Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Trans.' _publ_contact_author_name 'Dr Clara Vinas' _publ_contact_author_address ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; _publ_contact_author_phone '+ 34 93 5801853' _publ_contact_author_fax '+ 34 93 5805729' _publ_contact_author_email clara@icmab.es loop_ _publ_author_name _publ_author_address 'Anna Laromaine' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Francesc Teixidor' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Rajae Benakki' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Raikko Kivekas' ; Department of Chemistry P.O.Box 55 FIN-00014 University of Helsinki Finland ; 'Reijo Sillanpaa' ; Department of Chemistry University of Jyvaskyla FIN-40351 Jyvaskyla Finland ; 'Bohumir Gruner' ; Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 25056 Rez Czech Republic ; 'Clara Vinas' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; _publ_section_title ; Synthesis, Reactivity and Structural Studies of Carboranyl Thioethers and Disulfides. ; data_[2-Me-1,2-C~2~B~10~H~10~]~2~S _database_code_depnum_ccdc_archive 'CCDC 263591' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H26 B20 S' _chemical_formula_sum 'C6 H26 B20 S' _chemical_formula_weight 346.53 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' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.107(3) _cell_length_b 11.754(2) _cell_length_c 14.203(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.950(11) _cell_angle_gamma 90.00 _cell_volume 2060.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 19 _cell_measurement_theta_min 15.04 _cell_measurement_theta_max 16.90 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North, Phillips & Mathews 1968' _exptl_absorpt_correction_T_min 0.9468 _exptl_absorpt_correction_T_max 0.9687 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 3774 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3619 _reflns_number_gt 2252 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_data_reduction ; Texsan Process (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0798P)^2^+1.4700P] 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 3619 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.64422(7) 0.03401(7) 0.44634(7) 0.0410(3) Uani 1 d . . . C1 C 0.7672(2) 0.1084(3) 0.5287(2) 0.0321(7) Uani 1 d . . . C2 C 0.8027(3) 0.1276(3) 0.6615(3) 0.0381(8) Uani 1 d . . . B3 B 0.8860(3) 0.0516(3) 0.6273(3) 0.0348(9) Uani 1 d . . . H3 H 0.9007 -0.0403 0.6415 0.042 Uiso 1 calc R . . B4 B 0.8775(3) 0.1198(3) 0.5112(3) 0.0407(9) Uani 1 d . . . H4 H 0.8882 0.0721 0.4504 0.049 Uiso 1 calc R . . B5 B 0.7830(4) 0.2342(3) 0.4763(3) 0.0470(11) Uani 1 d . . . H5 H 0.7322 0.2610 0.3923 0.056 Uiso 1 calc R . . B6 B 0.7327(4) 0.2339(4) 0.5686(4) 0.0485(11) Uani 1 d . . . H6 H 0.6488 0.2583 0.5447 0.058 Uiso 1 calc R . . B7 B 0.9376(3) 0.1520(4) 0.7343(3) 0.0431(10) Uani 1 d . . . H7 H 0.9879 0.1254 0.8185 0.052 Uiso 1 calc R . . B8 B 0.9867(3) 0.1499(4) 0.6404(3) 0.0435(10) Uani 1 d . . . H8 H 1.0696 0.1222 0.6635 0.052 Uiso 1 calc R . . B9 B 0.9227(4) 0.2634(4) 0.5472(4) 0.0527(12) Uani 1 d . . . H9 H 0.9639 0.3098 0.5101 0.063 Uiso 1 calc R . . B10 B 0.8323(4) 0.3325(4) 0.5825(4) 0.0566(12) Uani 1 d . . . H10 H 0.8141 0.4238 0.5680 0.068 Uiso 1 calc R . . B11 B 0.8427(4) 0.2642(4) 0.6981(4) 0.0515(11) Uani 1 d . . . H11 H 0.8309 0.3106 0.7589 0.062 Uiso 1 calc R . . B12 B 0.9597(4) 0.2818(4) 0.6848(4) 0.0526(11) Uani 1 d . . . H12 H 1.0252 0.3401 0.7370 0.063 Uiso 1 calc R . . C13 C 0.7412(3) 0.0617(3) 0.7065(3) 0.0560(11) Uani 1 d . . . H13A H 0.6832 0.0202 0.6495 0.084 Uiso 1 calc R . . H13B H 0.7120 0.1138 0.7380 0.084 Uiso 1 calc R . . H13C H 0.7894 0.0095 0.7604 0.084 Uiso 1 calc R . . C21 C 0.6644(3) -0.1145(3) 0.4332(2) 0.0351(8) Uani 1 d . . . C22 C 0.6661(3) -0.1567(3) 0.3191(3) 0.0380(8) Uani 1 d . . . B23 B 0.7785(3) -0.1781(3) 0.4442(3) 0.0366(9) Uani 1 d . . . H23 H 0.8562 -0.1338 0.4720 0.044 Uiso 1 calc R . . B24 B 0.7265(3) -0.2129(3) 0.5326(3) 0.0424(10) Uani 1 d . . . H24 H 0.7715 -0.1925 0.6189 0.051 Uiso 1 calc R . . B25 B 0.5828(3) -0.2039(4) 0.4586(3) 0.0455(10) Uani 1 d . . . H25 H 0.5347 -0.1774 0.4968 0.055 Uiso 1 calc R . . B26 B 0.5472(3) -0.1636(4) 0.3243(3) 0.0435(10) Uani 1 d . . . H26 H 0.4767 -0.1093 0.2755 0.052 Uiso 1 calc R . . B27 B 0.7309(4) -0.2830(3) 0.3409(3) 0.0469(10) Uani 1 d . . . H27 H 0.7792 -0.3084 0.3026 0.056 Uiso 1 calc R . . B28 B 0.7681(4) -0.3214(4) 0.4754(4) 0.0494(11) Uani 1 d . . . H28 H 0.8408 -0.3726 0.5249 0.059 Uiso 1 calc R . . B29 B 0.6463(4) -0.3378(4) 0.4833(4) 0.0525(12) Uani 1 d . . . H29 H 0.6394 -0.4000 0.5375 0.063 Uiso 1 calc R . . B30 B 0.5350(4) -0.3063(4) 0.3547(3) 0.0517(12) Uani 1 d . . . H30 H 0.4553 -0.3470 0.3253 0.062 Uiso 1 calc R . . B31 B 0.5879(4) -0.2742(4) 0.2670(3) 0.0478(11) Uani 1 d . . . H31 H 0.5430 -0.2939 0.1805 0.057 Uiso 1 calc R . . B32 B 0.6496(4) -0.3816(4) 0.3653(4) 0.0541(12) Uani 1 d . . . H32 H 0.6450 -0.4719 0.3433 0.065 Uiso 1 calc R . . C33 C 0.6746(3) -0.0658(3) 0.2472(3) 0.0508(10) Uani 1 d . . . H33A H 0.6959 0.0051 0.2855 0.076 Uiso 1 calc R . . H33B H 0.6056 -0.0567 0.1838 0.076 Uiso 1 calc R . . H33C H 0.7277 -0.0883 0.2269 0.076 Uiso 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 S 0.0306(4) 0.0395(5) 0.0434(5) -0.0069(4) 0.0104(4) 0.0014(4) C1 0.0350(17) 0.0319(18) 0.0282(16) -0.0026(14) 0.0144(14) 0.0003(14) C2 0.044(2) 0.0399(19) 0.0329(18) -0.0060(15) 0.0208(16) -0.0002(16) B3 0.0332(19) 0.033(2) 0.035(2) -0.0006(16) 0.0143(16) 0.0017(16) B4 0.045(2) 0.042(2) 0.040(2) -0.0024(18) 0.024(2) -0.0052(18) B5 0.054(3) 0.038(2) 0.041(2) 0.0044(19) 0.017(2) -0.008(2) B6 0.051(3) 0.037(2) 0.057(3) -0.004(2) 0.026(2) 0.009(2) B7 0.042(2) 0.045(2) 0.034(2) -0.0055(19) 0.0126(18) -0.0054(19) B8 0.035(2) 0.049(3) 0.045(2) -0.003(2) 0.0184(19) -0.0054(19) B9 0.062(3) 0.048(3) 0.049(3) 0.003(2) 0.028(2) -0.015(2) B10 0.063(3) 0.029(2) 0.063(3) -0.004(2) 0.020(2) -0.002(2) B11 0.056(3) 0.046(3) 0.052(3) -0.017(2) 0.025(2) -0.007(2) B12 0.050(3) 0.047(3) 0.048(3) -0.009(2) 0.014(2) -0.015(2) C13 0.060(2) 0.069(3) 0.050(2) -0.005(2) 0.036(2) -0.010(2) C21 0.0368(19) 0.0388(19) 0.0298(17) -0.0053(14) 0.0161(15) -0.0066(15) C22 0.0424(19) 0.042(2) 0.0331(18) -0.0061(15) 0.0209(16) -0.0077(16) B23 0.036(2) 0.035(2) 0.039(2) -0.0043(17) 0.0179(18) -0.0033(17) B24 0.048(2) 0.040(2) 0.038(2) 0.0025(18) 0.0195(19) -0.0068(19) B25 0.044(2) 0.055(3) 0.043(2) -0.010(2) 0.026(2) -0.020(2) B26 0.038(2) 0.051(3) 0.037(2) -0.0093(19) 0.0154(18) -0.0107(19) B27 0.057(3) 0.037(2) 0.052(3) -0.012(2) 0.030(2) -0.006(2) B28 0.053(3) 0.036(2) 0.054(3) 0.002(2) 0.022(2) -0.001(2) B29 0.063(3) 0.047(3) 0.047(3) -0.005(2) 0.026(2) -0.020(2) B30 0.049(3) 0.055(3) 0.051(3) -0.018(2) 0.024(2) -0.023(2) B31 0.052(3) 0.049(3) 0.044(2) -0.017(2) 0.024(2) -0.016(2) B32 0.067(3) 0.041(2) 0.055(3) -0.010(2) 0.030(2) -0.014(2) C33 0.066(3) 0.051(2) 0.040(2) 0.0029(17) 0.0285(19) -0.0048(19) _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 S C1 1.783(3) . ? S C21 1.793(3) . ? C1 B4 1.696(5) . ? C1 C2 1.716(4) . ? C1 B3 1.716(5) . ? C1 B5 1.717(5) . ? C1 B6 1.732(5) . ? C2 C13 1.516(5) . ? C2 B7 1.693(5) . ? C2 B11 1.698(5) . ? C2 B3 1.722(5) . ? C2 B6 1.736(5) . ? B3 B8 1.769(5) . ? B3 B7 1.778(5) . ? B3 B4 1.783(5) . ? B3 H3 1.1000 . ? B4 B8 1.769(5) . ? B4 B5 1.787(6) . ? B4 B9 1.790(6) . ? B4 H4 1.1000 . ? B5 B10 1.754(6) . ? B5 B9 1.759(6) . ? B5 B6 1.767(6) . ? B5 H5 1.1000 . ? B6 B10 1.757(6) . ? B6 B11 1.776(6) . ? B6 H6 1.1000 . ? B7 B12 1.768(6) . ? B7 B11 1.768(6) . ? B7 B8 1.775(6) . ? B7 H7 1.1000 . ? B8 B12 1.782(6) . ? B8 B9 1.786(6) . ? B8 H8 1.1000 . ? B9 B12 1.775(6) . ? B9 B10 1.776(7) . ? B9 H9 1.1000 . ? B10 B11 1.769(7) . ? B10 B12 1.781(6) . ? B10 H10 1.1000 . ? B11 B12 1.762(6) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C21 B24 1.703(5) . ? C21 C22 1.707(4) . ? C21 B23 1.712(5) . ? C21 B25 1.720(5) . ? C21 B26 1.728(5) . ? C22 C33 1.522(4) . ? C22 B27 1.691(5) . ? C22 B31 1.697(5) . ? C22 B26 1.717(5) . ? C22 B23 1.734(5) . ? B23 B28 1.766(6) . ? B23 B27 1.780(5) . ? B23 B24 1.782(5) . ? B23 H23 1.1000 . ? B24 B28 1.759(6) . ? B24 B29 1.777(6) . ? B24 B25 1.778(6) . ? B24 H24 1.1000 . ? B25 B29 1.759(6) . ? B25 B30 1.766(6) . ? B25 B26 1.784(6) . ? B25 H25 1.1000 . ? B26 B30 1.761(6) . ? B26 B31 1.770(6) . ? B26 H26 1.1000 . ? B27 B31 1.769(6) . ? B27 B28 1.777(6) . ? B27 B32 1.778(6) . ? B27 H27 1.1000 . ? B28 B29 1.786(6) . ? B28 B32 1.792(6) . ? B28 H28 1.1000 . ? B29 B32 1.775(6) . ? B29 B30 1.778(6) . ? B29 H29 1.1000 . ? B30 B31 1.775(6) . ? B30 B32 1.784(6) . ? B30 H30 1.1000 . ? B31 B32 1.767(6) . ? B31 H31 1.1000 . ? B32 H32 1.1000 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 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 C1 S C21 113.14(15) . . ? B4 C1 C2 110.5(2) . . ? B4 C1 B3 63.0(2) . . ? C2 C1 B3 60.23(19) . . ? B4 C1 B5 63.1(2) . . ? C2 C1 B5 109.5(3) . . ? B3 C1 B5 114.1(3) . . ? B4 C1 B6 113.8(3) . . ? C2 C1 B6 60.5(2) . . ? B3 C1 B6 112.5(3) . . ? B5 C1 B6 61.6(2) . . ? B4 C1 S 127.8(2) . . ? C2 C1 S 117.4(2) . . ? B3 C1 S 126.9(2) . . ? B5 C1 S 115.3(2) . . ? B6 C1 S 107.1(2) . . ? C13 C2 B7 122.2(3) . . ? C13 C2 B11 121.8(3) . . ? B7 C2 B11 62.9(2) . . ? C13 C2 C1 118.3(3) . . ? B7 C2 C1 109.7(2) . . ? B11 C2 C1 109.8(3) . . ? C13 C2 B3 117.5(3) . . ? B7 C2 B3 62.7(2) . . ? B11 C2 B3 114.0(3) . . ? C1 C2 B3 59.90(19) . . ? C13 C2 B6 117.1(3) . . ? B7 C2 B6 113.5(3) . . ? B11 C2 B6 62.3(2) . . ? C1 C2 B6 60.2(2) . . ? B3 C2 B6 111.9(3) . . ? C1 B3 C2 59.87(19) . . ? C1 B3 B8 104.5(3) . . ? C2 B3 B8 104.7(3) . . ? C1 B3 B7 105.9(3) . . ? C2 B3 B7 57.9(2) . . ? B8 B3 B7 60.1(2) . . ? C1 B3 B4 57.9(2) . . ? C2 B3 B4 106.1(3) . . ? B8 B3 B4 59.7(2) . . ? B7 B3 B4 108.0(3) . . ? C1 B3 H3 123.7 . . ? C2 B3 H3 123.5 . . ? B8 B3 H3 123.4 . . ? B7 B3 H3 122.2 . . ? B4 B3 H3 122.1 . . ? C1 B4 B8 105.3(3) . . ? C1 B4 B3 59.0(2) . . ? B8 B4 B3 59.7(2) . . ? C1 B4 B5 59.0(2) . . ? B8 B4 B5 107.2(3) . . ? B3 B4 B5 107.6(3) . . ? C1 B4 B9 104.9(3) . . ? B8 B4 B9 60.2(2) . . ? B3 B4 B9 107.7(3) . . ? B5 B4 B9 58.9(2) . . ? C1 B4 H4 124.1 . . ? B8 B4 H4 122.4 . . ? B3 B4 H4 121.6 . . ? B5 B4 H4 122.2 . . ? B9 B4 H4 122.6 . . ? C1 B5 B10 106.0(3) . . ? C1 B5 B9 105.4(3) . . ? B10 B5 B9 60.7(3) . . ? C1 B5 B6 59.6(2) . . ? B10 B5 B6 59.9(3) . . ? B9 B5 B6 108.4(3) . . ? C1 B5 B4 57.9(2) . . ? B10 B5 B4 109.0(3) . . ? B9 B5 B4 60.6(2) . . ? B6 B5 B4 107.8(3) . . ? C1 B5 H5 124.3 . . ? B10 B5 H5 121.5 . . ? B9 B5 H5 121.7 . . ? B6 B5 H5 121.4 . . ? B4 B5 H5 121.6 . . ? C1 B6 C2 59.29(19) . . ? C1 B6 B10 105.2(3) . . ? C2 B6 B10 105.0(3) . . ? C1 B6 B5 58.8(2) . . ? C2 B6 B5 106.3(3) . . ? B10 B6 B5 59.7(3) . . ? C1 B6 B11 105.5(3) . . ? C2 B6 B11 57.8(2) . . ? B10 B6 B11 60.1(3) . . ? B5 B6 B11 107.7(3) . . ? C1 B6 H6 123.5 . . ? C2 B6 H6 123.6 . . ? B10 B6 H6 123.0 . . ? B5 B6 H6 122.0 . . ? B11 B6 H6 122.5 . . ? C2 B7 B12 105.4(3) . . ? C2 B7 B11 58.7(2) . . ? B12 B7 B11 59.8(3) . . ? C2 B7 B8 105.7(3) . . ? B12 B7 B8 60.4(2) . . ? B11 B7 B8 108.0(3) . . ? C2 B7 B3 59.4(2) . . ? B12 B7 B3 108.1(3) . . ? B11 B7 B3 107.9(3) . . ? B8 B7 B3 59.7(2) . . ? C2 B7 H7 124.0 . . ? B12 B7 H7 122.1 . . ? B11 B7 H7 121.8 . . ? B8 B7 H7 122.1 . . ? B3 B7 H7 121.5 . . ? B4 B8 B3 60.5(2) . . ? B4 B8 B7 108.7(3) . . ? B3 B8 B7 60.2(2) . . ? B4 B8 B12 108.3(3) . . ? B3 B8 B12 107.9(3) . . ? B7 B8 B12 59.6(2) . . ? B4 B8 B9 60.5(2) . . ? B3 B8 B9 108.5(3) . . ? B7 B8 B9 107.7(3) . . ? B12 