Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bohumir Gruner' _publ_contact_author_email GRUNER@IIC.CAS.CZ loop_ _publ_author_name B.Gruner J.Holub J.D.Kennedy J.Plesek B.Stibr M.Thornton-Pett # Attachment '(SMe2-4-Me C2B9) CCDC 220417.cif' data_cz2 _database_code_depnum_ccdc_archive 'CCDC 220147' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H19 B9 S' _chemical_formula_weight 208.55 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 ? _symmetry_space_group_name_H-M ? 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 6.65370(10) _cell_length_b 22.4790(3) _cell_length_c 8.86450(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.7170(7) _cell_angle_gamma 90.00 _cell_volume 1248.12(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19456 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8746 _exptl_absorpt_correction_T_max 0.9220 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4664 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2367 _reflns_number_gt 2312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0338P)^2^+0.3865P] 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 SHELXL _refine_ls_extinction_coef 0.021(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2367 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.52556(18) 0.15154(5) 1.27337(14) 0.0207(2) Uani 1 1 d . . . H1 H 0.689(2) 0.1633(6) 1.3443(16) 0.029(3) Uiso 1 1 d . . . B2 B 0.32311(19) 0.14831(6) 1.35827(14) 0.0225(3) Uani 1 1 d . . . H2 H 0.340(2) 0.1598(6) 1.4797(18) 0.036(4) Uiso 1 1 d . . . B3 B 0.3159(2) 0.20496(5) 1.22066(15) 0.0235(3) Uani 1 1 d . . . H3 H 0.317(2) 0.2529(7) 1.2433(16) 0.035(4) Uiso 1 1 d . . . B4 B 0.41089(18) 0.17564(5) 1.07068(14) 0.0193(2) Uani 1 1 d . . . C4 C 0.51418(19) 0.21843(5) 0.97482(15) 0.0317(3) Uani 1 1 d . . . H4A H 0.4021 0.2340 0.8801 0.048 Uiso 1 1 calc R . . H4B H 0.6185 0.1962 0.9411 0.048 Uiso 1 1 calc R . . H4C H 0.5858 0.2516 1.0439 0.048 Uiso 1 1 calc R . . B5 B 0.46476(17) 0.09920(5) 1.11349(13) 0.0177(2) Uani 1 1 d . . . H5 H 0.588(2) 0.0752(6) 1.0808(15) 0.026(3) Uiso 1 1 d . . . B6 B 0.40596(18) 0.08120(5) 1.29367(13) 0.0189(2) Uani 1 1 d . . . H6 H 0.495(2) 0.0482(6) 1.3778(16) 0.029(3) Uiso 1 1 d . . . C7 C 0.09400(17) 0.16384(5) 1.20399(13) 0.0231(2) Uani 1 1 d . . . H7 H -0.018(2) 0.1866(6) 1.2193(17) 0.033(4) Uiso 1 1 d . . . C8 C 0.13875(16) 0.17643(5) 1.04669(12) 0.0197(2) Uani 1 1 d . . . H8 H 0.050(2) 0.2072(6) 0.9784(15) 0.023(3) Uiso 1 1 d . . . B9 B 0.22029(18) 0.12002(5) 0.97512(13) 0.0165(2) Uani 1 1 d . . . S9 S 0.15538(4) 0.117786(11) 0.75118(3) 0.02034(13) Uani 1 1 d . . . C91 C 0.3053(2) 0.05532(6) 0.72128(14) 