####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_UDO11 _database_code_depnum_ccdc_archive 'CCDC 280344' _audit_creation_date 97-07-20 _audit_creation_method 'STADI4, X-RED' _chemical_name_systematic ; ? ; _chemical_name_common (5-(SMe2)-nido-B10H12) _chemical_formula_moiety ? _chemical_formula_sum 'C2 H18 B10 S' _chemical_formula_weight 182.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' H H 0.0000 0.0000 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 5.7777(4) _cell_length_b 12.9809(8) _cell_length_c 15.0483(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1128.62(11) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 30.3 _cell_measurement_theta_max 39.4 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 1.976 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5205 _exptl_absorpt_correction_T_max 0.6592 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_measurement_device 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 1.95 - 2.20, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5.3 _diffrn_reflns_number 1785 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.50 _diffrn_reflns_theta_max 64.45 _reflns_number_total 1785 _reflns_number_gt 1759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 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 w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.3707P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(19) _refine_ls_number_reflns 1785 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B -0.0934(4) 1.58119(16) 0.53259(15) 0.0191(5) Uani 1 d . . . H1 H -0.264(4) 1.6190(15) 0.5179(13) 0.023(6) Uiso 1 d . . . B2 B -0.0371(4) 1.53947(16) 0.64210(14) 0.0187(5) Uani 1 d . . . H2 H -0.165(5) 1.5393(18) 0.6915(16) 0.041(7) Uiso 1 d . . . B3 B -0.0456(4) 1.44728(17) 0.55570(15) 0.0178(5) Uani 1 d . . . H3 H -0.183(5) 1.3858(19) 0.5505(16) 0.042(7) Uiso 1 d . . . B4 B 0.0316(4) 1.49945(17) 0.44971(14) 0.0188(5) Uani 1 d . . . H4 H -0.073(4) 1.4748(18) 0.3929(16) 0.031(6) Uiso 1 d . . . B5 B 0.1073(4) 1.65007(17) 0.59980(14) 0.0198(5) Uani 1 d . . . H56 H 0.317(4) 1.6266(17) 0.6029(14) 0.030(6) Uiso 1 d . . . H5 H 0.089(4) 1.7324(16) 0.6177(13) 0.022(6) Uiso 1 d . . . B6 B 0.2574(4) 1.55974(16) 0.66658(14) 0.0186(5) Uani 1 d . . . H6 H 0.343(4) 1.5785(16) 0.7259(14) 0.028(6) Uiso 1 d . . . B7 B 0.1840(4) 1.44452(15) 0.62896(14) 0.0167(5) Uani 1 d . . . B8 B 0.2394(4) 1.42246(16) 0.51075(14) 0.0187(4) Uani 1 d . . . H8 H 0.299(4) 1.3433(17) 0.4898(15) 0.033(6) Uiso 1 d . . . H89 H 0.422(4) 1.4762(19) 0.5001(16) 0.034(7) Uiso 1 d . . . B9 B 0.3209(4) 1.52457(17) 0.43706(14) 0.0202(5) Uani 1 d . . . H9 H 0.429(4) 1.5156(18) 0.3822(16) 0.032(6) Uiso 1 d . . . H910 H 0.356(5) 1.6116(19) 0.4700(16) 0.038(7) Uiso 1 d . . . B10 B 0.1311(4) 1.62765(16) 0.46633(15) 0.0201(5) Uani 1 d . . . H10 H 0.107(4) 1.6926(16) 0.4257(13) 0.022(5) Uiso 1 d . . . S7 S 0.20829(8) 1.33655(3) 0.71203(3) 0.01884(15) Uani 1 d . . . C71 C 0.5145(4) 1.32294(18) 0.72508(14) 0.0321(5) Uani 1 d . . . H71A H 0.5475 1.2624 0.7618 0.048 Uiso 1 calc R . . H71B H 0.5772 1.3846 0.7540 0.048 Uiso 1 calc R . . H71C H 0.5867 1.3144 0.6666 0.048 Uiso 1 calc R . . C72 C 0.1391(4) 1.21946(14) 0.65559(14) 0.0295(5) Uani 1 d . . . H72A H 0.2322 1.2142 0.6013 0.044 Uiso 1 calc R . . H72B H -0.0256 1.2192 0.6400 0.044 Uiso 1 calc R . . H72C H 0.1729 1.1608 0.6944 0.044 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 B1 0.0131(11) 0.0185(10) 0.0258(11) 0.0005(9) -0.0029(9) 0.0001(9) B2 0.0157(12) 0.0197(10) 0.0207(10) -0.0043(8) 0.0019(9) 0.0012(9) B3 0.0128(11) 0.0190(10) 0.0217(10) -0.0026(8) 0.0010(9) -0.0004(8) B4 0.0176(12) 0.0187(10) 0.0200(10) 0.0021(8) -0.0019(9) -0.0023(9) B5 0.0137(11) 0.0190(10) 0.0267(10) -0.0015(9) -0.0033(9) -0.0004(9) B6 0.0142(12) 0.0215(10) 0.0201(10) -0.0013(8) -0.0020(9) -0.0002(9) B7 0.0148(11) 0.0172(9) 0.0180(10) 0.0001(8) 0.0015(9) 0.0009(9) B8 0.0146(12) 0.0213(10) 0.0202(10) 0.0001(8) 0.0033(9) 0.0012(9) B9 0.0171(13) 0.0241(10) 0.0194(10) 0.0021(8) 0.0011(9) -0.0002(9) B10 0.0164(11) 0.0184(10) 0.0256(11) 0.0034(8) -0.0057(9) -0.0030(9) S7 0.0204(3) 0.0184(2) 0.0177(2) 0.00062(17) 0.00224(17) 0.00055(18) C71 0.0212(11) 0.0381(11) 0.0371(12) 0.0136(10) -0.0004(9) 0.0059(10) C72 0.0443(15) 0.0155(9) 0.0287(11) -0.0007(8) -0.0040(10) -0.0018(9) _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 B10 1.744(3) . ? B1 B2 1.765(3) . ? B1 B5 1.780(3) . ? B1 B4 1.790(3) . ? B1 B3 1.794(3) . ? B1 H1 1.12(2) . ? B2 B6 1.761(3) . ? B2 B3 1.768(3) . ? B2 B5 1.778(3) . ? B2 B7 1.786(3) . ? B2 H2 1.05(3) . ? B3 B7 1.725(3) . ? B3 B4 1.789(3) . ? B3 B8 1.809(3) . ? B3 H3 1.13(3) . ? B4 B9 1.714(3) . ? B4 B10 1.778(3) . ? B4 B8 1.812(3) . ? B4 H4 1.09(2) . ? B5 B6 1.771(3) . ? B5 B10 2.034(3) . ? B5 H56 1.25(2) . ? B5 H5 1.11(2) . ? B6 B7 1.654(3) . ? B6 H56 1.34(2) . ? B6 H6 1.05(2) . ? B7 B8 1.830(3) . ? B7 S7 1.883(2) . ? B8 B9 1.791(3) . ? B8 H8 1.13(2) . ? B8 H89 1.28(3) . ? B9 B10 1.785(3) . ? B9 H89 1.28(2) . ? B9 H9 1.04(2) . ? B9 H910 1.25(2) . ? B10 H910 1.32(3) . ? B10 H10 1.05(2) . ? S7 C72 1.7863(19) . ? S7 C71 1.789(2) . ? 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 B10 B1 B2 120.20(17) . . ? B10 B1 B5 70.52(13) . . ? B2 B1 B5 60.23(12) . . ? B10 B1 B4 60.42(12) . . ? B2 B1 B4 113.23(15) . . ? B5 B1 B4 115.54(16) . . ? B10 B1 B3 109.35(16) . . ? B2 B1 B3 59.56(12) . . ? B5 B1 B3 106.04(15) . . ? B4 B1 B3 59.90(12) . . ? B10 B1 H1 112.9(11) . . ? B2 B1 H1 118.7(11) . . ? B5 B1 H1 117.6(10) . . ? B4 B1 H1 118.5(11) . . ? B3 B1 H1 126.7(11) . . ? B6 B2 B1 109.12(16) . . ? B6 B2 B3 106.36(15) . . ? B1 B2 B3 61.04(12) . . ? B6 B2 B5 60.05(12) . . ? B1 B2 B5 60.29(12) . . ? B3 B2 B5 107.23(15) . . ? B6 B2 B7 55.60(11) . . ? B1 B2 B7 103.89(15) . . ? B3 B2 B7 58.08(12) . . ? B5 B2 B7 100.48(15) . . ? B6 B2 H2 122.2(14) . . ? B1 B2 H2 122.2(14) . . ? B3 B2 H2 120.0(14) . . ? B5 B2 H2 125.9(13) . . ? B7 B2 H2 125.5(13) . . ? B7 B3 B2 61.50(12) . . ? B7 B3 B4 112.70(16) . . ? B2 B3 B4 113.11(15) . . ? B7 B3 B1 105.21(15) . . ? B2 B3 B1 59.40(12) . . ? B4 B3 B1 59.92(12) . . ? B7 B3 B8 62.32(13) . . ? B2 B3 B8 111.75(15) . . ? B4 B3 B8 60.48(12) . . ? B1 B3 B8 103.90(15) . . ? B7 B3 H3 124.8(13) . . ? B2 B3 H3 123.4(13) . . ? B4 B3 H3 112.4(12) . . ? B1 B3 H3 124.4(14) . . ? B8 B3 H3 119.2(14) . . ? B9 B4 B10 61.45(13) . . ? B9 B4 B3 114.46(16) . . ? B10 B4 B3 108.02(15) . . ? B9 B4 B1 110.99(16) . . ? B10 B4 B1 58.51(12) . . ? B3 B4 B1 60.17(12) . . ? B9 B4 B8 60.98(13) . . ? B10 B4 B8 103.33(15) . . ? B3 B4 B8 60.30(12) . . ? B1 B4 B8 103.95(15) . . ? B9 B4 H4 120.5(13) . . ? B10 B4 H4 124.2(12) . . ? B3 B4 H4 116.6(12) . . ? B1 B4 H4 119.7(13) . . ? B8 B4 H4 126.9(12) . . ? B6 B5 B2 59.48(12) . . ? B6 B5 B1 107.99(15) . . ? B2 B5 B1 59.48(12) . . ? B6 B5 B10 115.62(14) . . ? B2 B5 B10 105.65(14) . . ? B1 B5 B10 53.92(11) . . ? B6 B5 H56 48.9(10) . . ? B2 B5 H56 104.1(10) . . ? B1 B5 H56 122.0(10) . . ? B10 B5 H56 86.4(10) . . ? B6 B5 H5 123.2(11) . . ? B2 B5 H5 130.2(11) . . ? B1 B5 H5 124.1(12) . . ? B10 B5 H5 112.7(11) . . ? H56 B5 H5 108.7(16) . . ? B7 B6 B2 62.98(13) . . ? B7 B6 B5 106.20(16) . . ? B2 B6 B5 60.47(13) . . ? B7 B6 H56 114.1(10) . . ? B2 B6 H56 101.4(11) . . ? B5 B6 H56 44.9(10) . . ? B7 B6 H6 128.5(11) . . ? B2 B6 H6 132.0(13) . . ? B5 B6 H6 124.0(12) . . ? H56 B6 H6 109.6(15) . . ? B6 B7 B3 113.38(15) . . ? B6 B7 B2 61.42(12) . . ? B3 B7 B2 60.42(12) . . ? B6 B7 B8 115.43(15) . . ? B3 B7 B8 61.08(12) . . ? B2 B7 B8 109.92(15) . . ? B6 B7 S7 115.25(14) . . ? B3 B7 S7 119.79(14) . . ? B2 B7 S7 119.55(14) . . ? B8 B7 S7 121.05(13) . . ? B9 B8 B3 109.82(16) . . ? B9 B8 B4 56.80(12) . . ? B3 B8 B4 59.22(12) . . ? B9 B8 B7 122.14(15) . . ? B3 B8 B7 56.60(12) . . ? B4 B8 B7 106.89(15) . . ? B9 B8 H8 114.8(11) . . ? B3 B8 H8 123.1(12) . . ? B4 B8 H8 124.3(12) . . ? B7 B8 H8 117.9(11) . . ? B9 B8 H89 45.6(11) . . ? B3 B8 H89 134.7(11) . . ? B4 B8 H89 100.6(11) . . ? B7 B8 H89 100.5(11) . . ? H8 B8 H89 102.0(16) . . ? B4 B9 B10 61.05(13) . . ? B4 B9 B8 62.22(13) . . ? B10 B9 B8 103.90(16) . . ? B4 B9 H89 105.7(12) . . ? B10 B9 H89 117.8(11) . . ? B8 B9 H89 45.4(11) . . ? B4 B9 H9 130.7(13) . . ? B10 B9 H9 130.4(13) . . ? B8 B9 H9 124.4(13) . . ? H89 B9 H9 104.9(17) . . ? B4 B9 H910 106.6(13) . . ? B10 B9 H910 47.5(13) . . ? B8 B9 H910 117.8(11) . . ? H89 B9 H910 94.4(16) . . ? H9 B9 H910 108.6(18) . . ? B1 B10 B4 61.06(12) . . ? B1 B10 B9 109.81(15) . . ? B4 B10 B9 57.50(12) . . ? B1 B10 B5 55.57(11) . . ? B4 B10 B5 104.53(14) . . ? B9 