B8 B9 59.7(2) . . ? B4 B8 H8 121.0 . . ? B3 B8 H8 121.4 . . ? B7 B8 H8 121.7 . . ? B12 B8 H8 122.1 . . ? B9 B8 H8 121.7 . . ? B5 B9 B12 107.8(3) . . ? B5 B9 B10 59.5(3) . . ? B12 B9 B10 60.2(3) . . ? B5 B9 B8 107.6(3) . . ? B12 B9 B8 60.1(2) . . ? B10 B9 B8 107.9(3) . . ? B5 B9 B4 60.5(2) . . ? B12 B9 B4 107.7(3) . . ? B10 B9 B4 107.9(3) . . ? B8 B9 B4 59.3(2) . . ? B5 B9 H9 121.8 . . ? B12 B9 H9 121.7 . . ? B10 B9 H9 121.8 . . ? B8 B9 H9 122.0 . . ? B4 B9 H9 121.9 . . ? B5 B10 B6 60.4(2) . . ? B5 B10 B11 108.6(3) . . ? B6 B10 B11 60.5(3) . . ? B5 B10 B9 59.8(3) . . ? B6 B10 B9 108.1(3) . . ? B11 B10 B9 107.8(3) . . ? B5 B10 B12 107.7(3) . . ? B6 B10 B12 107.9(3) . . ? B11 B10 B12 59.5(3) . . ? B9 B10 B12 59.9(3) . . ? B5 B10 H10 121.5 . . ? B6 B10 H10 121.4 . . ? B11 B10 H10 121.6 . . ? B9 B10 H10 121.9 . . ? B12 B10 H10 122.1 . . ? C2 B11 B12 105.5(3) . . ? C2 B11 B7 58.4(2) . . ? B12 B11 B7 60.1(2) . . ? C2 B11 B10 106.2(3) . . ? B12 B11 B10 60.6(3) . . ? B7 B11 B10 108.6(3) . . ? C2 B11 B6 59.9(2) . . ? B12 B11 B6 107.8(3) . . ? B7 B11 B6 108.1(3) . . ? B10 B11 B6 59.4(2) . . ? C2 B11 H11 123.7 . . ? B12 B11 H11 122.1 . . ? B7 B11 H11 121.5 . . ? B10 B11 H11 121.8 . . ? B6 B11 H11 121.6 . . ? B11 B12 B7 60.1(2) . . ? B11 B12 B9 108.2(3) . . ? B7 B12 B9 108.5(3) . . ? B11 B12 B10 59.9(3) . . ? B7 B12 B10 108.1(3) . . ? B9 B12 B10 59.9(3) . . ? B11 B12 B8 107.9(3) . . ? B7 B12 B8 60.0(2) . . ? B9 B12 B8 60.3(2) . . ? B10 B12 B8 107.9(3) . . ? B11 B12 H12 121.7 . . ? B7 B12 H12 121.5 . . ? B9 B12 H12 121.4 . . ? B10 B12 H12 121.9 . . ? B8 B12 H12 121.8 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? B24 C21 C22 110.6(3) . . ? B24 C21 B23 62.9(2) . . ? C22 C21 B23 60.94(19) . . ? B24 C21 B25 62.6(2) . . ? C22 C21 B25 109.8(2) . . ? B23 C21 B25 114.1(3) . . ? B24 C21 B26 113.6(3) . . ? C22 C21 B26 60.0(2) . . ? B23 C21 B26 112.7(3) . . ? B25 C21 B26 62.3(2) . . ? B24 C21 S 128.3(2) . . ? C22 C21 S 117.2(2) . . ? B23 C21 S 127.2(2) . . ? B25 C21 S 114.7(2) . . ? B26 C21 S 106.7(2) . . ? C33 C22 B27 121.9(3) . . ? C33 C22 B31 121.6(3) . . ? B27 C22 B31 63.0(2) . . ? C33 C22 C21 118.3(3) . . ? B27 C22 C21 109.6(3) . . ? B31 C22 C21 110.2(2) . . ? C33 C22 B26 117.3(3) . . ? B27 C22 B26 113.8(3) . . ? B31 C22 B26 62.5(2) . . ? C21 C22 B26 60.60(19) . . ? C33 C22 B23 117.3(3) . . ? B27 C22 B23 62.6(2) . . ? B31 C22 B23 114.1(3) . . ? C21 C22 B23 59.67(19) . . ? B26 C22 B23 112.1(3) . . ? C21 B23 C22 59.39(19) . . ? C21 B23 B28 104.5(3) . . ? C22 B23 B28 104.5(3) . . ? C21 B23 B27 105.3(3) . . ? C22 B23 B27 57.5(2) . . ? B28 B23 B27 60.1(2) . . ? C21 B23 B24 58.3(2) . . ? C22 B23 B24 105.7(3) . . ? B28 B23 B24 59.4(2) . . ? B27 B23 B24 107.6(3) . . ? C21 B23 H23 123.8 . . ? C22 B23 H23 123.9 . . ? B28 B23 H23 123.4 . . ? B27 B23 H23 122.5 . . ? B24 B23 H23 122.3 . . ? C21 B24 B28 105.2(3) . . ? C21 B24 B29 105.1(3) . . ? B28 B24 B29 60.7(2) . . ? C21 B24 B25 59.2(2) . . ? B28 B24 B25 108.0(3) . . ? B29 B24 B25 59.3(2) . . ? C21 B24 B23 58.8(2) . . ? B28 B24 B23 59.8(2) . . ? B29 B24 B23 108.2(3) . . ? B25 B24 B23 108.1(3) . . ? C21 B24 H24 124.3 . . ? B28 B24 H24 122.1 . . ? B29 B24 H24 122.2 . . ? B25 B24 H24 121.6 . . ? B23 B24 H24 121.5 . . ? C21 B25 B29 105.1(3) . . ? C21 B25 B30 105.4(3) . . ? B29 B25 B30 60.6(3) . . ? C21 B25 B24 58.2(2) . . ? B29 B25 B24 60.3(2) . . ? B30 B25 B24 108.6(3) . . ? C21 B25 B26 59.0(2) . . ? B29 B25 B26 107.7(3) . . ? B30 B25 B26 59.5(2) . . ? B24 B25 B26 107.4(3) . . ? C21 B25 H25 124.4 . . ? B29 B25 H25 122.1 . . ? B30 B25 H25 121.9 . . ? B24 B25 H25 121.6 . . ? B26 B25 H25 122.0 . . ? C22 B26 C21 59.41(19) . . ? C22 B26 B30 105.6(3) . . ? C21 B26 B30 105.3(3) . . ? C22 B26 B31 58.2(2) . . ? C21 B26 B31 105.9(3) . . ? B30 B26 B31 60.4(2) . . ? C22 B26 B25 106.4(3) . . ? C21 B26 B25 58.6(2) . . ? B30 B26 B25 59.7(2) . . ? B31 B26 B25 108.1(3) . . ? C22 B26 H26 123.3 . . ? C21 B26 H26 123.5 . . ? B30 B26 H26 122.8 . . ? B31 B26 H26 122.1 . . ? B25 B26 H26 122.0 . . ? C22 B27 B31 58.7(2) . . ? C22 B27 B28 105.8(3) . . ? B31 B27 B28 108.1(3) . . ? C22 B27 B32 105.4(3) . . ? B31 B27 B32 59.7(2) . . ? B28 B27 B32 60.5(2) . . ? C22 B27 B23 59.9(2) . . ? B31 B27 B23 108.4(3) . . ? B28 B27 B23 59.5(2) . . ? B32 B27 B23 108.2(3) . . ? C22 B27 H27 123.8 . . ? B31 B27 H27 121.6 . . ? B28 B27 H27 122.1 . . ? B32 B27 H27 122.2 . . ? B23 B27 H27 121.2 . . ? B24 B28 B23 60.7(2) . . ? B24 B28 B27 108.7(3) . . ? B23 B28 B27 60.3(2) . . ? B24 B28 B29 60.2(2) . . ? B23 B28 B29 108.5(3) . . ? B27 B28 B29 107.6(3) . . ? B24 B28 B32 108.1(3) . . ? B23 B28 B32 108.2(3) . . ? B27 B28 B32 59.8(2) . . ? B29 B28 B32 59.5(2) . . ? B24 B28 H28 121.2 . . ? B23 B28 H28 121.1 . . ? B27 B28 H28 121.7 . . ? B29 B28 H28 121.9 . . ? B32 B28 H28 122.0 . . ? B25 B29 B32 108.3(3) . . ? B25 B29 B24 60.4(2) . . ? B32 B29 B24 108.0(3) . . ? B25 B29 B30 59.9(2) . . ? B32 B29 B30 60.3(3) . . ? B24 B29 B30 108.1(3) . . ? B25 B29 B28 107.7(3) . . ? B32 B29 B28 60.4(3) . . ? B24 B29 B28 59.2(2) . . ? B30 B29 B28 108.2(3) . . ? B25 B29 H29 121.7 . . ? B32 B29 H29 121.3 . . ? B24 B29 H29 121.9 . . ? B30 B29 H29 121.6 . . ? B28 B29 H29 122.0 . . ? B26 B30 B25 60.8(2) . . ? B26 B30 B31 60.1(2) . . ? B25 B30 B31 108.7(3) . . ? B26 B30 B29 107.9(3) . . ? B25 B30 B29 59.5(2) . . ? B31 B30 B29 107.6(3) . . ? B26 B30 B32 107.5(3) . . ? B25 B30 B32 107.6(3) . . ? B31 B30 B32 59.5(2) . . ? B29 B30 B32 59.8(3) . . ? B26 B30 H30 121.6 . . ? B25 B30 H30 121.4 . . ? B31 B30 H30 121.7 . . ? B29 B30 H30 122.1 . . ? B32 B30 H30 122.3 . . ? C22 B31 B32 105.6(3) . . ? C22 B31 B27 58.3(2) . . ? B32 B31 B27 60.4(2) . . ? C22 B31 B26 59.3(2) . . ? B32 B31 B26 107.8(3) . . ? B27 B31 B26 107.5(3) . . ? C22 B31 B30 105.9(3) . . ? B32 B31 B30 60.5(3) . . ? B27 B31 B30 108.5(3) . . ? B26 B31 B30 59.6(2) . . ? C22 B31 H31 124.0 . . ? B32 B31 H31 121.9 . . ? B27 B31 H31 121.7 . . ? B26 B31 H31 121.9 . . ? B30 B31 H31 121.9 . . ? B31 B32 B29 108.1(3) . . ? B31 B32 B27 59.9(2) . . ? B29 B32 B27 108.0(3) . . ? B31 B32 B30 60.0(3) . . ? B29 B32 B30 59.9(3) . . ? B27 B32 B30 107.7(3) . . ? B31 B32 B28 107.6(3) . . ? B29 B32 B28 60.1(2) . . ? B27 B32 B28 59.7(2) . . ? B30 B32 B28 107.6(3) . . ? B31 B32 H32 121.8 . . ? B29 B32 H32 121.6 . . ? B27 B32 H32 121.9 . . ? B30 B32 H32 121.9 . . ? B28 B32 H32 122.0 . . ? C22 C33 H33A 109.5 . . ? C22 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C22 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 S C1 C2 C13 11.7(4) . . . . ? S C21 C22 C33 12.7(4) . . . . ? C2 C1 S C21 -95.9(2) . . . . ? C22 C21 S C1 -99.1(2) . . . . ? C13 C2 C22 C33 152.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.871 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.052 #===END data_[1-S-1,2-C~2~B~10~H~11~]~2~ _database_code_depnum_ccdc_archive 'CCDC 263592' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C4 H22 B20 S2' _chemical_formula_sum 'C4 H22 B20 S2' _chemical_formula_weight 350.54 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' 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 n a 21' 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' _cell_length_a 23.5885(3) _cell_length_b 7.01160(10) _cell_length_c 11.5732(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1914.13(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1972 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 25.028 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 3194 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3194 _reflns_number_gt 2946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0404P)^2^+0.8844P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(8) _refine_ls_number_reflns 3192 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_all 0.1065 _refine_ls_wR_factor_ref 0.0799 _refine_ls_goodness_of_fit_all 1.033 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.319 _refine_ls_restrained_S_obs 1.033 _refine_ls_shift/su_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group S1 S 0.85112(2) 0.93294(9) 0.5923 0.02526(15) Uani 1 d . . S2 S 0.86761(2) 1.21332(8) 0.61636(8) 0.02442(15) Uani 1 d . . C1 C 0.78643(9) 0.8860(3) 0.6705(2) 0.0205(5) Uani 1 d . . C2 C 0.72986(9) 0.8473(3) 0.5876(2) 0.0237(5) Uani 1 d . . H2 H 0.73192(9) 0.8671(3) 0.4916(2) 0.028 Uiso 1 calc R . B3 B 0.76513(12) 0.6554(4) 0.6455(2) 0.0254(6) Uani 1 d . . H3 H 0.79015(12) 0.5491(4) 0.5943(2) 0.031 Uiso 1 calc R . B4 B 0.78681(11) 0.7330(4) 0.7850(3) 0.0236(6) Uani 1 d . . H4 H 0.82591(11) 0.6756(4) 0.8275(3) 0.028 Uiso 1 calc R . B5 B 0.76646(11) 0.9775(4) 0.8009(2) 0.0209(6) Uani 1 d . . H5 H 0.79222(11) 1.0801(4) 0.8533(2) 0.025 Uiso 1 calc R . B6 B 0.73135(11) 1.0488(4) 0.6711(2) 0.0217(6) Uani 1 d . . H6 H 0.73438(11) 1.1976(4) 0.6365(2) 0.026 Uiso 1 calc R . B7 B 0.68961(13) 0.6655(4) 0.6392(3) 0.0300(7) Uani 1 d . . H7 H 0.66465(13) 0.5637(4) 0.5847(3) 0.036 Uiso 1 calc R . B8 B 0.72456(13) 0.5931(4) 0.7681(3) 0.0302(7) Uani 1 d . . H8 H 0.72235(13) 0.4425(4) 0.8000(3) 0.036 Uiso 1 calc R . B9 B 0.72490(12) 0.7927(4) 0.8636(3) 0.0241(6) Uani 1 d . . H9 H 0.72266(12) 0.7734(4) 0.9595(3) 0.029 Uiso 1 calc R . B10 B 0.69087(12) 0.9889(4) 0.7940(2) 0.0227(6) Uani 1 d . . H10 H 0.66652(12) 1.0996(4) 0.8431(2) 0.027 Uiso 1 calc R . B11 B 0.66878(12) 0.9086(4) 0.6556(2) 0.0263(6) Uani 1 d . . H11 H 0.63000(12) 0.9660(4) 0.6119(2) 0.032 Uiso 1 calc R . B12 B 0.66471(12) 0.7508(4) 0.7750(3) 0.0266(6) Uani 1 d . . H12 H 0.62306(12) 0.7042(4) 0.8119(3) 0.032 Uiso 1 calc R . C21 C 0.92086(10) 1.2246(3) 0.7278(2) 0.0204(5) Uani 1 d . . C22 C 0.98365(10) 1.2990(4) 0.6825(2) 0.0279(6) Uani 1 d . . H22 H 0.99204(10) 1.3213(4) 0.5882(2) 0.034 Uiso 1 calc R . B23 B 0.93958(12) 1.4596(4) 0.7493(3) 0.0256(6) Uani 1 d . . H23 H 0.91864(12) 1.5841(4) 0.7061(3) 0.031 Uiso 1 calc R . B24 B 0.90509(12) 1.3222(4) 0.8588(2) 0.0221(6) Uani 1 d . . H24 H 0.86131(12) 1.3578(4) 0.8894(2) 0.026 Uiso 1 calc R . B25 B 0.92810(12) 1.0807(4) 0.8455(2) 0.0237(6) Uani 1 d . . H25 H 0.89948(12) 0.9583(4) 0.8670(2) 0.028 Uiso 1 calc R . B26 B 0.97732(12) 1.0672(4) 0.7281(3) 0.0271(6) Uani 1 d . . H26 H 0.98090(12) 0.9384(4) 0.6714(3) 0.032 Uiso 1 calc R . B27 B 1.01422(13) 1.4532(5) 0.7759(3) 0.0326(7) Uani 1 d . . H27 H 1.04256(13) 1.5747(5) 0.7512(3) 0.039 Uiso 1 calc R . B28 B 0.96471(13) 1.4672(4) 0.8930(3) 0.0284(7) Uani 1 d . . H28 H 0.96056(13) 1.5991(4) 0.9469(3) 0.034 Uiso 1 calc R . B29 B 0.95776(13) 1.2322(4) 0.9530(3) 0.0268(7) Uani 1 d . . H29 H 0.94917(13) 1.2092(4) 1.0471(3) 0.032 Uiso 1 calc R . B30 B 1.00232(12) 1.0746(4) 0.8726(3) 0.0288(7) Uani 1 d . . H30 H 1.02301(12) 0.9475(4) 0.9134(3) 0.035 Uiso 1 calc R . B31 B 1.03736(12) 1.2123(5) 0.7639(3) 0.0336(7) Uani 1 d . . H31 H 1.08088(12) 1.1768(5) 0.7317(3) 0.040 Uiso 1 calc R . B32 B 1.02503(12) 1.3136(5) 0.9028(3) 0.0320(7) Uani 1 d . . H32 H 1.06062(12) 1.3442(5) 0.9642(3) 0.038 Uiso 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 S1 0.0241(3) 0.0301(3) 0.0216(3) -0.0063(3) 0.0053(3) 0.0003(2) S2 0.0250(3) 0.0286(3) 0.0196(3) 0.0045(3) -0.0044(3) -0.0019(2) C1 0.0213(12) 0.0233(13) 0.0169(12) -0.0027(10) -0.0009(9) 0.0024(9) C2 0.0244(11) 0.0275(12) 0.0193(12) -0.0030(11) -0.0028(10) -0.0006(9) B3 0.033(2) 0.0185(14) 0.025(2) -0.0048(11) 0.0006(11) 0.0012(11) B4 0.0268(14) 0.0212(15) 0.0228(15) 0.0014(11) 0.0007(11) 0.0047(11) B5 0.0227(14) 0.0241(15) 0.0158(14) -0.0023(12) 0.0024(11) 0.0021(11) B6 0.0225(14) 0.025(2) 0.0177(14) 0.0005(12) 0.0004(11) 0.0047(11) B7 0.032(2) 0.029(2) 0.030(2) -0.0071(13) 0.0006(12) -0.0064(12) B8 