5) . ? C52 H49 0.9800 . ? C52 H50 0.9800 . ? C52 H51 0.9800 . ? O1 H52 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C4 107.24(17) . . ? N1 C1 H1 126.4 . . ? C4 C1 H1 126.4 . . ? C1 N1 C2 109.34(16) . . ? C1 N1 C19 123.80(17) . . ? C2 N1 C19 126.75(16) . . ? C3 C2 N1 109.09(18) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 C4 105.68(18) . . ? C2 C3 H3 127.2 . . ? C4 C3 H3 127.2 . . ? C1 C4 C3 108.64(17) . . ? C1 C4 S1 119.14(15) . . ? C3 C4 S1 132.20(15) . . ? C4 S1 C12 105.83(9) . . ? C4 S1 C5 105.92(10) . . ? C12 S1 C5 105.05(9) . . ? C10 C5 C6 121.75(19) . . ? C10 C5 S1 117.31(16) . . ? C6 C5 S1 120.53(16) . . ? C5 C6 C7 118.4(2) . . ? C5 C6 H4 120.8 . . ? C7 C6 H4 120.8 . . ? C6 C7 C8 121.3(2) . . ? C6 C7 H5 119.4 . . ? C8 C7 H5 119.4 . . ? C7 C8 C9 118.61(19) . . ? C7 C8 C11 120.9(2) . . ? C9 C8 C11 120.5(2) . . ? C10 C9 C8 120.9(2) . . ? C10 C9 H6 119.6 . . ? C8 C9 H6 119.6 . . ? C5 C10 C9 119.1(2) . . ? C5 C10 H7 120.4 . . ? C9 C10 H7 120.4 . . ? C8 C11 H8 109.5 . . ? C8 C11 H9 109.5 . . ? H8 C11 H9 109.5 . . ? C8 C11 H10 109.5 . . ? H8 C11 H10 109.5 . . ? H9 C11 H10 109.5 . . ? C17 C12 C13 121.79(18) . . ? C17 C12 S1 123.35(16) . . ? C13 C12 S1 114.72(15) . . ? C12 C13 C14 118.6(2) . . ? C12 C13 H11 120.7 . . ? C14 C13 H11 120.7 . . ? C15 C14 C13 121.1(2) . . ? C15 C14 H12 119.5 . . ? C13 C14 H12 119.5 . . ? C14 C15 C16 118.62(19) . . ? C14 C15 C18 120.8(2) . . ? C16 C15 C18 120.6(2) . . ? C17 C16 C15 121.5(2) . . ? C17 C16 H13 119.2 . . ? C15 C16 H13 119.2 . . ? C12 C17 C16 118.3(2) . . ? C12 C17 H14 120.8 . . ? C16 C17 H14 120.8 . . ? C15 C18 H15 109.5 . . ? C15 C18 H16 109.5 . . ? H15 C18 H16 109.5 . . ? C15 C18 H17 109.5 . . ? H15 C18 H17 109.5 . . ? H16 C18 H17 109.5 . . ? C24 C19 C20 122.73(19) . . ? C24 C19 N1 118.83(19) . . ? C20 C19 N1 118.40(18) . . ? C21 C20 C19 117.3(2) . . ? C21 C20 C25 121.2(2) . . ? C19 C20 C25 121.51(19) . . ? C20 C21 C22 122.2(2) . . ? C20 C21 H18 118.9 . . ? C22 C21 H18 118.9 . . ? C23 C22 C21 118.4(2) . . ? C23 C22 C26 121.6(2) . . ? C21 C22 C26 120.1(3) . . ? C22 C23 C24 122.2(2) . . ? C22 C23 H19 118.9 . . ? C24 C23 H19 118.9 . . ? C19 C24 C23 117.2(2) . . ? C19 C24 C27 121.4(2) . . ? C23 C24 C27 121.4(2) . . ? C20 C25 H20 109.5 . . ? C20 C25 H21 109.5 . . ? H20 C25 H21 109.5 . . ? C20 C25 H22 109.5 . . ? H20 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? C22 C26 H23 109.5 . . ? C22 C26 H24 109.5 . . ? H23 C26 H24 109.5 . . ? C22 C26 H25 109.5 . . ? H23 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C24 C27 H26 109.5 . . ? C24 C27 H27 109.5 . . ? H26 C27 H27 109.5 . . ? C24 C27 H28 109.5 . . ? H26 C27 H28 109.5 . . ? H27 C27 H28 109.5 . . ? C28 B1 C40 110.44(16) . . ? C28 B1 C46 107.16(16) . . ? C40 B1 C46 110.71(16) . . ? C28 B1 C34 110.63(16) . . ? C40 B1 C34 109.06(16) . . ? C46 B1 C34 108.81(15) . . ? C33 C28 C29 114.67(18) . . ? C33 C28 B1 124.80(18) . . ? C29 C28 B1 120.53(17) . . ? C30 C29 C28 123.45(19) . . ? C30 C29 H29 118.3 . . ? C28 C29 H29 118.3 . