Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'D.Valery Kalinin' _publ_contact_author_address ; A. N. Nesmeyanov Institute of Organoelement Compounds Russian Academy of Sciences 28 Vavilova str Moscow 119991 RUSSIAN FEDERATION ; _publ_contact_author_email VKALIN@INEOS.AC.RU _publ_section_title ; The first carborane triflates: synthesis and reactivity of 1-trifluoromethanesulfonylmethyl- and 1,2-bis(trifluoromethanesulfonylmethyl)-o-carborane ; loop_ _publ_author_name 'Evamarie Hey-Hawkins' A.A.Korlyukov V.A.Ol'shevskaya P.V.Petrovskii ; A.B.Ponomaryov ; 'Evgeny Rys' 'Zoya Starikova' D.D.Sung A.A.Tyutyunov data_posl_1 _database_code_depnum_ccdc_archive 'CCDC 227517' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common nido-7-((pyridinium)methyl)-7,8-dicarbaundecaborate _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H18 B9 N' _chemical_formula_weight 225.52 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 7.984(4) _cell_length_b 10.740(5) _cell_length_c 15.354(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.345(9) _cell_angle_gamma 90.00 _cell_volume 1314.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.290 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker SMART 1000 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 12170 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.99 _reflns_number_total 3145 _reflns_number_gt 2359 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0333P)^2^+1.2332P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3145 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 N1 N 0.28247(15) 0.77567(12) 0.07241(9) 0.0222(3) Uani 1 1 d . . . C1 C 0.5844(2) 0.73893(15) 0.23466(11) 0.0244(3) Uani 1 1 d . . . C2 C 0.53415(18) 0.83778(14) 0.16319(10) 0.0212(3) Uani 1 1 d . . . C3 C 0.34869(19) 0.86014(16) 0.14402(11) 0.0239(3) Uani 1 1 d . . . C4 C 0.2199(2) 0.82423(17) -0.00302(11) 0.0271(4) Uani 1 1 d . . . C5 C 0.1639(2) 0.74797(19) -0.07054(11) 0.0329(4) Uani 1 1 d . . . C6 C 0.1729(2) 0.62076(19) -0.06026(12) 0.0337(4) Uani 1 1 d . . . C7 C 0.2372(2) 0.57202(18) 0.01858(13) 0.0340(4) Uani 1 1 d . . . C8 C 0.2899(2) 0.65201(16) 0.08426(12) 0.0290(4) Uani 1 1 d . . . B1 B 0.7519(2) 0.66211(18) 0.21337(12) 0.0257(4) Uani 1 1 d . . . B2 B 0.8255(2) 0.73142(17) 0.11242(12) 0.0249(4) Uani 1 1 d . . . H10 H 0.696(4) 0.684(3) 0.1182(19) 0.091(10) Uiso 1 1 d . . . B3 B 0.6610(2) 0.84436(17) 0.08526(12) 0.0236(4) Uani 1 1 d . . . B4 B 0.7617(2) 0.78086(19) 0.29620(12) 0.0265(4) Uani 1 1 d . . . B5 B 0.9125(2) 0.77629(18) 0.21699(12) 0.0245(4) Uani 1 1 d . . . B6 B 0.8539(2) 0.89229(17) 0.13555(12) 0.0234(4) Uani 1 1 d . . . B7 B 0.6685(2) 0.96297(17) 0.16666(12) 0.0238(4) Uani 1 1 d . . . B8 B 0.6083(2) 0.89249(18) 0.26415(12) 0.0245(4) Uani 1 1 d . . . B9 B 0.8225(2) 0.92230(18) 0.24862(12) 0.0259(4) Uani 1 1 d . . . H1C H 0.489(3) 0.7023(18) 0.2656(13) 0.034(5) Uiso 1 1 d . . . H3CA H 0.283(2) 0.8434(17) 0.1948(12) 0.024(4) Uiso 1 1 d . . . H3CB H 0.330(2) 0.9444(17) 0.1246(11) 0.022(4) Uiso 1 1 d . . . H4C H 0.218(2) 0.9117(17) -0.0059(11) 0.021(4) Uiso 1 1 d . . . H5C H 0.126(3) 0.787(2) -0.1209(15) 0.048(6) Uiso 1 1 d . . . H6C H 0.138(3) 0.5675(19) -0.1064(13) 0.037(5) Uiso 1 1 d . . . H7C H 0.243(3) 0.487(2) 0.0270(14) 0.044(6) Uiso 1 1 d . . . H8C H 0.333(3) 0.6235(19) 0.1390(14) 0.037(5) Uiso 1 1 d . . . H1 H 0.771(2) 0.5682(19) 0.2338(12) 0.035(5) Uiso 1 1 d . . . H2 H 0.902(2) 0.6875(18) 0.0657(12) 0.032(5) Uiso 1 1 d . . . H3 H 0.612(2) 0.8704(18) 0.0196(12) 0.032(5) Uiso 1 1 d . . . H4 H 0.777(3) 0.751(2) 0.3634(14) 0.042(6) Uiso 1 1 d . . . H5 H 1.045(2) 0.7573(17) 0.2334(12) 0.028(5) Uiso 1 1 d . . . H6 H 0.946(2) 0.9437(18) 0.1020(12) 0.031(5) Uiso 1 1 d . . . H7 H 0.619(2) 1.0550(18) 0.1504(12) 0.030(5) Uiso 1 1 d . . . H8 H 0.525(2) 0.9362(16) 0.3072(11) 0.022(4) Uiso 1 1 d . . . H9 H 0.896(2) 0.9932(18) 0.2850(12) 0.031(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 N1 0.0187(6) 0.0243(7) 0.0231(7) -0.0013(5) -0.0018(5) -0.0006(5) C1 0.0235(7) 0.0247(8) 0.0244(8) 0.0036(6) -0.0031(6) -0.0027(6) C2 0.0213(7) 0.0211(7) 0.0209(7) -0.0010(6) -0.0024(6) -0.0013(6) C3 0.0216(7) 0.0248(8) 0.0250(8) -0.0050(6) -0.0016(6) -0.0006(6) C4 0.0249(8) 0.0285(9) 0.0277(8) 0.0058(7) -0.0011(6) -0.0022(6) C5 0.0316(9) 0.0448(11) 0.0217(8) 0.0034(8) -0.0036(7) -0.0069(8) C6 0.0298(9) 0.0414(10) 0.0298(9) -0.0115(8) -0.0005(7) -0.0062(8) C7 0.0326(9) 0.0255(9) 0.0431(11) -0.0046(8) -0.0047(8) -0.0004(7) C8 0.0288(8) 0.0262(8) 0.0310(9) 0.0019(7) -0.0071(7) 0.0007(7) B1 0.0255(8) 0.0229(9) 0.0286(9) 0.0032(7) -0.0006(7) -0.0002(7) B2 0.0258(9) 0.0240(9) 0.0249(9) -0.0004(7) 0.0012(7) 0.0002(7) B3 0.0232(8) 0.0248(9) 0.0224(8) 0.0005(7) -0.0008(7) 0.0007(7) B4 0.0244(8) 0.0323(10) 0.0221(9) 0.0031(7) -0.0040(7) -0.0041(7) B5 0.0210(8) 0.0275(9) 0.0246(9) 0.0025(7) -0.0014(7) -0.0011(7) B6 0.0219(8) 0.0229(8) 0.0254(9) 0.0028(7) 0.0009(7) -0.0019(7) B7 0.0239(8) 0.0216(8) 0.0259(9) -0.0005(7) 0.0004(7) -0.0019(7) B8 0.0232(8) 0.0278(9) 0.0225(8) -0.0042(7) -0.0001(7) -0.0041(7) B9 0.0232(8) 0.0289(9) 0.0252(9) -0.0034(8) -0.0013(7) -0.0049(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C4 1.340(2) . ? N1 C8 1.341(2) . ? N1 C3 1.498(2) . ? C1 C2 1.562(2) . ? C1 B1 1.621(3) . ? C1 B4 1.716(2) . ? C1 B8 1.718(3) . ? C2 C3 1.512(2) . ? C2 B3 1.614(2) . ? C2 B7 1.719(2) . ? C2 B8 1.729(2) . ? C4 C5 1.375(3) . ? C5 C6 1.377(3) . ? C6 C7 1.389(3) . ? C7 C8 1.372(2) . ? B1 B5 1.773(3) . ? B1 B4 1.800(3) . ? B1 B2 1.846(3) . ? B2 B6 1.776(3) . ? B2 B5 1.778(3) . ? B2 B3 1.818(3) . ? B3 B6 1.759(3) . ? B3 B7 1.783(3) . ? B4 B5 1.761(3) . ? B4 B8 1.764(3) . ? B4 B9 