0.0344(3) Uani 1 1 d . . . H91A H 0.2690 0.0200 0.7714 0.052 Uiso 1 1 calc R . . H91B H 0.4583 0.0636 0.7699 0.052 Uiso 1 1 calc R . . H91C H 0.2707 0.0483 0.6062 0.052 Uiso 1 1 calc R . . C92 C -0.1112(2) 0.08869(6) 0.67765(15) 0.0373(3) Uani 1 1 d . . . H92A H -0.1508 0.0803 0.5628 0.056 Uiso 1 1 calc R . . H92B H -0.2103 0.1180 0.6950 0.056 Uiso 1 1 calc R . . H92C H -0.1182 0.0519 0.7349 0.056 Uiso 1 1 calc R . . B10 B 0.22685(18) 0.05834(5) 1.10132(13) 0.0192(2) Uani 1 1 d . . . H10 H 0.224(2) 0.0104(6) 1.0750(16) 0.030(3) Uiso 1 1 d . . . H101 H 0.050(2) 0.0748(6) 1.1019(17) 0.036(4) Uiso 1 1 d . . . B11 B 0.12654(19) 0.09353(6) 1.25235(14) 0.0226(3) Uani 1 1 d . . . H11 H 0.038(2) 0.0711(6) 1.3229(17) 0.036(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0194(5) 0.0223(6) 0.0176(5) 0.0000(4) 0.0023(4) -0.0029(4) B2 0.0252(6) 0.0263(6) 0.0152(5) -0.0019(4) 0.0059(4) 0.0007(5) B3 0.0287(6) 0.0200(6) 0.0196(6) -0.0029(4) 0.0054(5) 0.0002(5) B4 0.0194(5) 0.0191(5) 0.0181(5) 0.0015(4) 0.0046(4) -0.0017(4) C4 0.0329(6) 0.0301(6) 0.0317(6) 0.0080(5) 0.0103(5) -0.0078(5) B5 0.0165(5) 0.0197(5) 0.0161(5) 0.0021(4) 0.0045(4) 0.0012(4) B6 0.0200(5) 0.0210(6) 0.0142(5) 0.0023(4) 0.0038(4) -0.0006(4) C7 0.0213(5) 0.0299(6) 0.0191(5) -0.0009(4) 0.0083(4) 0.0057(4) C8 0.0199(5) 0.0210(5) 0.0170(5) 0.0018(4) 0.0045(4) 0.0036(4) B9 0.0172(5) 0.0188(6) 0.0125(5) 0.0012(4) 0.0038(4) -0.0002(4) S9 0.02602(18) 0.02085(18) 0.01314(17) 0.00267(8) 0.00528(11) 0.00161(9) C91 0.0485(7) 0.0351(7) 0.0206(5) 0.0006(5) 0.0130(5) 0.0159(5) C92 0.0300(6) 0.0477(8) 0.0246(6) 0.0024(5) -0.0035(5) -0.0060(5) B10 0.0217(5) 0.0196(5) 0.0153(5) 0.0013(4) 0.0048(4) -0.0030(4) B11 0.0206(5) 0.0306(7) 0.0176(6) 0.0020(4) 0.0078(4) -0.0025(5) _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 B1 B2 1.7523(17) . ? B1 B3 1.7794(17) . ? B1 B5 1.7803(16) . ? B1 B4 1.7830(16) . ? B1 B6 1.8062(16) . ? B1 H1 1.090(13) . ? B2 C7 1.7057(15) . ? B2 B3 1.7529(17) . ? B2 B6 1.7666(17) . ? B2 B11 1.8111(17) . ? B2 H2 1.076(14) . ? B3 C7 1.7056(16) . ? B3 C8 1.7183(15) . ? B3 B4 1.7800(17) . ? B3 H3 1.095(15) . ? B4 C4 1.5854(15) . ? B4 C8 1.7506(15) . ? B4 B5 1.7701(16) . ? B4 B9 1.7788(16) . ? B5 B9 1.7388(15) . ? B5 B10 1.8016(16) . ? B5 B6 1.8137(15) . ? B5 H5 1.098(13) . ? B6 B11 1.7911(16) . ? B6 B10 1.7946(16) . ? B6 H6 1.077(14) . ? C7 C8 1.5471(14) . ? C7 B11 1.6329(17) . ? C7 H7 0.952(14) . ? C8 B9 1.5928(14) . ? C8 H8 0.974(13) . ? B9 B10 1.7728(15) . ? B9 S9 1.8845(11) . ? S9 C91 1.7932(12) . ? S9 C92 1.7942(12) . ? B10 B11 1.8618(16) . ? B10 H10 1.101(14) . ? B10 H101 1.235(14) . ? B11 H101 1.325(14) . ? B11 H11 1.114(14) . ? 