0.039(2) 0.021(2) 0.031(2) 0.0008(13) 0.0010(13) -0.0015(13) B9 0.0286(15) 0.026(2) 0.0181(14) 0.0025(12) 0.0005(11) -0.0014(12) B10 0.0219(13) 0.0262(15) 0.0201(14) -0.0013(12) 0.0016(11) 0.0024(11) B11 0.0217(14) 0.034(2) 0.0232(15) 0.0008(12) -0.0014(11) 0.0001(12) B12 0.0263(14) 0.029(2) 0.025(2) 0.0008(12) 0.0002(12) -0.0056(12) C21 0.0187(12) 0.0247(13) 0.0178(12) 0.0028(10) 0.0029(9) 0.0000(9) C22 0.0183(12) 0.040(2) 0.0254(13) 0.0028(12) 0.0043(10) -0.0021(11) B23 0.0258(15) 0.025(2) 0.026(2) 0.0032(13) 0.0001(12) -0.0026(12) B24 0.0235(14) 0.028(2) 0.0152(14) 0.0002(11) -0.0006(11) 0.0032(11) B25 0.0223(14) 0.028(2) 0.0207(14) 0.0044(12) 0.0003(11) 0.0064(12) B26 0.0195(14) 0.034(2) 0.0276(15) 0.0015(12) 0.0037(11) 0.0077(12) B27 0.025(2) 0.041(2) 0.032(2) 0.0037(14) -0.0021(13) -0.0074(13) B28 0.0266(15) 0.030(2) 0.029(2) -0.0038(13) -0.0046(12) 0.0001(13) B29 0.025(2) 0.034(2) 0.0210(14) 0.0033(13) -0.0022(11) 0.0048(12) B30 0.0220(14) 0.036(2) 0.028(2) 0.0028(15) -0.0026(12) 0.0084(13) B31 0.0194(15) 0.048(2) 0.033(2) 0.003(2) 0.0019(12) 0.0019(13) B32 0.022(2) 0.044(2) 0.030(2) -0.001(2) -0.0068(12) 0.0005(13) _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 S1 C1 1.805(2) . ? S1 S2 2.0232(8) . ? S2 C21 1.802(2) . ? C1 C2 1.666(3) . ? C1 B4 1.705(4) . ? C1 B5 1.706(3) . ? C1 B3 1.718(4) . ? C1 B6 1.729(3) . ? C2 B11 1.697(4) . ? C2 B7 1.698(4) . ? C2 B6 1.712(4) . ? C2 B3 1.718(4) . ? C2 H2 1.12 . ? B3 B8 1.767(4) . ? B3 B4 1.779(4) . ? B3 B7 1.784(4) . ? B3 H3 1.12 . ? B4 B9 1.770(4) . ? B4 B8 1.777(4) . ? B4 B5 1.790(4) . ? B4 H4 1.12 . ? B5 B9 1.779(4) . ? B5 B10 1.787(4) . ? B5 B6 1.787(4) . ? B5 H5 1.12 . ? B6 B10 1.764(4) . ? B6 B11 1.782(4) . ? B6 H6 1.12 . ? B7 B8 1.779(4) . ? B7 B12 1.781(4) . ? B7 B11 1.784(4) . ? B7 H7 1.12 . ? B8 B9 1.783(4) . ? B8 B12 1.795(4) . ? B8 H8 1.12 . ? B9 B12 1.775(4) . ? B9 B10 1.785(4) . ? B9 H9 1.12 . ? B10 B11 1.776(4) . ? B10 B12 1.794(4) . ? B10 H10 1.12 . ? B11 B12 1.773(4) . ? B11 H11 1.12 . ? B12 H12 1.12 . ? C21 C22 1.655(3) . ? C21 B25 1.704(4) . ? C21 B24 1.705(3) . ? C21 B23 1.724(4) . ? C21 B26 1.730(4) . ? C22 B27 1.690(4) . ? C22 B31 1.692(4) . ? C22 B26 1.715(4) . ? C22 B23 1.717(4) . ? C22 H22 1.12 . ? B23 B28 1.766(4) . ? B23 B24 1.788(4) . ? B23 B27 1.788(4) . ? B23 H23 1.12 . ? B24 B29 1.769(4) . ? B24 B28 1.780(4) . ? B24 B25 1.785(4) . ? B24 H24 1.12 . ? B25 B30 1.779(4) . ? B25 B29 1.779(4) . ? B25 B26 1.790(4) . ? B25 H25 1.12 . ? B26 B30 1.774(4) . ? B26 B31 1.792(4) . ? B26 H26 1.12 . ? B27 B31 1.781(5) . ? B27 B32 1.783(4) . ? B27 B28 1.791(4) . ? B27 H27 1.12 . ? B28 B32 1.788(4) . ? B28 B29 1.796(4) . ? B28 H28 1.12 . ? B29 B32 1.783(4) . ? B29 B30 1.787(4) . ? B29 H29 1.12 . ? B30 B31 1.788(4) . ? B30 B32 1.794(4) . ? B30 H30 1.12 . ? B31 B32 1.782(5) . ? B31 H31 1.12 . ? B32 H32 1.12 . ? 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 C1 S1 S2 105.70(8) . . ? C21 S2 S1 105.98(9) . . ? C2 C1 B4 110.5(2) . . ? C2 C1 B5 110.5(2) . . ? B4 C1 B5 63.3(2) . . ? C2 C1 B3 61.00(15) . . ? B4 C1 B3 62.6(2) . . ? B5 C1 B3 115.0(2) . . ? C2 C1 B6 60.52(15) . . ? B4 C1 B6 114.6(2) . . ? B5 C1 B6 62.69(15) . . ? B3 C1 B6 113.7(2) . . ? C2 C1 S1 114.70(15) . . ? B4 C1 S1 120.0(2) . . ? B5 C1 S1 127.5(2) . . ? B3 C1 S1 109.5(2) . . ? B6 C1 S1 121.1(2) . . ? C1 C2 B11 111.8(2) . . ? C1 C2 B7 111.6(2) . . ? B11 C2 B7 63.4(2) . . ? C1 C2 B6 61.57(14) . . ? B11 C2 B6 63.0(2) . . ? B7 C2 B6 115.6(2) . . ? C1 C2 B3 60.99(15) . . ? B11 C2 B3 115.4(2) . . ? B7 C2 B3 63.0(2) . . ? B6 C2 B3 114.6(2) . . ? C1 C2 H2 121.09(11) . . ? B11 C2 H2 117.73(13) . . ? B7 C2 H2 117.76(13) . . ? B6 C2 H2 117.18(13) . . ? B3 C2 H2 117.55(12) . . ? C1 B3 C2 58.01(14) . . ? C1 B3 B8 104.8(2) . . ? C2 B3 B8 104.2(2) . . ? C1 B3 B4 58.34(14) . . ? C2 B3 B4 104.7(2) . . ? B8 B3 B4 60.1(2) . . ? C1 B3 B7 105.2(2) . . ? C2 B3 B7 57.97(15) . . ? B8 B3 B7 60.1(2) . . ? B4 B3 B7 108.2(2) . . ? C1 B3 H3 124.14(12) . . ? C2 B3 H3 124.74(12) . . ? B8 B3 H3 123.08(13) . . ? B4 B3 H3 122.13(13) . . ? B7 B3 H3 122.08(13) . . ? C1 B4 B9 104.2(2) . . ? C1 B4 B8 104.9(2) . . ? B9 B4 B8 60.3(2) . . ? C1 B4 B3 59.0(2) . . ? B9 B4 B3 107.5(2) . . ? B8 B4 B3 59.6(2) . . ? C1 B4 B5 58.37(14) . . ? B9 B4 B5 60.0(2) . . ? B8 B4 B5 108.6(2) . . ? B3 B4 B5 108.0(2) . . ? C1 B4 H4 124.86(12) . . ? B9 B4 H4 122.62(13) . . ? B8 B4 H4 122.04(13) . . ? B3 B4 H4 121.68(13) . . ? B5 B4 H4 121.35(12) . . ? C1 B5 B9 103.8(2) . . ? C1 B5 B10 104.7(2) . . ? B9 B5 B10 60.1(2) . . ? C1 B5 B6 59.30(15) . . ? B9 B5 B6 106.9(2) . . ? B10 B5 B6 59.17(15) . . ? C1 B5 B4 58.34(15) . . ? B9 B5 B4 59.5(2) . . ? B10 B5 B4 107.8(2) . . ? B6 B5 B4 107.8(2) . . ? C1 B5 H5 124.79(12) . . ? B9 B5 H5 123.09(13) . . ? B10 B5 H5 122.46(13) . . ? B6 B5 H5 121.81(13) . . ? B4 B5 H5 121.68(12) . . ? C2 B6 C1 57.91(13) . . ? C2 B6 B10 104.4(2) . . ? C1 B6 B10 104.6(2) . . ? C2 B6 B11 58.08(14) . . ? C1 B6 B11 105.0(2) . . ? B10 B6 B11 60.1(2) . . ? C2 B6 B5 104.7(2) . . ? C1 B6 B5 58.02(14) . . ? B10 B6 B5 60.40(15) . . ? B11 B6 B5 108.3(2) . . ? C2 B6 H6 124.66(13) . . ? C1 B6 H6 124.45(12) . . ? B10 B6 H6 122.97(13) . . ? B11 B6 H6 122.06(13) . . ? B5 B6 H6 122.09(13) . . ? C2 B7 B8 104.5(2) . . ? C2 B7 B12 104.1(2) . . ? B8 B7 B12 60.6(2) . . ? C2 B7 B11 58.28(15) . . ? B8 B7 B11 108.1(2) . . ? B12 B7 B11 59.6(2) . . ? C2 B7 B3 59.07(15) . . ? B8 B7 B3 59.4(2) . . ? B12 B7 B3 107.8(2) . . ? B11 B7 B3 108.0(2) . . ? C2 B7 H7 125.05(13) . . ? B8 B7 H7 122.29(13) . . ? B12 B7 H7 122.52(13) . . ? B11 B7 H7 121.61(13) . . ? B3 B7 H7 121.51(13) . . ? B3 B8 B4 60.3(2) . . ? B3 B8 B7 60.4(2) . . ? B4 B8 B7 108.5(2) . . ? B3 B8 B9 107.5(2) . . ? B4 B8 B9 59.7(2) . . ? B7 B8 B9 107.3(2) . . ? B3 B8 B12 108.0(2) . . ? B4 B8 B12 107.8(2) . . ? B7 B8 B12 59.8(2) . . ? B9 B8 B12 59.5(2) . . ? B3 B8 H8 121.53(14) . . ? B4 B8 H8 121.52(13) . . ? B7 B8 H8 121.60(13) . . ? B9 B8 H8 122.44(14) . . ? B12 B8 H8 121.98(14) . . ? B4 B9 B12 108.9(2) . . ? B4 B9 B5 60.6(2) . . ? B12 B9 B5 109.0(2) . . ? B4 B9 B8 60.0(2) . . ? B12 B9 B8 60.6(2) . . ? B5 B9 B8 108.8(2) . . ? B4 B9 B10 108.8(2) . . ? B12 B9 B10 60.5(2) . . ? B5 B9 B10 60.16(15) . . ? B8 B9 B10 108.9(2) . . ? B4 B9 H9 121.29(13) . . ? B12 B9 H9 120.98(13) . . ? B5 B9 H9 121.19(13) . . ? B8 B9 H9 121.30(14) . . ? B10 B9 H9 121.26(13) . . ? B6 B10 B11 60.4(2) . . ? B6 B10 B9 107.7(2) . . ? B11 B10 B9 107.1(2) . . ? B6 B10 B5 60.42(15) . . ? B11 B10 B5 108.6(2) . . ? B9 B10 B5 59.8(2) . . ? B6 B10 B12 108.0(2) . . ? B11 B10 B12 59.6(2) . . ? B9 B10 B12 59.5(2) . . ? B5 B10 B12 107.9(2) . . ? B6 B10 H10 121.44(13) . . ? B11 B10 H10 121.76(13) . . ? B9 B10 H10 122.43(13) . . ? B5 B10 H10 121.36(13) . . ? B12 B10 H10 122.06(13) . . ? C2 B11 B12 104.4(2) . . ? C2 B11 B10 104.5(2) . . ? B12 B11 B10 60.7(2) . . ? C2 B11 B6 58.88(15) . . ? B12 B11 B6 108.1(2) . . ? B10 B11 B6 59.4(2) . . ? C2 B11 B7 58.3(2) . . ? B12 B11 B7 60.1(2) . . ? B10 B11 B7 108.5(2) . . ? B6 B11 B7 108.0(2) . . ? C2 B11 H11 125.10(13) . . ? B12 B11 H11 122.14(13) . . ? B10 B11 H11 122.20(13) . . ? B6 B11 H11 121.57(13) . . ? B7 B11 H11 121.35(13) . . ? B11 B12 B9 107.7(2) . . ? B11 B12 B7 60.3(2) . . ? B9 B12 B7 107.5(2) . . ? B11 B12 B10 59.7(2) . . ? B9 B12 B10 60.0(2) . . ? B7 B12 B10 107.9(2) . . ? B11 B12 B8 107.9(2) . . ? B9 B12 B8 59.9(2) . . ? B7 B12 B8 59.7(2) . . ? B10 B12 B8 108.0(2) . . ? B11 B12 H12 121.79(13) . . ? B9 B12 H12 121.97(13) . . ? B7 B12 H12 121.88(13) . . ? B10 B12 H12 121.76(13) . . ? B8 B12 H12 121.83(14) . . ? C22 C21 B25 110.5(2) . . ? C22 C21 B24 110.5(2) . . ? B25 C21 B24 63.2(2) . . ? C22 C21 B23 61.0(2) . . ? B25 C21 B23 115.2(2) . . ? B24 C21 B23 62.9(2) . . ? C22 C21 B26 60.8(2) . . ? B25 C21 B26 62.8(2) . . ? B24 C21 B26 115.0(2) . . ? B23 C21 B26 114.4(2) . . ? C22 C21 S2 114.3(2) . . ? B25 C21 S2 128.0(2) . . ? B24 C21 S2 120.1(2) . . ? B23 C21 S2 108.9(2) . . ? B26 C21 S2 120.7(2) . . ? C21 C22 B27 112.4(2) . . ? C21 C22 B31 112.4(2) . . ? B27 C22 B31 63.5(2) . . ? C21 C22 B26 61.73(15) . . ? B27 C22 B26 116.5(2) . . ? B31 C22 B26 63.5(2) . . ? C21 C22 B23 61.46(15) . . ? B27 C22 B23 63.3(2) . . ? B31 C22 B23 116.0(2) . . ? B26 C22 B23 115.5(2) . . ? C21 C22 H22 120.71(13) . . ? B27 C22 H22 117.28(14) . . ? B31 C22 H22 117.41(14) . . ? B26 C22 H22 116.60(14) . . ? B23 C22 H22 116.99(13) . . ? C22 B23 C21 57.51(14) . . ? C22 B23 B28 103.9(2) . . ? C21 B23 B28 104.5(2) . . ? C22 B23 B24 104.0(2) . . ? C21 B23 B24 58.05(15) . . ? B28 B23 B24 60.1(2) . . ? C22 B23 B27 57.6(2) . . ? C21 B23 B27 104.6(2) . . ? B28 B23 B27 60.5(2) . . ? B24 B23 B27 108.2(2) . . ? C22 B23 H23 125.27(13) . . ? C21 B23 H23 124.56(12) . . ? B28 B23 H23 122.98(14) . . ? B24 B23 H23 122.36(13) . . ? B27 B23 H23 122.07(14) . . ? C21 B24 B29 104.6(2) . . ? C21 B24 B28 104.7(2) . . ? B29 B24 B28 60.8(2) . . ? C21 B24 B25 58.40(15) . . ? B29 B24 B25 60.1(2) . . ? B28 B24 B25 108.7(2) . . ? C21 B24 B23 59.09(15) . . ? B29 B24 B23 108.0(2) . . ? B28 B24 B23 59.3(2) . . ? B25 B24 B23 108.2(2) . . ? C21 B24 H24 124.88(12) . . ? B29 B24 H24 122.16(14) . . ? B28 B24 H24 122.08(13) . . ? B25 B24 H24 121.27(13) . . ? B23 B24 H24 121.57(13) . . ? C21 B25 B30 104.7(2) . . ? C21 B25 B29 104.2(2) . . ? B30 B25 B29 60.3(2) . . ? C21 B25 B24 58.44(14) . . ? B30 B25 B24 107.9(2) . . ? B29 B25 B24 59.5(2) . . ? C21 B25 B26 59.28(15) . . ? B30 B25 B26 59.6(2) . . ? B29 B25 B26 107.9(2) . . ? B24 B25 B26 108.2(2) . . ? C21 B25 H25 124.82(13) . . ? B30 B25 H25 122.39(14) . . ? B29 B25 H25 122.65(14) . . ? B24 B25 H25 121.64(13) . . ? B26 B25 H25 121.28(14) . . ? C22 B26 C21 57.44(14) . . ? C22 B26 B30 103.5(2) . . ? C21 B26 B30 103.9(2) . . ? C22 B26 B25 103.9(2) . . ? C21 B26 B25 57.89(14) . . ? B30 B26 B25 59.9(2) . . ? C22 B26 B31 57.6(2) . . ? C21 B26 B31 104.3(2) . . ? B30 B26 B31 60.2(2) . . ? B25 B26 B31 107.9(2) . . ? C22 B26 H26 125.27(14) . . ? C21 B26 H26 124.86(13) . . ? B30 B26 H26 123.42(14) . . ? B25 B26 H26 122.44(14) . . ? B31 B26 H26 122.25(14) . . ? C22 B27 B31 58.3(2) . . ? C22 B27 B32 103.7(2) . . ? B31 B27 B32 60.0(2) . . ? C22 B27 B23 59.1(2) . . ? B31 B27 B23 108.2(2) . . ? B32 B27 B23 107.3(2) . . ? C22 B27 B28 103.9(2) . . ? B31 B27 B28 108.1(2) . . ? B32 B27 B28 60.0(2) . . ? B23 B27 B28 59.1(2) . . ? C22 B27 H27 125.30(14) . . ? B31 B27 H27 121.24(14) . . ? B32 B27 H27 122.83(14) . . ? B23 B27 H27 121.63(14) . . ? B28 B27 H27 122.70(15) . . ? B23 B28 B24 60.6(2) . . ? B23 B28 B32 108.0(2) . . ? B24 B28 B32 107.4(2) . . ? B23 B28 B27 60.3(2) . . ? B24 B28 B27 108.4(2) . . ? B32 B28 B27 59.8(2) . . ? B23 B28 B29 107.8(2) . . ? B24 B28 B29 59.3(2) . . ? B32 B28 B29 59.7(2) . . ? B27 B28 B29 107.5(2) . . ? B23 B28 H28 121.35(14) . . ? B24 B28 H28 121.76(13) . . ? B32 B28 H28 122.10(14) . . ? B27 B28 H28 121.60(14) . . ? B29 B28 H28 122.28(14) . . ? B24 B29 B25 60.4(2) . . ? B24 B29 B32 108.1(2) . . ? B25 B29 B32 108.3(2) . . ? B24 B29 B30 108.2(2) . . ? B25 B29 B30 59.8(2) . . ? B32 B29 B30 60.3(2) . . ? B24 B29 B28 59.9(2) . . ? B25 B29 B28 108.3(2) . . ? B32 B29 B28 60.0(2) . . ? B30 B29 B28 108.2(2) . . ? B24 B29 H29 121.59(14) . . ? B25 B29 H29 121.52(14) . . ? B32 B29 H29 121.59(14) . . ? B30 B29 H29 121.58(14) . . ? B28 B29 H29 121.70(14) . . ? B26 B30 B25 60.5(2) . . ? B26 B30 B29 108.3(2) . . ? B25 B30 B29 59.9(2) . . ? B26 B30 B31 60.4(2) . . ? B25 B30 B31 108.5(2) . . ? B29 B30 B31 107.7(2) . . ? B26 B30 B32 108.1(2) . . ? B25 B30 B32 107.8(2) . . ? B29 B30 B32 59.7(2) . . ? B31 B30 B32 59.7(2) . . ? B26 B30 H30 121.26(14) . . ? B25 B30 H30 121.48(14) . . ? B29 B30 H30 121.93(14) . . ? B31 B30 H30 121.63(13) . . ? B32 B30 H30 122.05(13) . . ? C22 B31 B27 58.2(2) . . ? C22 B31 B32 103.7(2) . . ? B27 B31 B32 60.1(2) . . ? C22 B31 B30 103.9(2) . . ? B27 B31 B30 108.4(2) . . ? B32 B31 B30 60.3(2) . . ? C22 B31 B26 58.9(2) . . ? B27 B31 B26 108.3(2) . . ? B32 B31 B26 107.8(2) . . ? B30 B31 B26 59.4(2) . . ? C22 B31 H31 125.54(13) . . ? B27 B31 H31 121.19(14) . . ? B32 B31 H31 122.56(13) . . ? B30 B31 H31 122.51(13) . . ? B26 B31 H31 121.43(14) . . ? B31 B32 B29 108.1(2) . . ? B31 B32 B27 59.9(2) . . ? B29 B32 B27 108.4(2) . . ? B31 B32 B28 108.2(2) . . ? B29 B32 B28 60.4(2) . . ? B27 B32 B28 60.2(2) . . ? B31 B32 B30 60.0(2) . . ? B29 B32 B30 59.9(2) . . ? B27 B32 B30 108.0(2) . . ? B28 B32 B30 108.2(2) . . ? B31 B32 H32 121.72(13) . . ? B29 B32 H32 121.47(14) . . ? B27 B32 H32 121.60(14) . . ? B28 B32 H32 121.44(14) . . ? B30 B32 H32 121.77(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 S1 S2 C21 100.20(11) . . . . ? C2 C1 S1 S2 108.6(2) . . . . ? C22 C21 S2 S1 111.