B10 B5 113.11(14) . . ? B1 B10 H910 130.9(11) . . ? B4 B10 H910 100.2(11) . . ? B9 B10 H910 44.4(11) . . ? B5 B10 H910 92.7(11) . . ? B1 B10 H10 120.9(12) . . ? B4 B10 H10 128.8(11) . . ? B9 B10 H10 122.6(12) . . ? B5 B10 H10 116.8(11) . . ? H910 B10 H10 106.3(16) . . ? B5 H56 B6 86.2(15) . . ? B8 H89 B9 89.1(16) . . ? B9 H910 B10 88.1(17) . . ? C72 S7 C71 100.92(12) . . ? C72 S7 B7 107.52(9) . . ? C71 S7 B7 102.71(10) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 64.45 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.170 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.039 data_k16597 _database_code_depnum_ccdc_archive 'CCDC 280345' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (6,9-(SMe2)2-arachno-B10H11-1-(6'-nido-B10H13)) _chemical_melting_point ? _chemical_formula_moiety 'C4 H36 B20 S2' _chemical_formula_sum 'C4 H36 B20 S2' _chemical_formula_weight 364.65 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.0367(1) _cell_length_b 32.4271(4) _cell_length_c 10.5289(1) _cell_angle_alpha 90.00 _cell_angle_beta 96.089(1) _cell_angle_gamma 90.00 _cell_volume 2388.93(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 24.0 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9431 _exptl_absorpt_correction_T_max 0.9979 _exptl_absorpt_process_details 'sadabs v2006/1' _exptl_special_details ; All cage H atoms were located and refined freely. All other H atoms were added in their calculated positions and were treated using appropriate riding models. ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36237 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4210 _reflns_number_gt 2737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker-SHELXTL (Sheldrick, 2005)' _computing_structure_refinement 'Bruker-SHELXTL (Sheldrick, 2005)' _computing_molecular_graphics 'Bruker-SHELXTL (Sheldrick, 2005)' _computing_publication_material 'Bruker-SHELXTL (Sheldrick, 2005)' _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^)+(0.0134P)^2^+3.1730P] 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 4210 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.101 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.01090(13) 0.40483(3) 0.88020(9) 0.0399(3) Uani 1 1 d . . . S2 S -0.03692(15) 0.23621(3) 0.46616(9) 0.0471(3) Uani 1 1 d . . . C11 C 0.0907(6) 0.45371(11) 0.8449(4) 0.0560(11) Uani 1 1 d . . . H11A H 0.2275 0.4531 0.8696 0.084 Uiso 1 1 calc R . . H11B H 0.0332 0.4753 0.8921 0.084 Uiso 1 1 calc R . . H11C H 0.0664 0.4592 0.7541 0.084 Uiso 1 1 calc R . . C12 C -0.2596(5) 0.41412(13) 0.8265(4) 0.0554(11) Uani 1 1 d . . . H12A H -0.3335 0.3896 0.8402 0.083 Uiso 1 1 calc R . . H12B H -0.2728 0.4208 0.7362 0.083 Uiso 1 1 calc R . . H12C H -0.3061 0.4369 0.8742 0.083 Uiso 1 1 calc R . . C21 C -0.0138(9) 0.19660(13) 0.5848(5) 0.103(2) Uani 1 1 d . . . H21A H 0.1205 0.1915 0.6106 0.155 Uiso 1 1 calc R . . H21B H -0.0737 0.1715 0.5498 0.155 Uiso 1 1 calc R . . H21C H -0.0758 0.2053 0.6583 0.155 Uiso 1 1 calc R . . C22 C -0.2909(6) 0.24071(17) 0.4327(6) 0.103(2) Uani 1 1 d . . . H22A H -0.3209 0.2618 0.3684 0.154 Uiso 1 1 calc R . . H22B H -0.3458 0.2482 0.5102 0.154 Uiso 1 1 calc R . . H22C H -0.3436 0.2145 0.4015 0.154 Uiso 1 1 calc R . . B1 B 0.2341(6) 0.36220(13) 0.5090(4) 0.0381(10) Uani 1 1 d . . . B2 B 0.2523(6) 0.37587(13) 0.6759(4) 0.0367(10) Uani 1 1 d . . . B3 B 0.3857(6) 0.33316(13) 0.6309(4) 0.0400(10) Uani 1 1 d . . . B4 B 0.2343(6) 0.30750(13) 0.5107(4) 0.0371(10) Uani 1 1 d . . . B5 B 0.0274(6) 0.38021(13) 0.5819(4) 0.0365(10) Uani 1 1 d . . . B6 B 0.0510(6) 0.36493(12) 0.7534(4) 0.0327(9) Uani 1 1 d . . . B7 B 0.2766(6) 0.33311(13) 0.7783(4) 0.0374(10) Uani 1 1 d . . . B8 B 0.2636(6) 0.28694(14) 0.6680(4) 0.0388(10) Uani 1 1 d . . . B9 B 0.0288(6) 0.28532(13) 0.5645(4) 0.0353(10) Uani 1 1 d . . . B10 B 0.0159(6) 0.33384(13) 0.4710(4) 0.0376(10) Uani 1 1 d . . . B1' B 0.4282(6) 0.41058(14) 0.1368(4) 0.0435(11) Uani 1 1 d . . . B2' B 0.2474(6) 0.40741(14) 0.2439(4) 0.0416(11) Uani 1 1 d . . . B3' B 0.3426(7) 0.45620(14) 0.2049(4) 0.0454(12) Uani 1 1 d . . . B4' B 0.5811(7) 0.45466(15) 0.1612(5) 0.0489(12) Uani 1 1 d . . . B5' B 0.4448(6) 0.37231(14) 0.2566(4) 0.0431(11) Uani 1 1 d . . . B6' B 0.3354(6) 0.39002(13) 0.3980(4) 0.0403(11) Uani 1 1 d . . . B7' B 0.3073(6) 0.44544(14) 0.3657(4) 0.0437(11) Uani 1 1 d . . . B8' B 0.5266(7) 0.47657(15) 0.3104(5) 0.0480(12) Uani 1 1 d . . . B9' B 0.7414(7) 0.44826(15) 0.2949(5) 0.0502(12) Uani 1 1 d . . . B10' B 0.6652(6) 0.40365(15) 0.1995(5) 0.0464(11) Uani 1 1 d . . . H2 H 0.316(4) 0.4070(9) 0.706(3) 0.031(8) Uiso 1 1 d . . . H3 H 0.542(4) 0.3345(9) 0.627(3) 0.034(9) Uiso 1 1 d . . . H4 H 0.282(4) 0.2902(9) 0.434(3) 0.032(8) Uiso 1 1 d . . . H5 H -0.041(5) 0.4096(11) 0.547(3) 0.052(10) Uiso 1 1 d . . . H6 H -0.064(4) 0.3413(9) 0.762(3) 0.032(8) Uiso 1 1 d . . . H7 H 0.364(4) 0.3330(10) 0.873(3) 0.044(9) Uiso 1 1 d . . . H8 H 0.349(4) 0.2605(10) 0.692(3) 0.038(9) Uiso 1 1 d . . . H9 H -0.078(4) 0.2897(10) 0.636(3) 0.044(9) Uiso 1 1 d . . . H10 H -0.059(4) 0.3369(9) 0.375(3) 0.035(9) Uiso 1 1 d . . . H78 H 0.178(5) 0.3003(11) 0.760(3) 0.054(10) Uiso 1 1 d . . . H510 H -0.091(5) 0.3510(11) 0.551(3) 0.056(11) Uiso 1 1 d . . . H1' H 0.393(4) 0.3985(10) 0.041(3) 0.043(9) Uiso 1 1 d . . . H2' H 0.102(5) 0.3987(9) 0.205(3) 0.040(9) Uiso 1 1 d . . . H3' H 0.247(5) 0.4781(11) 0.159(3) 0.060(11) Uiso 1 1 d . . . H4' H 0.621(5) 0.4733(10) 0.080(3) 0.050(10) Uiso 1 1 d . . . H5' H 0.455(5) 0.3373(12) 0.232(3) 0.065(12) Uiso 1 1 d . . . H7' H 0.206(5) 0.4639(10) 0.422(3) 0.047(10) Uiso 1 1 d . . . H8' H 0.536(5) 0.5083(12) 0.340(3) 0.062(12) Uiso 1 1 d . . . H9' H 0.885(5) 0.4586(10) 0.308(3) 0.044(10) Uiso 1 1 d . . . H10' H 0.769(5) 0.3858(10) 0.154(3) 0.047(10) Uiso 1 1 d . . . H56' H 0.510(5) 0.3745(11) 0.375(4) 0.064(11) Uiso 1 1 d . . . H67' H 0.423(4) 0.4269(10) 0.440(3) 0.043(9) Uiso 1 1 d . . . H89' H 0.649(4) 0.4572(9) 0.388(3) 0.032(8) Uiso 1 1 d . . . H91' H 0.728(5) 0.4092(11) 0.314(3) 0.056(11) 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 S1 0.0416(5) 0.0390(5) 0.0391(5) -0.0043(5) 0.0047(4) 0.0013(5) S2 0.0549(6) 0.0391(6) 0.0484(6) -0.0103(5) 0.0110(5) -0.0077(5) C11 0.058(3) 0.034(2) 0.076(3) -0.012(2) 0.009(2) -0.004(2) C12 0.035(2) 0.062(3) 0.070(3) -0.018(2) 0.010(2) 0.008(2) C21 0.189(6) 0.037(3) 0.081(4) 0.008(3) 0.002(4) -0.029(3) C22 0.054(3) 0.096(4) 0.155(5) -0.050(4) -0.008(3) -0.018(3) B1 0.037(2) 0.033(2) 0.046(3) 0.000(2) 0.013(2) -0.0027(19) B2 0.036(2) 0.033(2) 0.041(3) -0.001(2) 0.0028(19) -0.0036(19) B3 0.032(2) 0.041(3) 0.047(3) -0.001(2) 0.008(2) -0.003(2) B4 0.038(2) 0.035(2) 0.041(2) -0.003(2) 0.012(2) -0.0013(19) B5 0.039(3) 0.029(2) 0.042(3) 0.0011(19) 0.006(2) -0.0009(19) B6 0.037(2) 0.028(2) 0.034(2) -0.0019(18) 0.0036(19) 0.0007(19) B7 0.035(2) 0.037(3) 0.039(2) 0.000(2) -0.001(2) -0.002(2) B8 0.037(3) 0.035(3) 0.045(3) 0.000(2) 0.004(2) 0.004(2) B9 0.037(2) 0.031(2) 0.038(2) -0.0046(19) 0.007(2) -0.0026(19) B10 0.044(3) 0.037(2) 0.033(2) -0.001(2) 0.007(2) -0.002(2) B1' 0.041(3) 0.050(3) 0.040(3) 0.003(2) 0.005(2) 0.004(2) B2' 0.032(2) 0.049(3) 0.043(3) -0.004(2) 0.004(2) -0.001(2) B3' 0.046(3) 0.040(3) 0.050(3) 0.009(2) 0.005(2) 0.008(2) B4' 0.052(3) 0.050(3) 0.046(3) 0.004(2) 0.010(2) -0.007(2) B5' 0.041(3) 0.042(3) 0.048(3) 0.001(2) 0.015(2) 0.000(2) B6' 0.038(3) 0.035(2) 0.048(3) -0.005(2) 0.006(2) -0.0068(19) B7' 0.035(3) 0.046(3) 0.049(3) 0.000(2) 0.003(2) 0.005(2) B8' 0.051(3) 0.039(3) 0.055(3) 0.007(2) 0.011(2) -0.004(2) B9' 0.040(3) 0.048(3) 0.065(3) 0.013(3) 0.014(2) -0.005(2) B10' 0.041(3) 0.051(3) 0.050(3) 0.010(2) 0.014(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C11 1.794(4) . ? S1 C12 1.807(4) . ? S1 B6 1.942(4) . ? S2 C21 1.786(4) . ? S2 C22 1.790(5) . ? S2 B9 1.929(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? B1 B6' 1.693(6) . ? B1 B4 1.774(6) . ? B1 B10 1.798(6) . ? B1 B2 1.803(6) . ? B1 B5 1.811(6) . ? B1 B3 1.839(6) . ? B2 B6 1.744(6) . ? B2 B7 1.754(6) . ? B2 B3 1.766(6) . ? B2 B5 1.781(6) . ? B2 H2 1.14(3) . ? B3 B4 1.773(6) . ? B3 B8 1.791(6) . ? B3 B7 1.803(6) . ? B3 H3 1.11(3) . ? B4 B9 1.762(6) . ? B4 B10 1.769(6) . ? B4 B8 1.777(6) . ? B4 H4 1.07(3) . ? B5 B6 1.863(6) . ? B5 B10 1.900(6) . ? B5 H5 1.11(3) . ? B5 H510 1.28(3) . ? B6 B7 1.888(6) . ? B6 H6 1.12(3) . ? B7 B8 1.891(6) . ? B7 H7 1.12(3) . ? B7 H78 1.27(3) . ? B8 B9 1.881(6) . ? B8 H8 1.06(3) . ? B8 H78 1.27(3) . ? B9 B10 1.853(6) . ? B9 H9 1.12(3) . ? B10 H10 1.09(3) . ? B10 H510 1.31(3) . ? B1' B10' 1.742(6) . ? B1' B5' 1.764(6) . ? B1' B3' 1.777(6) . ? B1' B4' 1.791(7) . ? B1' B2' 1.791(6) . ? B1' H1' 1.09(3) . ? B2' B6' 1.766(6) . ? B2' B3' 1.783(6) . ? B2' B5' 1.790(6) . ? B2' B7' 1.797(6) . ? B2' H2' 1.10(3) . ? B3' B8' 1.744(7) . ? B3' B7' 1.772(6) . ? B3' B4' 1.787(6) . ? B3' H3' 1.06(4) . ? B4' B9' 1.721(7) . ? B4' B10' 1.789(7) . ? B4' B8' 1.802(7) . ? B4' H4' 1.11(3) . ? B5' B6' 1.839(6) . ? B5' B10' 1.999(6) . ? B5' H5' 1.17(4) . ? B5' H56' 1.28(4) . ? B6' B7' 1.836(6) . ? B6' H56' 1.37(4) . ? B6' H67' 1.40(3) . ? B7' B8' 1.982(6) . ? B7' H7' 1.14(3) . ? B7' H67' 1.23(3) . ? B8' B9' 1.791(7) . ? B8' H8' 1.08(4) . ? B8' H89' 1.29(3) . ? B9' B10' 1.809(7) . ? B9' H9' 1.06(3) . ? B9' H89' 1.27(3) . ? B9' H91' 1.29(3) . ? B10' H10' 1.08(3) . ? B10' H91' 1.26(3) . ? 