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 B2 B1 B3 59.51(7) . . ? B2 B1 B5 108.27(8) . . ? B3 B1 B5 106.83(8) . . ? B2 B1 B4 108.41(8) . . ? B3 B1 B4 59.95(7) . . ? B5 B1 B4 59.57(6) . . ? B2 B1 B6 59.51(7) . . ? B3 B1 B6 106.51(8) . . ? B5 B1 B6 60.75(6) . . ? B4 B1 B6 108.26(8) . . ? B2 B1 H1 121.7(7) . . ? B3 B1 H1 122.0(7) . . ? B5 B1 H1 122.3(7) . . ? B4 B1 H1 120.8(7) . . ? B6 B1 H1 122.9(7) . . ? C7 B2 B1 104.82(8) . . ? C7 B2 B3 59.08(7) . . ? B1 B2 B3 61.02(7) . . ? C7 B2 B6 101.96(8) . . ? B1 B2 B6 61.76(7) . . ? B3 B2 B6 109.45(8) . . ? C7 B2 B11 55.23(6) . . ? B1 B2 B11 109.32(8) . . ? B3 B2 B11 106.73(8) . . ? B6 B2 B11 60.07(7) . . ? C7 B2 H2 121.1(8) . . ? B1 B2 H2 125.7(8) . . ? B3 B2 H2 119.4(8) . . ? B6 B2 H2 126.2(8) . . ? B11 B2 H2 119.8(8) . . ? C7 B3 C8 53.72(6) . . ? C7 B3 B2 59.08(7) . . ? C8 B3 B2 101.70(8) . . ? C7 B3 B1 103.66(8) . . ? C8 B3 B1 102.91(8) . . ? B2 B3 B1 59.47(7) . . ? C7 B3 B4 104.46(8) . . ? C8 B3 B4 60.02(6) . . ? B2 B3 B4 108.52(8) . . ? B1 B3 B4 60.12(6) . . ? C7 B3 H3 120.2(7) . . ? C8 B3 H3 119.5(7) . . ? B2 B3 H3 126.2(7) . . ? B1 B3 H3 131.1(7) . . ? B4 B3 H3 121.1(7) . . ? C4 B4 C8 123.12(9) . . ? C4 B4 B5 127.65(9) . . ? C8 B4 B5 99.34(7) . . ? C4 B4 B9 122.65(9) . . ? C8 B4 B9 53.65(6) . . ? B5 B4 B9 58.67(6) . . ? C4 B4 B3 120.20(9) . . ? C8 B4 B3 58.24(6) . . ? B5 B4 B3 107.25(8) . . ? B9 B4 B3 103.90(8) . . ? C4 B4 B1 127.51(9) . . ? C8 B4 B1 101.48(8) . . ? B5 B4 B1 60.14(6) . . ? B9 B4 B1 105.08(8) . . ? B3 B4 B1 59.92(7) . . ? B4 C4 H4A 109.5 . . ? B4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? B4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? B9 B5 B4 60.91(6) . . ? B9 B5 B1 106.91(8) . . ? B4 B5 B1 60.29(6) . . ? B9 B5 B10 60.07(6) . . ? B4 B5 B10 111.82(8) . . ? B1 B5 B10 110.10(8) . . ? B9 B5 B6 104.65(7) . . ? B4 B5 B6 108.49(8) . . ? B1 B5 B6 60.33(6) . . ? B10 B5 B6 59.52(6) . . ? B9 B5 H5 123.3(7) . . ? B4 B5 H5 122.3(7) . . ? B1 B5 H5 123.0(7) . . ? B10 B5 H5 116.9(7) . . ? B6 B5 H5 121.7(7) . . ? B2 B6 B11 61.20(7) . . ? B2 B6 B10 111.88(8) . . ? B11 B6 B10 62.56(6) . . ? B2 B6 B1 58.73(7) . . ? B11 B6 B1 107.82(8) . . ? B10 B6 B1 109.25(8) . . ? B2 B6 B5 106.18(8) . . ? B11 B6 B5 107.62(8) . . ? B10 B6 B5 59.90(6) . . ? B1 B6 B5 58.92(6) . . ? B2 B6 H6 121.6(7) . . ? B11 B6 H6 122.7(7) . . ? B10 B6 H6 119.7(7) . . ? B1 B6 H6 120.8(7) . . ? B5 B6 H6 122.0(7) . . ? C8 C7 B11 111.40(8) . . ? C8 C7 B3 63.56(7) . . ? B11 C7 B3 117.87(9) . . ? C8 C7 B2 111.62(8) . . ? B11 C7 B2 65.66(7) . . ? B3 C7 B2 61.84(7) . . ? C8 C7 H7 115.4(8) . . ? B11 C7 H7 121.6(8) . . ? B3 C7 H7 113.3(8) . . ? B2 C7 H7 121.8(9) . . ? C7 