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.196 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.041 #===END data_[1-S-2-Me-1,2-C~2~B~10~H~10~]~2~ _database_code_depnum_ccdc_archive 'CCDC 263593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H26 B20 S2' _chemical_formula_sum 'C6 H26 B20 S2' _chemical_formula_weight 378.59 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' 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 'C 2/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 18.538(6) _cell_length_b 15.360(7) _cell_length_c 15.282(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.22(2) _cell_angle_gamma 90.00 _cell_volume 4351(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.02 _cell_measurement_theta_max 15.93 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North, Phillips & Mathews 1968' _exptl_absorpt_correction_T_min 0.9500 _exptl_absorpt_correction_T_max 0.9768 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 3955 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3828 _reflns_number_gt 2402 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_data_reduction ; Texsan Process (Molecular Structure Corporation, 1993) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0002P)^2^+34.0508P] 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 3828 _refine_ls_number_parameters 255 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1502 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.2130 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.147 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.63446(9) 0.84733(11) 0.27394(10) 0.0463(5) Uani 1 d . . . S2 S 0.65325(9) 0.76258(10) 0.37340(11) 0.0409(4) Uani 1 d . . . C1 C 0.6983(3) 0.9331(4) 0.2884(4) 0.0354(14) Uani 1 d . . . C2 C 0.7666(3) 0.9375(4) 0.2136(4) 0.0410(15) Uani 1 d . . . B3 B 0.6942(4) 1.0078(5) 0.2050(5) 0.0405(17) Uani 1 d . . . H3 H 0.6542 1.0056 0.1517 0.049 Uiso 1 calc R . . B4 B 0.6697(4) 1.0348(5) 0.3144(4) 0.0418(18) Uani 1 d . . . H4 H 0.6139 1.0516 0.3319 0.050 Uiso 1 calc R . . B5 B 0.7268(4) 0.9738(5) 0.3859(5) 0.0408(17) Uani 1 d . . . H5 H 0.7078 0.9508 0.4499 0.049 Uiso 1 calc R . . B6 B 0.7857(4) 0.9090(5) 0.3204(5) 0.0452(18) Uani 1 d . . . H6 H 0.8042 0.8441 0.3409 0.054 Uiso 1 calc R . . B7 B 0.7848(4) 1.0415(5) 0.1888(5) 0.0457(19) Uani 1 d . . . H7 H 0.8038 1.0631 0.1243 0.055 Uiso 1 calc R . . B8 B 0.7254(4) 1.1062(5) 0.2522(5) 0.0486(19) Uani 1 d . . . H8 H 0.7058 1.1699 0.2292 0.058 Uiso 1 calc R . . B9 B 0.7463(4) 1.0857(5) 0.3663(5) 0.0470(19) Uani 1 d . . . H9 H 0.7406 1.1358 0.4173 0.056 Uiso 1 calc R . . B10 B 0.8165(4) 1.0070(5) 0.3683(5) 0.050(2) Uani 1 d . . . H10 H 0.8566 1.0061 0.4215 0.060 Uiso 1 calc R . . B11 B 0.8407(4) 0.9811(5) 0.2591(5) 0.052(2) Uani 1 d . . . H11 H 0.8960 0.9633 0.2406 0.062 Uiso 1 calc R . . B12 B 0.8159(4) 1.0893(5) 0.2875(5) 0.0457(18) Uani 1 d . . . H12 H 0.8553 1.1428 0.2880 0.055 Uiso 1 calc R . . C13 C 0.7706(4) 0.8657(5) 0.1454(4) 0.0587(19) Uani 1 d . . . H13A H 0.7395 0.8186 0.1620 0.088 Uiso 1 calc R . . H13B H 0.8193 0.8449 0.1414 0.088 Uiso 1 calc R . . H13C H 0.7556 0.8881 0.0896 0.088 Uiso 1 calc R . . C21 C 0.5812(3) 0.7785(4) 0.4495(4) 0.0336(13) Uani 1 d . . . C22 C 0.5164(3) 0.6992(4) 0.4515(4) 0.0423(15) Uani 1 d . . . B23 B 0.5834(4) 0.7020(5) 0.5292(5) 0.0439(18) Uani 1 d . . . H23 H 0.6259 0.6522 0.5340 0.053 Uiso 1 calc R . . B24 B 0.5998(4) 0.8140(5) 0.5521(5) 0.0475(19) Uani 1 d . . . H24 H 0.6527 0.8379 0.5742 0.057 Uiso 1 calc R . . B25 B 0.5450(4) 0.8750(5) 0.4785(5) 0.0479(19) Uani 1 d . . . H25 H 0.5623 0.9382 0.4521 0.058 Uiso 1 calc R . . B26 B 0.4952(4) 0.7997(5) 0.4150(5) 0.0451(18) Uani 1 d . . . H26 H 0.4809 0.8133 0.3464 0.054 Uiso 1 calc R . . B27 B 0.4927(4) 0.6801(5) 0.5572(5) 0.051(2) Uani 1 d . . . H27 H 0.4762 0.6162 0.5826 0.062 Uiso 1 calc R . . B28 B 0.5437(4) 0.7535(6) 0.6218(5) 0.058(2) Uani 1 d U . . H28 H 0.5604 0.7379 0.6892 0.070 Uiso 1 calc R . . B29 B 0.5183(4) 0.8596(6) 0.5900(5) 0.054(2) Uani 1 d . . . H29 H 0.5175 0.9137 0.6371 0.064 Uiso 1 calc R . . B30 B 0.4540(4) 0.8523(5) 0.5045(5) 0.050(2) Uani 1 d . . . H30 H 0.4117 0.9017 0.4954 0.060 Uiso 1 calc R . . B31 B 0.4369(4) 0.7402(6) 0.4849(5) 0.053(2) Uani 1 d . . . H31 H 0.3838 0.7162 0.4631 0.063 Uiso 1 calc R . . B32 B 0.4533(4) 0.7766(6) 0.5938(5) 0.053(2) Uani 1 d . . . H32 H 0.4104 0.7764 0.6434 0.064 Uiso 1 calc R . . C33 C 0.5207(4) 0.6244(5) 0.3854(5) 0.065(2) Uani 1 d U . . H33A H 0.5315 0.6473 0.3285 0.097 Uiso 1 calc R . . H33B H 0.4753 0.5943 0.3834 0.097 Uiso 1 calc R . . H33C H 0.5580 0.5846 0.4029 0.097 Uiso 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 S1 0.0497(10) 0.0553(11) 0.0340(8) 0.0001(8) -0.0054(7) -0.0174(8) S2 0.0425(9) 0.0344(8) 0.0459(9) -0.0019(7) 0.0097(7) 0.0008(7) C1 0.033(3) 0.039(3) 0.034(3) 0.004(3) 0.000(3) 0.000(3) C2 0.046(4) 0.037(3) 0.040(4) 0.004(3) 0.009(3) 0.008(3) B3 0.042(4) 0.041(4) 0.038(4) 0.011(3) -0.006(3) 0.007(3) B4 0.044(4) 0.046(4) 0.036(4) -0.002(3) 0.004(3) 0.004(3) B5 0.043(4) 0.046(4) 0.033(4) 0.003(3) -0.002(3) -0.009(3) B6 0.040(4) 0.043(4) 0.052(5) 0.016(4) -0.010(3) -0.002(3) B7 0.057(5) 0.038(4) 0.043(4) 0.011(3) 0.011(4) -0.001(4) B8 0.061(5) 0.038(4) 0.047(4) 0.005(4) -0.006(4) 0.006(4) B9 0.062(5) 0.042(4) 0.037(4) 0.002(3) -0.003(4) -0.009(4) B10 0.044(4) 0.048(5) 0.058(5) 0.019(4) -0.018(4) -0.011(4) B11 0.040(4) 0.049(5) 0.067(6) 0.011(4) 0.000(4) -0.003(4) B12 0.052(5) 0.040(4) 0.045(4) 0.007(4) -0.004(4) -0.007(4) C13 0.069(5) 0.056(5) 0.051(4) -0.005(4) 0.012(4) 0.003(4) C21 0.034(3) 0.031(3) 0.035(3) -0.002(3) 0.002(3) -0.003(3) C22 0.040(4) 0.037(3) 0.050(4) -0.007(3) 0.004(3) -0.010(3) B23 0.050(5) 0.043(4) 0.038(4) 0.008(3) -0.006(3) 0.007(4) B24 0.048(5) 0.056(5) 0.038(4) -0.016(4) 0.001(3) -0.012(4) B25 0.048(5) 0.034(4) 0.061(5) -0.004(4) 0.016(4) 0.005(4) B26 0.037(4) 0.052(5) 0.046(4) 0.006(4) -0.003(3) 0.008(4) B27 0.054(5) 0.046(5) 0.054(5) 0.006(4) 0.010(4) -0.004(4) B28 0.061(5) 0.078(6) 0.036(4) 0.013(4) 0.007(4) 0.013(5) B29 0.050(5) 0.059(5) 0.052(5) -0.017(4) 0.011(4) -0.012(4) B30 0.040(4) 0.052(5) 0.058(5) 0.004(4) 0.011(4) 0.016(4) B31 0.039(4) 0.061(5) 0.057(5) -0.006(4) 0.002(4) -0.010(4) B32 0.042(4) 0.062(5) 0.056(5) 0.001(4) 0.009(4) 0.001(4) C33 0.065(4) 0.059(4) 0.070(4) -0.020(3) 0.007(3) -0.013(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 S1 C1 1.785(6) . ? S1 S2 2.030(2) . ? S2 C21 1.791(6) . ? C1 B4 1.697(9) . ? C1 B5 1.698(9) . ? C1 C2 1.710(8) . ? C1 B3 1.716(9) . ? C1 B6 1.731(9) . ? C2 C13 1.521(8) . ? C2 B11 1.676(10) . ? C2 B7 1.676(9) . ? C2 B6 1.726(9) . ? C2 B3 1.727(9) . ? B3 B8 1.771(10) . ? B3 B7 1.776(10) . ? B3 B4 1.783(10) . ? B3 H3 1.1000 . ? B4 B8 1.783(10) . ? B4 B5 1.785(10) . ? B4 B9 1.803(10) . ? B4 H4 1.1000 . ? B5 B10 1.761(10) . ? B5 B9 1.782(10) . ? B5 B6 1.786(11) . ? B5 H5 1.1000 . ? B6 B10 1.766(11) . ? B6 B11 1.775(10) . ? B6 H6 1.1000 . ? B7 B11 1.755(11) . ? B7 B12 1.772(11) . ? B7 B8 1.773(11) . ? B7 H7 1.1000 . ? B8 B12 1.779(11) . ? B8 B9 1.812(10) . ? B8 H8 1.1000 . ? B9 B12 1.770(11) . ? B9 B10 1.777(11) . ? B9 H9 1.1000 . ? B10 B12 1.767(10) . ? B10 B11 1.775(12) . ? B10 H10 1.1000 . ? B11 B12 1.779(11) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C21 B25 1.686(9) . ? C21 B23 1.693(9) . ? C21 B24 1.696(9) . ? C21 B26 1.708(9) . ? C21 C22 1.711(8) . ? C22 C33 1.532(9) . ? C22 B31 1.684(10) . ? C22 B26 1.688(10) . ? C22 B27 1.700(9) . ? C22 B23 1.716(9) . ? B23 B27 1.768(11) . ? B23 B24 1.781(11) . ? B23 B28 1.783(11) . ? B23 H23 1.1000 . ? B24 B28 1.757(11) . ? B24 B29 1.764(11) . ? B24 B25 1.778(11) . ? B24 H24 1.1000 . ? B25 B26 1.768(11) . ? B25 B30 1.770(10) . ? B25 B29 1.792(11) . ? B25 H25 1.1000 . ? B26 B30 1.765(10) . ? B26 B31 1.777(11) . ? B26 H26 1.1000 . ? B27 B32 1.746(11) . ? B27 B28 1.769(12) . ? B27 B31 1.770(11) . ? B27 H27 1.1000 . ? B28 B29 1.763(12) . ? B28 B32 1.764(11) . ? B28 H28 1.1000 . ? B29 B32 1.755(11) . ? B29 B30 1.770(11) . ? B29 H29 1.1000 . ? B30 B31 1.776(11) . ? B30 B32 1.791(11) . ? B30 H30 1.1000 . ? B31 B32 1.780(11) . ? B31 H31 1.1000 . ? B32 H32 1.1000 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 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 C1 S1 S2 105.6(2) . . ? C21 S2 S1 105.8(2) . . ? B4 C1 B5 63.4(4) . . ? B4 C1 C2 110.7(4) . . ? B5 C1 C2 110.1(5) . . ? B4 C1 B3 63.0(4) . . ? B5 C1 B3 114.8(5) . . ? C2 C1 B3 60.6(4) . . ? B4 C1 B6 115.1(5) . . ? B5 C1 B6 62.8(4) . . ? C2 C1 B6 60.2(4) . . ? B3 C1 B6 113.1(5) . . ? B4 C1 S1 120.0(4) . . ? B5 C1 S1 125.7(4) . . ? C2 C1 S1 116.0(4) . . ? B3 C1 S1 112.0(4) . . ? B6 C1 S1 119.8(4) . . ? C13 C2 B11 122.1(6) . . ? C13 C2 B7 121.7(5) . . ? B11 C2 B7 63.1(4) . . ? C13 C2 C1 117.9(5) . . ? B11 C2 C1 110.3(5) . . ? B7 C2 C1 109.8(5) . . ? C13 C2 B6 117.0(5) . . ? B11 C2 B6 62.9(4) . . ? B7 C2 B6 114.5(5) . . ? C1 C2 B6 60.5(4) . . ? C13 C2 B3 116.2(5) . . ? B11 C2 B3 114.7(5) . . ? B7 C2 B3 62.9(4) . . ? C1 C2 B3 59.9(4) . . ? B6 C2 B3 112.8(5) . . ? C1 B3 C2 59.5(3) . . ? C1 B3 B8 104.7(5) . . ? C2 B3 B8 104.4(5) . . ? C1 B3 B7 105.0(5) . . ? C2 B3 B7 57.2(4) . . ? B8 B3 B7 60.0(4) . . ? C1 B3 B4 58.0(4) . . ? C2 B3 B4 106.0(5) . . ? B8 B3 B4 60.2(4) . . ? B7 B3 B4 107.9(5) . . ? C1 B3 H3 123.9 . . ? C2 B3 H3 123.9 . . ? B8 B3 H3 123.1 . . ? B7 B3 H3 122.7 . . ? B4 B3 H3 121.9 . . ? C1 B4 B3 59.0(4) . . ? C1 B4 B8 105.0(5) . . ? B3 B4 B8 59.6(4) . . ? C1 B4 B5 58.3(4) . . ? B3 B4 B5 107.4(5) . . ? B8 B4 B5 107.8(5) . . ? C1 B4 B9 104.8(5) . . ? B3 B4 B9 108.1(5) . . ? B8 B4 B9 60.7(4) . . ? B5 B4 B9 59.6(4) . . ? C1 B4 H4 124.6 . . ? B3 B4 H4 121.7 . . ? B8 B4 H4 122.2 . . ? B5 B4 H4 122.1 . . ? B9 B4 H4 122.1 . . ? C1 B5 B10 105.3(5) . . ? C1 B5 B9 105.6(5) . . ? B10 B5 B9 60.2(4) . . ? C1 B5 B4 58.3(4) . . ? B10 B5 B4 108.2(5) . . ? B9 B5 B4 60.7(4) . . ? C1 B5 B6 59.5(4) . . ? B10 B5 B6 59.7(4) . . ? B9 B5 B6 108.6(5) . . ? B4 B5 B6 108.2(5) . . ? C1 B5 H5 124.3 . . ? B10 B5 H5 122.4 . . ? B9 B5 H5 121.7 . . ? B4 B5 H5 121.5 . . ? B6 B5 H5 121.2 . . ? C2 B6 C1 59.3(4) . . ? C2 B6 B10 103.9(5) . . ? C1 B6 B10 103.6(5) . . ? C2 B6 B11 57.2(4) . . ? C1 B6 B11 104.8(5) . . ? B10 B6 B11 60.2(4) . . ? C2 B6 B5 105.3(5) . . ? C1 B6 B5 57.7(4) . . ? B10 B6 B5 59.4(4) . . ? B11 B6 B5 107.6(5) . . ? C2 B6 H6 124.2 . . ? C1 B6 H6 124.4 . . ? B10 B6 H6 123.7 . . ? B11 B6 H6 122.5 . . ? B5 B6 H6 122.4 . . ? C2 B7 B11 58.4(4) . . ? C2 B7 B12 105.5(5) . . ? B11 B7 B12 