1.766(3) . ? B5 B9 1.803(3) . ? B5 B6 1.807(3) . ? B6 B7 1.755(3) . ? B6 B9 1.798(3) . ? B7 B9 1.762(3) . ? B7 B8 1.769(3) . ? B8 B9 1.770(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 C4 N1 C8 120.93(15) . . ? C4 N1 C3 119.77(14) . . ? C8 N1 C3 119.28(14) . . ? C2 C1 B1 112.67(13) . . ? C2 C1 B4 112.23(13) . . ? B1 C1 B4 65.21(11) . . ? C2 C1 B8 63.43(11) . . ? B1 C1 B8 117.50(13) . . ? B4 C1 B8 61.81(11) . . ? C3 C2 C1 116.94(13) . . ? C3 C2 B3 119.91(13) . . ? C1 C2 B3 113.83(13) . . ? C3 C2 B7 118.95(13) . . ? C1 C2 B7 112.06(12) . . ? B3 C2 B7 64.61(11) . . ? C3 C2 B8 113.61(13) . . ? C1 C2 B8 62.67(11) . . ? B3 C2 B8 116.94(13) . . ? B7 C2 B8 61.72(10) . . ? N1 C3 C2 110.27(13) . . ? N1 C4 C5 120.54(17) . . ? C4 C5 C6 119.48(17) . . ? C5 C6 C7 119.20(17) . . ? C8 C7 C6 119.10(18) . . ? N1 C8 C7 120.73(16) . . ? C1 B1 B5 104.20(14) . . ? C1 B1 B4 59.94(10) . . ? B5 B1 B4 59.07(11) . . ? C1 B1 B2 105.70(13) . . ? B5 B1 B2 58.83(10) . . ? B4 B1 B2 107.74(13) . . ? B6 B2 B5 61.12(10) . . ? B6 B2 B3 58.60(10) . . ? B5 B2 B3 105.38(13) . . ? B6 B2 B1 105.53(13) . . ? B5 B2 B1 58.52(11) . . ? B3 B2 B1 101.58(13) . . ? C2 B3 B6 104.99(13) . . ? C2 B3 B7 60.56(10) . . ? B6 B3 B7 59.38(10) . . ? C2 B3 B2 106.07(13) . . ? B6 B3 B2 59.50(10) . . ? B7 B3 B2 108.76(13) . . ? C1 B4 B5 100.81(13) . . ? C1 B4 B8 59.16(10) . . ? B5 B4 B8 108.54(13) . . ? C1 B4 B9 103.63(13) . . ? B5 B4 B9 61.51(11) . . ? B8 B4 B9 60.18(11) . . ? C1 B4 B1 54.85(10) . . ? B5 B4 B1 59.70(11) . . ? B8 B4 B1 106.48(13) . . ? B9 B4 B1 108.60(14) . . ? B4 B5 B1 61.23(11) . . ? B4 B5 B2 112.60(13) . . ? B1 B5 B2 62.64(11) . . ? B4 B5 B9 59.38(11) . . ? B1 B5 B9 108.13(13) . . ? B2 B5 B9 109.75(13) . . ? B4 B5 B6 107.40(13) . . ? B1 B5 B6 107.33(12) . . ? B2 B5 B6 59.37(10) . . ? B9 B5 B6 59.72(11) . . ? B7 B6 B3 60.99(11) . . ? B7 B6 B2 112.03(13) . . ? B3 B6 B2 61.90(10) . . ? B7 B6 B9 59.46(10) . . ? B3 B6 B9 107.95(13) . . ? B2 B6 B9 110.13(13) . . ? B7 B6 B5 107.35(13) . . ? B3 B6 B5 106.64(12) . . ? B2 B6 B5 59.51(10) . . ? B9 B6 B5 60.03(11) . . ? C2 B7 B6 100.84(13) . . ? C2 B7 B9 103.67(13) . . ? B6 B7 B9 61.49(11) . . ? C2 B7 B8 59.44(10) . . ? B6 B7 B8 108.70(13) . . ? B9 B7 B8 60.15(11) . . ? C2 B7 B3 54.83(10) . . ? B6 B7 B3 59.63(10) . . ? B9 B7 B3 108.48(13) . . ? B8 B7 B3 106.72(13) . . ? C1 B8 C2 53.90(9) . . ? C1 B8 B4 59.03(10) . . ? C2 B8 B4 102.41(13) . . ? C1 B8 B7 102.67(13) . . ? C2 B8 B7 58.85(10) . . ? B4 B8 B7 107.96(13) . . ? C1 B8 B9 103.38(13) . . ? C2 B8 B9 102.92(12) . . ? B4 B8 B9 59.97(11) . . ? B7 B8 B9 59.73(10) . . ? B7 B9 B4 108.16(13) . . ? B7 B9 B8 60.11(10) . . ? B4 B9 B8 59.84(11) . . ? B7 B9 B6 59.05(10) . . ? B4 B9 B6 107.61(13) . . ? B8 B9 B6 106.75(12) . . ? B7 B9 B5 107.20(13) . . ? B4 B9 B5 59.12(11) . . ? B8 B9 B5 106.40(13) . . ? B6 B9 B5 60.24(10) . . ? 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 B1 C1 C2 C3 145.41(14) . . . . ? B4 C1 C2 C3 -143.27(14) . . . . ? B8 C1 C2 C3 -104.07(15) . . . . ? B1 C1 C2 B3 -1.30(18) . . . . ? B4 C1 C2 B3 70.02(17) . . . . ? B8 C1 C2 B3 109.22(14) . . . . ? B1 C1 C2 B7 -72.23(17) . . . . ? B4 C1 C2 B7 -0.91(18) . . . . ? B8 C1 C2 B7 38.29(12) . . . . ? B1 C1 C2 B8 -110.52(14) . . . . ? B4 C1 C2 B8 -39.20(13) . . . . ? C4 N1 C3 C2 -116.98(16) . . . . ? C8 N1 C3 C2 61.67(19) . . . . ? C1 C2 C3 N1 -90.84(17) . . . . ? B3 C2 C3 N1 53.77(19) . . . . ? B7 C2 C3 N1 129.46(14) . . . . ? B8 C2 C3 N1 -160.97(13) . . . . ? C8 N1 C4 C5 -0.9(2) . . . . ? C3 N1 C4 C5 177.76(15) . . . . ? N1 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C7 0.6(3) . . . . ? C5 C6 C7 C8 0.1(3) . . . . ? C4 N1 C8 C7 1.5(3) . . . . ? C3 N1 C8 C7 -177.10(15) . . . . ? C6 C7 C8 N1 -1.1(3) . . . . ? C2 C1 B1 B5 64.37(16) . . . . ? B4 C1 B1 B5 -40.62(12) . . . . ? B8 C1 B1 B5 -6.42(18) . . . . ? C2 C1 B1 B4 104.99(14) . . . . ? B8 C1 B1 B4 34.21(13) . . . . ? C2 C1 B1 B2 3.27(17) . . . . ? B4 C1 B1 B2 -101.72(14) . . . . ? B8 C1 B1 B2 -67.51(17) . . . . ? C1 B1 B2 B6 56.61(15) . . . . ? B5 B1 B2 B6 -40.73(12) . . . . ? B4 B1 B2 B6 -6.24(16) . . . . ? C1 B1 B2 B5 97.34(14) . . . . ? B4 B1 B2 B5 34.49(12) . . . . ? C1 B1 B2 B3 -3.73(15) . . . . ? B5 B1 B2 B3 -101.06(13) . . . . ? B4 B1 B2 B3 -66.57(15) . . . . ? C3 C2 B3 B6 151.02(14) . . . . ? C1 C2 B3 B6 -63.35(16) . . . . ? B7 C2 B3 B6 40.82(12) . . . . ? B8 C2 B3 B6 6.86(18) . . . . ? C3 C2 B3 B7 110.19(16) . . . . ? C1 C2 B3 B7 -104.17(14) . . . . ? B8 C2 B3 B7 -33.96(13) . . . . ? C3 C2 B3 B2 -146.99(14) . . . . ? C1 C2 B3 B2 -1.36(17) . . . . ? B7 C2 B3 B2 102.81(13) . . . . ? B8 C2 B3 B2 68.85(17) . . . . ? B6 B2 B3 C2 -98.21(14) . . . . ? B5 B2 B3 C2 -57.20(15) . . . . ? B1 B2 B3 C2 3.04(15) . . . . ? B5 B2 B3 B6 41.01(12) . . . . ? B1 B2 B3 B6 101.25(13) . . . . ? B6 B2 B3 B7 -34.47(12) . . . . ? B5 B2 B3 B7 6.55(16) . . . . ? B1 B2 B3 B7 66.78(15) . . . . ? C2 C1 B4 B5 -65.35(16) . . . . ? B1 C1 B4 B5 40.30(12) . . . . ? B8 C1 B4 B5 -105.24(14) . . . . ? C2 C1 B4 B8 39.89(13) . . . . ? B1 C1 B4 B8 145.54(14) . . . . ? C2 C1 B4 B9 -2.31(18) . . . . ? B1 C1 B4 B9 103.34(14) . . . . ? B8 C1 B4 B9 -42.21(12) . . . . ? C2 C1 B4 B1 -105.65(15) . . . . ? B8 C1 B4 B1 -145.54(14) . . . . ? B5 B1 B4 C1 132.62(14) . . . . ? B2 B1 B4 C1 98.23(14) . . . . ? C1 B1 B4 B5 -132.62(14) . . . . ? B2 B1 B4 B5 -34.39(12) . . . . ? C1 B1 B4 B8 -30.44(12) . . . . ? B5 B1 B4 B8 102.18(14) . . . . ? B2 B1 B4 B8 67.79(15) . . . . ? C1 B1 B4 B9 -93.85(14) . . . . ? B5 B1 B4 B9 38.77(12) . . . . ? B2 B1 B4 B9 4.38(17) . . . . ? C1 B4 B5 B1 -37.78(11) . . . . ? B8 B4 B5 B1 -98.67(14) . . . . ? B9 B4 B5 B1 -137.52(13) . . . . ? C1 B4 B5 B2 -0.56(17) . . . . ? B8 B4 B5 B2 -61.45(17) . . . . ? B9 B4 B5 B2 -100.31(14) . . . . ? B1 B4 B5 B2 37.22(13) . . . . ? C1 B4 B5 B9 99.75(13) . . . . ? B8 B4 B5 B9 38.85(12) . . . . ? B1 B4 B5 B9 137.52(13) . . . . ? C1 B4 B5 B6 62.83(15) . . . . ? B8 B4 B5 B6 1.93(17) . . . . ? B9 B4 B5 B6 -36.92(12) . . . . ? B1 B4 B5 B6 100.60(14) . . . . ? C1 B1 B5 B4 41.07(12) . . . . ? B2 B1 B5 B4 141.04(13) . . . . ? C1 B1 B5 B2 -99.98(13) . . . . ? B4 B1 B5 B2 -141.04(13) . . . . ? C1 B1 B5 B9 3.37(17) . . . . ? B4 B1 B5 B9 -37.70(12) . . . . ? B2 B1 B5 B9 103.35(14) . . . . ? C1 B1 B5 B6 -59.65(16) . . . . ? B4 B1 B5 B6 -100.72(14) . . . . ? B2 B1 B5 B6 40.32(12) . . . . ? B6 B2 B5 B4 97.46(15) . . . . ? B3 B2 B5 B4 57.70(17) . . . . ? B1 B2 B5 B4 -36.65(13) . . . . ? B6 B2 B5 B1 134.12(13) . . . . ? B3 B2 B5 B1 94.35(14) . . . . ? B6 B2 B5 B9 33.37(12) . . . . ? B3 B2 B5 B9 -6.40(16) . . . . ? B1 B2 B5 B9 -100.75(14) . . . . ? B3 B2 B5 B6 -39.77(12) . . . . ? B1 B2 B5 B6 -134.12(13) . . . . ? C2 B3 B6 B7 -41.42(12) . . . . ? B2 B3 B6 B7 -141.49(13) . . . . ? C2 B3 B6 B2 100.07(14) . . . . ? B7 B3 B6 B2 141.49(13) . . . . ? C2 B3 B6 B9 -3.64(17) . . . . ? B7 B3 B6 B9 37.77(12) . . . . ? B2 B3 B6 B9 -103.71(14) . . . . ? C2 B3 B6 B5 59.54(16) . . . . ? B7 B3 B6 B5 100.96(14) . . . . ? B2 B3 B6 B5 -40.53(12) . . . . ? B5 B2 B6 B7 -97.76(14) . . . . ? B3 B2 B6 B7 35.98(13) . . . . ? B1 B2 B6 B7 -58.30(16) . . . . ? B5 B2 B6 B3 -133.73(13) . . . . ? B1 B2 B6 B3 -94.28(13) . . . . ? B5 B2 B6 B9 -33.58(12) . . . . ? B3 B2 B6 B9 100.16(14) . . . . ? B1 B2 B6 B9 5.88(16) . . . . ? B3 B2 B6 B5 133.73(13) . . . . ? B1 B2 B6 B5 39.46(11) . . . . ? B4 B5 B6 B7 -0.61(16) . . . . ? B1 B5 B6 B7 63.88(16) . . . . ? B2 B5 B6 B7 105.79(14) . . . . ? B9 B5 B6 B7 -37.38(12) . . . . ? B4 B5 B6 B3 -64.70(16) . . . . ? B1 B5 B6 B3 -0.21(17) . . . . ? B2 B5 B6 B3 41.70(12) . . . . ? B9 B5 B6 B3 -101.47(14) . . . . ? B4 B5 B6 B2 -106.40(14) . . . . ? B1 B5 B6 B2 -41.91(12) . . . . ? B9 B5 B6 B2 -143.17(13) . . . . ? B4 B5 B6 B9 36.77(12) . . . . ? B1 B5 B6 B9 101.26(14) . . . . ? B2 B5 B6 B9 143.17(13) . . . . ? C3 C2 B7 B6 -151.74(14) . . . . ? C1 C2 B7 B6 66.73(15) . . . . ? B3 C2 B7 B6 -40.14(12) . . . . ? B8 C2 B7 B6 105.43(13) . . . . ? C3 C2 B7 B9 145.24(14) . . . . ? C1 C2 B7 B9 3.71(17) . . . . ? B3 C2 B7 B9 -103.16(14) . . . . ? B8 C2 B7 B9 42.40(12) . . . . ? C3 C2 B7 B8 102.84(15) . . . . ? C1 C2 B7 B8 -38.69(13) . . . . ? B3 C2 B7 B8 -145.56(13) . . . . ? C3 C2 B7 B3 -111.60(16) . . . . ? C1 C2 B7 B3 106.87(15) . . . . ? B8 C2 B7 B3 145.56(13) . . . . ? B3 B6 B7 C2 37.64(11) . . . . ? B2 B6 B7 C2 1.31(16) . . . . ? B9 B6 B7 C2 -99.78(13) . . . . ? B5 B6 B7 C2 -62.14(14) . . . . ? B3 B6 B7 B9 137.42(13) . . . . ? B2 B6 B7 B9 101.08(14) . . . . ? B5 B6 B7 B9 37.64(12) . . . . ? B3 B6 B7 B8 98.84(14) . . . . ? B2 B6 B7 B8 62.50(16) . . . . ? B9 B6 B7 B8 -38.58(12) . . . . ? B5 B6 B7 B8 -0.94(16) . . . . ? B2 B6 B7 B3 -36.34(13) . . . . ? B9 B6 B7 B3 -137.42(13) . . . . ? B5 B6 B7 B3 -99.78(14) . . . . ? B6 B3 B7 C2 -132.80(13) . . . . ? B2 B3 B7 C2 -98.28(14) . . . . ? C2 B3 B7 B6 132.80(13) . . . . ? B2 B3 B7 B6 34.52(12) . . . . ? C2 B3 B7 B9 93.97(14) . . . . ? B6 B3 B7 B9 -38.82(12) . . . . ? B2 B3 B7 B9 -4.31(17) . . . . ? C2 B3 B7 B8 30.56(12) . . . . ? B6 B3 B7 B8 -102.24(14) . . . . ? B2 B3 B7 B8 -67.72(15) . . . . ? B1 C1 B8 C2 103.03(15) . . . . ? B4 C1 B8 C2 138.41(13) . . . . ? C2 C1 B8 B4 -138.41(13) . . . . ? B1 C1 B8 B4 -35.38(14) . . . . ? C2 C1 B8 B7 -34.89(11) . . . . ? B1 C1 B8 B7 68.14(16) . . . . ? B4 C1 B8 B7 103.52(14) . . . . ? C2 C1 B8 B9 -96.37(13) . . . . ? B1 C1 B8 B9 6.66(18) . . . . ? B4 C1 B8 B9 42.04(12) . . . . ? C3 C2 B8 C1 109.31(15) . . . . ? B3 C2 B8 C1 -104.33(15) . . . . ? B7 C2 B8 C1 -139.30(13) . . . . ? C3 C2 B8 B4 144.96(13) . . . . ? C1 C2 B8 B4 35.65(12) . . . . ? B3 C2 B8 B4 -68.69(16) . . . . ? B7 C2 B8 B4 -103.65(14) . . . . ? C3 C2 B8 B7 -111.39(15) . . . . ? C1 C2 B8 B7 139.30(13) . . . . ? B3 C2 B8 B7 34.96(14) . . . . ? C3 C2 B8 B9 -153.41(14) . . . . ? C1 C2 B8 B9 97.27(14) . . . . ? B3 C2 B8 B9 -7.06(18) . . . . ? B7 C2 B8 B9 -42.02(12) . . . . ? B5 B4 B8 C1 91.74(14) . . . . ? B9 B4 B8 C1 131.19(13) . . . . ? B1 B4 B8 C1 28.85(12) . . . . ? C1 B4 B8 C2 -33.31(11) . . . . ? B5 B4 B8 C2 58.43(15) . . . . ? B9 B4 B8 C2 97.88(13) . . . . ? B1 B4 B8 C2 -4.46(15) . . . . ? C1 B4 B8 B7 -94.26(13) . . . . ? B5 B4 B8 B7 -2.53(17) . . . . ? B9 B4 B8 B7 36.93(12) . . . . ? B1 B4 B8 B7 -65.42(15) . . . . ? C1 B4 B8 B9 -131.19(13) . . . . ? B5 B4 B8 B9 -39.46(12) . . . . ? B1 B4 B8 B9 -102.35(14) . . . . ? C2 B7 B8 C1 32.69(10) . . . . ? B6 B7 B8 C1 -59.07(15) . . . . ? B9 B7 B8 C1 -98.25(13) . . . . ? B3 B7 B8 C1 3.83(15) . . . . ? B6 B7 B8 C2 -91.76(13) . . . . ? B9 B7 B8 C2 -130.94(13) . . . . ? B3 B7 B8 C2 -28.86(11) . . . . ? C2 B7 B8 B4 93.90(14) . . . . ? B6 B7 B8 B4 2.14(16) . . . . ? B9 B7 B8 B4 -37.04(12) . . . . ? B3 B7 B8 B4 65.04(15) . . . . ? C2 B7 B8 B9 130.94(13) . . . . ? B6 B7 B8 B9 39.18(12) . . . . ? B3 B7 B8 B9 102.07(13) . . . . ? C2 B7 B9 B4 -5.00(16) . . . . ? B6 B7 B9 B4 -100.05(14) . . . . ? B8 B7 B9 B4 37.03(13) . . . . ? B3 B7 B9 B4 -62.06(16) . . . . ? C2 B7 B9 B8 -42.02(11) . . . . ? B6 B7 B9 B8 -137.08(13) . . . . ? B3 B7 B9 B8 -99.09(14) . . . . ? C2 B7 B9 B6 95.05(13) . . . . ? B8 B7 B9 B6 137.08(13) . . . . ? B3 B7 B9 B6 37.99(12) . . . . ? C2 B7 B9 B5 57.36(15) . . . . ? B6 B7 B9 B5 -37.69(12) . . . . ? B8 B7 B9 B5 99.39(14) . . . . ? B3 B7 B9 B5 0.30(17) . . . . ? C1 B4 B9 B7 4.52(17) . . . . ? B5 B4 B9 B7 99.57(14) . . . . ? B8 B4 B9 B7 -37.14(12) . . . . ? B1 B4 B9 B7 61.61(16) . . . . ? C1 B4 B9 B8 41.67(12) . . . . ? B5 