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 C11 S1 C12 100.50(19) . . ? C11 S1 B6 108.84(19) . . ? C12 S1 B6 100.16(18) . . ? C21 S2 C22 102.2(3) . . ? C21 S2 B9 102.7(2) . . ? C22 S2 B9 102.5(2) . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? B6' B1 B4 122.6(3) . . ? B6' B1 B10 122.1(3) . . ? B4 B1 B10 59.4(2) . . ? B6' B1 B2 123.4(3) . . ? B4 B1 B2 103.7(3) . . ? B10 B1 B2 108.3(3) . . ? B6' B1 B5 122.4(3) . . ? B4 B1 B5 108.6(3) . . ? B10 B1 B5 63.5(2) . . ? B2 B1 B5 59.0(2) . . ? B6' B1 B3 119.9(3) . . ? B4 B1 B3 58.8(2) . . ? B10 B1 B3 108.2(3) . . ? B2 B1 B3 58.0(2) . . ? B5 B1 B3 107.6(3) . . ? B6 B2 B7 65.3(2) . . ? B6 B2 B3 116.5(3) . . ? B7 B2 B3 61.6(2) . . ? B6 B2 B5 63.8(2) . . ? B7 B2 B5 115.3(3) . . ? B3 B2 B5 112.3(3) . . ? B6 B2 B1 115.3(3) . . ? B7 B2 B1 113.4(3) . . ? B3 B2 B1 62.0(2) . . ? B5 B2 B1 60.7(2) . . ? B6 B2 H2 111.4(15) . . ? B7 B2 H2 121.5(15) . . ? B3 B2 H2 124.7(15) . . ? B5 B2 H2 112.5(15) . . ? B1 B2 H2 118.4(15) . . ? B2 B3 B4 105.3(3) . . ? B2 B3 B8 108.5(3) . . ? B4 B3 B8 59.8(2) . . ? B2 B3 B7 58.8(2) . . ? B4 B3 B7 109.6(3) . . ? B8 B3 B7 63.5(2) . . ? B2 B3 B1 60.0(2) . . ? B4 B3 B1 58.8(2) . . ? B8 B3 B1 108.9(3) . . ? B7 B3 B1 109.4(3) . . ? B2 B3 H3 122.7(16) . . ? B4 B3 H3 120.9(16) . . ? B8 B3 H3 122.9(16) . . ? B7 B3 H3 123.4(16) . . ? B1 B3 H3 117.2(16) . . ? B9 B4 B10 63.3(2) . . ? B9 B4 B3 114.4(3) . . ? B10 B4 B3 112.5(3) . . ? B9 B4 B1 114.3(3) . . ? B10 B4 B1 61.0(2) . . ? B3 B4 B1 62.5(2) . . ? B9 B4 B8 64.2(2) . . ? B10 B4 B8 114.4(3) . . ? B3 B4 B8 60.6(2) . . ? B1 B4 B8 112.6(3) . . ? B9 B4 H4 111.3(16) . . ? B10 B4 H4 114.2(16) . . ? B3 B4 H4 125.1(16) . . ? B1 B4 H4 121.2(16) . . ? B8 B4 H4 119.7(16) . . ? B2 B5 B1 60.3(2) . . ? B2 B5 B6 57.2(2) . . ? B1 B5 B6 109.4(3) . . ? B2 B5 B10 104.9(3) . . ? B1 B5 B10 57.9(2) . . ? B6 B5 B10 112.3(3) . . ? B2 B5 H5 125.2(17) . . ? B1 B5 H5 118.5(17) . . ? B6 B5 H5 122.4(17) . . ? B10 B5 H5 119.3(17) . . ? B2 B5 H510 126.9(15) . . ? B1 B5 H510 100.6(16) . . ? B6 B5 H510 92.4(15) . . ? B10 B5 H510 43.4(16) . . ? H5 B5 H510 108(2) . . ? B2 B6 B5 59.1(2) . . ? B2 B6 B7 57.6(2) . . ? B5 B6 B7 105.5(3) . . ? B2 B6 S1 116.0(3) . . ? B5 B6 S1 119.1(2) . . ? B7 B6 S1 121.0(2) . . ? B2 B6 H6 143.4(15) . . ? B5 B6 H6 105.7(15) . . ? B7 B6 H6 102.5(15) . . ? S1 B6 H6 100.5(15) . . ? B2 B7 B3 59.5(2) . . ? B2 B7 B6 57.1(2) . . ? B3 B7 B6 108.0(3) . . ? B2 B7 B8 104.7(3) . . ? B3 B7 B8 57.9(2) . . ? B6 B7 B8 111.2(3) . . ? B2 B7 H7 124.2(17) . . ? B3 B7 H7 121.7(17) . . ? B6 B7 H7 120.1(17) . . ? B8 B7 H7 122.2(17) . . ? B2 B7 H78 123.7(15) . . ? B3 B7 H78 98.5(16) . . ? B6 B7 H78 90.0(15) . . ? B8 B7 H78 42.0(16) . . ? H7 B7 H78 112(2) . . ? B4 B8 B3 59.6(2) . . ? B4 B8 B9 57.5(2) . . ? B3 B8 B9 108.0(3) . . ? B4 B8 B7 105.6(3) . . ? B3 B8 B7 58.6(2) . . ? B9 B8 B7 111.1(3) . . ? B4 B8 H8 122.2(17) . . ? B3 B8 H8 117.2(17) . . ? B9 B8 H8 123.7(17) . . ? B7 B8 H8 120.3(17) . . ? B4 B8 H78 124.6(15) . . ? B3 B8 H78 99.2(16) . . ? B9 B8 H78 89.7(15) . . ? B7 B8 H78 42.0(16) . . ? H8 B8 H78 113(2) . . ? B4 B9 B10 58.5(2) . . ? B4 B9 B8 58.3(2) . . ? B10 B9 B8 105.9(3) . . ? B4 B9 S2 108.8(3) . . ? B10 B9 S2 114.9(2) . . ? B8 B9 S2 118.7(3) . . ? B4 B9 H9 142.4(17) . . ? B10 B9 H9 104.3(16) . . ? B8 B9 H9 102.7(16) . . ? S2 B9 H9 108.8(16) . . ? B4 B10 B1 59.6(2) . . ? B4 B10 B9 58.1(2) . . ? B1 B10 B9 108.9(3) . . ? B4 B10 B5 104.9(3) . . ? B1 B10 B5 58.6(2) . . ? B9 B10 B5 110.4(3) . . ? B4 B10 H10 125.7(16) . . ? B1 B10 H10 118.3(16) . . ? B9 B10 H10 124.1(16) . . ? B5 B10 H10 118.7(16) . . ? B4 B10 H510 126.8(15) . . ? B1 B10 H510 100.2(16) . . ? B9 B10 H510 91.1(15) . . ? B5 B10 H510 42.4(15) . . ? H10 B10 H510 107(2) . . ? B10' B1' B5' 69.5(3) . . ? B10' B1' B3' 107.8(3) . . ? B5' B1' B3' 107.2(3) . . ? B10' B1' B4' 60.8(3) . . ? B5' B1' B4' 117.7(3) . . ? B3' B1' B4' 60.1(3) . . ? B10' B1' B2' 118.0(3) . . ? B5' B1' B2' 60.5(2) . . ? B3' B1' B2' 60.0(2) . . ? B4' B1' B2' 114.3(3) . . ? B10' B1' H1' 115.0(17) . . ? B5' B1' H1' 113.7(17) . . ? B3' B1' H1' 128.4(17) . . ? B4' B1' H1' 119.8(17) . . ? B2' B1' H1' 117.1(17) . . ? B6' B2' B3' 113.0(3) . . ? B6' B2' B5' 62.3(2) . . ? B3' B2' B5' 105.9(3) . . ? B6' B2' B1' 113.2(3) . . ? B3' B2' B1' 59.6(3) . . ? B5' B2' B1' 59.0(2) . . ? B6' B2' B7' 62.0(2) . . ? B3' B2' B7' 59.3(3) . . ? B5' B2' B7' 105.2(3) . . ? B1' B2' B7' 106.4(3) . . ? B6' B2' H2' 119.0(16) . . ? B3' B2' H2' 120.0(17) . . ? B5' B2' H2' 123.2(17) . . ? B1' B2' H2' 118.2(16) . . ? B7' B2' H2' 125.7(16) . . ? B8' B3' B7' 68.7(3) . . ? B8' B3' B1' 108.2(3) . . ? B7' B3' B1' 108.1(3) . . ? B8' B3' B2' 117.5(3) . . ? B7' B3' B2' 60.7(2) . . ? B1' B3' B2' 60.4(2) . . ? B8' B3' B4' 61.4(3) . . ? B7' B3' B4' 118.1(3) . . ? B1' B3' B4' 60.3(3) . . ? B2' B3' B4' 114.9(3) . . ? B8' B3' H3' 115(2) . . ? B7' B3' H3' 115(2) . . ? B1' B3' H3' 127(2) . . ? B2' B3' H3' 118(2) . . ? B4' B3' H3' 118(2) . . ? B9' B4' B3' 110.1(3) . . ? B9' B4' B10' 62.0(3) . . ? B3' B4' B10' 105.4(3) . . ? B9' B4' B1' 110.6(3) . . ? B3' B4' B1' 59.6(3) . . ? B10' B4' B1' 58.2(3) . . ? B9' B4' B8' 61.1(3) . . ? B3' B4' B8' 58.1(3) . . ? B10' B4' B8' 105.3(3) . . ? B1' B4' B8' 105.0(3) . . ? B9' B4' H4' 119.7(17) . . ? B3' B4' H4' 120.5(17) . . ? B10' B4' H4' 125.1(18) . . ? B1' B4' H4' 121.8(17) . . ? B8' B4' H4' 123.4(18) . . ? B1' B5' B2' 60.5(2) . . ? B1' B5' B6' 110.9(3) . . ? B2' B5' B6' 58.2(2) . . ? B1' B5' B10' 54.7(2) . . ? B2' B5' B10' 106.0(3) . . ? B6' B5' B10' 119.3(3) . . ? B1' B5' H5' 121.5(18) . . ? B2' B5' H5' 131.7(18) . . ? B6' B5' H5' 121.7(18) . . ? B10' B5' H5' 111.0(18) . . ? B1' B5' H56' 130.2(16) . . ? B2' B5' H56' 103.2(16) . . ? B6' B5' H56' 48.0(16) . . ? B10' B5' H56' 93.3(16) . . ? H5' B5' H56' 104(2) . . ? B1 B6' B2' 132.2(3) . . ? B1 B6' B7' 127.2(3) . . ? B2' B6' B7' 59.8(2) . . ? B1 B6' B5' 129.5(3) . . ? B2' B6' B5' 59.5(2) . . ? B7' B6' B5' 101.7(3) . . ? B1 B6' H56' 112.1(15) . . ? B2' B6' H56' 100.9(16) . . ? B7' B6' H56' 114.1(15) . . ? B5' B6' H56' 44.3(15) . . ? B1 B6' H67' 116.1(13) . . ? B2' B6' H67' 96.8(13) . . ? B7' B6' H67' 41.9(13) . . ? B5' B6' H67' 108.4(13) . . ? H56' B6' H67' 90(2) . . ? B3' B7' B2' 59.9(3) . . ? B3' B7' B6' 110.2(3) . . ? B2' B7' B6' 58.2(2) . . ? B3' B7' B8' 55.0(2) . . ? B2' B7' B8' 105.7(3) . . ? B6' B7' B8' 118.7(3) . . ? B3' B7' H7' 123.4(16) . . ? B2' B7' H7' 128.2(17) . . ? B6' B7' H7' 118.6(17) . . ? B8' B7' H7' 115.6(17) . . ? B3' B7' H67' 123.8(15) . . ? B2' B7' H67' 102.0(15) . . ? B6' B7' H67' 49.5(15) . . ? B8' B7' H67' 87.3(15) . . ? H7' B7' H67' 110(2) . . ? B3' B8' B9' 109.0(4) . . ? B3' B8' B4' 60.5(3) . . ? B9' B8' B4' 57.2(3) . . ? B3' B8' B7' 56.3(2) . . ? B9' B8' B7' 117.2(3) . . ? B4' B8' B7' 107.4(3) . . ? B3' B8' H8' 125(2) . . ? B9' B8' H8' 119(2) . . ? B4' B8' H8' 128(2) . . ? B7' B8' H8' 115(2) . . ? B3' B8' H89' 128.5(14) . . ? B9' B8' H89' 44.9(13) . . ? B4' B8' H89' 99.8(14) . . ? B7' B8' H89' 93.2(13) . . ? H8' B8' H89' 105(2) . . ? B4' B9' B8' 61.7(3) . . ? B4' B9' B10' 60.8(3) . . ? B8' B9' B10' 104.9(3) . . ? B4' B9' H9' 127.2(18) . . ? B8' B9' H9' 129.0(18) . . ? B10' B9' H9' 123.2(18) . . ? B4' B9' H89' 105.1(14) . . ? B8' B9' H89' 45.9(13) . . ? B10' B9' H89' 117.9(14) . . ? H9' B9' H89' 113(2) . . ? B4' B9' H91' 101.4(16) . . ? B8' B9' H91' 114.5(15) . . ? B10' B9' H91' 44.0(16) . . ? H9' B9' H91' 112(2) . . ? H89' B9' H91' 93(2) . . ? B1' B10' B4' 60.9(3) . . ? B1' B10' B9' 108.8(3) . . ? B4' B10' B9' 57.2(3) . . ? B1' B10' B5' 55.8(2) . . ? B4' B10' B5' 106.8(3) . . ? B9' B10' B5' 115.7(3) . . ? B1' B10' H10' 124.4(18) . . ? B4' B10' H10' 128.2(18) . . ? B9' B10' H10' 119.9(18) . . ? B5' B10' H10' 116.2(18) . . ? B1' B10' H91' 125.0(16) . . ? B4' B10' H91' 99.2(17) . . ? B9' B10' H91' 45.4(16) . . ? B5' B10' H91' 89.5(16) . . ? H10' B10' H91' 108(2) . . ? 