C8 B9 114.11(8) . . ? C7 C8 B3 62.72(7) . . ? B9 C8 B3 115.59(8) . . ? C7 C8 B4 113.23(8) . . ? B9 C8 B4 64.08(7) . . ? B3 C8 B4 61.74(7) . . ? C7 C8 H8 115.5(7) . . ? B9 C8 H8 122.1(7) . . ? B3 C8 H8 112.3(7) . . ? B4 C8 H8 117.7(7) . . ? C8 B9 B5 107.25(8) . . ? C8 B9 B10 108.09(8) . . ? B5 B9 B10 61.73(6) . . ? C8 B9 B4 62.27(6) . . ? B5 B9 B4 60.41(6) . . ? B10 B9 B4 112.79(8) . . ? C8 B9 S9 116.93(7) . . ? B5 B9 S9 124.29(7) . . ? B10 B9 S9 126.30(7) . . ? B4 B9 S9 113.18(7) . . ? C91 S9 C92 101.08(7) . . ? C91 S9 B9 103.61(5) . . ? C92 S9 B9 103.86(6) . . ? S9 C91 H91A 109.5 . . ? S9 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? S9 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? S9 C92 H92A 109.5 . . ? S9 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? S9 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? B9 B10 B6 104.05(8) . . ? B9 B10 B5 58.21(6) . . ? B6 B10 B5 60.57(6) . . ? B9 B10 B11 100.55(8) . . ? B6 B10 B11 58.63(6) . . ? B5 B10 B11 105.15(8) . . ? B9 B10 H10 129.5(7) . . ? B6 B10 H10 116.1(7) . . ? B5 B10 H10 117.7(7) . . ? B11 B10 H10 125.7(7) . . ? B9 B10 H101 87.0(7) . . ? B6 B10 H101 103.8(7) . . ? B5 B10 H101 131.7(7) . . ? B11 B10 H101 45.3(7) . . ? H10 B10 H101 110.2(10) . . ? C7 B11 B6 103.89(8) . . ? C7 B11 B2 59.10(7) . . ? B6 B11 B2 58.73(6) . . ? C7 B11 B10 105.69(8) . . ? B6 B11 B10 58.81(6) . . ? B2 B11 B10 106.88(8) . . ? C7 B11 H101 94.1(6) . . ? B6 B11 H101 100.1(6) . . ? B2 B11 H101 134.6(6) . . ? B10 B11 H101 41.5(6) . . ? C7 B11 H11 122.4(7) . . ? B6 B11 H11 121.6(7) . . ? B2 B11 H11 116.3(7) . . ? B10 B11 H11 126.7(7) . . ? H101 B11 H11 109.0(10) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.227 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.031 data_cz3 _database_code_depnum_ccdc_archive 'CCDC 220148' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H19 B9 S' _chemical_formula_weight 208.55 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 12.4930(2) _cell_length_b 12.1073(4) _cell_length_c 16.4857(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2493.57(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17901 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8745 _exptl_absorpt_correction_T_max 0.9608 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12059 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2429 _reflns_number_gt 2315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0422P)^2^+0.7099P] 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 2429 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.92142(10) 0.69718(10) 0.50296(7) 0.0229(3) Uani 1 1 d . . . H1 H 0.9685(11) 