B4 B9 B8 136.72(13) . . . . ? B1 B4 B9 B8 98.75(13) . . . . ? C1 B4 B9 B6 -57.85(16) . . . . ? B5 B4 B9 B6 37.20(12) . . . . ? B8 B4 B9 B6 -99.52(13) . . . . ? B1 B4 B9 B6 -0.77(17) . . . . ? C1 B4 B9 B5 -95.05(14) . . . . ? B8 B4 B9 B5 -136.72(13) . . . . ? B1 B4 B9 B5 -37.97(12) . . . . ? C1 B8 B9 B7 97.02(13) . . . . ? C2 B8 B9 B7 41.55(12) . . . . ? B4 B8 B9 B7 138.57(14) . . . . ? C1 B8 B9 B4 -41.55(12) . . . . ? C2 B8 B9 B4 -97.02(13) . . . . ? B7 B8 B9 B4 -138.57(14) . . . . ? C1 B8 B9 B6 59.43(15) . . . . ? C2 B8 B9 B6 3.96(16) . . . . ? B4 B8 B9 B6 100.98(14) . . . . ? B7 B8 B9 B6 -37.59(12) . . . . ? C1 B8 B9 B5 -3.72(16) . . . . ? C2 B8 B9 B5 -59.19(15) . . . . ? B4 B8 B9 B5 37.83(12) . . . . ? B7 B8 B9 B5 -100.74(14) . . . . ? B3 B6 B9 B7 -38.46(12) . . . . ? B2 B6 B9 B7 -104.34(14) . . . . ? B5 B6 B9 B7 -137.72(13) . . . . ? B7 B6 B9 B4 101.01(14) . . . . ? B3 B6 B9 B4 62.55(16) . . . . ? B2 B6 B9 B4 -3.33(17) . . . . ? B5 B6 B9 B4 -36.70(12) . . . . ? B7 B6 B9 B8 38.07(12) . . . . ? B3 B6 B9 B8 -0.39(17) . . . . ? B2 B6 B9 B8 -66.27(16) . . . . ? B5 B6 B9 B8 -99.65(14) . . . . ? B7 B6 B9 B5 137.72(13) . . . . ? B3 B6 B9 B5 99.25(13) . . . . ? B2 B6 B9 B5 33.38(12) . . . . ? B4 B5 B9 B7 -101.25(14) . . . . ? B1 B5 B9 B7 -62.73(16) . . . . ? B2 B5 B9 B7 3.93(17) . . . . ? B6 B5 B9 B7 37.16(12) . . . . ? B1 B5 B9 B4 38.52(12) . . . . ? B2 B5 B9 B4 105.18(14) . . . . ? B6 B5 B9 B4 138.41(13) . . . . ? B4 B5 B9 B8 -38.17(12) . . . . ? B1 B5 B9 B8 0.36(17) . . . . ? B2 B5 B9 B8 67.02(16) . . . . ? B6 B5 B9 B8 100.25(13) . . . . ? B4 B5 B9 B6 -138.41(13) . . . . ? B1 B5 B9 B6 -99.89(13) . . . . ? B2 B5 B9 B6 -33.23(12) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.355 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.052 _publ_section_references ; Bruker (1998a). SAINTPlus. Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; data_posl_2 _database_code_depnum_ccdc_archive 'CCDC 227518' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1,2-Bis(trifluoromethanesulfonyl)-o-carborane _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H14 B10 F6 O6 S2' _chemical_formula_weight 468.39 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 6.8212(14) _cell_length_b 26.485(5) _cell_length_c 10.634(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.37(3) _cell_angle_gamma 90.00 _cell_volume 1905.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Rebuild Syntex P2~1~/Siemens P3 four-circle diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6818 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3709 _reflns_number_gt 3290 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens P3/PC (Siemens, 1989)' _computing_cell_refinement 'Siemens P3/PC (Siemens, 1989)' _computing_data_reduction 'Siemens P3/PC (Siemens, 1989)' _computing_structure_solution 'SHELXTL PLUS 5 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL PLUS 5 (Sheldrick, 1998)' _computing_molecular_graphics 'SHELXTL PLUS 5 (Sheldrick, 1998)' _computing_publication_material 'SHELXTL PLUS 5 (Sheldrick, 1998)' _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^)+(0.0733P)^2^+0.8047P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3709 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 S1 S 0.28682(7) 0.37187(2) 0.64782(5) 0.03132(16) Uani 1 1 d . . . S2 S 0.28870(7) 0.498245(15) 0.32344(4) 0.02340(14) Uani 1 1 d . . . F1 F 0.3456(3) 0.38667(8) 0.89022(14) 0.0709(6) Uani 1 1 d . . . F2 F 0.0621(2) 0.35452(8) 0.82096(14) 0.0610(5) Uani 1 1 d . . . F3 F 0.3239(3) 0.30876(7) 0.83613(16) 0.0688(5) Uani 1 1 d . . . F4 F 0.3029(3) 0.49340(8) 0.08029(14) 0.0677(5) Uani 1 1 d . . . F5 F 0.0288(2) 0.52116(6) 0.13140(13) 0.0518(4) Uani 1 1 d . . . F6 F 0.2861(3) 0.56845(6) 0.15580(16) 0.0649(5) Uani 1 1 d . . . O1 O 0.1413(2) 0.33434(5) 0.57213(13) 0.0318(3) Uani 1 1 d . . . O2 O 0.2168(3) 0.42211(6) 0.63072(19) 0.0521(5) Uani 1 1 d . . . O3 O 0.4798(2) 0.35868(9) 0.62989(16) 0.0546(5) Uani 1 1 d . . . O4 O 0.1890(2) 0.44514(5) 0.31277(13) 0.0277(3) Uani 1 1 d . . . O5 O 0.4948(2) 0.49070(5) 0.33892(16) 0.0384(4) Uani 1 1 d . . . O6 O 0.1934(2) 0.53026(5) 0.40310(14) 0.0346(3) Uani 1 1 d . . . C1 C -0.1099(3) 0.34026(6) 0.38887(16) 0.0190(3) Uani 1 1 d . . . C2 C -0.0849(3) 0.38808(6) 0.28781(16) 0.0201(3) Uani 1 1 d . . . C13 C -0.0643(3) 0.34814(7) 0.53017(16) 0.0225(4) Uani 1 1 d . . . C14 C 0.2526(4) 0.35447(11) 0.8098(2) 0.0442(6) Uani 1 1 d . . . C15 C -0.0152(3) 0.43911(7) 0.33921(18) 0.0255(4) Uani 1 1 d . . . C16 C 0.2225(3) 0.52146(9) 0.1617(2) 0.0387(5) Uani 1 1 d . . . B3 B 0.0801(3) 0.33851(7) 0.29645(19) 0.0215(4) Uani 1 1 d . . . B4 B -0.0633(3) 0.28402(7) 0.32209(19) 0.0242(4) Uani 1 1 d . . . B5 B -0.3102(3) 0.30393(8) 0.33416(19) 0.0239(4) Uani 1 1 d . . . B6 B -0.3189(3) 0.37087(7) 0.31739(19) 0.0225(4) Uani 1 1 d . . . B7 B -0.0199(3) 0.36583(8) 0.14860(19) 0.0241(4) Uani 1 1 d . . . B8 B -0.0082(3) 0.29906(8) 0.1675(2) 0.0255(4) Uani 1 1 d . . . B9 B -0.2505(3) 0.27771(9) 0.1901(2) 0.0285(4) Uani 1 1 d . . . B10 B -0.4100(3) 0.33141(9) 0.1878(2) 0.0271(4) Uani 1 1 d . . . B11 B -0.2671(3) 0.38529(8) 0.16117(19) 0.0258(4) Uani 1 1 d . . . B12 B -0.2237(3) 0.32805(9) 0.0833(2) 0.0277(4) Uani 1 1 d . . . H3 H 0.232(3) 0.3455(8) 0.344(2) 0.024(5) Uiso 1 1 d . . . H4 H 0.010(3) 0.2546(9) 0.388(2) 0.032(6) Uiso 1 1 d . . . H5 H -0.384(3) 0.2877(9) 0.410(2) 0.034(6) Uiso 1 1 d . . . H6 H -0.392(3) 0.3954(8) 0.375(2) 0.026(5) Uiso 1 1 d . . . H7 H 0.078(4) 0.3879(9) 0.102(2) 0.038(6) Uiso 1 1 d . . . H8 H 0.092(3) 0.2777(9) 0.123(2) 0.035(6) Uiso 1 1 d . . . H9 H -0.302(4) 0.2403(10) 0.157(2) 0.041(7) Uiso 1 1 d . . . H10 H -0.556(4) 