60.6(4) . . ? C2 B7 B8 106.5(5) . . ? B11 B7 B8 109.2(6) . . ? B12 B7 B8 60.2(4) . . ? C2 B7 B3 60.0(4) . . ? B11 B7 B3 108.5(5) . . ? B12 B7 B3 107.9(5) . . ? B8 B7 B3 59.9(4) . . ? C2 B7 H7 123.8 . . ? B11 B7 H7 121.1 . . ? B12 B7 H7 122.2 . . ? B8 B7 H7 121.5 . . ? B3 B7 H7 121.3 . . ? B3 B8 B7 60.1(4) . . ? B3 B8 B12 107.8(5) . . ? B7 B8 B12 59.8(4) . . ? B3 B8 B4 60.2(4) . . ? B7 B8 B4 108.0(5) . . ? B12 B8 B4 107.2(5) . . ? B3 B8 B9 108.2(5) . . ? B7 B8 B9 107.3(5) . . ? B12 B8 B9 59.0(4) . . ? B4 B8 B9 60.2(4) . . ? B3 B8 H8 121.4 . . ? B7 B8 H8 121.8 . . ? B12 B8 H8 122.4 . . ? B4 B8 H8 121.7 . . ? B9 B8 H8 122.1 . . ? B12 B9 B10 59.8(4) . . ? B12 B9 B5 107.0(5) . . ? B10 B9 B5 59.3(4) . . ? B12 B9 B4 106.8(5) . . ? B10 B9 B4 106.8(5) . . ? B5 B9 B4 59.7(4) . . ? B12 B9 B8 59.5(4) . . ? B10 B9 B8 106.8(5) . . ? B5 B9 B8 106.6(5) . . ? B4 B9 B8 59.1(4) . . ? B12 B9 H9 122.2 . . ? B10 B9 H9 122.4 . . ? B5 B9 H9 122.4 . . ? B4 B9 H9 122.5 . . ? B8 B9 H9 122.6 . . ? B5 B10 B6 60.9(4) . . ? B5 B10 B12 108.1(5) . . ? B6 B10 B12 108.6(5) . . ? B5 B10 B11 108.7(5) . . ? B6 B10 B11 60.1(4) . . ? B12 B10 B11 60.3(4) . . ? B5 B10 B9 60.5(4) . . ? B6 B10 B9 109.7(5) . . ? B12 B10 B9 59.9(4) . . ? B11 B10 B9 108.9(5) . . ? B5 B10 H10 121.3 . . ? B6 B10 H10 120.8 . . ? B12 B10 H10 121.8 . . ? B11 B10 H10 121.3 . . ? B9 B10 H10 120.9 . . ? C2 B11 B7 58.4(4) . . ? C2 B11 B6 59.9(4) . . ? B7 B11 B6 108.3(5) . . ? C2 B11 B10 105.6(5) . . ? B7 B11 B10 107.8(6) . . ? B6 B11 B10 59.7(4) . . ? C2 B11 B12 105.2(5) . . ? B7 B11 B12 60.2(4) . . ? B6 B11 B12 107.7(6) . . ? B10 B11 B12 59.6(4) . . ? C2 B11 H11 123.9 . . ? B7 B11 H11 121.6 . . ? B6 B11 H11 121.2 . . ? B10 B11 H11 122.4 . . ? B12 B11 H11 122.5 . . ? B10 B12 B9 60.3(4) . . ? B10 B12 B7 107.4(5) . . ? B9 B12 B7 109.3(5) . . ? B10 B12 B11 60.1(4) . . ? B9 B12 B11 109.1(5) . . ? B7 B12 B11 59.2(4) . . ? B10 B12 B8 108.6(5) . . ? B9 B12 B8 61.4(4) . . ? B7 B12 B8 59.9(4) . . ? B11 B12 B8 107.8(5) . . ? B10 B12 H12 121.8 . . ? B9 B12 H12 120.3 . . ? B7 B12 H12 122.0 . . ? B11 B12 H12 121.9 . . ? B8 B12 H12 121.3 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? B25 C21 B23 115.4(5) . . ? B25 C21 B24 63.4(4) . . ? B23 C21 B24 63.4(4) . . ? B25 C21 B26 62.8(4) . . ? B23 C21 B26 112.0(5) . . ? B24 C21 B26 114.2(5) . . ? B25 C21 C22 110.0(5) . . ? B23 C21 C22 60.5(4) . . ? B24 C21 C22 110.6(5) . . ? B26 C21 C22 59.2(4) . . ? B25 C21 S2 126.1(4) . . ? B23 C21 S2 110.9(4) . . ? B24 C21 S2 119.6(4) . . ? B26 C21 S2 121.6(4) . . ? C22 C21 S2 116.1(4) . . ? C33 C22 B31 121.9(5) . . ? C33 C22 B26 118.7(6) . . ? B31 C22 B26 63.6(4) . . ? C33 C22 B27 120.8(6) . . ? B31 C22 B27 63.1(4) . . ? B26 C22 B27 114.3(5) . . ? C33 C22 C21 118.9(5) . . ? B31 C22 C21 110.8(5) . . ? B26 C22 C21 60.3(4) . . ? B27 C22 C21 108.9(5) . . ? C33 C22 B23 115.9(6) . . ? B31 C22 B23 114.4(5) . . ? B26 C22 B23 111.9(5) . . ? B27 C22 B23 62.3(4) . . ? C21 C22 B23 59.2(4) . . ? C21 B23 C22 60.2(4) . . ? C21 B23 B27 106.6(5) . . ? C22 B23 B27 58.4(4) . . ? C21 B23 B24 58.4(4) . . ? C22 B23 B24 106.4(5) . . ? B27 B23 B24 107.3(6) . . ? C21 B23 B28 104.8(5) . . ? C22 B23 B28 105.1(5) . . ? B27 B23 B28 59.7(5) . . ? B24 B23 B28 59.1(4) . . ? C21 B23 H23 123.1 . . ? C22 B23 H23 123.0 . . ? B27 B23 H23 122.2 . . ? B24 B23 H23 122.5 . . ? B28 B23 H23 123.6 . . ? C21 B24 B28 105.8(5) . . ? C21 B24 B29 105.1(5) . . ? B28 B24 B29 60.1(5) . . ? C21 B24 B25 58.0(4) . . ? B28 B24 B25 108.9(6) . . ? B29 B24 B25 60.8(4) . . ? C21 B24 B23 58.2(4) . . ? B28 B24 B23 60.5(4) . . ? B29 B24 B23 107.6(6) . . ? B25 B24 B23 106.7(5) . . ? C21 B24 H24 124.7 . . ? B28 B24 H24 121.4 . . ? B29 B24 H24 122.1 . . ? B25 B24 H24 121.7 . . ? B23 B24 H24 122.2 . . ? C21 B25 B26 59.2(4) . . ? C21 B25 B30 105.4(5) . . ? B26 B25 B30 59.8(4) . . ? C21 B25 B24 58.5(4) . . ? B26 B25 B24 107.4(5) . . ? B30 B25 B24 107.3(5) . . ? C21 B25 B29 104.2(5) . . ? B26 B25 B29 106.9(5) . . ? B30 B25 B29 59.6(4) . . ? B24 B25 B29 59.2(4) . . ? C21 B25 H25 124.2 . . ? B26 B25 H25 121.8 . . ? B30 B25 H25 122.3 . . ? B24 B25 H25 122.1 . . ? B29 B25 H25 123.2 . . ? C22 B26 C21 60.5(4) . . ? C22 B26 B30 105.2(5) . . ? C21 B26 B30 104.7(5) . . ? C22 B26 B25 107.2(5) . . ? C21 B26 B25 58.0(4) . . ? B30 B26 B25 60.1(4) . . ? C22 B26 B31 58.1(4) . . ? C21 B26 B31 106.6(5) . . ? B30 B26 B31 60.2(4) . . ? B25 B26 B31 108.9(5) . . ? C22 B26 H26 122.9 . . ? C21 B26 H26 123.4 . . ? B30 B26 H26 123.3 . . ? B25 B26 H26 121.5 . . ? B31 B26 H26 121.7 . . ? C22 B27 B32 105.6(6) . . ? C22 B27 B23 59.3(4) . . ? B32 B27 B23 108.4(6) . . ? C22 B27 B28 106.4(5) . . ? B32 B27 B28 60.2(5) . . ? B23 B27 B28 60.5(4) . . ? C22 B27 B31 58.0(4) . . ? B32 B27 B31 60.8(5) . . ? B23 B27 B31 107.7(5) . . ? B28 B27 B31 109.0(6) . . ? C22 B27 H27 124.2 . . ? B32 B27 H27 121.8 . . ? B23 B27 H27 121.4 . . ? B28 B27 H27 121.3 . . ? B31 B27 H27 121.5 . . ? B24 B28 B29 60.1(5) . . ? B24 B28 B32 108.1(6) . . ? B29 B28 B32 59.7(5) . . ? B24 B28 B27 108.3(5) . . ? B29 B28 B27 107.1(6) . . ? B32 B28 B27 59.2(5) . . ? B24 B28 B23 60.4(4) . . ? B29 B28 B23 107.5(5) . . ? B32 B28 B23 107.0(6) . . ? B27 B28 B23 59.7(4) . . ? B24 B28 H28 121.1 . . ? B29 B28 H28 122.1 . . ? B32 B28 H28 122.3 . . ? B27 B28 H28 122.1 . . ? B23 B28 H28 122.1 . . ? B32 B29 B28 60.2(5) . . ? B32 B29 B24 108.2(6) . . ? B28 B29 B24 59.8(5) . . ? B32 B29 B30 61.1(5) . . ? B28 B29 B30 108.8(6) . . ? B24 B29 B30 107.9(5) . . ? B32 B29 B25 108.6(6) . . ? B28 B29 B25 108.0(6) . . ? B24 B29 B25 60.0(4) . . ? B30 B29 B25 59.6(4) . . ? B32 B29 H29 121.1 . . ? B28 B29 H29 121.6 . . ? B24 B29 H29 121.9 . . ? B30 B29 H29 121.3 . . ? B25 B29 H29 121.8 . . ? B26 B30 B29 108.0(5) . . ? B26 B30 B25 60.0(4) . . ? B29 B30 B25 60.8(4) . . ? B26 B30 B31 60.2(4) . . ? B29 B30 B31 107.8(6) . . ? B25 B30 B31 108.8(5) . . ? B26 B30 B32 107.3(6) . . ? B29 B30 B32 59.0(4) . . ? B25 B30 B32 107.9(5) . . ? B31 B30 B32 59.9(5) . . ? B26 B30 H30 121.9 . . ? B29 B30 H30 121.9 . . ? B25 B30 H30 121.1 . . ? B31 B30 H30 121.4 . . ? B32 B30 H30 122.4 . . ? C22 B31 B27 58.9(4) . . ? C22 B31 B30 104.9(5) . . ? B27 B31 B30 107.2(6) . . ? C22 B31 B26 58.3(4) . . ? B27 B31 B26 106.7(5) . . ? B30 B31 B26 59.6(4) . . ? C22 B31 B32 104.7(5) . . ? B27 B31 B32 58.9(4) . . ? B30 B31 B32 60.5(5) . . ? B26 B31 B32 107.3(5) . . ? C22 B31 H31 124.4 . . ? B27 B31 H31 122.4 . . ? B30 B31 H31 122.3 . . ? B26 B31 H31 122.3 . . ? B32 B31 H31 122.6 . . ? B27 B32 B29 108.5(6) . . ? B27 B32 B28 60.5(5) . . ? B29 B32 B28 60.1(5) . . ? B27 B32 B31 60.3(5) . . ? B29 B32 B31 108.2(6) . . ? B28 B32 B31 108.8(6) . . ? B27 B32 B30 107.6(6) . . ? B29 B32 B30 59.9(5) . . ? B28 B32 B30 107.8(6) . . ? B31 B32 B30 59.6(5) . . ? B27 B32 H32 121.5 . . ? B29 B32 H32 121.5 . . ? B28 B32 H32 121.3 . . ? B31 B32 H32 121.4 . . ? B30 B32 H32 122.3 . . ? C22 C33 H33A 109.5 . . ? C22 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C22 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 S1 C1 C2 C13 -4.0(7) . . . . ? S2 C21 C22 C33 -4.2(7) . . . . ? C2 C1 S1 S2 109.0(4) . . . . ? C22 C21 S2 S1 105.6(4) . . . . ? C1 S1 S2 C21 105.1(3) . . . . ? C13 C2 C22 C33 1.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.337 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.069 #===END data_[1-S-2-Ph-1,2-C~2~B~10~H~10~]~2~ _database_code_depnum_ccdc_archive 'CCDC 263594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H30 B20 S2' _chemical_formula_sum 'C16 H30 B20 S2' _chemical_formula_weight 502.72 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' 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 11.579(3) _cell_length_b 12.917(4) _cell_length_c 10.511(5) _cell_angle_alpha 110.95(3) _cell_angle_beta 102.28(3) _cell_angle_gamma 85.09(3) _cell_volume 1434.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 19 _cell_measurement_theta_min 4.42 _cell_measurement_theta_max 10.36 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9402 _exptl_absorpt_correction_T_max 0.9695 _exptl_absorpt_process_details 'North, Phillips & Mathews 1968' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5059 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.3254 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5059 _reflns_number_gt 2640 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_data_reduction ; Texsan Process (Molecular Structure Corporation, 1993) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0775P)^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 5059 _refine_ls_number_parameters 346 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1754 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1837 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1A S 0.00685(9) 0.66752(9) 0.23097(12) 0.0421(3) Uani 0.934(2) d P A 1 S2A S 0.03703(10) 0.82653(10) 0.35907(12) 0.0460(4) Uani 0.934(2) d P A 1 C1 C -0.1387(3) 0.6684(3) 0.1274(4) 0.0320(10) Uani 0.934(2) d P A 1 C2 C -0.2445(3) 0.5948(3) 0.1592(4) 0.0306(9) Uani 0.934(2) d P A 1 B3 B -0.2561(4) 0.7371(4) 0.2005(5) 0.0391(12) Uani 0.934(2) d P A 1 H3 H -0.2462 0.7953 0.3082 0.047 Uiso 0.934(2) calc PR A 1 B4 B -0.2048(4) 0.7688(4) 0.0695(5) 0.0402(12) Uani 0.934(2) d P A 1 H4 H -0.1635 0.8485 0.0913 0.048 Uiso 0.934(2) calc PR A 1 B5 B -0.1569(4) 0.6442(4) -0.0454(5) 0.0416(13) Uani 0.934(2) d P A 1 H5 H -0.0847 0.6422 -0.0994 0.050 Uiso 0.934(2) calc PR A 1 B6 B -0.1745(4) 0.5365(4) 0.0178(5) 0.0342(11) Uani 0.934(2) d P A 1 H6 H -0.1120 0.4663 0.0085 0.041 Uiso 0.934(2) calc PR A 1 B7 B -0.3804(4) 0.6478(4) 0.1186(5) 0.0394(12) Uani 0.934(2) d P A 1 H7 H -0.4536 0.6493 0.1710 0.047 Uiso 0.934(2) calc PR A 1 B8 B -0.3583(4) 0.7575(4) 0.0616(5) 0.0400(12) Uani 0.934(2) d P A 1 H8 H -0.4172 0.8306 0.0781 0.048 Uiso 0.934(2) calc PR A 1 B9 B -0.2973(4) 0.6986(4) -0.0915(5) 0.0402(12) Uani 0.934(2) d P A 1 H9 H -0.3177 0.7331 -0.1757 0.048 Uiso 0.934(2) calc PR A 1 B10 B -0.2784(4) 0.5542(4) -0.1252(5) 0.0418(12) Uani 0.934(2) d P A 1 H10 H -0.2855 0.4938 -0.2314 0.050 Uiso 0.934(2) calc PR A 1 B11 B -0.3285(4) 0.5230(4) 0.0058(5) 0.0348(11) Uani 0.934(2) d P A 1 H11 H -0.3669 0.4422 -0.0149 0.042 Uiso 0.934(2) calc PR A 1 B12 B -0.4044(4) 0.6235(4) -0.0624(5) 0.0394(12) Uani 0.934(2) d P A 1 H12 H -0.4933 0.6089 -0.1279 0.047 Uiso 0.934(2) calc PR A 1 C13 C -0.2114(4) 0.5489(4) 0.2766(4) 0.0386(10) Uani 0.934(2) d P A 1 C14 C -0.2287(5) 0.6101(4) 0.4085(5) 0.0719(17) Uani 0.934(2) d P A 1 H14 H -0.2572 0.6825 0.4271 0.086 Uiso 0.934(2) calc PR A 1 C15 C -0.2048(6) 0.5668(5) 0.5132(6) 0.094(2) Uani 0.934(2) d PD A 1 H15 H -0.2172 0.6092 0.6017 0.112 Uiso 0.934(2) calc PR A 1 C16 C -0.1624(6) 0.4602(6) 0.4855(7) 0.090(2) Uani 0.934(2) d PD A 1 H16 H -0.1442 0.4308 0.5563 0.109 Uiso 0.934(2) calc PR A 1 C17 C -0.1467(5) 0.3973(5) 0.3555(7) 0.0822(19) Uani 0.934(2) d P A 1 H17 H -0.1197 0.3245 0.3371 0.099 Uiso 0.934(2) calc PR A 1 C18 C -0.1713(5) 0.4421(4) 0.2497(6) 0.0603(14) Uani 0.934(2) d P A 1 H18 H -0.1603 0.3991 0.1608 0.072 Uiso 0.934(2) calc PR A 1 C21 C 0.1325(3) 0.8807(3) 0.2833(4) 0.0364(10) Uani 0.934(2) d P A 1 C22 C 0.2798(3) 0.9010(3) 0.3751(4) 0.0311(9) Uani 0.934(2) d P A 1 B23 B 0.2435(5) 0.8024(4) 0.2103(5) 0.0419(13) Uani 0.934(2) d P A 1 H23 H 0.2537 0.7129 0.1912 0.050 Uiso 0.934(2) calc PR A 1 B24 B 0.1259(5) 0.8557(4) 0.1139(5) 0.0459(14) Uani 0.934(2) d P A 1 H24 H 0.0603 0.8011 0.0303 0.055 Uiso 0.934(2) calc PR A 1 B25 B 0.0843(5) 0.9867(5) 0.2240(6) 0.0525(15) Uani 0.934(2) d P A 1 H25 H -0.0073 1.0181 0.2128 0.063 Uiso 0.934(2) calc PR A 1 B26 B 