0.6599(13) 0.5519(9) 0.038(4) Uiso 1 1 d . . . B2 B 0.78341(10) 0.67444(10) 0.49245(8) 0.0224(3) Uani 1 1 d . . . H2 H 0.7305(11) 0.6300(11) 0.5336(8) 0.031(3) Uiso 1 1 d . . . B3 B 0.82857(9) 0.80732(10) 0.51988(7) 0.0209(3) Uani 1 1 d . . . C3 C 0.79798(10) 0.87030(11) 0.60015(7) 0.0328(3) Uani 1 1 d . . . H3A H 0.7488 0.9309 0.5873 0.049 Uiso 1 1 calc R . . H3B H 0.8629 0.9002 0.6253 0.049 Uiso 1 1 calc R . . H3C H 0.7632 0.8190 0.6378 0.049 Uiso 1 1 calc R . . B4 B 0.94959(9) 0.83139(10) 0.46576(7) 0.0200(2) Uani 1 1 d . . . H4 H 1.0063(11) 0.8886(12) 0.4899(8) 0.032(4) Uiso 1 1 d . . . B5 B 0.97705(9) 0.71549(10) 0.40477(8) 0.0222(3) Uani 1 1 d . . . H5 H 1.0559(11) 0.6908(12) 0.3885(8) 0.035(4) Uiso 1 1 d . . . B6 B 0.87067(10) 0.61591(10) 0.41955(8) 0.0246(3) Uani 1 1 d . . . H6 H 0.8867(12) 0.5254(13) 0.4175(9) 0.044(4) Uiso 1 1 d . . . C7 C 0.73729(8) 0.78796(9) 0.44339(6) 0.0204(2) Uani 1 1 d . . . H7 H 0.6697(11) 0.8177(11) 0.4588(8) 0.027(3) Uiso 1 1 d . . . C8 C 0.82784(8) 0.87197(8) 0.42580(6) 0.0184(2) Uani 1 1 d . . . H8 H 0.8071(10) 0.9472(11) 0.4299(8) 0.025(3) Uiso 1 1 d . . . B9 B 0.91476(9) 0.83025(9) 0.36227(7) 0.0192(2) Uani 1 1 d . . . S9 S 0.98430(2) 0.93825(2) 0.299242(16) 0.02405(12) Uani 1 1 d . . . C91 C 1.09297(11) 0.86491(13) 0.25323(10) 0.0474(4) Uani 1 1 d . . . H91A H 1.0659 0.7973 0.2278 0.071 Uiso 1 1 calc R . . H91B H 1.1459 0.8457 0.2948 0.071 Uiso 1 1 calc R . . H91C H 1.1266 0.9116 0.2119 0.071 Uiso 1 1 calc R . . C92 C 0.89694(11) 0.95632(11) 0.21422(8) 0.0342(3) Uani 1 1 d . . . H92A H 0.9329 1.0009 0.1728 0.051 Uiso 1 1 calc R . . H92B H 0.8315 0.9939 0.2318 0.051 Uiso 1 1 calc R . . H92C H 0.8786 0.8840 0.1915 0.051 Uiso 1 1 calc R . . B10 B 0.87564(10) 0.69634(10) 0.32874(8) 0.0248(3) Uani 1 1 d . . . H10 H 0.8960(11) 0.6531(11) 0.2708(8) 0.036(4) Uiso 1 1 d . . . H101 H 0.7837(12) 0.7353(12) 0.3218(9) 0.041(4) Uiso 1 1 d . . . B11 B 0.74804(10) 0.67890(10) 0.38624(8) 0.0247(3) Uani 1 1 d . . . H11 H 0.6796(11) 0.6297(11) 0.3686(8) 0.032(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0203(6) 0.0230(6) 0.0254(6) 0.0056(5) -0.0028(5) 0.0016(5) B2 0.0207(6) 0.0197(5) 0.0267(6) 0.0044(5) -0.0007(5) -0.0020(4) B3 0.0194(6) 0.0219(6) 0.0212(6) 0.0016(5) 0.0003(4) -0.0014(4) C3 0.0364(7) 0.0368(7) 0.0253(6) -0.0051(5) 0.0064(5) -0.0050(5) B4 0.0174(5) 0.0202(6) 0.0223(6) 0.0000(5) -0.0012(4) -0.0018(4) B5 0.0193(6) 0.0203(6) 0.0270(6) 0.0010(5) 0.0016(5) 0.0030(4) B6 0.0259(6) 0.0152(5) 0.0327(7) 0.0009(5) 0.0005(5) 0.0011(5) C7 0.0148(5) 0.0199(5) 0.0266(5) 0.0025(4) -0.0013(4) 0.0002(4) C8 0.0178(5) 0.0143(5) 0.0229(5) 0.0014(4) -0.0003(4) 0.0009(4) B9 