0.3291(9) 0.160(2) 0.037(6) Uiso 1 1 d . . . H11 H -0.313(4) 0.4189(10) 0.123(3) 0.043(7) Uiso 1 1 d . . . H12 H -0.267(4) 0.3241(9) -0.022(2) 0.035(6) Uiso 1 1 d . . . H13A H -0.133(3) 0.3250(9) 0.570(2) 0.024(5) Uiso 1 1 d . . . H13B H -0.089(4) 0.3806(10) 0.554(2) 0.036(6) Uiso 1 1 d . . . H15A H -0.017(3) 0.4409(9) 0.427(2) 0.033(6) Uiso 1 1 d . . . H15B H -0.097(3) 0.4648(8) 0.294(2) 0.021(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 S1 0.0266(3) 0.0404(3) 0.0256(3) 0.00239(19) -0.00180(19) -0.00561(19) S2 0.0307(3) 0.0155(2) 0.0225(2) -0.00156(15) -0.00196(17) -0.00293(16) F1 0.0665(11) 0.1093(15) 0.0344(8) -0.0245(8) -0.0032(7) -0.0344(10) F2 0.0429(8) 0.1063(14) 0.0353(8) -0.0071(8) 0.0107(6) -0.0197(8) F3 0.0718(11) 0.0729(11) 0.0553(10) 0.0314(9) -0.0164(8) -0.0095(9) F4 0.0791(12) 0.0964(14) 0.0308(7) -0.0092(8) 0.0194(7) -0.0089(10) F5 0.0498(8) 0.0650(9) 0.0356(7) 0.0159(6) -0.0140(6) -0.0085(7) F6 0.0828(12) 0.0510(9) 0.0570(9) 0.0295(7) -0.0066(8) -0.0285(8) O1 0.0359(8) 0.0285(7) 0.0277(7) -0.0041(5) -0.0085(6) 0.0058(6) O2 0.0522(10) 0.0305(8) 0.0670(12) 0.0057(8) -0.0172(8) -0.0128(7) O3 0.0299(9) 0.0948(15) 0.0385(9) -0.0016(9) 0.0021(7) 0.0005(9) O4 0.0318(7) 0.0155(6) 0.0362(7) -0.0037(5) 0.0065(6) -0.0036(5) O5 0.0307(8) 0.0262(7) 0.0560(9) -0.0027(6) -0.0032(7) -0.0041(6) O6 0.0500(9) 0.0223(7) 0.0316(7) -0.0082(5) 0.0062(6) -0.0014(6) C1 0.0231(8) 0.0141(7) 0.0195(8) -0.0001(6) 0.0009(6) -0.0004(6) C2 0.0249(8) 0.0167(8) 0.0191(8) 0.0013(6) 0.0038(6) 0.0015(6) C13 0.0267(9) 0.0210(8) 0.0192(8) -0.0004(6) 0.0013(7) -0.0019(7) C14 0.0379(12) 0.0678(16) 0.0252(10) -0.0037(10) -0.0023(9) -0.0172(11) C15 0.0327(10) 0.0176(8) 0.0275(9) -0.0010(7) 0.0087(7) -0.0015(7) C16 0.0461(12) 0.0416(12) 0.0274(10) 0.0064(9) 0.0011(9) -0.0127(10) B3 0.0223(9) 0.0185(9) 0.0232(9) -0.0031(7) 0.0013(7) 0.0003(7) B4 0.0289(10) 0.0165(9) 0.0266(10) -0.0044(7) 0.0012(8) 0.0010(8) B5 0.0256(10) 0.0212(9) 0.0240(9) -0.0034(7) 0.0001(7) -0.0045(8) B6 0.0225(9) 0.0229(9) 0.0219(9) 0.0004(7) 0.0022(7) 0.0028(7) B7 0.0276(10) 0.0265(10) 0.0182(9) -0.0021(7) 0.0033(7) 0.0001(8) B8 0.0264(10) 0.0249(10) 0.0250(10) -0.0089(8) 0.0030(8) -0.0011(8) B9 0.0294(10) 0.0287(11) 0.0266(10) -0.0100(8) 0.0004(8) -0.0053(8) B10 0.0218(10) 0.0365(11) 0.0223(9) -0.0027(8) -0.0004(7) -0.0015(8) B11 0.0270(10) 0.0305(11) 0.0189(9) 0.0031(8) -0.0002(8) 0.0046(8) B12 0.0258(10) 0.0360(11) 0.0203(9) -0.0057(8) -0.0004(7) -0.0023(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 S1 O3 1.3986(18) . ? S1 O2 1.4176(18) . ? S1 O1 1.5546(14) . ? S1 C14 1.827(2) . ? S2 O5 1.4089(16) . ? S2 O6 1.4142(15) . ? S2 O4 1.5601(13) . ? S2 C16 1.828(2) . ? F1 C14 1.312(3) . ? F2 C14 1.320(3) . ? F3 C14 1.321(3) . ? F4 C16 1.313(3) . ? F5 C16 1.320(3) . ? F6 C16 1.322(3) . ? O1 C13 1.463(2) . ? O4 C15 1.465(2) . ? C1 C13 1.509(2) . ? C1 C2 1.684(2) . ? C1 B4 1.698(2) . ? C1 B5 1.711(2) . ? C1 B3 1.725(3) . ? C1 B6 1.729(3) . ? C2 C15 1.511(2) . ? C2 B7 1.704(3) . ? C2 B11 1.713(3) . ? C2 B3 1.724(2) . ? C2 B6 1.727(3) . ? B3 B8 1.767(3) . ? B3 B4 1.784(3) . ? B3 B7 1.785(3) . ? B4 B8 1.778(3) . ? B4 B9 1.780(3) . ? B4 B5 1.785(3) . ? B5 B10 1.773(3) . ? B5 B9 1.776(3) . ? B5 B6 1.782(3) . ? B6 B10 1.777(3) . ? B6 B11 1.784(3) . ? B7 B12 1.780(3) . ? B7 B8 1.781(3) . ? B7 B11 1.784(3) . ? B8 B9 1.792(3) . ? B8 B12 1.793(3) . ? B9 B12 1.776(3) . ? B9 B10 1.789(3) . ? B10 B11 1.771(3) . ? B10 B12 1.795(3) . ? B11 B12 1.771(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 O3 S1 O2 121.64(13) . . ? O3 S1 O1 108.64(11) . . ? O2 S1 O1 110.57(9) . . ? O3 S1 C14 107.57(12) . . ? O2 S1 C14 106.02(13) . . ? O1 S1 C14 100.17(10) . . ? O5 S2 O6 122.92(10) . . ? O5 S2 O4 107.45(8) . . ? O6 S2 O4 110.76(8) . . ? O5 S2 C16 106.25(11) . . ? O6 S2 C16 106.56(10) . . ? O4 S2 C16 100.49(9) . . ? C13 O1 S1 121.46(12) . . ? C15 O4 S2 120.05(11) . . ? C13 C1 C2 120.44(13) . . ? C13 C1 B4 120.79(14) . . ? C2 C1 B4 110.69(13) . . ? C13 C1 B5 118.02(15) . . ? C2 C1 B5 110.36(13) . . ? B4 C1 B5 63.17(11) . . ? C13 C1 B3 119.80(14) . . ? C2 C1 B3 60.76(10) . . ? B4 C1 B3 62.82(11) . . ? B5 C1 B3 114.64(13) . . ? C13 C1 B6 115.20(14) . . ? C2 C1 B6 60.80(10) . . ? B4 C1 B6 114.56(13) . . ? B5 C1 B6 62.40(11) . . ? B3 C1 B6 113.56(13) . . ? C15 C2 C1 119.65(14) . . ? C15 C2 B7 121.24(15) . . ? C1 C2 B7 110.69(13) . . ? C15 C2 B11 119.06(15) . . ? C1 C2 B11 110.27(13) . . ? B7 C2 B11 62.96(12) . . ? C15 C2 B3 119.26(15) . . ? C1 C2 B3 60.80(10) . . ? B7 C2 B3 62.75(11) . . ? B11 C2 B3 114.32(13) . . ? C15 C2 B6 115.16(14) . . ? C1 C2 B6 60.90(10) . . ? B7 C2 B6 114.60(14) . . ? B11 C2 B6 62.45(12) . . ? B3 C2 B6 113.68(13) . . ? O1 C13 C1 109.64(15) . . ? F1 C14 F2 109.9(2) . . ? F1 C14 F3 108.9(2) . . ? F2 C14 F3 108.8(2) . . ? F1 C14 S1 109.92(17) . . ? F2 C14 S1 109.30(16) . . ? F3 C14 S1 110.04(18) . . ? O4 C15 C2 106.90(14) . . ? F4 C16 F5 109.02(19) . . ? F4 C16 F6 109.5(2) . . ? F5 C16 F6 108.6(2) . . ? F4 C16 S2 110.87(17) . . ? F5 C16 S2 110.25(14) . . ? F6 C16 S2 108.55(15) . . ? C2 B3 C1 58.44(10) . . ? C2 B3 B8 104.69(14) . . ? C1 B3 B8 104.57(13) . . ? C2 B3 B4 104.90(14) . . ? C1 B3 B4 57.84(10) . . ? B8 B3 B4 60.08(11) . . ? C2 B3 B7 58.07(10) . . ? C1 B3 B7 105.10(14) . . ? B8 B3 B7 60.17(12) . . ? B4 B3 B7 107.90(14) . . ? C1 B4 B8 105.27(14) . . ? C1 B4 B9 104.96(14) . . ? B8 B4 B9 60.49(12) . . ? C1 B4 B3 59.34(11) . . ? B8 B4 B3 59.49(11) . . ? B9 B4 B3 107.91(15) . . ? C1 B4 B5 58.78(11) . . ? B8 B4 B5 108.28(15) . . ? B9 B4 B5 59.75(12) . . ? B3 B4 B5 108.24(14) . . ? C1 B5 B10 105.51(14) . . ? C1 B5 B9 104.57(14) . . ? B10 B5 B9 60.54(12) . . ? C1 B5 B6 59.30(10) . . ? B10 