0.1784(4) 1.0108(4) 0.3888(6) 0.0445(13) Uani 0.934(2) d P A 1 H26 H 0.1467 1.0560 0.4856 0.053 Uiso 0.934(2) calc PR A 1 B27 B 0.3674(5) 0.8921(5) 0.2617(6) 0.0469(14) Uani 0.934(2) d P A 1 H27 H 0.4594 0.8618 0.2738 0.056 Uiso 0.934(2) calc PR A 1 B28 B 0.2729(5) 0.8628(5) 0.0962(6) 0.0565(16) Uani 0.934(2) d P A 1 H28 H 0.3040 0.8126 0.0005 0.068 Uiso 0.934(2) calc PR A 1 B29 B 0.1751(5) 0.9782(5) 0.1030(6) 0.0568(16) Uani 0.934(2) d P A 1 H29 H 0.1432 1.0038 0.0123 0.068 Uiso 0.934(2) calc PR A 1 B30 B 0.2065(5) 1.0748(5) 0.2764(7) 0.0617(17) Uani 0.934(2) d P A 1 H30 H 0.1939 1.1646 0.2995 0.074 Uiso 0.934(2) calc PR A 1 B31 B 0.3258(5) 1.0220(4) 0.3724(6) 0.0502(15) Uani 0.934(2) d P A 1 H31 H 0.3902 1.0769 0.4574 0.060 Uiso 0.934(2) calc PR A 1 B32 B 0.3218(5) 1.0006(5) 0.1954(6) 0.0574(16) Uani 0.934(2) d P A 1 H32 H 0.3844 1.0416 0.1638 0.069 Uiso 0.934(2) calc PR A 1 C33 C 0.3193(3) 0.8628(4) 0.4960(5) 0.0396(11) Uani 0.934(2) d P A 1 C34 C 0.2994(5) 0.9260(4) 0.6276(5) 0.0604(14) Uani 0.934(2) d P A 1 H34 H 0.2590 0.9933 0.6402 0.073 Uiso 0.934(2) calc PR A 1 C35 C 0.3372(5) 0.8924(5) 0.7394(6) 0.0786(18) Uani 0.934(2) d PD A 1 H35 H 0.3229 0.9364 0.8265 0.094 Uiso 0.934(2) calc PR A 1 C36 C 0.3962(5) 0.7935(5) 0.7218(7) 0.0787(18) Uani 0.934(2) d PD A 1 H36 H 0.4199 0.7691 0.7967 0.094 Uiso 0.934(2) calc PR A 1 C37 C 0.4207(5) 0.7302(5) 0.5951(7) 0.0794(18) Uani 0.934(2) d PD A 1 H37 H 0.4640 0.6646 0.5847 0.095 Uiso 0.934(2) calc PR A 1 C38 C 0.3805(4) 0.7644(4) 0.4806(5) 0.0650(15) Uani 0.934(2) d PD A 1 H38 H 0.3952 0.7203 0.3938 0.078 Uiso 0.934(2) calc PR A 1 S1B S -0.0430(4) 0.7581(4) 0.3220(5) 0.028(4) Uiso 0.066(2) d PR A 2 S2B S 0.1124(4) 0.7164(4) 0.2574(5) 0.040(5) Uiso 0.066(2) d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1A 0.0329(6) 0.0443(7) 0.0519(8) 0.0231(6) 0.0011(5) -0.0057(5) S2A 0.0382(7) 0.0614(8) 0.0345(7) 0.0069(6) 0.0100(5) -0.0158(6) C1 0.027(2) 0.037(2) 0.035(2) 0.0152(19) 0.0025(18) -0.0106(18) C2 0.028(2) 0.030(2) 0.037(2) 0.0135(19) 0.0112(18) -0.0029(17) B3 0.045(3) 0.035(3) 0.037(3) 0.011(2) 0.011(2) 0.000(2) B4 0.040(3) 0.036(3) 0.047(3) 0.020(2) 0.002(2) -0.007(2) B5 0.033(3) 0.062(4) 0.044(3) 0.035(3) 0.009(2) -0.002(2) B6 0.033(3) 0.036(3) 0.037(3) 0.015(2) 0.010(2) -0.001(2) B7 0.026(3) 0.040(3) 0.052(3) 0.015(3) 0.010(2) -0.001(2) B8 0.032(3) 0.037(3) 0.051(3) 0.018(3) 0.007(2) 0.005(2) B9 0.031(3) 0.048(3) 0.047(3) 0.027(3) -0.002(2) -0.006(2) B10 0.041(3) 0.044(3) 0.036(3) 0.010(2) 0.005(2) -0.005(2) B11 0.032(3) 0.039(3) 0.031(3) 0.008(2) 0.003(2) -0.010(2) B12 0.031(3) 0.044(3) 0.043(3) 0.019(2) -0.003(2) -0.006(2) C13 0.037(2) 0.048(3) 0.039(3) 0.023(2) 0.005(2) -0.013(2) C14 0.114(5) 0.062(4) 0.044(3) 0.019(3) 0.020(3) -0.007(3) C15 0.157(7) 0.092(5) 0.042(4) 0.034(4) 0.021(4) -0.005(5) C16 0.109(5) 0.119(6) 0.077(5) 0.078(5) 0.007(4) -0.013(4) C17 0.093(5) 0.083(4) 0.102(5) 0.069(4) 0.026(4) 0.012(4) C18 0.074(4) 0.056(3) 0.064(4) 0.034(3) 0.018(3) 0.002(3) C21 0.030(2) 0.047(3) 0.032(2) 0.014(2) -0.0016(18) -0.0157(19) C22 0.023(2) 0.034(2) 0.034(2) 0.0087(18) 0.0040(17) -0.0033(17) B23 0.050(3) 0.036(3) 0.035(3) 0.004(2) 0.015(2) -0.003(2) B24 0.046(3) 0.061(4) 0.030(3) 0.015(3) 0.001(2) -0.015(3) B25 0.047(3) 0.055(4) 0.056(4) 0.031(3) -0.009(3) -0.002(3) B26 0.034(3) 0.044(3) 0.043(3) 0.005(3) 0.000(2) -0.002(2) B27 0.032(3) 0.065(4) 0.049(3) 0.022(3) 0.012(2) -0.006(3) B28 0.056(4) 0.077(4) 0.039(3) 0.019(3) 0.011(3) -0.014(3) B29 0.051(3) 0.074(4) 0.055(4) 0.038(3) -0.004(3) -0.025(3) B30 0.070(4) 0.041(3) 0.074(4) 0.028(3) -0.003(3) -0.007(3) B31 0.040(3) 0.037(3) 0.069(4) 0.018(3) -0.005(3) -0.016(2) B32 0.049(3) 0.069(4) 0.070(4) 0.044(3) 0.002(3) -0.022(3) C33 0.026(2) 0.044(3) 0.049(3) 0.020(2) -0.002(2) -0.008(2) C34 0.074(4) 0.069(4) 0.040(3) 0.025(3) 0.003(3) -0.006(3) C35 0.093(5) 0.101(5) 0.045(3) 0.034(3) 0.003(3) -0.014(4) C36 0.062(4) 0.102(5) 0.090(5) 0.063(4) -0.003(3) -0.011(4) C37 0.066(4) 0.083(4) 0.103(5) 0.058(4) 0.005(4) 0.016(3) C38 0.054(3) 0.075(4) 0.072(4) 0.039(3) 0.004(3) 0.008(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 S1A C1 1.803(4) . ? S1A S2A 2.0245(19) . ? S2A C21 1.803(4) . ? C1 B4 1.684(6) . ? C1 B5 1.699(6) . ? C1 B6 1.707(6) . ? C1 B3 1.726(6) . ? C1 C2 1.766(5) . ? C2 C13 1.517(5) . ? C2 B11 1.681(6) . ? C2 B7 1.693(6) . ? C2 B3 1.732(6) . ? C2 B6 1.744(6) . ? B3 B8 1.757(7) . ? B3 B7 1.787(7) . ? B3 B4 1.792(7) . ? B3 H3 1.1000 . ? B4 B5 1.761(7) . ? B4 B9 1.770(7) . ? B4 B8 1.778(7) . ? B4 H4 1.1000 . ? B5 B9 1.757(7) . ? B5 B10 1.765(7) . ? B5 B6 1.785(6) . ? B5 H5 1.1000 . ? B6 B11 1.780(6) . ? B6 B10 1.785(7) . ? B6 H6 1.1000 . ? B7 B11 1.771(7) . ? B7 B8 1.780(7) . ? B7 B12 1.777(7) . ? B7 H7 1.1000 . ? B8 B9 1.784(7) . ? B8 B12 1.797(7) . ? B8 H8 1.1000 . ? B9 B10 1.774(7) . ? B9 B12 1.776(7) . ? B9 H9 1.1000 . ? B10 B12 1.769(7) . ? B10 B11 1.781(7) . ? B10 H10 1.1000 . ? B11 B12 1.781(7) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C13 C18 1.367(6) . ? C13 C14 1.376(6) . ? C14 C15 1.374(7) . ? C14 H14 0.9300 . ? C15 C16 1.371(5) . ? C15 H15 0.9300 . ? C16 C17 1.359(8) . ? C16 H16 0.9300 . ? C17 C18 1.397(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C21 B24 1.678(6) . ? C21 B26 1.704(6) . ? C21 B23 1.705(6) . ? C21 B25 1.705(6) . ? C21 C22 1.763(5) . ? C22 C33 1.493(6) . ? C22 B27 1.691(6) . ? C22 B31 1.705(6) . ? C22 B23 1.733(6) . ? C22 B26 1.747(6) . ? B23 B28 1.748(7) . ? B23 B24 1.763(7) . ? B23 B27 1.789(7) . ? B23 H23 1.1000 . ? B24 B28 1.765(8) . ? B24 B25 1.769(8) . ? B24 B29 1.776(7) . ? B24 H24 1.1000 . ? B25 B30 1.760(8) . ? B25 B29 1.784(8) . ? B25 B26 1.776(7) . ? B25 H25 1.1000 . ? B26 B30 1.759(8) . ? B26 B31 1.775(7) . ? B26 H26 1.1000 . ? B27 B31 1.762(8) . ? B27 B32 1.773(8) . ? B27 B28 1.778(8) . ? B27 H27 1.1000 . ? B28 B32 1.780(8) . ? B28 B29 1.782(9) . ? B28 H28 1.1000 . ? B29 B32 1.759(8) . ? B29 B30 1.783(8) . ? B29 H29 1.1000 . ? B30 B32 1.762(9) . ? B30 B31 1.770(8) . ? B30 H30 1.1000 . ? B31 B32 1.771(8) . ? B31 H31 1.1000 . ? B32 H32 1.1000 . ? C33 C38 1.375(6) . ? C33 C34 1.390(6) . ? C34 C35 1.369(7) . ? C34 H34 0.9300 . ? C35 C36 1.367(5) . ? C35 H35 0.9300 . ? C36 C37 1.365(8) . ? C36 H36 0.9300 . ? C37 C38 1.403(5) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? S1B S2B 2.0202 . ? 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 C1 S1A S2A 105.41(15) . . ? C21 S2A S1A 105.20(15) . . ? B4 C1 B5 62.7(3) . . ? B4 C1 B6 114.7(3) . . ? B5 C1 B6 63.2(3) . . ? B4 C1 B3 63.4(3) . . ? B5 C1 B3 114.1(3) . . ? B6 C1 B3 111.9(3) . . ? B4 C1 C2 110.5(3) . . ? B5 C1 C2 110.3(3) . . ? B6 C1 C2 60.3(2) . . ? B3 C1 C2 59.5(2) . . ? B4 C1 S1A 128.5(3) . . ? B5 C1 S1A 120.6(3) . . ? B6 C1 S1A 109.2(3) . . ? B3 C1 S1A 121.8(3) . . ? C2 C1 S1A 113.9(2) . . ? C13 C2 B11 121.7(3) . . ? C13 C2 B7 122.4(3) . . ? B11 C2 B7 63.3(3) . . ? C13 C2 B3 118.6(3) . . ? B11 C2 B3 113.7(3) . . ? B7 C2 B3 62.9(3) . . ? C13 C2 B6 117.4(3) . . ? B11 C2 B6 62.6(3) . . ? B7 C2 B6 113.6(3) . . ? B3 C2 B6 109.8(3) . . ? C13 C2 C1 119.5(3) . . ? B11 C2 C1 108.1(3) . . ? B7 C2 C1 108.8(3) . . ? B3 C2 C1 59.1(2) . . ? B6 C2 C1 58.2(2) . . ? C1 B3 C2 61.4(2) . . ? C1 B3 B8 104.6(3) . . ? C2 B3 B8 105.4(3) . . ? C1 B3 B7 106.4(3) . . ? C2 B3 B7 57.5(3) . . ? B8 B3 B7 60.3(3) . . ? C1 B3 B4 57.2(3) . . ? C2 B3 B4 107.1(3) . . ? B8 B3 B4 60.1(3) . . ? B7 B3 B4 108.3(4) . . ? C1 B3 H3 123.4 . . ? C2 B3 H3 122.7 . . ? B8 B3 H3 123.2 . . ? B7 B3 H3 122.1 . . ? B4 B3 H3 122.0 . . ? C1 B4 B5 59.0(3) . . ? C1 B4 B9 105.3(3) . . ? B5 B4 B9 59.7(3) . . ? C1 B4 B8 105.4(3) . . ? B5 B4 B8 108.1(3) . . ? B9 B4 B8 60.4(3) . . ? C1 B4 B3 59.4(3) . . ? B5 B4 B3 107.9(3) . . ? B9 B4 B3 107.3(3) . . ? B8 B4 B3 59.0(3) . . ? C1 B4 H4 123.8 . . ? B5 B4 H4 121.5 . . ? B9 B4 H4 122.4 . . ? B8 B4 H4 122.3 . . ? B3 B4 H4 122.0 . . ? C1 B5 B9 105.3(4) . . ? C1 B5 B4 58.2(3) . . ? B9 B5 B4 60.4(3) . . ? C1 B5 B10 105.7(3) . . ? B9 B5 B10 60.5(3) . . ? B4 B5 B10 108.7(4) . . ? C1 B5 B6 58.6(2) . . ? B9 B5 B6 108.3(3) . . ? B4 B5 B6 107.3(3) . . ? B10 B5 B6 60.4(3) . . ? C1 B5 H5 124.5 . . ? B9 B5 H5 121.9 . . ? B4 B5 H5 121.7 . . ? B10 B5 H5 121.5 . . ? B6 B5 H5 121.7 . . ? C1 B6 C2 61.5(2) . . ? C1 B6 B5 58.2(3) . . ? C2 B6 B5 107.4(3) . . ? C1 B6 B11 106.3(3) . . ? C2 B6 B11 57.0(2) . . ? B5 B6 B11 107.7(3) . . ? C1 B6 B10 104.4(3) . . ? C2 B6 B10 104.4(3) . . ? B5 B6 B10 59.2(3) . . ? B11 B6 B10 60.0(3) . . ? C1 B6 H6 122.9 . . ? C2 B6 H6 122.9 . . ? B5 B6 H6 122.0 . . ? B11 B6 H6 122.6 . . ? B10 B6 H6 123.9 . . ? C2 B7 B11 58.0(3) . . ? C2 B7 B8 106.0(3) . . ? B11 B7 B8 108.2(4) . . ? C2 B7 B12 105.7(3) . . ? B11 B7 B12 60.3(3) . . ? B8 B7 B12 60.7(3) . . ? C2 B7 B3 59.6(2) . . ? B11 B7 B3 106.8(3) . . ? B8 B7 B3 59.0(3) . . ? B12 B7 B3 107.4(3) . . ? C2 B7 H7 123.8 . . ? B11 B7 H7 122.1 . . ? B8 B7 H7 121.9 . . ? B12 B7 H7 121.9 . . ? B3 B7 H7 122.3 . . ? B3 B8 B4 60.9(3) . . ? B3 B8 B7 60.7(3) . . ? B4 B8 B7 109.3(3) . . ? B3 B8 B9 108.2(3) . . ? B4 B8 B9 59.6(3) . . ? B7 B8 B9 107.7(4) . . ? B3 B8 B12 107.9(3) . . ? B4 B8 B12 107.5(4) . . ? B7 B8 B12 59.6(3) . . ? B9 B8 B12 59.5(3) . . ? B3 B8 H8 121.1 . . ? B4 B8 H8 121.3 . . ? B7 B8 H8 121.2 . . ? B9 B8 H8 122.2 . . ? B12 B8 H8 122.4 . . ? B5 B9 B4 59.9(3) . . ? B5 B9 B10 60.0(3) . . ? B4 B9 B10 107.9(3) . . ? B5 B9 B12 108.3(3) . . ? B4 B9 B12 108.7(4) . . ? B10 B9 B12 59.8(3) . . ? B5 B9 B8 107.9(4) . . ? B4 B9 B8 60.0(3) . . ? B10 B9 B8 107.9(3) . . ? B12 B9 B8 60.6(3) . . ? B5 B9 H9 121.8 . . ? B4 B9 H9 121.6 . . ? B10 B9 H9 122.0 . . ? B12 B9 H9 121.2 . . ? B8 B9 H9 121.6 . . ? B12 B10 B5 108.2(4) . . ? B12 B10 B9 60.2(3) . . ? B5 B10 B9 59.6(3) . . ? B12 B10 B11 60.2(3) . . ? B5 B10 B11 108.5(3) . . ? B9 B10 B11 108.1(4) . . ? B12 B10 B6 108.0(4) . . ? B5 B10 B6 60.4(3) . . ? B9 B10 B6 107.6(3) . . ? B11 B10 B6 59.9(3) . . ? B12 B10 H10 121.5 . . ? B5 B10 H10 121.5 . . ? B9 B10 H10 122.0 . . ? B11 B10 H10 121.5 . . ? B6 B10 H10 121.9 . . ? C2 B11 B7 58.7(3) . . ? C2 B11 B12 106.1(3) . . ? B7 B11 B12 60.0(3) . . ? C2 B11 B6 60.5(2) . . ? B7 B11 B6 108.2(3) . . ? B12 B11 B6 107.7(3) . . ? C2 B11 B10 107.3(3) . . ? B7 B11 B10 107.9(3) . . ? B12 B11 B10 59.5(3) . . ? B6 B11 B10 60.2(3) . . ? C2 B11 H11 122.8 . . ? B7 B11 H11 121.8 . . ? B12 B11 H11 122.5 . . ? B6 B11 H11 121.2 . . ? B10 B11 H11 121.8 . . ? B10 B12 B9 60.0(3) . . ? B10 B12 B7 108.2(3) . . ? B9 B12 B7 108.3(3) . . ? B10 B12 B11 60.2(3) . . ? B9 B12 B11 108.0(3) . . ? B7 B12 B11 59.7(3) . . ? B10 B12 B8 107.6(3) . . ? B9 B12 B8 59.9(3) . . ? B7 B12 B8 59.7(3) . . ? B11 B12 B8 107.0(3) . . ? B10 B12 H12 121.6 . . ? B9 B12 H12 121.5 . . ? B7 B12 H12 121.6 . . ? B11 B12 H12 122.0 . . ? B8 B12 H12 122.3 . . ? C18 C13 C14 118.8(4) . . ? C18 C13 C2 119.7(4) . . ? C14 C13 C2 121.3(4) . . ? C15 C14 C13 121.5(5) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 119.9(6) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 120.1(5) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? B24 C21 B26 114.1(3) . . ? B24 C21 B23 62.8(3) . . ? B26 C21 B23 111.9(3) . . ? B24 C21 B25 63.1(3) . . ? B26 C21 B25 62.8(3) . . ? B23 C21 B25 114.3(3) . . ? B24 C21 C22 110.6(3) . . ? B26 C21 C22 60.5(2) . . ? B23 C21 C22 60.0(2) . . ? B25 C21 C22 111.1(3) . . ? B24 C21 S2A 127.2(3) . . ? B26 C21 S2A 111.0(3) . . ? B23 C21 S2A 121.5(3) . . ? B25 C21 S2A 119.9(3) . . ? C22 C21 S2A 114.6(3) . . ? C33 C22 B27 122.5(4) . . ? C33 C22 B31 122.9(3) . . ? B27 C22 B31 62.5(3) . . ? C33 C22 B23 118.7(3) . . ? B27 C22 B23 63.0(3) . . ? B31 C22 B23 112.5(3) . . ? C33 