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 119.1(2) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 120.5(2) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 122.6(2) . . ? C32 C33 H33 118.7 . . ? C28 C33 H33 118.7 . . ? C39 C34 C35 114.74(18) . . ? C39 C34 B1 125.27(17) . . ? C35 C34 B1 119.85(17) . . ? C36 C35 C34 122.81(19) . . ? C36 C35 H34 118.6 . . ? C34 C35 H34 118.6 . . ? C37 C36 C35 120.5(2) . . ? C37 C36 H35 119.8 . . ? C35 C36 H35 119.8 . . ? C36 C37 C38 118.66(19) . . ? C36 C37 H36 120.7 . . ? C38 C37 H36 120.7 . . ? C37 C38 C39 120.3(2) . . ? C37 C38 H37 119.8 . . ? C39 C38 H37 119.8 . . ? C38 C39 C34 122.98(19) . . ? C38 C39 H38 118.5 . . ? C34 C39 H38 118.5 . . ? C41 C40 C45 113.86(19) . . ? C41 C40 B1 123.96(18) . . ? C45 C40 B1 122.13(18) . . ? C40 C41 C42 123.3(2) . . ? C40 C41 H39 118.3 . . ? C42 C41 H39 118.3 . . ? C43 C42 C41 120.6(2) . . ? C43 C42 H40 119.7 . . ? C41 C42 H40 119.7 . . ? C42 C43 C44 118.2(2) . . ? C42 C43 H41 120.9 . . ? C44 C43 H41 120.9 . . ? C43 C44 C45 120.3(2) . . ? C43 C44 H42 119.9 . . ? C45 C44 H42 119.9 . . ? C44 C45 C40 123.8(2) . . ? C44 C45 H43 118.1 . . ? C40 C45 H43 118.1 . . ? C51 C46 C47 114.82(18) . . ? C51 C46 B1 124.24(17) . . ? C47 C46 B1 120.94(17) . . ? C48 C47 C46 122.95(19) . . ? C48 C47 H44 118.5 . . ? C46 C47 H44 118.5 . . ? C47 C48 C49 120.4(2) . . ? C47 C48 H45 119.8 . . ? C49 C48 H45 119.8 . . ? C50 C49 C48 118.7(2) . . ? C50 C49 H46 120.7 . . ? C48 C49 H46 120.7 . . ? C49 C50 C51 120.4(2) . . ? C49 C50 H47 119.8 . . ? C51 C50 H47 119.8 . . ? C50 C51 C46 122.8(2) . . ? C50 C51 H48 118.6 . . ? C46 C51 H48 118.6 . . ? O1 C52 H49 109.5 . . ? O1 C52 H50 109.5 . . ? H49 C52 H50 109.5 . . ? O1 C52 H51 109.5 . . ? H49 C52 H51 109.5 . . ? H50 C52 H51 109.5 . . ? C52 O1 H52 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 C4 C1 N1 C2 -0.1(2) . . . . ? C4 C1 N1 C19 -176.55(17) . . . . ? C1 N1 C2 C3 0.1(2) . . . . ? C19 N1 C2 C3 176.41(18) . . . . ? N1 C2 C3 C4 0.0(2) . . . . ? N1 C1 C4 C3 0.1(2) . . . . ? N1 C1 C4 S1 -178.41(13) . . . . ? C2 C3 C4 C1 0.0(2) . . . . ? C2 C3 C4 S1 178.19(17) . . . . ? C1 C4 S1 C12 127.39(17) . . . . ? C3 C4 S1 C12 -50.7(2) . . . . ? C1 C4 S1 C5 -121.42(16) . . . . ? C3 C4 S1 C5 60.5(2) . . . . ? C4 S1 C5 C10 -162.41(16) . . . . ? C12 S1 C5 C10 -50.66(18) . . . . ? C4 S1 C5 C6 24.80(19) . . . . ? C12 S1 C5 C6 136.54(17) . . . . ? C10 C5 C6 C7 1.5(3) . . . . ? S1 C5 C6 C7 173.94(15) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C6 C7 C8 C9 -1.5(3) . . . . ? C6 C7 C8 C11 176.9(2) . . . . ? C7 C8 C9 C10 0.9(3) . . . . ? C11 C8 C9 C10 -177.4(2) . . . . ? C6 C5 C10 C9 -2.0(3) . . . . ? S1 C5 C10 C9 -174.71(15) . . . . ? C8 C9 C10 C5 0.8(3) . . . . ? C4 S1 C12 C17 69.36(19) . . . . ? C5 S1 C12 C17 -42.45(19) . . . . ? C4 S1 C12 C13 -106.39(16) . . . . ? C5 S1 C12 C13 141.80(15) . . . . ? C17 C12 C13 C14 -1.0(3) . . . . ? S1 C12 C13 C14 174.81(15) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 