0.0208(6) 0.0165(5) 0.0203(5) 0.0019(4) 0.0012(4) -0.0007(4) S9 0.02454(18) 0.02283(18) 0.02476(18) 0.00407(10) 0.00286(10) -0.00366(10) C91 0.0329(7) 0.0539(8) 0.0555(9) 0.0188(7) 0.0234(6) 0.0118(6) C92 0.0359(7) 0.0389(7) 0.0279(6) 0.0114(5) -0.0023(5) -0.0018(5) B10 0.0290(6) 0.0215(6) 0.0238(6) -0.0038(5) 0.0007(5) -0.0001(5) B11 0.0234(6) 0.0213(6) 0.0293(6) -0.0003(5) -0.0045(5) -0.0042(5) _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 B1 B2 1.7545(17) . ? B1 B4 1.7721(17) . ? B1 B5 1.7756(17) . ? B1 B3 1.7893(17) . ? B1 B6 1.8057(18) . ? B1 H1 1.096(14) . ? B2 C7 1.6956(15) . ? B2 B3 1.7638(16) . ? B2 B6 1.7705(18) . ? B2 B11 1.8066(17) . ? B2 H2 1.089(13) . ? B3 C3 1.5744(16) . ? B3 C7 1.7162(15) . ? B3 C8 1.7372(15) . ? B3 B4 1.7796(17) . ? B4 C8 1.7288(15) . ? B4 B5 1.7600(17) . ? B4 B9 1.7606(16) . ? B4 H4 1.067(14) . ? B5 B9 1.7397(16) . ? B5 B10 1.7971(17) . ? B5 B6 1.8109(17) . ? B5 H5 1.064(14) . ? B6 B10 1.7871(18) . ? B6 B11 1.7972(18) . ? B6 H6 1.115(16) . ? C7 C8 1.5487(14) . ? C7 B11 1.6277(16) . ? C7 H7 0.952(13) . ? C8 B9 1.5910(15) . ? C8 H8 0.949(13) . ? B9 B10 1.7812(16) . ? B9 S9 1.8827(11) . ? S9 C92 1.7899(13) . ? S9 C91 1.7908(13) . ? B10 B11 1.8667(18) . ? B10 H10 1.118(14) . ? B10 H101 1.248(15) . ? B11 H101 1.339(15) . ? B11 H11 1.082(14) . ? 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 B2 B1 B4 107.75(8) . . ? B2 B1 B5 108.31(9) . . ? B4 B1 B5 59.48(7) . . ? B2 B1 B3 59.69(7) . . ? B4 B1 B3 59.95(7) . . ? B5 B1 B3 107.62(8) . . ? B2 B1 B6 59.62(7) . . ? B4 B1 B6 107.81(8) . . ? B5 B1 B6 60.74(7) . . ? B3 B1 B6 107.29(8) . . ? B2 B1 H1 122.4(8) . . ? B4 B1 H1 121.7(8) . . ? B5 B1 H1 120.8(8) . . ? B3 B1 H1 122.7(8) . . ? B6 B1 H1 121.6(8) . . ? C7 B2 B1 104.71(8) . . ? C7 B2 B3 59.44(6) . . ? B1 B2 B3 61.14(7) . . ? C7 B2 B6 102.12(8) . . ? B1 B2 B6 61.63(7) . . ? B3 B2 B6 110.01(8) . . ? C7 B2 B11 55.28(6) . . ? B1 B2 B11 109.35(9) . . ? B3 B2 B11 107.42(8) . . ? B6 B2 B11 60.31(7) . . ? C7 B2 H2 119.4(7) . . ? B1 B2 H2 127.8(7) . . ? B3 B2 H2 119.0(7) . . ? B6 B2 H2 126.8(7) . . ? B11 B2 H2 118.0(7) . . ? C3 B3 C7 121.50(9) . . ? C3 B3 C8 122.07(9) . . ? C7 B3 C8 53.29(6) . . ? C3 B3 B2 125.42(10) . . ? C7 B3 B2 58.30(6) . . ? C8 B3 B2 100.40(8) . . ? C3 B3 B4 123.25(9) . . ? C7 B3 B4 102.63(8) . . ? C8 B3 B4 58.87(6) . . ? B2 B3 B4 107.01(8) . . ? C3 B3 B1 130.49(10) . . ? C7 B3 B1 102.38(8) . . ? C8 B3 B1 101.54(8) . . ? B2 B3 B1 59.18(7) . . ? B4 B3 B1 59.54(7) . . ? C8 B4 B5 100.39(8) . . ? C8 B4 B9 54.24(6) . . ? B5 B4 B9 59.23(7) . . ? C8 B4 B1 102.57(8) . . ? B5 B4 B1 60.35(7) . . ? B9 B4 B1 106.20(8) . . ? C8 B4 B3 59.34(6) . . ? B5 B4 B3 