B5 B6 59.97(12) . . ? B9 B5 B6 108.12(15) . . ? C1 B5 B4 58.05(10) . . ? B10 B5 B4 108.52(14) . . ? B9 B5 B4 59.98(12) . . ? B6 B5 B4 107.83(14) . . ? C2 B6 C1 58.30(10) . . ? C2 B6 B10 104.68(14) . . ? C1 B6 B10 104.58(14) . . ? C2 B6 B5 105.13(13) . . ? C1 B6 B5 58.30(10) . . ? B10 B6 B5 59.75(12) . . ? C2 B6 B11 58.37(11) . . ? C1 B6 B11 105.01(14) . . ? B10 B6 B11 59.67(12) . . ? B5 B6 B11 107.34(14) . . ? C2 B7 B12 104.86(14) . . ? C2 B7 B8 104.97(14) . . ? B12 B7 B8 60.48(12) . . ? C2 B7 B11 58.76(11) . . ? B12 B7 B11 59.57(12) . . ? B8 B7 B11 107.91(15) . . ? C2 B7 B3 59.18(11) . . ? B12 B7 B3 107.88(15) . . ? B8 B7 B3 59.42(11) . . ? B11 B7 B3 108.02(14) . . ? B3 B8 B4 60.43(11) . . ? B3 B8 B7 60.42(11) . . ? B4 B8 B7 108.38(13) . . ? B3 B8 B9 108.13(14) . . ? B4 B8 B9 59.83(12) . . ? B7 B8 B9 107.44(15) . . ? B3 B8 B12 108.10(14) . . ? B4 B8 B12 107.52(15) . . ? B7 B8 B12 59.75(12) . . ? B9 B8 B12 59.39(12) . . ? B5 B9 B12 108.19(15) . . ? B5 B9 B4 60.27(12) . . ? B12 B9 B4 108.15(15) . . ? B5 B9 B10 59.64(12) . . ? B12 B9 B10 60.46(12) . . ? B4 B9 B10 108.04(14) . . ? B5 B9 B8 108.04(14) . . ? B12 B9 B8 60.33(12) . . ? B4 B9 B8 59.68(12) . . ? B10 B9 B8 108.49(15) . . ? B11 B10 B5 108.29(14) . . ? B11 B10 B6 60.35(12) . . ? B5 B10 B6 60.28(11) . . ? B11 B10 B9 107.23(15) . . ? B5 B10 B9 59.83(12) . . ? B6 B10 B9 107.79(14) . . ? B11 B10 B12 59.53(12) . . ? B5 B10 B12 107.50(15) . . ? B6 B10 B12 107.73(14) . . ? B9 B10 B12 59.41(12) . . ? C2 B11 B12 104.89(14) . . ? C2 B11 B10 105.53(14) . . ? B12 B11 B10 60.90(13) . . ? C2 B11 B6 59.18(11) . . ? B12 B11 B6 108.51(15) . . ? B10 B11 B6 59.97(12) . . ? C2 B11 B7 58.28(11) . . ? B12 B11 B7 60.10(12) . . ? B10 B11 B7 108.92(15) . . ? B6 B11 B7 108.07(14) . . ? B11 B12 B9 107.83(15) . . ? B11 B12 B7 60.33(12) . . ? B9 B12 B7 108.16(14) . . ? B11 B12 B8 107.95(14) . . ? B9 B12 B8 60.28(12) . . ? B7 B12 B8 59.77(12) . . ? B11 B12 B10 59.57(12) . . ? B9 B12 B10 60.12(12) . . ? B7 B12 B10 108.05(14) . . ? B8 B12 B10 108.18(15) . . ? 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 O3 S1 O1 C13 -155.70(15) . . . . ? O2 S1 O1 C13 -19.81(18) . . . . ? C14 S1 O1 C13 91.71(16) . . . . ? O5 S2 O4 C15 159.11(14) . . . . ? O6 S2 O4 C15 22.35(16) . . . . ? C16 S2 O4 C15 -90.00(15) . . . . ? C13 C1 C2 C15 0.3(2) . . . . ? B4 C1 C2 C15 -148.60(15) . . . . ? B5 C1 C2 C15 143.39(15) . . . . ? B3 C1 C2 C15 -109.04(17) . . . . ? B6 C1 C2 C15 104.06(17) . . . . ? C13 C1 C2 B7 148.86(16) . . . . ? B4 C1 C2 B7 -0.07(19) . . . . ? B5 C1 C2 B7 -68.08(17) . . . . ? B3 C1 C2 B7 39.49(13) . . . . ? B6 C1 C2 B7 -107.41(15) . . . . ? C13 C1 C2 B11 -143.39(16) . . . . ? B4 C1 C2 B11 67.68(17) . . . . ? B5 C1 C2 B11 -0.33(18) . . . . ? B3 C1 C2 B11 107.24(15) . . . . ? B6 C1 C2 B11 -39.65(13) . . . . ? C13 C1 C2 B3 109.37(17) . . . . ? B4 C1 C2 B3 -39.56(13) . . . . ? B5 C1 C2 B3 -107.57(14) . . . . ? B6 C1 C2 B3 -146.90(13) . . . . ? C13 C1 C2 B6 -103.73(17) . . . . ? B4 C1 C2 B6 107.34(15) . . . . ? B5 C1 C2 B6 39.33(13) . . . . ? B3 C1 C2 B6 146.90(13) . . . . ? S1 O1 C13 C1 125.34(14) . . . . ? C2 C1 C13 O1 -92.87(18) . . . . ? B4 C1 C13 O1 52.9(2) . . . . ? B5 C1 C13 O1 126.79(16) . . . . ? B3 C1 C13 O1 -21.3(2) . . . . ? B6 C1 C13 O1 -162.45(14) . . . . ? O3 S1 C14 F1 74.7(2) . . . . ? O2 S1 C14 F1 -56.9(2) . . . . ? O1 S1 C14 F1 -171.91(18) . . . . ? O3 S1 C14 F2 -164.62(18) . . . . ? O2 S1 C14 F2 63.8(2) . . . . ? O1 S1 C14 F2 -51.2(2) . . . . ? O3 S1 C14 F3 -45.2(2) . . . . ? O2 S1 C14 F3 -176.79(16) . . . . ? O1 S1 C14 F3 68.19(17) . . . . ? S2 O4 C15 C2 165.22(12) . . . . ? C1 C2 C15 O4 106.59(17) . . . . ? B7 C2 C15 O4 -38.6(2) . . . . ? B11 C2 C15 O4 -112.83(17) . . . . ? B3 C2 C15 O4 35.5(2) . . . . ? B6 C2 C15 O4 176.04(13) . . . . ? O5 S2 C16 F4 48.19(18) . . . . ? O6 S2 C16 F4 -179.17(15) . . . . ? O4 S2 C16 F4 -63.63(17) . . . . ? O5 S2 C16 F5 169.01(16) . . . . ? O6 S2 C16 F5 -58.35(18) . . . . ? O4 S2 C16 F5 57.19(18) . . . . ? O5 S2 C16 F6 -72.18(19) . . . . ? O6 S2 C16 F6 60.45(19) . . . . ? O4 S2 C16 F6 176.00(17) . . . . ? C15 C2 B3 C1 109.67(16) . . . . ? B7 C2 B3 C1 -137.99(14) . . . . ? B11 C2 B3 C1 -100.55(15) . . . . ? B6 C2 B3 C1 -31.40(13) . . . . ? C15 C2 B3 B8 -152.04(15) . . . . ? C1 C2 B3 B8 98.29(14) . . . . ? B7 C2 B3 B8 -39.70(13) . . . . ? B11 C2 B3 B8 -2.26(19) . . . . ? B6 C2 B3 B8 66.89(17) . . . . ? C15 C2 B3 B4 145.59(15) . . . . ? C1 C2 B3 B4 35.93(12) . . . . ? B7 C2 B3 B4 -102.06(15) . . . . ? B11 C2 B3 B4 -64.62(17) . . . . ? B6 C2 B3 B4 4.53(18) . . . . ? C15 C2 B3 B7 -112.34(17) . . . . ? C1 C2 B3 B7 137.99(14) . . . . ? B11 C2 B3 B7 37.44(14) . . . . ? B6 C2 B3 B7 106.59(15) . . . . ? C13 C1 B3 C2 -110.39(16) . . . . ? B4 C1 B3 C2 137.95(14) . . . . ? B5 C1 B3 C2 100.48(15) . . . . ? B6 C1 B3 C2 31.34(13) . . . . ? C13 C1 B3 B8 151.11(15) . . . . ? C2 C1 B3 B8 -98.50(14) . . . . ? B4 C1 B3 B8 39.45(13) . . . . ? B5 C1 B3 B8 1.98(18) . . . . ? B6 C1 B3 B8 -67.16(17) . . . . ? C13 C1 B3 B4 111.66(17) . . . . ? C2 C1 B3 B4 -137.95(14) . . . . ? B5 C1 B3 B4 -37.47(14) . . . . ? B6 C1 B3 B4 -106.61(15) . . . . ? C13 C1 B3 B7 -146.43(15) . . . . ? C2 C1 B3 B7 -36.04(12) . . . . ? B4 C1 B3 B7 101.91(14) . . . . ? B5 C1 B3 B7 64.45(17) . . . . ? B6 C1 B3 B7 -4.70(17) . . . . ? C13 C1 B4 B8 -149.46(16) . . . . ? C2 C1 B4 B8 -0.65(18) . . . . ? B5 C1 B4 B8 102.40(15) . . . . ? B3 C1 B4 B8 -39.32(13) . . . . ? B6 C1 B4 B8 65.72(18) . . . . ? C13 C1 B4 B9 147.65(16) . . . . ? C2 C1 B4 B9 -63.55(17) . . . . ? B5 C1 B4 B9 39.50(14) . . . . ? B3 C1 B4 B9 -102.21(15) . . . . ? B6 C1 B4 B9 2.82(19) . . . . ? C13 C1 B4 B3 -110.14(18) . . . . ? C2 C1 B4 B3 38.66(13) . . . . ? B5 