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 B6' B1 B2 B6 145.0(3) . . . . ? B4 B1 B2 B6 -69.4(4) . . . . ? B10 B1 B2 B6 -7.5(4) . . . . ? B5 B1 B2 B6 34.3(3) . . . . ? B3 B1 B2 B6 -108.0(3) . . . . ? B6' B1 B2 B7 -142.4(3) . . . . ? B4 B1 B2 B7 3.3(4) . . . . ? B10 B1 B2 B7 65.1(4) . . . . ? B5 B1 B2 B7 106.9(3) . . . . ? B3 B1 B2 B7 -35.3(3) . . . . ? B6' B1 B2 B3 -107.0(4) . . . . ? B4 B1 B2 B3 38.6(3) . . . . ? B10 B1 B2 B3 100.4(3) . . . . ? B5 B1 B2 B3 142.2(3) . . . . ? B6' B1 B2 B5 110.7(4) . . . . ? B4 B1 B2 B5 -103.6(3) . . . . ? B10 B1 B2 B5 -41.8(3) . . . . ? B3 B1 B2 B5 -142.2(3) . . . . ? B6 B2 B3 B4 67.1(4) . . . . ? B7 B2 B3 B4 104.0(3) . . . . ? B5 B2 B3 B4 -3.7(4) . . . . ? B1 B2 B3 B4 -38.9(3) . . . . ? B6 B2 B3 B8 4.4(4) . . . . ? B7 B2 B3 B8 41.2(3) . . . . ? B5 B2 B3 B8 -66.4(4) . . . . ? B1 B2 B3 B8 -101.7(3) . . . . ? B6 B2 B3 B7 -36.9(3) . . . . ? B5 B2 B3 B7 -107.7(3) . . . . ? B1 B2 B3 B7 -142.9(3) . . . . ? B6 B2 B3 B1 106.0(3) . . . . ? B7 B2 B3 B1 142.9(3) . . . . ? B5 B2 B3 B1 35.2(3) . . . . ? B6' B1 B3 B2 112.9(4) . . . . ? B4 B1 B3 B2 -134.9(3) . . . . ? B10 B1 B3 B2 -100.6(3) . . . . ? B5 B1 B3 B2 -33.4(3) . . . . ? B6' B1 B3 B4 -112.2(4) . . . . ? B10 B1 B3 B4 34.3(3) . . . . ? B2 B1 B3 B4 134.9(3) . . . . ? B5 B1 B3 B4 101.4(3) . . . . ? B6' B1 B3 B8 -146.2(3) . . . . ? B4 B1 B3 B8 -34.0(3) . . . . ? B10 B1 B3 B8 0.3(4) . . . . ? B2 B1 B3 B8 100.9(3) . . . . ? B5 B1 B3 B8 67.4(4) . . . . ? B6' B1 B3 B7 146.1(3) . . . . ? B4 B1 B3 B7 -101.7(3) . . . . ? B10 B1 B3 B7 -67.4(4) . . . . ? B2 B1 B3 B7 33.2(3) . . . . ? B5 B1 B3 B7 -0.3(4) . . . . ? B2 B3 B4 B9 -66.3(4) . . . . ? B8 B3 B4 B9 36.5(3) . . . . ? B7 B3 B4 B9 -4.5(4) . . . . ? B1 B3 B4 B9 -105.8(3) . . . . ? B2 B3 B4 B10 3.5(4) . . . . ? B8 B3 B4 B10 106.2(3) . . . . ? B7 B3 B4 B10 65.3(4) . . . . ? B1 B3 B4 B10 -36.1(3) . . . . ? B2 B3 B4 B1 39.5(3) . . . . ? B8 B3 B4 B1 142.3(3) . . . . ? B7 B3 B4 B1 101.3(3) . . . . ? B2 B3 B4 B8 -102.8(3) . . . . ? B7 B3 B4 B8 -40.9(3) . . . . ? B1 B3 B4 B8 -142.3(3) . . . . ? B6' B1 B4 B9 -146.2(3) . . . . ? B10 B1 B4 B9 -35.5(3) . . . . ? B2 B1 B4 B9 67.8(4) . . . . ? B5 B1 B4 B9 6.3(4) . . . . ? B3 B1 B4 B9 106.0(3) . . . . ? B6' B1 B4 B10 -110.7(4) . . . . ? B2 B1 B4 B10 103.4(3) . . . . ? B5 B1 B4 B10 41.8(3) . . . . ? B3 B1 B4 B10 141.6(3) . . . . ? B6' B1 B4 B3 107.7(4) . . . . ? B10 B1 B4 B3 -141.6(3) . . . . ? B2 B1 B4 B3 -38.2(3) . . . . ? B5 B1 B4 B3 -99.7(3) . . . . ? B6' B1 B4 B8 143.0(4) . . . . ? B10 B1 B4 B8 -106.3(3) . . . . ? B2 B1 B4 B8 -3.0(4) . . . . ? B5 B1 B4 B8 -64.5(4) . . . . ? B3 B1 B4 B8 35.3(3) . . . . ? B6 B2 B5 B1 -145.4(3) . . . . ? B7 B2 B5 B1 -103.8(3) . . . . ? B3 B2 B5 B1 -35.8(3) . . . . ? B7 B2 B5 B6 41.7(3) . . . . ? B3 B2 B5 B6 109.7(3) . . . . ? B1 B2 B5 B6 145.4(3) . . . . ? B6 B2 B5 B10 -107.2(3) . . . . ? B7 B2 B5 B10 -65.5(4) . . . . ? B3 B2 B5 B10 2.5(4) . . . . ? B1 B2 B5 B10 38.3(3) . . . . ? B6' B1 B5 B2 -112.3(4) . . . . ? B4 B1 B5 B2 95.1(3) . . . . ? B10 B1 B5 B2 135.0(3) . . . . ? B3 B1 B5 B2 33.0(3) . . . . ? B6' B1 B5 B6 -142.6(3) . . . . ? B4 B1 B5 B6 64.8(4) . . . . ? B10 B1 B5 B6 104.7(3) . . . . ? B2 B1 B5 B6 -30.3(3) . . . . ? B3 B1 B5 B6 2.7(4) . . . . ? B6' B1 B5 B10 112.7(4) . . . . ? B4 B1 B5 B10 -39.9(3) . . . . ? B2 B1 B5 B10 -135.0(3) . . . . ? B3 B1 B5 B10 -102.0(3) . . . . ? B7 B2 B6 B5 -138.6(3) . . . . ? B3 B2 B6 B5 -103.1(3) . . . . ? B1 B2 B6 B5 -33.2(3) . . . . ? B3 B2 B6 B7 35.5(3) . . . . ? B5 B2 B6 B7 138.6(3) . . . . ? B1 B2 B6 B7 105.4(3) . . . . ? B7 B2 B6 S1 111.7(3) . . . . ? B3 B2 B6 S1 147.2(3) . . . . ? B5 B2 B6 S1 -109.7(3) . . . . ? B1 B2 B6 S1 -142.9(3) . . . . ? B1 B5 B6 B2 31.5(3) . . . . ? B10 B5 B6 B2 93.8(3) . . . . ? B2 B5 B6 B7 -35.4(3) . . . . ? B1 B5 B6 B7 -3.9(4) . . . . ? B10 B5 B6 B7 58.4(4) . . . . ? B2 B5 B6 S1 104.6(3) . . . . ? B1 B5 B6 S1 136.1(3) . . . . ? B10 B5 B6 S1 -161.6(2) . . . . ? C11 S1 B6 B2 23.6(3) . . . . ? C12 S1 B6 B2 128.4(3) . . . . ? C11 S1 B6 B5 -43.9(3) . . . . ? C12 S1 B6 B5 61.0(3) . . . . ? C11 S1 B6 B7 89.8(3) . . . . ? C12 S1 B6 B7 -165.3(3) . . . . ? B6 B2 B7 B3 143.8(3) . . . . ? B5 B2 B7 B3 102.8(3) . . . . ? B1 B2 B7 B3 35.5(3) . . . . ? B3 B2 B7 B6 -143.8(3) . . . . ? B5 B2 B7 B6 -41.0(3) . . . . ? B1 B2 B7 B6 -108.3(3) . . . . ? B6 B2 B7 B8 106.1(3) . . . . ? B3 B2 B7 B8 -37.7(3) . . . . ? B5 B2 B7 B8 65.0(4) . . . . ? B1 B2 B7 B8 -2.3(4) . . . . ? B4 B3 B7 B2 -96.4(3) . . . . ? B8 B3 B7 B2 -135.7(3) . . . . ? B1 B3 B7 B2 -33.6(3) . . . . ? B2 B3 B7 B6 31.4(3) . . . . ? B4 B3 B7 B6 -65.0(4) . . . . ? B8 B3 B7 B6 -104.2(3) . . . . ? B1 B3 B7 B6 -2.2(4) . . . . ? B2 B3 B7 B8 135.7(3) . . . . ? B4 B3 B7 B8 39.3(3) . . . . ? B1 B3 B7 B8 102.0(3) . . . . ? B5 B6 B7 B2 36.1(3) . . . . ? S1 B6 B7 B2 -103.0(3) . . . . ? B2 B6 B7 B3 -32.3(3) . . . . ? B5 B6 B7 B3 3.7(4) . . . . ? S1 B6 B7 B3 -135.3(3) . . . . ? B2 B6 B7 B8 -94.1(3) . . . . ? B5 B6 B7 B8 -58.1(4) . . . . ? S1 B6 B7 B8 162.9(3) . . . . ? B9 B4 B8 B3 -143.1(3) . . . . ? B10 B4 B8 B3 -103.1(3) . . . . ? B1 B4 B8 B3 -36.0(3) . . . . ? B10 B4 B8 B9 39.9(3) . . . . ? B3 B4 B8 B9 143.1(3) . . . . ? B1 B4 B8 B9 107.1(3) . . . . ? B9 B4 B8 B7 -105.4(3) . . . . ? B10 B4 B8 B7 -65.5(4) . . . . ? B3 B4 B8 B7 37.7(3) . . . . ? B1 B4 B8 B7 1.7(4) . . . . ? B2 B3 B8 B4 97.3(3) . . . . ? B7 B3 B8 B4 136.4(3) . . . . ? B1 B3 B8 B4 33.6(3) . . . . ? B2 B3 B8 B9 65.1(4) . . . . ? B4 B3 B8 B9 -32.2(3) . . . . ? B7 B3 B8 B9 104.2(3) . . . . ? B1 B3 B8 B9 1.4(4) . . . . ? B2 B3 B8 B7 -39.1(3) . . . . ? B4 B3 B8 B7 -136.4(3) . . . . ? B1 B3 B8 B7 -102.8(3) . . . . ? B2 B7 B8 B4 0.4(4) . . . . ? B3 B7 B8 B4 -38.1(3) . . . . ? B6 B7 B8 B4 60.3(4) . . . . ? B2 B7 B8 B3 38.5(3) . . . . ? B6 B7 B8 B3 98.5(3) . . . . ? B2 B7 B8 B9 -60.3(4) . . . . ? B3 B7 B8 B9 -98.8(3) . . . . ? B6 B7 B8 B9 -0.3(4) . . . . ? B3 B4 B9 B10 104.1(3) . . . . ? B1 B4 B9 B10 34.7(3) . . . . ? B8 B4 B9 B10 139.1(3) . . . . ? B10 B4 B9 B8 -139.1(3) . . . . ? B3 B4 B9 B8 -35.1(3) . . . . ? B1 B4 B9 B8 -104.5(4) . . . . ? B10 B4 B9 S2 108.2(3) . . . . ? B3 B4 B9 S2 -147.8(3) . . . . ? B1 B4 B9 S2 142.9(3) . . . . ? B8 B4 B9 S2 -112.7(3) . . . . ? B3 B8 B9 B4 33.0(3) . . . . ? B7 B8 B9 B4 95.5(3) . . . . ? B4 B8 B9 B10 -35.5(3) . . . . ? B3 B8 B9 B10 -2.5(4) . . . . ? B7 B8 B9 B10 60.0(3) . . . . ? B4 B8 B9 S2 95.4(3) . . . . ? B3 B8 B9 S2 128.4(3) . . . . ? B7 B8 B9 S2 -169.1(3) . . . . ? C21 S2 B9 B4 117.8(3) . . . . ? C22 S2 B9 B4 -136.5(3) . . . . ? C21 S2 B9 B10 -178.9(3) . . . . ? C22 S2 B9 B10 -73.2(3) . . . . ? C21 S2 B9 B8 54.3(4) . . . . ? C22 S2 B9 B8 160.0(3) . . . . ? B9 B4 B10 B1 143.6(3) . . . . ? B3 B4 B10 B1 36.6(3) . . . . ? B8 B4 B10 B1 103.3(3) . . . . ? B3 B4 B10 B9 -107.0(3) . . . . ? B1 B4 B10 B9 -143.6(3) . . . . ? B8 B4 B10 B9 -40.3(3) . . . . ? B9 B4 B10 B5 105.1(3) . . . . ? B3 B4 B10 B5 -1.9(4) . . . . ? B1 B4 B10 B5 -38.6(3) . . . . ? B8 B4 B10 B5 64.8(4) . . . . ? B6' B1 B10 B4 111.6(4) . . . . ? B2 B1 B10 B4 -95.4(3) . . . . ? B5 B1 B10 B4 -135.1(3) . . . . ? B3 B1 B10 B4 -34.0(3) . . . . ? B6' B1 B10 B9 143.8(3) . . . . ? B4 B1 B10 B9 32.2(3) . . . . ? B2 B1 B10 B9 -63.2(4) . . . . ? B5 B1 B10 B9 -102.9(3) . . . . ? B3 B1 B10 B9 -1.9(4) . . . . ? B6' B1 B10 B5 -113.3(4) . . . . ? B4 B1 B10 B5 135.1(3) . . . . ? B2 B1 B10 B5 39.7(3) . . . . ? B3 B1 B10 B5 101.1(3) . . . . ? B8 B9 B10 B4 35.4(3) . . . . ? S2 B9 B10 B4 -97.7(3) . . . . ? B4 B9 B10 B1 -32.7(3) . . . . ? B8 B9 B10 B1 2.6(4) . . . . ? S2 B9 B10 B1 -130.4(3) . . . . ? B4 B9 B10 B5 -95.3(3) . . . . ? B8 B9 B10 B5 -59.9(3) . . . . ? S2 B9 B10 B5 167.0(2) . . . . ? B2 B5 B10 B4 -0.3(4) . . . . ? B1 B5 B10 B4 39.1(3) . . . . ? B6 B5 B10 B4 -60.5(4) . . . . ? B2 B5 B10 B1 -39.4(3) . . . . ? B6 B5 B10 B1 -99.6(3) . . . . ? B2 B5 B10 B9 60.7(3) . . . . ? B1 B5 B10 B9 100.2(3) . . . . ? B6 B5 B10 B9 0.6(4) . . . . ? B10' B1' B2' B6' -8.7(5) . . . . ? B5' B1' B2' B6' 32.1(3) . . . . ? B3' B1' B2' B6' -104.0(4) . . . . ? B4' B1' B2' B6' -77.2(4) . . . . ? B10' B1' B2' B3' 95.3(4) . . . . ? B5' B1' B2' B3' 136.2(3) . . . . ? B4' B1' B2' B3' 26.8(3) . . . . ? B10' B1' B2' B5' -40.8(4) . . . . ? B3' B1' B2' B5' -136.2(3) . . . . ? B4' B1' B2' B5' -109.3(4) . . . . ? B10' B1' B2' B7' 57.4(4) . . . . ? B5' B1' B2' B7' 98.2(3) . . . . ? B3' B1' B2' B7' -38.0(3) . . . . ? B4' B1' B2' B7' -11.2(4) . . . . ? B10' B1' B3' B8' -0.7(4) . . . . ? B5' B1' B3' B8' 72.7(4) . . . . ? B4' B1' B3' B8' -39.9(3) . . . . ? B2' B1' B3' B8' 