C22 B26 119.0(3) . . ? B27 C22 B26 112.1(3) . . ? B31 C22 B26 61.9(3) . . ? B23 C22 B26 108.5(3) . . ? C33 C22 C21 119.9(3) . . ? B27 C22 C21 108.2(3) . . ? B31 C22 C21 107.4(3) . . ? B23 C22 C21 58.4(2) . . ? B26 C22 C21 58.1(2) . . ? C21 B23 C22 61.7(2) . . ? C21 B23 B28 105.3(4) . . ? C22 B23 B28 105.9(4) . . ? C21 B23 B24 57.9(3) . . ? C22 B23 B24 108.1(4) . . ? B28 B23 B24 60.4(3) . . ? C21 B23 B27 106.4(3) . . ? C22 B23 B27 57.3(3) . . ? B28 B23 B27 60.3(3) . . ? B24 B23 B27 108.5(4) . . ? C21 B23 H23 123.0 . . ? C22 B23 H23 122.3 . . ? B28 B23 H23 122.8 . . ? B24 B23 H23 121.5 . . ? B27 B23 H23 122.4 . . ? C21 B24 B28 105.7(4) . . ? C21 B24 B23 59.3(3) . . ? B28 B24 B23 59.4(3) . . ? C21 B24 B25 59.2(3) . . ? B28 B24 B25 108.7(4) . . ? B23 B24 B25 108.3(4) . . ? C21 B24 B29 106.2(4) . . ? B28 B24 B29 60.4(3) . . ? B23 B24 B29 108.0(4) . . ? B25 B24 B29 60.4(3) . . ? C21 B24 H24 123.7 . . ? B28 B24 H24 122.1 . . ? B23 B24 H24 121.7 . . ? B25 B24 H24 121.1 . . ? B29 B24 H24 121.8 . . ? C21 B25 B30 104.9(4) . . ? C21 B25 B24 57.7(3) . . ? B30 B25 B24 107.6(4) . . ? C21 B25 B29 104.7(4) . . ? B30 B25 B29 60.4(3) . . ? B24 B25 B29 60.0(3) . . ? C21 B25 B26 58.6(3) . . ? B30 B25 B26 59.7(3) . . ? B24 B25 B26 106.3(4) . . ? B29 B25 B26 107.6(4) . . ? C21 B25 H25 124.8 . . ? B30 B25 H25 122.1 . . ? B24 B25 H25 122.4 . . ? B29 B25 H25 122.1 . . ? B26 B25 H25 122.3 . . ? C21 B26 C22 61.4(3) . . ? C21 B26 B30 105.0(4) . . ? C22 B26 B30 105.6(4) . . ? C21 B26 B31 106.8(4) . . ? C22 B26 B31 57.9(3) . . ? B30 B26 B31 60.1(3) . . ? C21 B26 B25 58.6(3) . . ? C22 B26 B25 108.5(4) . . ? B30 B26 B25 59.7(3) . . ? B31 B26 B25 108.6(4) . . ? C21 B26 H26 122.8 . . ? C22 B26 H26 122.1 . . ? B30 B26 H26 123.4 . . ? B31 B26 H26 122.1 . . ? B25 B26 H26 121.3 . . ? C22 B27 B31 59.1(3) . . ? C22 B27 B32 106.4(4) . . ? B31 B27 B32 60.1(3) . . ? C22 B27 B28 106.4(4) . . ? B31 B27 B28 108.2(4) . . ? B32 B27 B28 60.2(3) . . ? C22 B27 B23 59.7(3) . . ? B31 B27 B23 107.2(4) . . ? B32 B27 B23 106.5(4) . . ? B28 B27 B23 58.7(3) . . ? C22 B27 H27 122.9 . . ? B31 B27 H27 121.6 . . ? B32 B27 H27 122.3 . . ? B28 B27 H27 122.1 . . ? B23 B27 H27 122.7 . . ? B23 B28 B24 60.3(3) . . ? B23 B28 B27 61.0(3) . . ? B24 B28 B27 109.0(4) . . ? B23 B28 B32 108.0(4) . . ? B24 B28 B32 107.2(4) . . ? B27 B28 B32 59.8(3) . . ? B23 B28 B29 108.5(4) . . ? B24 B28 B29 60.1(3) . . ? B27 B28 B29 108.1(4) . . ? B32 B28 B29 59.2(3) . . ? B23 B28 H28 121.1 . . ? B24 B28 H28 121.6 . . ? B27 B28 H28 121.1 . . ? B32 B28 H28 122.6 . . ? B29 B28 H28 121.9 . . ? B32 B29 B25 107.4(4) . . ? B32 B29 B24 107.6(4) . . ? B25 B29 B24 59.6(3) . . ? B32 B29 B30 59.7(3) . . ? B25 B29 B30 59.1(3) . . ? B24 B29 B30 106.4(4) . . ? B32 B29 B28 60.3(3) . . ? B25 B29 B28 107.2(4) . . ? B24 B29 B28 59.5(3) . . ? B30 B29 B28 107.1(4) . . ? B32 B29 H29 121.6 . . ? B25 B29 H29 122.3 . . ? B24 B29 H29 122.4 . . ? B30 B29 H29 122.8 . . ? B28 B29 H29 122.0 . . ? B26 B30 B25 60.6(3) . . ? B26 B30 B32 107.9(4) . . ? B25 B30 B32 108.4(4) . . ? B26 B30 B31 60.4(3) . . ? B25 B30 B31 109.6(4) . . ? B32 B30 B31 60.2(3) . . ? B26 B30 B29 108.4(4) . . ? B25 B30 B29 60.5(3) . . ? B32 B30 B29 59.5(3) . . ? B31 B30 B29 108.4(4) . . ? B26 B30 H30 121.5 . . ? B25 B30 H30 120.8 . . ? B32 B30 H30 122.0 . . ? B31 B30 H30 120.9 . . ? B29 B30 H30 121.7 . . ? C22 B31 B27 58.3(3) . . ? C22 B31 B30 107.0(4) . . ? B27 B31 B30 108.1(4) . . ? C22 B31 B32 105.8(4) . . ? B27 B31 B32 60.2(3) . . ? B30 B31 B32 59.7(3) . . ? C22 B31 B26 60.2(3) . . ? B27 B31 B26 107.4(3) . . ? B30 B31 B26 59.5(3) . . ? B32 B31 B26 106.9(4) . . ? C22 B31 H31 123.1 . . ? B27 B31 H31 121.9 . . ? B30 B31 H31 121.8 . . ? B32 B31 H31 122.6 . . ? B26 B31 H31 122.0 . . ? B30 B32 B29 60.9(3) . . ? B30 B32 B27 108.0(4) . . ? B29 B32 B27 109.3(4) . . ? B30 B32 B31 60.1(3) . . ? B29 B32 B31 109.5(4) . . ? B27 B32 B31 59.6(3) . . ? B30 B32 B28 108.1(4) . . ? B29 B32 B28 60.5(3) . . ? B27 B32 B28 60.0(3) . . ? B31 B32 B28 107.7(4) . . ? B30 B32 H32 121.6 . . ? B29 B32 H32 120.3 . . ? B27 B32 H32 121.6 . . ? B31 B32 H32 121.6 . . ? B28 B32 H32 121.9 . . ? C38 C33 C34 117.8(4) . . ? C38 C33 C22 120.4(4) . . ? C34 C33 C22 121.8(4) . . ? C35 C34 C33 122.1(5) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C36 C35 C34 119.4(6) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.5(6) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 119.8(5) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C33 C38 C37 120.4(5) . . ? C33 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? 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 C13 C2 C22 C33 -1.3(3) . . . . ? S1A C1 C2 C13 6.5(5) . . . . ? C1 S1A S2A C21 -101.7(2) . . . . ? S2A C21 C22 C33 6.3(5) . . . . ? C2 C1 S1A S2A -113.4(2) . . . . ? C22 C21 S2A S1A -107.8(3) . . . . ? C1 C2 C13 C14 90.6(5) . . . . ? C1 C2 C13 C18 -94.0(5) . . . . ? C21 C22 C33 C34 -82.4(5) . . . . ? C21 C22 C33 C38 99.7(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 0.282 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.063 #===END data_[NMe~4~][(2-Me-1,2-closo-C~2~B~10~H~10~)S(8-Me-7,8-nido-C~2~B~9~H~10~)] _database_code_depnum_ccdc_archive 'CCDC 263595' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H26 B19 S, C4 H12 N' _chemical_formula_sum 'C10 H38 B19 N S' _chemical_formula_weight 409.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.209(7) _cell_length_b 13.046(8) _cell_length_c 19.001(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.93(7) _cell_angle_gamma 90.00 _cell_volume 2500(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 13.3 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7001 _exptl_absorpt_correction_T_max 0.8528 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 4636 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 65.04 _reflns_number_total 4184 _reflns_number_gt 2987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _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 ; w=1/[\s^2^(Fo^2^)+(0.1288P)^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 4184 _refine_ls_number_parameters 298 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1935 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.101 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.03179(8) 0.52679(5) 0.88668(4) 0.0339(3) Uani 1 d . . . N N 0.2269(3) 0.1883(2) 0.93522(14) 0.0383(7) Uani 1 d . . . C1 C -0.0736(3) 0.5279(2) 0.80154(15) 0.0298(7) Uani 1 d . . . C2 C -0.2388(3) 0.5036(2) 0.80396(17) 0.0341(7) Uani 1 d . . . B3 B -0.1927(4) 0.6241(3) 0.77982(19) 0.0338(8) Uani 1 d . . . H3 H -0.2005 0.6944 0.8127 0.041 Uiso 1 calc R . . B4 B -0.0585(4) 0.6040(3) 0.73122(19) 0.0335(8) Uani 1 d . . . H4 H 0.0223 0.6622 0.7314 0.040 Uiso 1 calc R . . B5 B -0.0264(4) 0.4689(3) 0.72929(19) 0.0349(8) Uani 1 d . . . H5 H 0.0753 0.4377 0.7275 0.042 Uiso 1 calc R . . B6 B -0.1381(4) 0.4084(3) 0.7792(2) 0.0375(9) Uani 1 d . . . H6 H -0.1096 0.3384 0.8122 0.045 Uiso 1 calc R . . B7 B -0.3345(4) 0.5618(3) 0.7338(2) 0.0402(9) Uani 1 d . . . H7 H -0.4367 0.5922 0.7352 0.048 Uiso 1 calc R . . B8 B -0.2230(4) 0.6247(3) 0.6860(2) 0.0395(9) Uani 1 d . . . H8 H -0.2505 0.6970 0.6554 0.047 Uiso 1 calc R . . B9 B -0.1218(4) 0.5287(3) 0.6545(2) 0.0384(9) Uani 1 d . . . H9 H -0.0830 0.5376 0.6029 0.046 Uiso 1 calc R . . B10 B -0.1705(4) 0.4070(3) 0.6849(2) 0.0393(9) Uani 1 d . . . H10 H -0.1638 0.3349 0.6536 0.047 Uiso 1 calc R . . B11 B -0.3023(4) 0.4277(3) 0.7340(2) 0.0393(9) Uani 1 d . . . H11 H -0.3822 0.3694 0.7359 0.047 Uiso 1 calc R . . B12 B -0.2922(4) 0.5028(3) 0.6566(2) 0.0400(9) Uani 1 d . . . H12 H -0.3654 0.4943 0.6066 0.048 Uiso 1 calc R . . C13 C -0.2852(4) 0.4936(3) 0.87513(18) 0.0444(8) Uani 1 d . . . H13A H -0.3733 0.5246 0.8725 0.067 Uiso 1 calc R . . H13B H -0.2228 0.5288 0.9116 0.067 Uiso 1 calc R . . H13C H -0.2899 0.4209 0.8876 0.067 Uiso 1 calc R . . B21 B 0.3202(4) 0.7396(3) 0.9865(2) 0.0417(9) Uani 1 d . . . H21 H 0.3800 0.7486 1.0407 0.050 Uiso 1 calc R . . B22 B 0.1548(4) 0.6972(3) 0.9749(2) 0.0385(9) Uani 1 d . . . H22 H 0.1060 0.6757 1.0217 0.046 Uiso 1 calc R . . B23 B 0.2789(4) 0.6182(3) 0.94763(19) 0.0373(9) Uani 1 d . . . H23 H 0.3100 0.5439 0.9747 0.045 Uiso 1 calc R . . B24 B 0.3913(4) 0.6979(3) 0.9134(2) 0.0439(9) Uani 1 d . . . H24 H 0.4992 0.6780 0.9195 0.053 Uiso 1 calc R . . B25 B 0.3367(4) 0.8252(3) 0.9141(2) 0.0456(10) Uani 1 d . . . H25 H 0.4095 0.8900 0.9198 0.055 Uiso 1 calc R . . B26 B 0.1866(4) 0.8251(3) 0.9538(2) 0.0421(9) Uani 1 d . . . H26 H 0.1575 0.8897 0.9870 0.051 Uiso 1 calc R . . C27 C 0.1295(3) 0.6409(2) 0.89110(16) 0.0317(7) Uani 1 d . . . C28 C 0.2632(3) 0.6392(2) 0.85779(16) 0.0351(7) Uani 1 d . . . B29 B 0.3021(4) 0.7533(3) 0.8341(2) 0.0414(9) Uani 1 d D . . H29 H 0.353(3) 0.761(3) 0.7864(11) 0.050 Uiso 1 d D . . B30 B 0.1799(5) 0.8429(3) 0.8609(2) 0.0460(10) Uani 1 d D . . H30A H 0.153(3) 0.9196(12) 0.8365(17) 0.055 Uiso 1 d D . . H30B H 0.136(3) 0.784(2) 0.8215(14) 0.055 Uiso 1 d D . . B31 B 0.0656(4) 0.7550(3) 0.89592(19) 0.0358(9) Uani 1 d D . . H31 H -0.0420(9) 0.773(2) 0.8947(17) 0.043 Uiso 1 d D . . C32 C 0.2970(4) 0.5469(3) 0.81596(18) 0.0436(8) Uani 1 d . . . H32A H 0.2741 0.4841 0.8397 0.065 Uiso 1 calc R . . H32B H 0.3922 0.5470 0.8135 0.065 Uiso 1 calc R . . H32C H 0.2468 0.5496 0.7677 0.065 Uiso 1 calc R . . C33 C 0.2325(5) 0.2896(4) 0.9692(3) 0.0987(18) Uani 1 d U . . H33A H 0.3243 0.3143 0.9769 0.148 Uiso 1 calc R . . H33B H 0.2004 0.2844 1.0151 0.148 Uiso 1 calc R . . H33C H 0.1766 0.3377 0.9383 0.148 Uiso 1 calc R . . C34 C 0.0908(5) 0.1493(4) 0.9190(4) 0.105(2) Uani 1 d U . . H34A H 0.0373 0.1963 0.8860 0.157 Uiso 1 calc R . . H34B H 0.0526 0.1443 0.9631 0.157 Uiso 1 calc R . . H34C H 0.0915 0.0814 0.8971 0.157 Uiso 1 calc R . . C35 C 0.3069(7) 0.1175(4) 0.9816(4) 0.131(3) Uani 1 d U . . H35A H 0.3025 0.0495 0.9595 0.197 Uiso 1 calc R . . H35B H 0.2736 0.1136 1.0272 0.197 Uiso 1 calc R . . H35C H 0.3991 0.1413 0.9898 0.197 Uiso 1 calc R . . C36 C 0.2879(10) 0.1895(8) 0.8715(4) 0.182(4) Uani 1 d U . . H36A H 0.3750 0.2224 0.8818 0.273 Uiso 1 calc R . . H36B H 0.2315 0.2278 0.8341 0.273 Uiso 1 calc R . . H36C H 0.2984 0.1190 0.8554 0.273 Uiso 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 S 0.0451(5) 0.0210(4) 0.0325(4) 0.0052(3) -0.0036(3) -0.0031(3) N 0.0480(17) 0.0298(14) 0.0332(14) -0.0020(11) -0.0059(12) -0.0003(12) C1 0.0403(17) 0.0184(14) 0.0311(15) 0.0024(12) 0.0063(13) -0.0020(12) C2 0.0377(18) 0.0274(16) 0.0356(16) 0.0061(12) 0.0012(14) -0.0010(13) B3 0.045(2) 0.0227(17) 0.0315(18) 0.0036(14) -0.0007(16) 0.0061(15) B4 0.047(2) 0.0208(16) 0.0324(18) 0.0000(14) 0.0052(16) -0.0005(15) B5 0.045(2) 0.0202(16) 0.0389(19) -0.0035(14) 0.0040(16) 0.0007(15) B6 0.048(2) 0.0194(17) 0.043(2) 0.0024(15) -0.0015(18) -0.0025(16) B7 0.040(2) 0.037(2) 0.041(2) 0.0042(16) -0.0034(17) 0.0069(16) B8 0.058(2) 0.0239(18) 0.0340(19) 0.0025(15) -0.0004(18) 0.0009(17) B9 0.053(2) 0.0285(18) 0.0331(18) -0.0032(15) 0.0041(17) -0.0030(17) B10 0.051(2) 0.0238(17) 0.040(2) -0.0033(15) -0.0028(18) -0.0039(16) B11 0.045(2) 0.0292(19) 0.040(2) 0.0014(15) -0.0032(17) -0.0054(16) B12 0.052(2) 0.0305(19) 0.035(2) 0.0001(15) -0.0009(18) -0.0010(16) C13 0.046(2) 0.051(2) 0.0361(18) 0.0074(15) 0.0052(15) -0.0004(16) B21 0.049(2) 0.040(2) 0.0329(19) -0.0055(16) -0.0052(18) -0.0054(18) B22 0.053(2) 0.0290(19) 0.0317(19) -0.0046(15) 0.0008(17) -0.0011(17) B23 0.044(2) 0.0308(18) 0.0327(19) 0.0025(15) -0.0091(16) 0.0000(16) B24 0.045(2) 0.042(2) 0.041(2) -0.0019(17) -0.0053(18) -0.0072(18) B25 0.056(3) 