C1 B4 B3 141.71(14) . . . . ? B6 C1 B4 B3 105.03(15) . . . . ? C13 C1 B4 B5 108.15(18) . . . . ? C2 C1 B4 B5 -103.05(15) . . . . ? B3 C1 B4 B5 -141.71(14) . . . . ? B6 C1 B4 B5 -36.68(14) . . . . ? C2 B3 B4 C1 -36.20(12) . . . . ? B8 B3 B4 C1 -134.81(14) . . . . ? B7 B3 B4 C1 -96.91(14) . . . . ? C2 B3 B4 B8 98.61(14) . . . . ? C1 B3 B4 B8 134.81(14) . . . . ? B7 B3 B4 B8 37.90(13) . . . . ? C2 B3 B4 B9 60.91(17) . . . . ? C1 B3 B4 B9 97.11(15) . . . . ? B8 B3 B4 B9 -37.70(14) . . . . ? B7 B3 B4 B9 0.20(19) . . . . ? C2 B3 B4 B5 -2.29(17) . . . . ? C1 B3 B4 B5 33.91(12) . . . . ? B8 B3 B4 B5 -100.90(16) . . . . ? B7 B3 B4 B5 -63.00(17) . . . . ? C13 C1 B5 B10 145.18(15) . . . . ? C2 C1 B5 B10 1.12(17) . . . . ? B4 C1 B5 B10 -102.44(15) . . . . ? B3 C1 B5 B10 -65.11(17) . . . . ? B6 C1 B5 B10 39.75(13) . . . . ? C13 C1 B5 B9 -151.90(15) . . . . ? C2 C1 B5 B9 64.04(16) . . . . ? B4 C1 B5 B9 -39.52(14) . . . . ? B3 C1 B5 B9 -2.20(19) . . . . ? B6 C1 B5 B9 102.67(15) . . . . ? C13 C1 B5 B6 105.43(16) . . . . ? C2 C1 B5 B6 -38.63(13) . . . . ? B4 C1 B5 B6 -142.19(14) . . . . ? B3 C1 B5 B6 -104.86(15) . . . . ? C13 C1 B5 B4 -112.38(16) . . . . ? C2 C1 B5 B4 103.56(14) . . . . ? B3 C1 B5 B4 37.33(14) . . . . ? B6 C1 B5 B4 142.19(14) . . . . ? B8 B4 B5 C1 -97.13(15) . . . . ? B9 B4 B5 C1 -134.65(15) . . . . ? B3 B4 B5 C1 -34.14(12) . . . . ? C1 B4 B5 B10 97.09(15) . . . . ? B8 B4 B5 B10 -0.03(18) . . . . ? B9 B4 B5 B10 -37.56(14) . . . . ? B3 B4 B5 B10 62.96(17) . . . . ? C1 B4 B5 B9 134.65(15) . . . . ? B8 B4 B5 B9 37.53(14) . . . . ? B3 B4 B5 B9 100.52(16) . . . . ? C1 B4 B5 B6 33.62(13) . . . . ? B8 B4 B5 B6 -63.50(17) . . . . ? B9 B4 B5 B6 -101.03(16) . . . . ? B3 B4 B5 B6 -0.51(18) . . . . ? C15 C2 B6 C1 -111.35(16) . . . . ? B7 C2 B6 C1 100.94(15) . . . . ? B11 C2 B6 C1 137.53(14) . . . . ? B3 C2 B6 C1 31.37(13) . . . . ? C15 C2 B6 B10 150.36(15) . . . . ? C1 C2 B6 B10 -98.28(14) . . . . ? B7 C2 B6 B10 2.66(18) . . . . ? B11 C2 B6 B10 39.25(13) . . . . ? B3 C2 B6 B10 -66.91(17) . . . . ? C15 C2 B6 B5 -147.58(15) . . . . ? C1 C2 B6 B5 -36.22(12) . . . . ? B7 C2 B6 B5 64.72(17) . . . . ? B11 C2 B6 B5 101.31(15) . . . . ? B3 C2 B6 B5 -4.85(18) . . . . ? C15 C2 B6 B11 111.11(16) . . . . ? C1 C2 B6 B11 -137.53(14) . . . . ? B7 C2 B6 B11 -36.60(14) . . . . ? B3 C2 B6 B11 -106.16(15) . . . . ? C13 C1 B6 C2 112.23(15) . . . . ? B4 C1 B6 C2 -100.92(15) . . . . ? B5 C1 B6 C2 -137.90(14) . . . . ? B3 C1 B6 C2 -31.32(13) . . . . ? C13 C1 B6 B10 -149.30(15) . . . . ? C2 C1 B6 B10 98.46(14) . . . . ? B4 C1 B6 B10 -2.46(19) . . . . ? B5 C1 B6 B10 -39.44(13) . . . . ? B3 C1 B6 B10 67.14(17) . . . . ? C13 C1 B6 B5 -109.87(16) . . . . ? C2 C1 B6 B5 137.90(14) . . . . ? B4 C1 B6 B5 36.97(14) . . . . ? B3 C1 B6 B5 106.57(15) . . . . ? C13 C1 B6 B11 148.76(15) . . . . ? C2 C1 B6 B11 36.52(12) . . . . ? B4 C1 B6 B11 -64.40(17) . . . . ? B5 C1 B6 B11 -101.37(15) . . . . ? B3 C1 B6 B11 5.20(18) . . . . ? C1 B5 B6 C2 36.22(12) . . . . ? B10 B5 B6 C2 -98.41(15) . . . . ? B9 B5 B6 C2 -60.30(17) . . . . ? B4 B5 B6 C2 3.10(18) . . . . ? B10 B5 B6 C1 -134.63(14) . . . . ? B9 B5 B6 C1 -96.53(15) . . . . ? B4 B5 B6 C1 -33.12(12) . . . . ? C1 B5 B6 B10 134.63(14) . . . . ? B9 B5 B6 B10 38.11(14) . . . . ? B4 B5 B6 B10 101.51(15) . . . . ? C1 B5 B6 B11 97.23(15) . . . . ? B10 B5 B6 B11 -37.40(14) . . . . ? B9 B5 B6 B11 0.71(19) . . . . ? B4 B5 B6 B11 64.11(17) . . . . ? C15 C2 B7 B12 -148.47(16) . . . . ? C1 C2 B7 B12 63.58(17) . . . . ? B11 C2 B7 B12 -39.32(14) . . . . ? B3 C2 B7 B12 102.22(15) . . . . ? B6 C2 B7 B12 -2.91(19) . . . . ? C15 C2 B7 B8 148.71(16) . . . . ? C1 C2 B7 B8 0.76(18) . . . . ? B11 C2 B7 B8 -102.13(15) . . . . ? B3 C2 B7 B8 39.40(13) . . . . ? B6 C2 B7 B8 -65.73(17) . . . . ? C15 C2 B7 B11 -109.15(18) . . . . ? C1 C2 B7 B11 102.89(15) . . . . ? B3 C2 B7 B11 141.54(14) . . . . ? B6 C2 B7 B11 36.40(14) . . . . ? C15 C2 B7 B3 109.31(18) . . . . ? C1 C2 B7 B3 -38.64(13) . . . . ? B11 C2 B7 B3 -141.54(14) . . . . ? B6 C2 B7 B3 -105.13(15) . . . . ? C1 B3 B7 C2 36.20(12) . . . . ? B8 B3 B7 C2 134.58(15) . . . . ? B4 B3 B7 C2 96.72(15) . . . . ? C2 B3 B7 B12 -96.97(15) . . . . ? C1 B3 B7 B12 -60.76(16) . . . . ? B8 B3 B7 B12 37.61(14) . . . . ? B4 B3 B7 B12 -0.24(18) . . . . ? C2 B3 B7 B8 -134.58(15) . . . . ? C1 B3 B7 B8 -98.38(14) . . . . ? B4 B3 B7 B8 -37.86(13) . . . . ? C2 B3 B7 B11 -34.01(13) . . . . ? C1 B3 B7 B11 2.20(17) . . . . ? B8 B3 B7 B11 100.57(16) . . . . ? B4 B3 B7 B11 62.71(17) . . . . ? C2 B3 B8 B4 -98.96(15) . . . . ? C1 B3 B8 B4 -38.36(13) . . . . ? B7 B3 B8 B4 -137.64(15) . . . . ? C2 B3 B8 B7 38.68(13) . . . . ? C1 B3 B8 B7 99.28(14) . . . . ? B4 B3 B8 B7 137.64(15) . . . . ? C2 B3 B8 B9 -61.50(18) . . . . ? C1 B3 B8 B9 -0.90(18) . . . . ? B4 B3 B8 B9 37.46(14) . . . . ? B7 B3 B8 B9 -100.18(16) . . . . ? C2 B3 B8 B12 1.33(18) . . . . ? C1 B3 B8 B12 61.93(17) . . . . ? B4 B3 B8 B12 100.29(16) . . . . ? B7 B3 B8 B12 -37.35(14) . . . . ? C1 B4 B8 B3 39.24(13) . . . . ? B9 B4 B8 B3 138.04(15) . . . . ? B5 B4 B8 B3 100.83(15) . . . . ? C1 B4 B8 B7 1.11(19) . . . . ? B9 B4 B8 B7 99.91(16) . . . . ? B3 B4 B8 B7 -38.13(14) . . . . ? B5 B4 B8 B7 62.70(17) . . . . ? C1 B4 B8 B9 -98.80(15) . . . . ? B3 B4 B8 B9 -138.04(15) . . . . ? B5 B4 B8 B9 -37.21(13) . . . . ? C1 B4 B8 B12 -62.03(17) . . . . ? B9 B4 B8 B12 36.77(14) . . . . ? B3 B4 B8 B12 -101.27(15) . . . . ? B5 B4 B8 B12 -0.44(18) . . . . ? C2 B7 B8 B3 -39.29(13) . . . . ? B12 B7 B8 B3 -138.12(15) . . . . ? B11 B7 B8 B3 -100.75(15) . . . . ? C2 B7 B8 B4 -1.15(19) . . . . ? B12 B7 B8 B4 -99.98(16) . . . . ? B11 B7 B8 B4 -62.61(18) . . . . ? B3 B7 B8 B4 38.14(14) . . . . ? C2 