111.8(3) . . . . ? B10' B1' B3' B7' -73.5(4) . . . . ? B5' B1' B3' B7' -0.1(4) . . . . ? B4' B1' B3' B7' -112.6(4) . . . . ? B2' B1' B3' B7' 39.0(3) . . . . ? B10' B1' B3' B2' -112.5(3) . . . . ? B5' B1' B3' B2' -39.1(3) . . . . ? B4' B1' B3' B2' -151.7(3) . . . . ? B10' B1' B3' B4' 39.2(3) . . . . ? B5' B1' B3' B4' 112.6(3) . . . . ? B2' B1' B3' B4' 151.7(3) . . . . ? B6' B2' B3' B8' 8.0(5) . . . . ? B5' B2' B3' B8' -58.1(4) . . . . ? B1' B2' B3' B8' -96.3(4) . . . . ? B7' B2' B3' B8' 40.4(3) . . . . ? B6' B2' B3' B7' -32.4(3) . . . . ? B5' B2' B3' B7' -98.5(3) . . . . ? B1' B2' B3' B7' -136.6(3) . . . . ? B6' B2' B3' B1' 104.3(3) . . . . ? B5' B2' B3' B1' 38.1(3) . . . . ? B7' B2' B3' B1' 136.6(3) . . . . ? B6' B2' B3' B4' 77.3(4) . . . . ? B5' B2' B3' B4' 11.1(4) . . . . ? B1' B2' B3' B4' -27.0(3) . . . . ? B7' B2' B3' B4' 109.6(4) . . . . ? B8' B3' B4' B9' 33.4(3) . . . . ? B7' B3' B4' B9' -7.0(5) . . . . ? B1' B3' B4' B9' -102.7(4) . . . . ? B2' B3' B4' B9' -75.7(4) . . . . ? B8' B3' B4' B10' 98.7(3) . . . . ? B7' B3' B4' B10' 58.3(4) . . . . ? B1' B3' B4' B10' -37.4(3) . . . . ? B2' B3' B4' B10' -10.4(4) . . . . ? B8' B3' B4' B1' 136.1(3) . . . . ? B7' B3' B4' B1' 95.7(4) . . . . ? B2' B3' B4' B1' 27.0(3) . . . . ? B7' B3' B4' B8' -40.3(4) . . . . ? B1' B3' B4' B8' -136.1(3) . . . . ? B2' B3' B4' B8' -109.0(4) . . . . ? B10' B1' B4' B9' -34.6(3) . . . . ? B5' B1' B4' B9' 7.0(5) . . . . ? B3' B1' B4' B9' 101.8(4) . . . . ? B2' B1' B4' B9' 75.1(4) . . . . ? B10' B1' B4' B3' -136.5(3) . . . . ? B5' B1' B4' B3' -94.8(4) . . . . ? B2' B1' B4' B3' -26.8(3) . . . . ? B5' B1' B4' B10' 41.7(3) . . . . ? B3' B1' B4' B10' 136.5(3) . . . . ? B2' B1' B4' B10' 109.7(4) . . . . ? B10' B1' B4' B8' -98.9(3) . . . . ? B5' B1' B4' B8' -57.2(4) . . . . ? B3' B1' B4' B8' 37.6(3) . . . . ? B2' B1' B4' B8' 10.8(4) . . . . ? B10' B1' B5' B2' 142.0(3) . . . . ? B3' B1' B5' B2' 38.9(3) . . . . ? B4' B1' B5' B2' 103.7(4) . . . . ? B10' B1' B5' B6' 111.8(4) . . . . ? B3' B1' B5' B6' 8.7(4) . . . . ? B4' B1' B5' B6' 73.5(4) . . . . ? B2' B1' B5' B6' -30.2(3) . . . . ? B3' B1' B5' B10' -103.1(4) . . . . ? B4' B1' B5' B10' -38.3(3) . . . . ? B2' B1' B5' B10' -142.0(3) . . . . ? B6' B2' B5' B1' -146.5(3) . . . . ? B3' B2' B5' B1' -38.4(3) . . . . ? B7' B2' B5' B1' -100.2(3) . . . . ? B3' B2' B5' B6' 108.1(3) . . . . ? B1' B2' B5' B6' 146.5(3) . . . . ? B7' B2' B5' B6' 46.2(3) . . . . ? B6' B2' B5' B10' -114.9(3) . . . . ? B3' B2' B5' B10' -6.9(4) . . . . ? B1' B2' B5' B10' 31.6(3) . . . . ? B7' B2' B5' B10' -68.7(4) . . . . ? B4 B1 B6' B2' 86.8(5) . . . . ? B10 B1 B6' B2' 15.0(6) . . . . ? B2 B1 B6' B2' -133.8(4) . . . . ? B5 B1 B6' B2' -62.0(6) . . . . ? B3 B1 B6' B2' 156.8(4) . . . . ? B4 B1 B6' B7' 167.4(3) . . . . ? B10 B1 B6' B7' 95.6(4) . . . . ? B2 B1 B6' B7' -53.2(5) . . . . ? B5 B1 B6' B7' 18.6(6) . . . . ? B3 B1 B6' B7' -122.6(4) . . . . ? B4 B1 B6' B5' 4.9(6) . . . . ? B10 B1 B6' B5' -66.9(5) . . . . ? B2 B1 B6' B5' 144.2(4) . . . . ? B5 B1 B6' B5' -143.9(4) . . . . ? B3 B1 B6' B5' 74.9(5) . . . . ? B3' B2' B6' B1 146.0(4) . . . . ? B5' B2' B6' B1 -117.5(5) . . . . ? B1' B2' B6' B1 -148.5(4) . . . . ? B7' B2' B6' B1 114.6(5) . . . . ? B3' B2' B6' B7' 31.4(3) . . . . ? B5' B2' B6' B7' 127.9(3) . . . . ? B1' B2' B6' B7' 96.9(4) . . . . ? B3' B2' B6' B5' -96.5(3) . . . . ? B1' B2' B6' B5' -31.0(3) . . . . ? B7' B2' B6' B5' -127.9(3) . . . . ? B1' B5' B6' B1 152.7(4) . . . . ? B2' B5' B6' B1 121.7(4) . . . . ? B10' B5' B6' B1 -146.9(4) . . . . ? B1' B5' B6' B2' 31.0(3) . . . . ? B10' B5' B6' B2' 91.3(4) . . . . ? B1' B5' B6' B7' -13.2(4) . . . . ? B2' B5' B6' B7' -44.2(3) . . . . ? B10' B5' B6' B7' 47.2(4) . . . . ? B8' B3' B7' B2' -141.9(3) . . . . ? B1' B3' B7' B2' -38.9(3) . . . . ? B4' B3' B7' B2' -104.3(4) . . . . ? B8' B3' B7' B6' -111.6(3) . . . . ? B1' B3' B7' B6' -8.6(4) . . . . ? B2' B3' B7' B6' 30.3(3) . . . . ? B4' B3' B7' B6' -74.0(4) . . . . ? B1' B3' B7' B8' 103.0(4) . . . . ? B2' B3' B7' B8' 141.9(3) . . . . ? B4' B3' B7' B8' 37.6(3) . . . . ? B6' B2' B7' B3' 146.1(3) . . . . ? B5' B2' B7' B3' 99.7(3) . . . . ? B1' B2' B7' B3' 38.1(3) . . . . ? B3' B2' B7' B6' -146.1(3) . . . . ? B5' B2' B7' B6' -46.4(3) . . . . ? B1' B2' B7' B6' -108.0(3) . . . . ? B6' B2' B7' B8' 114.4(3) . . . . ? B3' B2' B7' B8' -31.7(3) . . . . ? B5' B2' B7' B8' 68.0(4) . . . . ? B1' B2' B7' B8' 6.5(4) . . . . ? B1 B6' B7' B3' -153.3(4) . . . . ? B2' B6' B7' B3' -31.0(3) . . . . ? B5' B6' B7' B3' 13.0(4) . . . . ? B1 B6' B7' B2' -122.3(4) . . . . ? B5' B6' B7' B2' 44.0(3) . . . . ? B1 B6' B7' B8' 146.4(4) . . . . ? B2' B6' B7' B8' -91.3(4) . . . . ? B5' B6' B7' B8' -47.3(4) . . . . ? B7' B3' B8' B9' 110.6(3) . . . . ? B1' B3' B8' B9' 7.7(4) . . . . ? B2' B3' B8' B9' 73.2(4) . . . . ? B4' B3' B8' B9' -31.6(3) . . . . ? B7' B3' B8' B4' 142.2(3) . . . . ? B1' B3' B8' B4' 39.4(3) . . . . ? B2' B3' B8' B4' 104.8(4) . . . . ? B1' B3' B8' B7' -102.8(3) . . . . ? B2' B3' B8' B7' -37.4(3) . . . . ? B4' B3' B8' B7' -142.2(3) . . . . ? B9' B4' B8' B3' -143.9(4) . . . . ? B10' B4' B8' B3' -98.8(3) . . . . ? B1' B4' B8' B3' -38.3(3) . . . . ? B3' B4' B8' B9' 143.9(4) . . . . ? B10' B4' B8' B9' 45.0(3) . . . . ? B1' B4' B8' B9' 105.6(4) . . . . ? B9' B4' B8' B7' -111.5(3) . . . . ? B3' B4' B8' B7' 32.3(3) . . . . ? B10' B4' B8' B7' -66.5(4) . . . . ? B1' B4' B8' B7' -5.9(4) . . . . ? B2' B7' B8' B3' 33.7(3) . . . . ? B6' B7' B8' B3' 95.6(4) . . . . ? B3' B7' B8' B9' -95.6(4) . . . . ? B2' B7' B8' B9' -61.9(4) . . . . ? B6' B7' B8' B9' 0.1(5) . . . . ? B3' B7' B8' B4' -34.0(3) . . . . ? B2' B7' B8' B4' -0.3(4) . . . . ? B6' B7' B8' B4' 61.6(4) . . . . ? B3' B4' B9' B8' -32.2(3) . . . . ? B10' B4' B9' B8' -129.4(3) . . . . ? B1' B4' B9' B8' -96.2(4) . . . . ? B3' B4' B9' B10' 97.2(4) . . . . ? B1' B4' B9' B10' 33.2(3) . . . . ? B8' B4' B9' B10' 129.4(3) . . . . ? B3' B8' B9' B4' 32.9(3) . . . . ? B7' B8' B9' B4' 94.0(4) . . . . ? B3' B8' B9' B10' -11.4(4) . . . . ? B4' B8' B9' B10' -44.3(3) . . . . ? B7' B8' B9' B10' 49.8(4) . . . . ? B5' B1' B10' B4' -141.1(3) . . . . ? B3' B1' B10' B4' -38.8(3) . . . . ? B2' B1' B10' B4' -103.7(4) . . . . ? B5' B1' B10' B9' -108.8(3) . . . . ? B3' B1' B10' B9' -6.5(4) . . . . ? B4' B1' B10' B9' 32.3(3) . . . . ? B2' B1' B10' B9' -71.4(4) . . . . ? B3' B1' B10' B5' 102.3(3) . . . . ? B4' B1' B10' B5' 141.1(3) . . . . ? B2' B1' B10' B5' 37.4(3) . . . . ? B9' B4' B10' B1' 143.0(3) . . . . ? B3' B4' B10' B1' 38.0(3) . . . . ? B8' B4' B10' B1' 98.5(3) . . . . ? B3' B4' B10' B9' -105.0(3) . . . . ? B1' B4' B10' B9' -143.0(3) . . . . ? B8' B4' B10' B9' -44.5(3) . . . . ? B9' B4' B10' B5' 110.1(3) . . . . ? B3' B4' B10' B5' 5.1(4) . . . . ? B1' B4' B10' B5' -32.9(3) . . . . ? B8' B4' B10' B5' 65.6(4) . . . . ? B4' B9' B10' B1' -33.8(3) . . . . ? B8' B9' B10' B1' 11.0(4) . . . . ? B8' B9' B10' B4' 44.8(3) . . . . ? B4' B9' B10' B5' -94.1(4) . . . . ? B8' B9' B10' B5' -49.3(4) . . . . ? B2' B5' B10' B1' -33.9(3) . . . . ? B6' B5' B10' B1' -96.0(4) . . . . ? B1' B5' B10' B4' 35.0(3) . . . . ? B2' B5' B10' B4' 1.1(4) . . . . ? B6' B5' B10' B4' -61.0(4) . . . . ? B1' B5' B10' B9' 96.1(4) . . . . ? B2' B5' B10' B9' 62.2(4) . . . . ? B6' B5' B10' B9' 0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.254 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.051 data_mlb20 _database_code_depnum_ccdc_archive 'CCDC 280346' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common "[1,6'-(nido-B10H13)2]" _chemical_melting_point ? _chemical_formula_moiety 'B20 H26' _chemical_formula_sum 'B20 H26' _chemical_formula_weight 242.