0.5(3) . . . . ? C13 C14 C15 C18 -178.41(19) . . . . ? C14 C15 C16 C17 -0.3(3) . . . . ? C18 C15 C16 C17 178.64(19) . . . . ? C13 C12 C17 C16 1.2(3) . . . . ? S1 C12 C17 C16 -174.22(15) . . . . ? C15 C16 C17 C12 -0.6(3) . . . . ? C1 N1 C19 C24 -77.7(3) . . . . ? C2 N1 C19 C24 106.4(2) . . . . ? C1 N1 C19 C20 100.0(2) . . . . ? C2 N1 C19 C20 -75.8(3) . . . . ? C24 C19 C20 C21 1.3(3) . . . . ? N1 C19 C20 C21 -176.33(18) . . . . ? C24 C19 C20 C25 -179.7(2) . . . . ? N1 C19 C20 C25 2.6(3) . . . . ? C19 C20 C21 C22 -0.9(3) . . . . ? C25 C20 C21 C22 -179.8(2) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? C20 C21 C22 C26 -178.8(2) . . . . ? C21 C22 C23 C24 0.3(3) . . . . ? C26 C22 C23 C24 179.2(2) . . . . ? C20 C19 C24 C23 -1.0(3) . . . . ? N1 C19 C24 C23 176.69(18) . . . . ? C20 C19 C24 C27 179.4(2) . . . . ? N1 C19 C24 C27 -2.9(3) . . . . ? C22 C23 C24 C19 0.1(3) . . . . ? C22 C23 C24 C27 179.7(2) . . . . ? C40 B1 C28 C33 7.6(3) . . . . ? C46 B1 C28 C33 128.27(19) . . . . ? C34 B1 C28 C33 -113.2(2) . . . . ? C40 B1 C28 C29 -171.95(17) . . . . ? C46 B1 C28 C29 -51.3(2) . . . . ? C34 B1 C28 C29 67.2(2) . . . . ? C33 C28 C29 C30 1.5(3) . . . . ? B1 C28 C29 C30 -178.91(18) . . . . ? C28 C29 C30 C31 -2.1(3) . . . . ? C29 C30 C31 C32 0.8(3) . . . . ? C30 C31 C32 C33 0.9(3) . . . . ? C31 C32 C33 C28 -1.5(3) . . . . ? C29 C28 C33 C32 0.3(3) . . . . ? B1 C28 C33 C32 -179.27(19) . . . . ? C28 B1 C34 C39 -16.8(3) . . . . ? C40 B1 C34 C39 -138.43(19) . . . . ? C46 B1 C34 C39 100.7(2) . . . . ? C28 B1 C34 C35 167.74(17) . . . . ? C40 B1 C34 C35 46.1(2) . . . . ? C46 B1 C34 C35 -74.8(2) . . . . ? C39 C34 C35 C36 0.2(3) . . . . ? B1 C34 C35 C36 176.16(19) . . . . ? C34 C35 C36 C37 0.4(3) . . . . ? C35 C36 C37 C38 -0.8(3) . . . . ? C36 C37 C38 C39 0.6(3) . . . . ? C37 C38 C39 C34 0.0(3) . . . . ? C35 C34 C39 C38 -0.4(3) . . . . ? B1 C34 C39 C38 -176.07(19) . . . . ? C28 B1 C40 C41 94.1(2) . . . . ? C46 B1 C40 C41 -24.4(3) . . . . ? C34 B1 C40 C41 -144.1(2) . . . . ? C28 B1 C40 C45 -83.2(2) . . . . ? C46 B1 C40 C45 158.24(19) . . . . ? C34 B1 C40 C45 38.5(3) . . . . ? C45 C40 C41 C42 0.0(4) . . . . ? B1 C40 C41 C42 -177.5(2) . . . . ? C40 C41 C42 C43 -0.8(4) . . . . ? C41 C42 C43 C44 1.1(4) . . . . ? C42 C43 C44 C45 -0.8(4) . . . . ? C43 C44 C45 C40 0.0(4) . . . . ? C41 C40 C45 C44 0.4(3) . . . . ? B1 C40 C45 C44 178.0(2) . . . . ? C28 B1 C46 C51 133.98(19) . . . . ? C40 B1 C46 C51 -105.5(2) . . . . ? C34 B1 C46 C51 14.3(3) . . . . ? C28 B1 C46 C47 -45.8(2) . . . . ? C40 B1 C46 C47 74.7(2) . . . . ? C34 B1 C46 C47 -165.44(17) . . . . ? C51 C46 C47 C48 1.0(3) . . . . ? B1 C46 C47 C48 -179.21(18) . . . . ? C46 C47 C48 C49 -0.9(3) . . . . ? C47 C48 C49 C50 -0.1(3) . . . . ? C48 C49 C50 C51 1.0(3) . . . . ? C49 C50 C51 C46 -0.9(3) . . . . ? C47 C46 C51 C50 -0.1(3) . . . . ? B1 C46 C51 C50 -179.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.692 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.047