108.75(8) . . ? B9 B4 B3 105.93(8) . . ? B1 B4 B3 60.50(7) . . ? C8 B4 H4 122.7(8) . . ? B5 B4 H4 126.9(7) . . ? B9 B4 H4 122.0(8) . . ? B1 B4 H4 126.7(8) . . ? B3 B4 H4 118.9(7) . . ? B9 B5 B4 60.40(7) . . ? B9 B5 B1 106.96(8) . . ? B4 B5 B1 60.16(7) . . ? B9 B5 B10 60.45(7) . . ? B4 B5 B10 111.34(8) . . ? B1 B5 B10 110.11(8) . . ? B9 B5 B6 104.93(8) . . ? B4 B5 B6 108.11(8) . . ? B1 B5 B6 60.45(7) . . ? B10 B5 B6 59.38(7) . . ? B9 B5 H5 122.5(8) . . ? B4 B5 H5 123.3(8) . . ? B1 B5 H5 123.9(8) . . ? B10 B5 H5 116.1(8) . . ? B6 B5 H5 121.7(8) . . ? B2 B6 B10 111.84(8) . . ? B2 B6 B11 60.84(7) . . ? B10 B6 B11 62.77(7) . . ? B2 B6 B1 58.75(7) . . ? B10 B6 B1 109.19(8) . . ? B11 B6 B1 107.50(8) . . ? B2 B6 B5 106.07(8) . . ? B10 B6 B5 59.93(7) . . ? B11 B6 B5 107.57(8) . . ? B1 B6 B5 58.81(7) . . ? B2 B6 H6 121.6(8) . . ? B10 B6 H6 120.3(8) . . ? B11 B6 H6 124.1(8) . . ? B1 B6 H6 119.7(8) . . ? B5 B6 H6 121.3(8) . . ? C8 C7 B11 111.35(9) . . ? C8 C7 B2 111.93(8) . . ? B11 C7 B2 65.82(7) . . ? C8 C7 B3 64.05(7) . . ? B11 C7 B3 118.77(8) . . ? B2 C7 B3 62.26(7) . . ? C8 C7 H7 116.7(8) . . ? B11 C7 H7 122.3(8) . . ? B2 C7 H7 118.7(8) . . ? B3 C7 H7 109.9(8) . . ? C7 C8 B9 114.41(8) . . ? C7 C8 B4 112.63(8) . . ? B9 C8 B4 63.90(7) . . ? C7 C8 B3 62.66(7) . . ? B9 C8 B3 116.17(8) . . ? B4 C8 B3 61.79(6) . . ? C7 C8 H8 114.7(8) . . ? B9 C8 H8 122.5(8) . . ? B4 C8 H8 119.1(8) . . ? B3 C8 H8 111.7(8) . . ? C8 B9 B5 107.08(8) . . ? C8 B9 B4 61.86(7) . . ? B5 B9 B4 60.37(7) . . ? C8 B9 B10 107.82(8) . . ? B5 B9 B10 61.37(7) . . ? B4 B9 B10 112.07(8) . . ? C8 B9 S9 117.24(7) . . ? B5 B9 S9 124.79(8) . . ? B4 B9 S9 114.54(7) . . ? B10 B9 S9 125.98(8) . . ? C92 S9 C91 101.02(7) . . ? C92 S9 B9 103.64(6) . . ? C91 S9 B9 103.84(6) . . ? B9 B10 B6 104.21(8) . . ? B9 B10 B5 58.18(7) . . ? B6 B10 B5 60.69(7) . . ? B9 B10 B11 100.35(8) . . ? B6 B10 B11 58.88(7) . . ? B5 B10 B11 105.21(8) . . ? B9 B10 H10 129.0(7) . . ? B6 B10 H10 117.9(7) . . ? B5 B10 H10 119.7(7) . . ? B11 B10 H10 125.1(7) . . ? B9 B10 H101 86.4(7) . . ? B6 B10 H101 104.5(7) . . ? B5 B10 H101 131.6(7) . . ? B11 B10 H101 45.8(7) . . ? H10 B10 H101 107.9(10) . . ? C7 B11 B6 103.75(8) . . ? C7 B11 B2 58.90(7) . . ? B6 B11 B2 58.85(7) . . ? C7 B11 B10 105.82(8) . . ? B6 B11 B10 58.35(7) . . ? B2 B11 B10 106.66(8) . . ? C7 B11 H101 94.2(6) . . ? B6 B11 H101 100.1(6) . . ? B2 B11 H101 134.7(6) . . ? B10 B11 H101 41.9(6) . . ? C7 B11 H11 122.5(7) . . ? B6 B11 H11 121.5(7) . . ? B2 B11 H11 115.9(7) . . ? B10 B11 H11 126.9(7) . . ? H101 B11 H11 109.3(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.240 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.035