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3252(3) _cell_length_b 14.0450(4) _cell_length_c 20.8013(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3308.71(17) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9929 _exptl_absorpt_correction_T_max 0.9982 _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 ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _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 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligable _diffrn_reflns_number 23355 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3235 _reflns_number_gt 2371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1999)' _computing_molecular_graphics ORTEX _computing_publication_material 'WinCIF (Thornton-Pett, 2000)' _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^)+(0.0541P)^2^+1.1222P] 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 3235 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.28143(15) 0.07443(13) 0.35502(8) 0.0189(4) Uani 1 1 d . . . B2 B 0.28180(16) -0.05262(13) 0.34476(9) 0.0222(4) Uani 1 1 d . . . H2 H 0.2436(15) -0.0977(12) 0.3822(9) 0.031(5) Uiso 1 1 d . . . B3 B 0.18650(15) 0.01947(13) 0.29694(9) 0.0206(4) Uani 1 1 d . . . H3 H 0.0903(16) 0.0086(13) 0.3014(9) 0.032(5) Uiso 1 1 d . . . B4 B 0.23797(16) 0.13793(13) 0.28384(9) 0.0216(4) Uani 1 1 d . . . H4 H 0.1772(15) 0.1968(12) 0.2872(8) 0.026(4) Uiso 1 1 d . . . B5 B 0.41673(15) 0.01320(14) 0.35155(9) 0.0227(4) Uani 1 1 d . . . H5 H 0.4799(14) 0.0119(11) 0.3905(8) 0.025(4) Uiso 1 1 d . . . B6 B 0.40296(17) -0.08883(14) 0.30006(10) 0.0263(4) Uani 1 1 d . . . H6 H 0.4570(16) -0.1529(13) 0.3015(9) 0.036(5) Uiso 1 1 d . . . B7 B 0.26373(17) -0.07372(14) 0.26002(9) 0.0252(4) Uani 1 1 d . . . H7 H 0.2207(16) -0.1346(14) 0.2379(9) 0.034(5) Uiso 1 1 d . . . B8 B 0.23571(16) 0.05292(14) 0.22006(9) 0.0240(4) Uani 1 1 d . . . H8 H 0.1803(16) 0.0525(13) 0.1772(10) 0.038(5) Uiso 1 1 d . . . B9 B 0.35084(17) 0.13959(14) 0.22807(9) 0.0260(4) Uani 1 1 d . . . H9 H 0.3729(16) 0.1917(13) 0.1934(9) 0.036(5) Uiso 1 1 d . . . B10 B 0.38780(16) 0.13928(14) 0.31186(9) 0.0234(4) Uani 1 1 d . . . H10 H 0.4312(15) 0.1996(13) 0.3323(9) 0.031(5) Uiso 1 1 d . . . H56 H 0.4710(15) -0.0193(13) 0.3027(9) 0.032(5) Uiso 1 1 d . . . H67 H 0.3691(17) -0.0755(13) 0.2401(9) 0.039(5) Uiso 1 1 d . . . H89 H 0.3427(16) 0.0575(13) 0.2000(9) 0.034(5) Uiso 1 1 d . . . H910 H 0.4419(16) 0.1159(14) 0.2625(9) 0.039(5) Uiso 1 1 d . . . B1' B 0.18208(17) 0.10211(14) 0.56277(9) 0.0238(4) Uani 1 1 d . . . H1' H 0.1693(15) 0.0461(13) 0.5984(9) 0.034(5) Uiso 1 1 d . . . B2' B 0.14021(16) 0.07674(13) 0.48202(9) 0.0231(4) Uani 1 1 d . . . H2' H 0.0932(15) 0.0128(13) 0.4692(9) 0.032(5) Uiso 1 1 d . . . B3' B 0.07100(16) 0.17105(14) 0.52526(9) 0.0232(4) Uani 1 1 d . . . H3' H -0.0230(17) 0.1675(13) 0.5342(9) 0.036(5) Uiso 1 1 d . . . B4' B 0.16010(16) 0.22241(14) 0.58673(9) 0.0236(4) Uani 1 1 d . . . H4' H 0.1233(15) 0.2400(13) 0.6323(9) 0.030(5) Uiso 1 1 d . . . B5' B 0.29209(16) 0.07965(13) 0.50533(9) 0.0223(4) Uani 1 1 d . . . H5' H 0.3537(15) 0.0203(13) 0.5082(8) 0.029(5) Uiso 1 1 d . . . B6' B 0.24321(15) 0.11899(13) 0.42732(8) 0.0193(4) Uani 1 1 d . . . B7' B 0.11405(16) 0.18921(14) 0.44504(9) 0.0231(4) Uani 1 1 d . . . H7' H 0.0523(15) 0.2032(13) 0.4070(9) 0.033(5) Uiso 1 1 d . . . B8' B 0.12587(17) 0.28642(14) 0.51476(9) 0.0243(4) Uani 1 1 d . . . H8' H 0.0683(16) 0.3462(13) 0.5096(9) 0.035(5) Uiso 1 1 d . . . B9' B 0.26611(17) 0.29566(14) 0.55346(9) 0.0252(4) Uani 1 1 d . . . H9' H 0.3071(16) 0.3597(14) 0.5701(9) 0.038(5) Uiso 1 1 d . . . B10' B 0.30531(16) 0.17571(14) 0.57412(9) 0.0248(4) Uani 1 1 d . . . H10' H 0.3719(15) 0.1624(12) 0.6106(9) 0.031(5) Uiso 1 1 d . . . H56' H 0.3343(15) 0.1354(13) 0.4641(8) 0.030(5) Uiso 1 1 d . . . H67' H 0.2121(15) 0.2081(13) 0.4256(8) 0.029(5) Uiso 1 1 d . . . H89' H 0.2279(16) 0.3123(13) 0.4967(9) 0.034(5) Uiso 1 1 d . . . H91' H 0.3460(15) 0.2370(12) 0.5358(8) 0.026(5) 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 0.0171(8) 0.0203(9) 0.0191(9) 0.0002(7) -0.0016(7) -0.0009(7) B2 0.0237(9) 0.0212(9) 0.0217(10) 0.0019(7) -0.0014(7) 0.0004(7) B3 0.0178(8) 0.0226(9) 0.0213(9) 0.0003(7) -0.0012(7) -0.0005(7) B4 0.0232(9) 0.0215(9) 0.0201(9) 0.0011(7) -0.0010(7) 0.0002(7) B5 0.0183(9) 0.0290(10) 0.0209(9) -0.0010(8) -0.0006(7) 0.0018(7) B6 0.0292(10) 0.0240(10) 0.0257(10) -0.0011(8) -0.0003(8) 0.0036(8) B7 0.0275(10) 0.0249(10) 0.0232(10) -0.0022(8) -0.0021(8) -0.0015(8) B8 0.0236(9) 0.0285(10) 0.0200(9) -0.0010(8) -0.0015(7) 0.0009(8) B9 0.0297(10) 0.0272(10) 0.0210(10) 0.0019(8) 0.0025(8) -0.0015(8) B10 0.0218(9) 0.0266(10) 0.0219(10) -0.0021(8) 0.0025(7) -0.0034(7) B1' 0.0263(10) 0.0252(10) 0.0199(10) 0.0027(8) 0.0034(7) 0.0005(7) B2' 0.0232(9) 0.0223(10) 0.0239(10) -0.0014(8) 0.0030(7) -0.0026(7) B3' 0.0183(9) 0.0283(10) 0.0231(10) -0.0006(8) 0.0032(7) -0.0011(7) B4' 0.0218(9) 0.0277(10) 0.0213(10) -0.0017(8) 0.0030(7) 0.0022(8) B5' 0.0236(9) 0.0226(10) 0.0206(9) 0.0003(8) -0.0004(7) 0.0028(7) B6' 0.0182(8) 0.0204(9) 0.0194(9) 0.0000(7) -0.0008(7) -0.0012(7) B7' 0.0184(9) 0.0289(10) 0.0221(9) 0.0007(8) 0.0000(7) 0.0015(7) B8' 0.0230(10) 0.0238(10) 0.0263(10) -0.0010(8) 0.0023(7) 0.0026(7) B9' 0.0242(9) 0.0266(10) 0.0248(10) -0.0061(8) 0.0015(7) -0.0010(8) B10' 0.0243(9) 0.0305(11) 0.0196(9) -0.0034(8) 0.0000(7) 0.0024(8) _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 B6' 1.686(2) . ? B1 B10 1.757(2) . ? B1 B5 1.759(2) . ? B1 B3 1.792(2) . ? B1 B2 1.797(3) . ? B1 B4 1.797(2) . ? B2 B6 1.734(3) . ? B2 B3 1.783(3) . ? B2 B5 1.792(2) . ? B2 B7 1.799(3) . ? B3 B7 1.751(3) . ? B3 B8 1.757(3) . ? B3 B4 1.784(3) . ? B4 B9 1.726(3) . ? B4 B8 1.785(3) . ? B4 B10 1.794(3) . ? B5 B6 1.796(3) . ? B5 B10 1.981(3) . ? B6 B7 1.796(3) . ? B7 B8 1.989(3) . ? B8 B9 1.791(3) . ? B9 B10 1.793(3) . ? B1' B10' 1.753(3) . ? B1' B5' 1.755(3) . ? B1' B3' 1.769(3) . ? B1' B4' 1.779(3) . ? B1' B2' 1.781(3) . ? B2' B6' 1.734(2) . ? B2' B7' 1.782(3) . ? B2' B3' 1.783(3) . ? B2' B5' 1.788(3) . ? B3' B8' 1.749(3) . ? B3' B7' 1.757(3) . ? B3' B4' 1.782(3) . ? B4' B9' 1.726(3) . ? B4' B8' 1.789(3) . ? B4' B10' 1.790(3) . ? B5' B6' 1.801(2) . ? B5' B10' 1.972(3) . ? B6' B7' 1.802(2) . ? B7' B8' 1.996(3) . ? B8' B9' 1.785(3) . ? B9' B10' 1.794(3) . ? 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 B6' B1 B10 116.07(13) . . ? B6' B1 B5 116.23(13) . . ? B10 B1 B5 68.60(11) . . ? B6' B1 B3 127.41(13) . . ? B10 B1 B3 106.87(13) . . ? B5 B1 B3 106.52(12) . . ? B6' B1 B2 118.37(13) . . ? B10 B1 B2 116.91(13) . . ? B5 B1 B2 60.50(10) . . ? B3 B1 B2 59.58(10) . . ? B6' B1 B4 118.72(13) . . ? B10 B1 B4 60.63(10) . . ? B5 B1 B4 116.58(13) . . ? B3 B1 B4 59.61(10) . . ? B2 B1 B4 113.31(13) . . ? B6 B2 B3 110.26(13) . . ? B6 B2 B5 61.22(10) . . ? B3 B2 B5 105.50(13) . . ? B6 B2 B1 110.90(13) . . ? B3 B2 B1 60.07(10) . . ? B5 B2 B1 58.69(10) . . ? B6 B2 B7 61.07(11) . . ? B3 B2 B7 58.54(10) . . ? B5 B2 B7 105.02(13) . . ? B1 B2 B7 106.23(12) . . ? B7 B3 B8 69.05(11) . . ? B7 B3 B2 61.19(11) . . ? B8 B3 B2 117.88(13) . . ? B7 B3 B4 117.83(13) . . ? B8 B3 B4 60.53(10) . . ? B2 B3 B4 114.65(13) . . ? B7 B3 B1 108.54(12) . . ? B8 B3 B1 107.94(12) . . ? B2 B3 B1 60.35(10) . . ? B4 B3 B1 60.34(10) . . ? B9 B4 B3 110.92(13) . . ? B9 B4 B8 61.33(11) . . ? B3 B4 B8 59.00(10) . . ? B9 B4 B10 61.18(11) . . ? B3 B4 B10 105.62(13) . . ? B8 B4 B10 105.19(13) . . ? B9 B4 B1 110.95(13) . . ? B3 B4 B1 60.05(10) . . ? B8 B4 B1 106.51(13) . . ? B10 B4 B1 58.58(10) . . ? B1 B5 B2 60.81(10) . . ? B1 B5 B6 109.82(13) . . ? B2 B5 B6 57.81(10) . . ? B1 B5 B10 55.66(9) . . ? B2 B5 B10 106.70(12) . . ? B6 B5 B10 116.77(13) . . ? B2 B6 B5 60.97(10) . . ? B2 B6 B7 61.26(11) . . ? B5 B6 B7 104.98(13) . . ? B3 B7 B6 108.87(13) . . ? B3 B7 B2 60.27(10) . . ? B6 B7 B2 57.67(10) . . ? B3 B7 B8 55.61(10) . . ? B6 B7 B8 116.08(13) . . ? B2 B7 B8 106.28(12) . . ? B3 B8 B4 60.47(10) . . ? B3 B8 B9 109.14(13) . . ? B4 B8 B9 57.72(10) . . ? B3 B8 B7 55.33(10) . . ? B4 B8 B7 106.58(12) . . ? B9 B8 B7 116.91(13) . . ? B4 B9 B8 60.95(11) . . ? B4 B9 B10 61.28(10) . . ? B8 B9 B10 105.00(13) . . ? B1 B10 B9 109.75(13) . . ? B1 B10 B4 60.80(10) . . ? B9 B10 B4 57.54(10) . . ? B1 B10 B5 55.74(9) . . ? B9 B10 B5 116.48(13) . . ? B4 B10 B5 106.40(12) . . ? B10' B1' B5' 68.43(11) . . ? B10' B1' B3' 107.63(13) . . ? B5' B1' B3' 107.63(13) . . ? B10' B1' B4' 60.89(11) . . ? B5' B1' B4' 117.44(13) . . ? B3' B1' B4' 60.28(11) . . ? B10' B1' B2' 117.19(13) . . ? B5' B1' B2' 60.73(10) . . ? B3' B1' B2' 60.27(10) . . ? B4' B1' B2' 114.64(13) . . ? B6' B2' B1' 111.79(13) . . ? B6' B2' B7' 61.65(10) . . ? B1' B2' B7' 105.91(13) . . ? B6' B2' B3' 111.87(13) . . ? B1' B2' B3' 59.52(10) . . ? B7' B2' B3' 59.07(10) . . ? B6' B2' B5' 61.50(10) . . ? B1' B2' B5' 58.90(10) . . ? B7' B2' B5' 104.88(13) . . ? B3' B2' B5' 105.62(13) . . ? B8' B3' B7' 69.41(11) . . ? B8' B3' B1' 108.03(13) . . ? B7' B3' B1' 107.52(13) . . ? B8' B3' B4' 60.88(11) . . ? B7' B3' B4' 117.76(13) . . ? B1' B3' B4' 60.14(11) . . ? B8' B3' B2' 117.98(13) . . ? B7' B3' B2' 60.44(10) . . ? B1' B3' B2' 60.21(10) . . ? B4' B3' B2' 114.46(13) . . ? B9' B4' B1' 110.88(13) . . ? B9' B4' B3' 110.33(14) . . ? B1' B4' B3' 59.58(11) . . ? B9' B4' B8' 61.02(11) . . ? B1' B4' B8' 105.85(13) . . ? B3' B4' B8' 58.67(10) . . ? B9' B4' B10' 61.35(11) . . ? B1' B4' B10' 58.82(10) . . ? B3' B4' B10' 105.47(13) . . ? B8' B4' B10' 105.11(13) . . ? B1' B5' B2' 60.37(10) . . ? B1' B5' B6' 109.88(13) . . ? B2' B5' B6' 57.79(10) . . ? B1' B5' B10' 