0.035(2) 0.044(2) -0.0052(17) 0.0030(19) -0.0132(19) B26 0.057(3) 0.0274(19) 0.040(2) -0.0067(16) 0.0003(19) -0.0047(17) C27 0.0425(18) 0.0193(14) 0.0307(15) 0.0003(12) -0.0024(13) -0.0001(13) C28 0.0422(19) 0.0312(17) 0.0309(16) -0.0022(13) 0.0022(14) -0.0025(14) B29 0.053(2) 0.034(2) 0.0358(19) -0.0015(16) 0.0038(18) -0.0136(17) B30 0.070(3) 0.0240(18) 0.040(2) -0.0012(15) -0.003(2) -0.0054(19) B31 0.050(2) 0.0180(16) 0.0361(19) -0.0003(14) -0.0024(17) -0.0009(15) C32 0.047(2) 0.0356(18) 0.047(2) -0.0072(15) 0.0054(16) -0.0030(15) C33 0.087(3) 0.051(3) 0.152(5) -0.040(3) 0.000(3) -0.001(3) C34 0.065(3) 0.083(3) 0.159(5) -0.045(3) -0.005(3) -0.006(3) C35 0.128(5) 0.067(3) 0.169(6) 0.043(4) -0.071(5) -0.014(3) C36 0.230(8) 0.239(9) 0.095(5) -0.041(5) 0.083(5) -0.105(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C27 1.787(3) . ? S C1 1.799(3) . ? N C35 1.440(5) . ? N C36 1.445(7) . ? N C34 1.467(6) . ? N C33 1.468(5) . ? C1 B4 1.691(4) . ? C1 B5 1.708(5) . ? C1 B6 1.719(4) . ? C1 C2 1.723(4) . ? C1 B3 1.752(4) . ? C2 C13 1.507(4) . ? C2 B11 1.703(5) . ? C2 B7 1.705(5) . ? C2 B6 1.723(5) . ? C2 B3 1.724(4) . ? B3 B8 1.761(5) . ? B3 B7 1.769(5) . ? B3 B4 1.787(5) . ? B3 H3 1.1200 . ? B4 B8 1.784(6) . ? B4 B9 1.793(5) . ? B4 B5 1.795(5) . ? B4 H4 1.1200 . ? B5 B10 1.773(5) . ? B5 B9 1.774(5) . ? B5 B6 1.777(5) . ? B5 H5 1.1200 . ? B6 B10 1.772(5) . ? B6 B11 1.779(6) . ? B6 H6 1.1200 . ? B7 B8 1.765(6) . ? B7 B12 1.768(6) . ? B7 B11 1.780(5) . ? B7 H7 1.1200 . ? B8 B9 1.784(5) . ? B8 B12 1.793(5) . ? B8 H8 1.1200 . ? B9 B12 1.778(6) . ? B9 B10 1.786(5) . ? B9 H9 1.1200 . ? B10 B11 1.773(6) . ? B10 B12 1.785(5) . ? B10 H10 1.1200 . ? B11 B12 1.782(5) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? B21 B24 1.751(6) . ? B21 B22 1.757(6) . ? B21 B23 1.770(5) . ? B21 B26 1.796(6) . ? B21 B25 1.800(6) . ? B21 H21 1.1200 . ? B22 C27 1.736(5) . ? B22 B26 1.757(5) . ? B22 B23 1.772(6) . ? B22 B31 1.796(5) . ? B22 H22 1.1200 . ? B23 C28 1.712(5) . ? B23 B24 1.747(6) . ? B23 C27 1.749(5) . ? B23 H23 1.1200 . ? B24 C28 1.727(5) . ? B24 B25 1.752(6) . ? B24 B29 1.788(6) . ? B24 H24 1.1200 . ? B25 B30 1.770(6) . ? B25 B29 1.773(6) . ? B25 B26 1.811(6) . ? B25 H25 1.1200 . ? B26 B30 1.771(6) . ? B26 B31 1.774(5) . ? B26 H26 1.1200 . ? C27 C28 1.591(5) . ? C27 B31 1.634(4) . ? C28 C32 1.513(4) . ? C28 B29 1.622(5) . ? B29 B30 1.837(6) . ? B29 H29 1.1199(13) . ? B30 B31 1.832(6) . ? B30 H30A 1.1200(13) . ? B30 H30B 1.1200(12) . ? B31 H31 1.1200(13) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 C27 S C1 106.70(14) . . ? C35 N C36 104.1(6) . . ? C35 N C34 109.6(4) . . ? C36 N C34 110.2(5) . . ? C35 N C33 109.2(4) . . ? C36 N C33 111.5(5) . . ? C34 N C33 112.0(4) . . ? B4 C1 B5 63.75(19) . . ? B4 C1 B6 114.6(2) . . ? B5 C1 B6 62.5(2) . . ? B4 C1 C2 109.8(2) . . ? B5 C1 C2 109.8(2) . . ? B6 C1 C2 60.06(19) . . ? B4 C1 B3 62.5(2) . . ? B5 C1 B3 114.0(2) . . ? B6 C1 B3 111.5(2) . . ? C2 C1 B3 59.48(18) . . ? B4 C1 S 126.9(2) . . ? B5 C1 S 121.0(2) . . ? B6 C1 S 111.5(2) . . ? C2 C1 S 115.2(2) . . ? B3 C1 S 120.9(2) . . ? C13 C2 B11 121.1(3) . . ? C13 C2 B7 121.2(3) . . ? B11 C2 B7 63.0(2) . . ? C13 C2 B6 117.8(3) . . ? B11 C2 B6 62.6(2) . . ? B7 C2 B6 113.7(3) . . ? C13 C2 C1 119.0(3) . . ? B11 C2 C1 110.0(3) . . ? B7 C2 C1 110.0(2) . . ? B6 C2 C1 59.86(19) . . ? C13 C2 B3 117.0(3) . . ? B11 C2 B3 114.1(3) . . ? B7 C2 B3 62.1(2) . . ? B6 C2 B3 112.7(3) . . ? C1 C2 B3 61.08(18) . . ? C2 B3 C1 59.44(18) . . ? C2 B3 B8 105.1(2) . . ? C1 B3 B8 104.4(3) . . ? C2 B3 B7 58.4(2) . . ? C1 B3 B7 105.8(2) . . ? B8 B3 B7 60.0(2) . . ? C2 B3 B4 105.4(2) . . ? C1 B3 B4 57.09(18) . . ? B8 B3 B4 60.4(2) . . ? B7 B3 B4 108.2(3) . . ? C2 B3 H3 123.5 . . ? C1 B3 H3 124.2 . . ? B8 B3 H3 123.0 . . ? B7 B3 H3 121.9 . . ? B4 B3 H3 122.4 . . ? C1 B4 B8 105.9(3) . . ? C1 B4 B3 60.41(19) . . ? B8 B4 B3 59.1(2) . . ? C1 B4 B9 104.8(2) . . ? B8 B4 B9 59.8(2) . . ? B3 B4 B9 107.0(3) . . ? C1 B4 B5 58.58(19) . . ? B8 B4 B5 107.5(3) . . ? B3 B4 B5 108.2(2) . . ? B9 B4 B5 59.3(2) . . ? C1 B4 H4 123.6 . . ? B8 B4 H4 122.4 . . ? B3 B4 H4 121.5 . . ? B9 B4 H4 123.1 . . ? B5 B4 H4 121.9 . . ? C1 B5 B10 105.7(3) . . ? C1 B5 B9 104.9(2) . . ? B10 B5 B9 60.5(2) . . ? C1 B5 B6 59.1(2) . . ? B10 B5 B6 59.9(2) . . ? B9 B5 B6 107.7(3) . . ? C1 B5 B4 57.67(18) . . ? B10 B5 B4 108.4(3) . . ? B9 B5 B4 60.3(2) . . ? B6 B5 B4 106.9(3) . . ? C1 B5 H5 124.5 . . ? B10 B5 H5 121.6 . . ? B9 B5 H5 122.1 . . ? B6 B5 H5 122.0 . . ? B4 B5 H5 122.0 . . ? C1 B6 C2 60.07(18) . . ? C1 B6 B10 105.2(2) . . ? C2 B6 B10 104.9(2) . . ? C1 B6 B5 58.44(19) . . ? C2 B6 B5 106.6(2) . . ? B10 B6 B5 59.9(2) . . ? C1 B6 B11 106.7(2) . . ? C2 B6 B11 58.2(2) . . ? B10 B6 B11 59.9(2) . . ? B5 B6 B11 108.3(3) . . ? C1 B6 H6 123.0 . . ? C2 B6 H6 123.3 . . ? B10 B6 H6 123.3 . . ? B5 B6 H6 121.9 . . ? B11 B6 H6 121.9 . . ? C2 B7 B8 105.8(3) . . ? C2 B7 B12 105.7(3) . . ? B8 B7 B12 61.0(2) . . ? C2 B7 B3 59.47(19) . . ? B8 B7 B3 59.8(2) . . ? B12 B7 B3 108.8(3) . . ? C2 B7 B11 58.48(19) . . ? B8 B7 B11 108.9(3) . . ? B12 B7 B11 60.3(2) . . ? B3 B7 B11 108.3(3) . . ? C2 B7 H7 124.2 . . ? B8 B7 H7 121.7 . . ? B12 B7 H7 121.6 . . ? B3 B7 H7 121.2 . . ? B11 B7 H7 121.4 . . ? B3 B8 B7 60.2(2) . . ? B3 B8 B4 60.5(2) . . ? B7 B8 B4 108.4(3) . . ? B3 B8 B9 108.4(3) . . ? B7 B8 B9 107.4(3) . . ? B4 B8 B9 60.3(2) . . ? B3 B8 B12 108.0(3) . . ? B7 B8 B12 59.6(2) . . ? B4 B8 B12 108.1(3) . . ? B9 B8 B12 59.6(2) . . ? B3 B8 H8 121.3 . . ? B7 B8 H8 121.9 . . ? B4 B8 H8 121.2 . . ? B9 B8 H8 121.9 . . ? B12 B8 H8 122.0 . . ? B5 B9 B12 108.4(3) . . ? B5 B9 B8 108.4(3) . . ? B12 B9 B8 60.4(2) . . ? B5 B9 B10 59.7(2) . . ? B12 B9 B10 60.1(2) . . ? B8 B9 B10 108.1(3) . . ? B5 B9 B4 60.4(2) . . ? B12 B9 B4 108.4(3) . . ? B8 B9 B4 59.8(2) . . ? B10 B9 B4 107.9(3) . . ? B5 B9 H9 121.5 . . ? B12 B9 H9 121.3 . . ? B8 B9 H9 121.5 . . ? B10 B9 H9 121.9 . . ? B4 B9 H9 121.6 . . ? B6 B10 B5 60.2(2) . . ? B6 B10 B11 60.2(2) . . ? B5 B10 B11 108.8(3) . . ? B6 B10 B12 108.0(3) . . ? B5 B10 B12 108.2(3) . . ? B11 B10 B12 60.1(2) . . ? B6 B10 B9 107.5(2) . . ? B5 B10 B9 59.8(2) . . ? B11 B10 B9 107.9(3) . . ? B12 B10 B9 59.7(2) . . ? B6 B10 H10 121.8 . . ? B5 B10 H10 121.3 . . ? B11 B10 H10 121.3 . . ? B12 B10 H10 121.7 . . ? B9 B10 H10 122.2 . . ? C2 B11 B10 105.7(3) . . ? C2 B11 B6 59.2(2) . . ? B10 B11 B6 59.9(2) . . ? C2 B11 B7 58.5(2) . . ? B10 B11 B7 107.7(3) . . ? B6 B11 B7 107.4(3) . . ? C2 B11 B12 105.1(3) . . ? B10 B11 B12 60.3(2) . . ? B6 B11 B12 107.8(3) . . ? B7 B11 B12 59.5(2) . . ? C2 B11 H11 124.0 . . ? B10 B11 H11 122.0 . . ? B6 B11 H11 121.7 . . ? B7 B11 H11 122.1 . . ? B12 B11 H11 122.4 . . ? B7 B12 B9 107.6(3) . . ? B7 B12 B11 60.2(2) . . ? B9 B12 B11 107.8(3) . . ? B7 B12 B10 107.7(3) . . ? B9 B12 B10 60.2(2) . . ? B11 B12 B10 59.6(2) . . ? B7 B12 B8 59.4(2) . . ? B9 B12 B8 60.0(2) . . ? B11 B12 B8 107.6(3) . . ? B10 B12 B8 107.8(3) . . ? B7 B12 H12 122.0 . . ? B9 B12 H12 121.8 . . ? B11 B12 H12 121.9 . . ? B10 B12 H12 121.8 . . ? B8 B12 H12 122.1 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? B24 B21 B22 108.2(3) . . ? B24 B21 B23 59.5(2) . . ? B22 B21 B23 60.3(2) . . ? B24 B21 B26 107.8(3) . . ? B22 B21 B26 59.3(2) . . ? B23 B21 B26 107.0(3) . . ? B24 B21 B25 59.1(2) . . ? B22 B21 B25 107.6(3) . . ? B23 B21 B25 106.3(3) . . ? B26 B21 B25 60.5(2) . . ? B24 B21 H21 121.9 . . ? B22 B21 H21 121.6 . . ? B23 B21 H21 122.6 . . ? B26 B21 H21 122.0 . . ? B25 B21 H21 122.4 . . ? C27 B22 B21 104.6(3) . . ? C27 B22 B26 101.5(3) . . ? B21 B22 B26 61.5(2) . . ? C27 B22 B23 59.8(2) . . ? B21 B22 B23 60.2(2) . . ? B26 B22 B23 108.7(3) . . ? C27 B22 B31 55.06(18) . . ? B21 B22 B31 109.0(3) . . ? B26 B22 B31 59.9(2) . . ? B23 B22 B31 107.0(3) . . ? C27 B22 H22 126.9 . . ? B21 B22 H22 121.1 . . ? B26 B22 H22 122.7 . . ? B23 B22 H22 120.8 . . ? B31 B22 H22 122.6 . . ? C28 B23 B24 59.9(2) . . ? C28 B23 C27 54.75(18) . . ? B24 B23 C27 103.4(2) . . ? C28 B23 B21 104.6(3) . . ? B24 B23 B21 59.7(2) . . ? C27 B23 B21 103.5(3) . . ? C28 B23 B22 103.8(2) . . ? B24 B23 B22 107.7(3) . . ? C27 B23 B22 59.1(2) . . ? B21 B23 B22 59.5(2) . . ? C28 B23 H23 124.9 . . ? B24 B23 H23 122.0 . . ? C27 B23 H23 125.9 . . ? B21 B23 H23 123.4 . . ? B22 B23 H23 122.2 . . ? C28 B24 B23 59.0(2) . . ? C28 B24 B21 104.8(3) . . ? B23 B24 B21 60.8(2) . . ? C28 B24 B25 102.3(3) . . ? B23 B24 B25 109.4(3) . . ? B21 B24 B25 61.8(2) . . ? C28 B24 B29 54.9(2) . . ? B23 B24 B29 106.0(3) . . ? B21 B24 B29 108.8(3) . . ? B25 B24 B29 60.1(2) . . ? C28 B24 H24 126.9 . . ? B23 B24 H24 121.1 . . ? B21 B24 H24 120.8 . . ? B25 B24 H24 121.8 . . ? B29 B24 H24 123.1 . . ? B24 B25 B30 112.3(3) . . ? B24 B25 B29 60.9(2) . . ? B30 B25 B29 62.5(2) . . ? B24 B25 B21 59.0(2) . . ? B30 B25 B21 109.5(3) . . ? B29 B25 B21 107.3(3) . . ? B24 B25 B26 107.0(3) . . ? B30 B25 B26 59.3(2) . . ? B29 B25 B26 106.7(3) . . ? B21 B25 B26 59.6(2) . . ? B24 B25 H25 120.7 . . ? B30 B25 H25 119.0 . . ? B29 B25 H25 121.6 . . ? B21 B25 H25 122.3 . . ? B26 B25 H25 123.5 . . ? B22 B26 B30 111.8(3) . . ? B22 B26 B31 61.1(2) . . ? B30 B26 B31 62.2(2) . . ? B22 B26 B21 59.3(2) . . ? B30 B26 B21 109.6(3) . . ? B31 B26 B21 108.2(3) . . ? B22 B26 B25 107.1(3) . . ? B30 B26 B25 59.2(3) . . ? B31 B26 B25 107.1(3) . . ? B21 B26 B25 59.9(2) . . ? B22 B26 H26 120.8 . . ? B30 B26 H26 119.3 . . ? B31 B26 H26 121.1 . . ? B21 B26 H26 121.7 . . ? B25 B26 H26 123.3 . . ? C28 C27 B31 114.2(3) . . ? C28 C27 B22 110.8(3) . . ? B31 C27 B22 64.3(2) . . ? C28 C27 B23 61.4(2) . . ? B31 C27 B23 115.9(2) . . ? B22 C27 B23 61.1(2) . . ? C28 C27 S 118.5(2) . . ? B31 C27 S 122.5(2) . . ? B22 C27 S 113.5(2) . . ? B23 C27 S 108.4(2) . . ? C32 C28 C27 120.0(3) . . ? C32 C28 B29 120.0(3) . . ? C27 C28 B29 111.1(3) . . ? C32 C28 B23 113.7(3) . . ? C27 C28 B23 63.8(2) . . ? B29 C28 B23 115.7(3) . . ? C32 C28 B24 117.5(3) . . ? C27 C28 B24 111.4(3) . . ? B29 C28 B24 64.4(2) . . ? B23 C28 B24 61.1(2) . . ? C28 B29 B25 105.8(3) . . ? C28 B29 B24 60.6(2) . . ? B25 B29 B24 59.0(2) . . ? C28 B29 B30 107.5(3) . . ? B25 B29 B30 58.7(2) . . ? B24 B29 B30 107.6(3) . . ? C28 B29 H29 118.1(18) . . ? B25 B29 H29 126.2(18) . . ? B24 B29 H29 118.6(18) . . ? B30 B29 H29 126.2(18) . . ? B25 B30 B26 61.5(2) . . ? B25 B30 B31 106.4(3) . . ? B26 B30 B31 59.0(2) . . ? B25 B30 B29 58.8(2) . . ? B26 B30 B29 105.7(3) . . ? B31 B30 B29 101.6(3) . . ? B25 B30 H30A 119.9(19) . . ? B26 B30 H30A 119.9(19) . . ? B31 B30 H30A 125(2) . . ? B29 B30 H30A 126.1(19) . . ? B25 B30 H30B 121.5(19) . . ? B26 B30 H30B 121.6(19) . . ? B31 B30 H30B 66.4(19) . . ? B29 B30 H30B 66.0(19) . . ? H30A B30 H30B 107(3) . . ? C27 B31 B26 105.0(3) . . ? C27 B31 B22 60.60(19) . . ? B26 B31 B22 59.0(2) . . ? C27 B31 B30 105.5(3) . . ? B26 B31 B30 58.8(2) . . ? B22 B31 B30 107.3(3) . . ? C27 B31 H31 125.8(18) . . ? B26 B31 H31 119.6(17) . . ? B22 B31 H31 118.2(17) . . ? B30 B31 H31 122.8(17) . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N C33 H33A 109.5 . . ? N C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N C34 H34A 109.5 . . ? N C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N C35 H35A 109.5 . . ? N C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N C36 H36A 109.5 . . ? N C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 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 S C1 C2 C13 5.8(3) . . . . ? S C27 C28 C32 7.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 65.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.510 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.065 #===END