55.73(10) . . ? B2' B5' B10' 106.58(12) . . ? B6' B5' B10' 117.84(13) . . ? B1 B6' B2' 129.13(14) . . ? B1 B6' B5' 127.66(13) . . ? B2' B6' B5' 60.71(10) . . ? B1 B6' B7' 126.45(13) . . ? B2' B6' B7' 60.47(10) . . ? B5' B6' B7' 103.48(12) . . ? B3' B7' B2' 60.49(11) . . ? B3' B7' B6' 109.88(13) . . ? B2' B7' B6' 57.88(10) . . ? B3' B7' B8' 55.11(10) . . ? B2' B7' B8' 106.35(13) . . ? B6' B7' B8' 117.93(12) . . ? B3' B8' B9' 109.09(14) . . ? B3' B8' B4' 60.46(11) . . ? B9' B8' B4' 57.75(10) . . ? B3' B8' B7' 55.48(10) . . ? B9' B8' B7' 115.91(13) . . ? B4' B8' B7' 106.19(13) . . ? B4' B9' B8' 61.23(11) . . ? B4' B9' B10' 61.08(11) . . ? B8' B9' B10' 105.06(13) . . ? B1' B10' B4' 60.28(11) . . ? B1' B10' B9' 108.94(13) . . ? B4' B10' B9' 57.57(10) . . ? B1' B10' B5' 55.84(10) . . ? B4' B10' B5' 106.70(12) . . ? B9' B10' B5' 116.72(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.239 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.039 data_jb6-6 _database_code_depnum_ccdc_archive 'CCDC 280347' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common "[5-(SMe2)-4-(2'-nido-B10H13)-nido-B10H11]" _chemical_melting_point ? _chemical_formula_moiety 'C2 H30 B20 S' _chemical_formula_sum 'C2 H30 B20 S' _chemical_formula_weight 302.52 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 P21/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 6.9622(2) _cell_length_b 26.4999(6) _cell_length_c 10.6444(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.6540(10) _cell_angle_gamma 90.00 _cell_volume 1950.64(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourles _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9404 _exptl_absorpt_correction_T_max 0.9928 _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 ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 100(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 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligable _diffrn_reflns_number 12704 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3820 _reflns_number_gt 3188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _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 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0602P)^2^+0.4244P] 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 3820 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.9560(2) 1.07679(7) 0.08377(16) 0.0186(4) Uani 1 1 d . . . H1 H 0.927(2) 1.0522(6) 0.0040(15) 0.019(4) Uiso 1 1 d . . . B2 B 1.1615(2) 1.06906(7) 0.19702(17) 0.0223(4) Uani 1 1 d . . . H2 H 1.273(2) 1.0392(7) 0.1841(17) 0.031(5) Uiso 1 1 d . . . B3 B 1.1418(2) 1.12407(7) 0.10164(17) 0.0218(4) Uani 1 1 d . . . H3 H 1.253(3) 1.1329(7) 0.0372(17) 0.034(5) Uiso 1 1 d . . . B4 B 0.8956(2) 1.14211(7) 0.04786(16) 0.0195(4) Uani 1 1 d . . . B5 B 0.9215(2) 1.05999(7) 0.23677(16) 0.0199(4) Uani 1 1 d . . . S5 S 0.83226(5) 0.994402(15) 0.26842(4) 0.02143(15) Uani 1 1 d . . . C51 C 0.6506(3) 1.00628(7) 0.37215(17) 0.0283(4) Uani 1 1 d . . . H51A H 0.5583 1.0313 0.3334 0.042 Uiso 1 1 calc R . . H51B H 0.7123 1.0192 0.4532 0.042 Uiso 1 1 calc R . . H51C H 0.5823 0.9748 0.3863 0.042 Uiso 1 1 calc R . . C52 C 0.6829(2) 0.97482(6) 0.12811(15) 0.0248(4) Uani 1 1 d . . . H52A H 0.6231 0.9422 0.1433 0.037 Uiso 1 1 calc R . . H52B H 0.7623 0.9715 0.0583 0.037 Uiso 1 1 calc R . . H52C H 0.5817 1.0001 0.1061 0.037 Uiso 1 1 calc R . . B6 B 1.0881(3) 1.08293(7) 0.34605(17) 0.0247(4) Uani 1 1 d . . . H6 H 1.145(2) 1.0694(7) 0.4424(17) 0.030(5) Uiso 1 1 d . . . H67 H 1.101(3) 1.1307(8) 0.3496(18) 0.039(5) Uiso 1 1 d . . . B7 B 1.2169(3) 1.12900(8) 0.26696(18) 0.0281(4) Uani 1 1 d . . . H7 H 1.361(3) 1.1460(7) 0.3053(17) 0.032(5) Uiso 1 1 d . . . B8 B 1.0462(3) 1.17879(7) 0.15916(18) 0.0273(4) Uani 1 1 d . . . H89 H 0.941(3) 1.1843(8) 0.2493(19) 0.042(5) Uiso 1 1 d . . . H8 H 1.110(3) 1.2162(8) 0.1407(18) 0.038(5) Uiso 1 1 d . . . B9 B 0.7942(3) 1.17174(7) 0.16888(18) 0.0266(4) Uani 1 1 d . . . H9 H 0.684(3) 1.2003(8) 0.1620(18) 0.037(5) Uiso 1 1 d . . . H910 H 0.750(3) 1.1369(8) 0.243(2) 0.045(6) Uiso 1 1 d . . . B10 B 0.7552(3) 1.10528(7) 0.14993(17) 0.0214(4) Uani 1 1 d . . . H10 H 0.608(3) 1.0942(7) 0.1245(16) 0.029(5) Uiso 1 1 d . . . B1' B 0.7206(3) 1.11947(7) -0.22384(18) 0.0239(4) Uani 1 1 d . . . H1' H 0.674(3) 1.0830(8) -0.1962(17) 0.038(5) Uiso 1 1 d . . . B2' B 0.8317(2) 1.16088(7) -0.10340(17) 0.0201(4) Uani 1 1 d . . . B3' B 0.9594(3) 1.14086(7) -0.23188(17) 0.0203(4) Uani 1 1 d . . . H3' H 1.095(2) 1.1187(7) -0.2095(16) 0.026(4) Uiso 1 1 d . . . B4' B 0.8091(3) 1.12444(7) -0.37361(18) 0.0261(4) Uani 1 1 d . . . H4' H 0.842(3) 1.0906(8) -0.4273(18) 0.041(5) Uiso 1 1 d . . . B5' B 0.5868(3) 1.17043(8) -0.17494(18) 0.0285(4) Uani 1 1 d . . . H56' H 0.597(3) 1.2159(8) -0.2088(18) 0.039(5) Uiso 1 1 d . . . H5' H 0.450(3) 1.1659(8) -0.129(2) 0.050(6) Uiso 1 1 d . . . B6' B 0.7470(3) 1.22190(8) -0.13420(18) 0.0286(4) Uani 1 1 d . . . H6' H 0.726(3) 1.2519(7) -0.0678(18) 0.038(5) Uiso 1 1 d . . . H67' H 0.850(3) 1.2392(8) -0.2220(18) 0.043(6) Uiso 1 1 d . . . B7' B 0.9704(3) 1.20434(7) -0.18813(17) 0.0235(4) Uani 1 1 d . . . H7' H 1.104(3) 1.2251(7) -0.1486(17) 0.032(5) Uiso 1 1 d . . . B8' B 0.9555(3) 1.18007(7) -0.36534(18) 0.0264(4) Uani 1 1 d . . . H8' H 1.079(3) 1.1858(8) -0.4149(19) 0.043(5) Uiso 1 1 d . . . H89' H 0.827(3) 1.2131(8) -0.404(2) 0.052(6) Uiso 1 1 d . . . B9' B 0.7201(3) 1.17764(8) -0.45327(19) 0.0304(4) Uani 1 1 d . . . H9' H 0.688(3) 1.1848(8) -0.5587(18) 0.038(5) Uiso 1 1 d . . . H91' H 0.574(3) 1.1916(8) -0.3944(19) 0.046(6) Uiso 1 1 d . . . B10' B 0.5713(3) 1.14560(8) -0.35182(19) 0.0306(4) Uani 1 1 d . . . H10' H 0.435(3) 1.1272(7) -0.3920(18) 0.038(5) 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 0.0167(8) 0.0193(9) 0.0198(9) 0.0010(7) 0.0017(6) 0.0016(6) B2 0.0186(9) 0.0264(10) 0.0216(9) 0.0020(7) 0.0015(7) 0.0003(7) B3 0.0207(9) 0.0240(10) 0.0201(9) 0.0007(7) 0.0004(7) -0.0040(7) B4 0.0201(9) 0.0174(9) 0.0212(9) 0.0007(7) 0.0039(7) -0.0001(7) B5 0.0196(9) 0.0191(9) 0.0209(9) 0.0022(7) 0.0020(7) 0.0000(6) S5 0.0203(2) 0.0193(2) 0.0244(2) 0.00411(15) 0.00124(16) 0.00088(14) C51 0.0301(9) 0.0324(10) 0.0235(9) 0.0020(7) 0.0073(7) -0.0048(7) C52 0.0260(8) 0.0229(9) 0.0257(9) -0.0040(7) 0.0039(6) -0.0038(7) B6 0.0267(9) 0.0273(10) 0.0201(9) 0.0011(7) 0.0022(7) 0.0005(7) B7 0.0274(10) 0.0317(11) 0.0242(10) -0.0006(8) -0.0006(7) -0.0071(8) B8 0.0387(11) 0.0232(10) 0.0196(10) -0.0006(7) 0.0017(8) -0.0059(8) B9 0.0382(11) 0.0212(10) 0.0213(10) 0.0015(7) 0.0073(8) 0.0052(8) B10 0.0228(9) 0.0194(9) 0.0224(9) 0.0010(7) 0.0052(7) 0.0023(7) B1' 0.0244(9) 0.0228(10) 0.0237(10) 0.0032(7) -0.0003(7) -0.0039(7) B2' 0.0209(9) 0.0178(9) 0.0220(9) 0.0000(7) 0.0047(7) 0.0002(7) B3' 0.0231(9) 0.0180(9) 0.0206(9) 0.0002(7) 0.0053(7) 0.0008(7) B4' 0.0341(10) 0.0226(10) 0.0210(9) -0.0034(7) 0.0002(7) 0.0001(8) B5' 0.0245(10) 0.0356(12) 0.0259(10) 0.0068(8) 0.0046(8) 0.0047(8) B6' 0.0432(11) 0.0231(10) 0.0201(10) 0.0020(8) 0.0057(8) 0.0090(8) B7' 0.0310(10) 0.0184(9) 0.0211(9) 0.0024(7) 0.0031(7) -0.0039(7) B8' 0.0332(10) 0.0243(10) 0.0229(10) 0.0019(8) 0.0085(8) 0.0009(8) B9' 0.0391(11) 0.0279(11) 0.0235(10) -0.0002(8) 0.0005(8) 0.0031(9) B10' 0.0291(10) 0.0318(11) 0.0294(11) 0.0025(8) -0.0030(8) -0.0017(8) _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 B5 1.732(2) . ? B1 B2 1.773(2) . ? B1 B3 1.795(2) . ? B1 B10 1.802(2) . ? B1 B4 1.812(2) . ? B1 H1 1.071(16) . ? B2 B6 1.761(3) . ? B2 B3 1.773(3) . ? B2 B7 1.777(3) . ? B2 B5 1.787(2) . ? B2 H2 1.129(18) . ? B3 B8 1.736(3) . ? B3 B7 1.781(3) . ? B3 B4 1.808(2) . ? B3 H3 1.118(18) . ? B4 B2' 1.695(2) . ? B4 B9 1.728(2) . ? B4 B8 1.778(3) . ? B4 B10 1.826(2) . ? B5 B6 1.660(3) . ? B5 B10 1.840(2) . ? B5 S5 1.8890(18) . ? S5 C52 1.7949(16) . ? S5 C51 1.8006(17) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? B6 B7 1.783(3) . ? B6 H6 1.115(18) . ? B6 H67 1.27(2) . ? B7 B8 2.038(3) . ? B7 H67 1.263(19) . ? B7 H7 1.133(18) . ? B8 B9 1.779(3) . ? B8 H89 1.282(19) . ? B8 H8 1.11(2) . ? B9 B10 1.790(3) . ? B9 H89 1.30(2) . ? B9 H9 1.08(2) . ? B9 H910 1.27(2) . ? B10 H910 1.30(2) . ? B10 H10 1.072(18) . ? B1' B5' 1.754(3) . ? B1' B10' 1.757(3) . ? B1' B3' 1.768(2) . ? B1' B4' 1.779(3) . ? B1' B2' 1.793(3) . ? B1' H1' 1.07(2) . ? B2' B6' 1.739(3) . ? B2' B3' 1.796(2) . ? B2' B5' 1.803(3) . ? B2' B7' 1.809(2) . ? B3' B7' 1.745(2) . ? B3' B8' 1.758(3) . ? B3' B4' 1.787(3) . ? B3' H3' 1.115(18) . ? B4' B9' 1.723(3) . ? B4' B10' 1.788(3) . ? B4' B8' 1.788(3) . ? B4' H4' 1.10(2) . ? B5' B6' 1.783(3) . ? B5' B10' 1.986(3) . ? B5' H56' 1.26(2) . ? B5' H5' 1.13(2) . ? B6' B7' 1.781(3) . ? B6' H56' 1.25(2) . ? B6' H6' 1.09(2) . ? B6' H67' 1.325(19) . ? B7' B8' 1.984(3) . ? B7' H67' 1.27(2) . ? B7' H7' 1.117(19) . ? B8' B9' 1.791(3) . ? B8' H8' 1.07(2) . ? B8' H89' 1.29(2) . ? B9' B10' 1.794(3) . ? B9' H89' 1.27(2) . ? B9' H9' 1.134(19) . ? B9' H91' 1.31(2) . ? B10' H91' 1.30(2) . ? B10' H10' 1.108(19) . ? 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 B5 B1 B2 61.30(10) . . ? B5 B1 B3 104.87(12) . . ? B2 B1 B3 59.58(10) . . ? B5 B1 B10 62.73(10) . . ? B2 B1 B10 112.58(12) . . ? B3 B1 B10 104.38(12) . . ? B5 B1 B4 112.95(12) . . ? B2 B1 B4 113.78(13) . . ? B3 B1 B4 60.16(10) . . ? B10 B1 B4 60.70(9) . . ? B5 B1 H1 123.7(9) . . ? B2 B1 H1 122.2(9) . . ? B3 B1 H1 125.3(9) . . ? B10 B1 H1 118.7(9) . . ? B4 B1 H1 113.3(9) . . ? B6 B2 B1 107.05(12) . . ? B6 B2 B3 109.46(13) . . ? B1 B2 B3 60.84(10) . . ? B6 B2 B7 60.50(11) . . ? B1 B2 B7 107.49(13) . . ? B3 B2 B7 60.24(11) . . ? B6 B2 B5 55.80(10) . . ? B1 B2 B5 58.23(9) . . ? B3 B2 B5 103.54(12) . . ? B7 B2 B5 100.64(12) . . ? B6 B2 H2 122.1(9) . . ? B1 B2 H2 120.7(9) . . ? B3 B2 H2 121.0(9) . . ? B7 B2 H2 123.9(9) . . ? B5 B2 H2 127.7(9) . . ? B8 B3 B2 119.48(13) . . ? B8 B3 B7 70.79(12) . . ? B2 B3 B7 60.01(11) . . ? B8 B3 B1 108.62(13) . . ? B2 B3 B1 59.58(10) . . ? B7 B3 B1 106.33(12) . . ? B8 B3 B4 60.17(10) . . ? B2 B3 B4 113.97(12) . . ? B7 B3 B4 116.89(13) . . ? B1 B3 B4 60.37(9) . . ? B8 B3 H3 111.3(10) . . ? B2 B3 H3 120.7(10) . . ? B7 B3 H3 116.4(10) . . ? B1 B3 H3 128.6(10) . . ? B4 B3 H3 116.8(9) . . ? B2' B4 B9 119.35(13) . . ? B2' B4 B8 122.84(13) . . ? B9 B4 B8 60.99(11) . . ? B2' B4 B3 120.89(13) . . ? B9 B4 B3 109.78(13) . . ? B8 B4 B3 57.93(10) . . ? B2' B4 B1 120.66(13) . . ? B9 B4 B1 112.45(12) . . ? B8 B4 B1 106.09(12) . . ? B3 B4 B1 59.47(9) . . ? B2' B4 B10 128.50(13) . . ? B9 B4 B10 60.41(10) . . ? B8 B4 B10 102.17(12) . . ? B3 B4 B10 102.92(12) . . ? B1 B4 B10 59.40(9) . . ? B6 B5 B1 113.75(13) . . ? B6 B5 B2 61.30(10) . . ? B1 B5 B2 60.47(10) . . ? B6 B5 B10 117.44(13) . . ? B1 B5 B10 60.51(9) . . ? B2 B5 B10 110.14(12) . . ? B6 B5 S5 115.44(12) . . ? B1 B5 S5 119.25(11) . . ? B2 B5 S5 120.13(11) . . ? B10 B5 S5 119.27(11) . . ? C52 S5 C51 100.39(8) . . ? C52 S5 B5 106.76(8) . . ? C51 S5 B5 102.56(8) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? B5 B6 B2 62.90(10) . . ? B5 B6 B7 105.60(13) . . ? B2 B6 B7 60.22(11) . . ? B5 B6 H6 132.1(10) . . ? B2 B6 H6 130.8(9) . . ? B7 B6 H6 120.8(9) . . ? B5 B6 H67 115.2(9) . . ? B2 B6 H67 102.0(9) . . ? B7 B6 H67 45.1(9) . . ? H6 B6 H67 106.2(13) . . ? B2 B7 B3 59.75(10) . . ? B2 B7 B6 59.28(10) . . ? B3 B7 B6 108.07(13) . . ? B2 B7 B8 104.99(12) . . ? B3 B7 B8 53.57(10) . . ? B6 B7 B8 114.64(13) . . ? B2 B7 H67 101.5(9) . . ? B3 B7 H67 123.5(9) . . ? B6 B7 H67 45.4(9) . . ? B8 B7 H67 89.4(9) . . ? B2 B7 H7 130.3(10) . . ? B3 B7 H7 122.1(9) . . ? B6 B7 H7 125.1(9) . . ? B8 B7 H7 112.3(10) . . ? H67 B7 H7 110.3(13) . . ? B3 B8 B4 61.90(10) . . ? B3 B8 B9 110.71(13) . . ? B4 B8 B9 58.12(10) . . ? B3 B8 B7 55.64(10) . . ? B4 B8 B7 106.36(12) . . ? B9 B8 B7 114.44(13) . . ? B3 B8 H89 129.4(9) . . ? B4 B8 H89 102.5(9) . . ? B9 B8 H89 46.7(9) . . ? B7 B8 H89 90.0(9) . . ? B3 B8 H8 120.4(10) . . ? B4 B8 H8 125.9(10) . . ? B9 B8 H8 121.3(10) . . ? B7 B8 H8 117.3(10) . . ? H89 B8 H8 107.8(14) . . ? B4 B9 B8 60.89(10) . . ? B4 B9 B10 62.52(10) . . ? B8 B9 B10 103.56(13) . . ? B4 B9 H89 104.5(9) . . ? B8 B9 H89 46.0(9) . . ? B10 B9 H89 115.1(9) . . ? B4 B9 H9 128.3(10) . . ? B8 B9 H9 128.7(11) . . ? B10 B9 H9 125.9(11) . . ? H89 B9 H9 111.5(14) . . ? B4 B9 H910 106.2(10) . . ? B8 B9 H910 115.0(9) . . ? B10 B9 H910 46.5(10) . . ? H89 B9 H910 90.4(13) . . ? H9 B9 H910 109.2(14) . . ? B9 B10 B1 109.98(12) . . ? B9 B10 B4 57.07(10) . . ? B1 B10 B4 59.90(9) . . ? B9 B10 B5 120.45(13) . . ? B1 B10 B5 56.76(9) . . ? B4 B10 B5 107.37(12) . . ? B9 B10 H910 45.3(9) . . ? B1 B10 H910 131.2(9) . . ? B4 B10 H910 99.8(9) . . ? B5 B10 H910 96.4(9) . . ? B9 B10 H10 115.3(10) . . ? B1 B10 H10 123.4(10) . . ? B4 B10 H10 124.0(9) . . ? B5 B10 H10 118.4(10) . . ? H910 B10 H10 105.0(13) . . ? B5' B1' B10' 68.88(12) . . ? B5' B1' B3' 107.61(13) . . ? B10' B1' B3' 108.14(13) . . ? B5' B1' B4' 117.38(14) . . ? B10' B1' B4' 60.75(11) . . ? B3' B1' B4' 60.51(10) . . ? B5' B1' B2' 61.09(11) . . ? B10' B1' B2' 118.71(14) . . ? B3' B1' B2' 60.55(10) . . ? B4' B1' B2' 115.45(13) . . ? B5' B1' H1' 115.1(10) . . ? B10' B1' H1' 113.3(10) . . ? B3' B1' H1' 128.3(10) . . ? B4' B1' H1' 117.4(10) . . ? B2' B1' H1' 118.4(10) . . ? B4 B2' B6' 119.86(14) . . ? B4 B2' B1' 122.92(13) . . ? B6' B2' B1' 109.00(13) . . ? B4 B2' B3' 122.56(13) . . ? B6' B2' B3' 108.55(12) . . ? B1' B2' B3' 59.03(10) . . ? B4 B2' B5' 125.01(13) . . ? B6' B2' B5' 60.43(11) . . ? B1' B2' B5' 58.37(10) . . ? B3' B2' B5' 104.33(12) . . ? B4 B2' B7' 124.33(13) . . ? B6' B2' B7' 60.21(11) . . ? B1' B2' B7' 104.12(12) . . ? B3' B2' B7' 57.89(10) . . ? B5' B2' B7' 103.50(12) . . ? B7' B3' B8' 69.01(11) . . ? B7' B3' B1' 107.97(13) . . ? B8' B3' B1' 107.57(13) . . ? B7' B3' B4' 117.59(13) . . ? B8' B3' B4' 60.59(11) . . ? B1' B3' B4' 60.05(10) . . ? B7' B3' B2' 61.45(10) . . ? B8' B3' B2' 118.55(13) . . ? B1' B3' B2' 60.42(10) . . ? B4' B3' B2' 114.93(13) . . ? B7' B3' H3' 116.2(9) . . ? B8' B3' H3' 114.7(9) . . ? B1' B3' H3' 126.8(9) . . ? B4' B3' H3' 116.8(9) . . ? B2' B3' H3' 118.4(9) . . ? B9' B4' B1' 111.07(14) . . ? B9' B4' B3' 111.00(14) . . ? B1' B4' B3' 59.44(10) . . ? B9' B4' B10' 61.44(12) . . ? B1' B4' B10' 59.01(11) . . ? B3' B4' B10' 105.94(13) . . ? B9' B4' B8' 61.32(12) . . ? B1' B4' B8' 105.75(13) . . ? B3' B4' B8' 58.89(10) . . ? B10' B4' B8' 105.43(14) . . ? B9' B4' H4' 119.7(10) . . ? B1' B4' H4' 121.3(10) . . ? B3' B4' H4' 119.9(10) . . ? B10' B4' H4' 125.1(10) . . ? B8' B4' H4' 123.0(10) . . ? B1' B5' B6' 108.79(13) . . ? B1' B5' B2' 60.54(10) . . ? B6' B5' B2' 58.01(10) . . ? B1' B5' B10' 55.64(10) . . ? B6' B5' B10' 116.59(13) . . ? B2' B5' B10' 107.37(12) . . ? B1' B5' H56' 127.0(9) . . ? B6' B5' H56' 44.5(9) . . ? B2' B5' H56' 100.1(9) . . ? B10' B5' H56' 92.5(9) . . ? B1' B5' H5' 123.6(11) . . ? B6' B5' H5' 120.7(11) . . ? B2' B5' H5' 127.3(11) . . ? B10' B5' H5' 115.1(11) . . ? H56' B5' H5' 107.5(14) . . ? B2' B6' B7' 61.86(10) . . ? B2' B6' B5' 61.56(11) . . ? B7' B6' B5' 105.48(13) . . ? B2' B6' H56' 104.0(9) . . ? B7' B6' H56' 117.5(9) . . ? B5' B6' H56' 45.0(9) . . ? B2' B6' H6' 128.8(10) . . ? B7' B6' H6' 126.3(10) . . ? B5' B6' H6' 126.1(10) . . ? H56' B6' H6' 109.8(13) . . ? B2' B6' H67' 104.8(9) . . ? B7' B6' H67' 45.5(9) . . ? B5' B6' H67' 117.9(9) . . ? H56' B6' H67' 94.5(12) . . ? H6' B6' H67' 109.4(14) . . ? B3' B7' B6' 108.97(13) . . ? B3' B7' B2' 60.66(10) . . ? B6' B7' B2' 57.94(10) . . ? B3' B7' B8' 55.80(10) . . ? B6' B7' B8' 116.08(13) . . ? B2' B7' B8' 107.18(12) . . ? B3' B7' H67' 128.2(9) . . ? B6' B7' H67' 47.9(9) . . ? B2' B7' H67' 103.4(9) . . ? B8' B7' H67' 90.3(9) . . ? B3' B7' H7' 125.7(10) . . ? B6' B7' H7' 117.9(9) . . ? B2' B7' H7' 126.4(10) . . ? B8' B7' H7' 117.8(9) . . ? H67' B7' H7' 103.9(14) . . ? B3' B8' B4' 60.53(10) . . ? B3' B8' B9' 109.19(13) . . ? B4' B8' B9' 57.53(11) . . ? B3' B8' B7' 55.19(9) . . ? B4' B8' B7' 106.31(12) . . ? B9' B8' B7' 116.90(13) . . ? B3' B8' H8' 122.9(11) . . ? B4' B8' H8' 125.4(11) . . ? B9' B8' H8' 119.1(11) . . ? B7' B8' H8' 117.7(11) . . ? B3' B8' H89' 127.4(10) . . ? B4' B8' H89' 100.0(10) . . ? B9' B8' H89' 45.2(10) . . ? B7' B8' H89' 92.5(10) . . ? H8' B8' H89' 108.4(15) . . ? B4' B9' B8' 61.14(11) . . ? B4' B9' B10' 61.08(12) . . ? B8' B9' B10' 105.04(13) . . ? B4' B9' H89' 104.2(10) . . ? B8' B9' H89' 46.0(10) . . ? B10' B9' H89' 117.0(10) . . ? B4' B9' H9' 129.9(10) . . ? B8' B9' H9' 124.9(10) . . ? B10' B9' H9' 127.9(10) . . ? H89' B9' H9' 108.6(14) . . ? B4' B9' H91' 104.6(9) . . ? B8' B9' H91' 117.0(9) . . ? B10' B9' H91' 46.5(9) . . ? H89' B9' H91' 92.4(14) . . ? H9' B9' H91' 110.7(13) . . ? B1' B10' B4' 60.24(11) . . ? B1' B10' B9' 108.79(14) . . ? B4' B10' B9' 57.49(11) . . ? B1' B10' B5' 55.48(10) . . ? B4' B10' B5' 106.12(13) . . ? B9' B10' B5' 116.25(14) . . ? B1' B10' H91' 127.4(9) . . ? B4' B10' H91' 101.3(9) . . ? B9' B10' H91' 46.7(9) . . ? B5' B10' H91' 91.1(9) . . ? B1' B10' H10' 121.9(10) . . ? B4' B10' H10' 125.2(10) . . ? B9' B10' H10' 120.3(10) . . ? B5' B10' H10' 117.5(10) . . ? H91' B10' H10' 109.0(14) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.427 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.057