B7 B8 B9 62.06(17) . . . . ? B12 B7 B8 B9 -36.78(13) . . . . ? B11 B7 B8 B9 0.60(18) . . . . ? B3 B7 B8 B9 101.35(15) . . . . ? C2 B7 B8 B12 98.84(15) . . . . ? B11 B7 B8 B12 37.37(13) . . . . ? B3 B7 B8 B12 138.12(15) . . . . ? C1 B5 B9 B12 -62.36(17) . . . . ? B10 B5 B9 B12 37.46(14) . . . . ? B6 B5 B9 B12 -0.40(19) . . . . ? B4 B5 B9 B12 -100.95(16) . . . . ? C1 B5 B9 B4 38.59(13) . . . . ? B10 B5 B9 B4 138.40(15) . . . . ? B6 B5 B9 B4 100.55(15) . . . . ? C1 B5 B9 B10 -99.82(15) . . . . ? B6 B5 B9 B10 -37.85(14) . . . . ? B4 B5 B9 B10 -138.40(15) . . . . ? C1 B5 B9 B8 1.47(19) . . . . ? B10 B5 B9 B8 101.29(17) . . . . ? B6 B5 B9 B8 63.44(19) . . . . ? B4 B5 B9 B8 -37.11(14) . . . . ? C1 B4 B9 B5 -39.03(13) . . . . ? B8 B4 B9 B5 -138.35(15) . . . . ? B3 B4 B9 B5 -101.09(15) . . . . ? C1 B4 B9 B12 61.99(18) . . . . ? B8 B4 B9 B12 -37.33(14) . . . . ? B3 B4 B9 B12 -0.08(19) . . . . ? B5 B4 B9 B12 101.01(16) . . . . ? C1 B4 B9 B10 -1.98(19) . . . . ? B8 B4 B9 B10 -101.30(16) . . . . ? B3 B4 B9 B10 -64.05(18) . . . . ? B5 B4 B9 B10 37.04(14) . . . . ? C1 B4 B9 B8 99.32(15) . . . . ? B3 B4 B9 B8 37.25(13) . . . . ? B5 B4 B9 B8 138.35(15) . . . . ? B3 B8 B9 B5 -0.4(2) . . . . ? B4 B8 B9 B5 37.37(14) . . . . ? B7 B8 B9 B5 -64.15(18) . . . . ? B12 B8 B9 B5 -101.08(16) . . . . ? B3 B8 B9 B12 100.72(16) . . . . ? B4 B8 B9 B12 138.45(15) . . . . ? B7 B8 B9 B12 36.93(13) . . . . ? B3 B8 B9 B4 -37.73(14) . . . . ? B7 B8 B9 B4 -101.52(15) . . . . ? B12 B8 B9 B4 -138.45(15) . . . . ? B3 B8 B9 B10 62.79(18) . . . . ? B4 B8 B9 B10 100.52(15) . . . . ? B7 B8 B9 B10 -1.00(19) . . . . ? B12 B8 B9 B10 -37.93(14) . . . . ? C1 B5 B10 B11 -1.48(19) . . . . ? B9 B5 B10 B11 -99.71(16) . . . . ? B6 B5 B10 B11 37.94(14) . . . . ? B4 B5 B10 B11 -62.40(18) . . . . ? C1 B5 B10 B6 -39.42(13) . . . . ? B9 B5 B10 B6 -137.65(15) . . . . ? B4 B5 B10 B6 -100.33(15) . . . . ? C1 B5 B10 B9 98.23(15) . . . . ? B6 B5 B10 B9 137.65(15) . . . . ? B4 B5 B10 B9 37.32(14) . . . . ? C1 B5 B10 B12 61.40(18) . . . . ? B9 B5 B10 B12 -36.83(14) . . . . ? B6 B5 B10 B12 100.82(16) . . . . ? B4 B5 B10 B12 0.49(19) . . . . ? C2 B6 B10 B11 -38.62(13) . . . . ? C1 B6 B10 B11 -99.08(15) . . . . ? B5 B6 B10 B11 -137.81(15) . . . . ? C2 B6 B10 B5 99.19(14) . . . . ? C1 B6 B10 B5 38.73(12) . . . . ? B11 B6 B10 B5 137.81(15) . . . . ? C2 B6 B10 B9 61.48(17) . . . . ? C1 B6 B10 B9 1.02(18) . . . . ? B5 B6 B10 B9 -37.71(14) . . . . ? B11 B6 B10 B9 100.10(16) . . . . ? C2 B6 B10 B12 -1.24(18) . . . . ? C1 B6 B10 B12 -61.69(18) . . . . ? B5 B6 B10 B12 -100.42(16) . . . . ? B11 B6 B10 B12 37.38(14) . . . . ? B5 B9 B10 B11 101.53(15) . . . . ? B12 B9 B10 B11 -36.86(13) . . . . ? B4 B9 B10 B11 64.21(18) . . . . ? B8 B9 B10 B11 1.01(19) . . . . ? B12 B9 B10 B5 -138.39(15) . . . . ? B4 B9 B10 B5 -37.32(14) . . . . ? B8 B9 B10 B5 -100.52(15) . . . . ? B5 B9 B10 B6 37.91(14) . . . . ? B12 B9 B10 B6 -100.48(16) . . . . ? B4 B9 B10 B6 0.6(2) . . . . ? B8 B9 B10 B6 -62.61(18) . . . . ? B5 B9 B10 B12 138.39(15) . . . . ? B4 B9 B10 B12 101.07(16) . . . . ? B8 B9 B10 B12 37.87(14) . . . . ? C15 C2 B11 B12 152.06(15) . . . . ? C1 C2 B11 B12 -63.97(17) . . . . ? B7 C2 B11 B12 39.57(14) . . . . ? B3 C2 B11 B12 2.21(19) . . . . ? B6 C2 B11 B12 -102.94(16) . . . . ? C15 C2 B11 B10 -144.58(15) . . . . ? C1 C2 B11 B10 -0.62(18) . . . . ? B7 C2 B11 B10 102.93(16) . . . . ? B3 C2 B11 B10 65.57(18) . . . . ? B6 C2 B11 B10 -39.58(13) . . . . ? C15 C2 B11 B6 -104.99(16) . . . . ? C1 C2 B11 B6 38.97(13) . . . . ? B7 C2 B11 B6 142.51(14) . . . . ? B3 C2 B11 B6 105.15(15) . . . . ? C15 C2 B11 B7 112.49(17) . . . . ? C1 C2 B11 B7 -103.55(14) . . . . ? B3 C2 B11 B7 -37.36(14) . . . . ? B6 C2 B11 B7 -142.51(14) . . . . ? B5 B10 B11 C2 1.30(19) . . . . ? B6 B10 B11 C2 39.20(13) . . . . ? B9 B10 B11 C2 -61.85(17) . . . . ? B12 B10 B11 C2 -98.66(15) . . . . ? B5 B10 B11 B12 99.96(16) . . . . ? B6 B10 B11 B12 137.86(15) . . . . ? B9 B10 B11 B12 36.81(14) . . . . ? B5 B10 B11 B6 -37.90(14) . . . . ? B9 B10 B11 B6 -101.05(15) . . . . ? B12 B10 B11 B6 -137.86(15) . . . . ? B5 B10 B11 B7 62.51(18) . . . . ? B6 B10 B11 B7 100.41(15) . . . . ? B9 B10 B11 B7 -0.64(18) . . . . ? B12 B10 B11 B7 -37.45(13) . . . . ? C1 B6 B11 C2 -36.49(12) . . . . ? B10 B6 B11 C2 -134.84(14) . . . . ? B5 B6 B11 C2 -97.40(14) . . . . ? C2 B6 B11 B12 96.65(15) . . . . ? C1 B6 B11 B12 60.15(17) . . . . ? B10 B6 B11 B12 -38.19(14) . . . . ? B5 B6 B11 B12 -0.76(19) . . . . ? C2 B6 B11 B10 134.84(14) . . . . ? C1 B6 B11 B10 98.34(15) . . . . ? B5 B6 B11 B10 37.43(14) . . . . ? C2 B6 B11 B7 32.99(13) . . . . ? C1 B6 B11 B7 -3.50(18) . . . . ? B10 B6 B11 B7 -101.84(16) . . . . ? B5 B6 B11 B7 -64.41(18) . . . . ? B12 B7 B11 C2 134.75(15) . . . . ? B8 B7 B11 C2 96.97(15) . . . . ? B3 B7 B11 C2 34.18(13) . . . . ? C2 B7 B11 B12 -134.75(15) . . . . ? B8 B7 B11 B12 -37.77(14) . . . . ? B3 B7 B11 B12 -100.57(15) . . . . ? C2 B7 B11 B10 -96.95(15) . . . . ? B12 B7 B11 B10 37.80(14) . . . . ? B8 B7 B11 B10 0.02(18) . . . . ? B3 B7 B11 B10 -62.77(17) . . . . ? C2 B7 B11 B6 -33.35(13) . . . . ? B12 B7 B11 B6 101.40(16) . . . . ? B8 B7 B11 B6 63.63(18) . . . . ? B3 B7 B11 B6 0.83(19) . . . . ? C2 B11 B12 B9 62.47(18) . . . . ? B10 B11 B12 B9 -37.26(14) . . . . ? B6 B11 B12 B9 0.51(19) . . . . ? B7 B11 B12 B9 101.16(16) . . . . ? C2 B11 B12 B7 -38.69(13) . . . . ? B10 B11 B12 B7 -138.43(15) . . . . ? B6 B11 B12 B7 -100.65(15) . . . . ? C2 B11 B12 B8 -1.22(19) . . . . ? B10 B11 B12 B8 -100.95(16) . . . . ? B6 B11 B12 B8 -63.18(18) . . . . ? B7 B11 B12 B8 37.47(14) . . . . ? C2 B11 B12 B10 99.74(15) . . . . ? B6 B11 B12 B10 37.78(14) . . . . ? B7 B11 B12 B10 138.43(15) . . . . ? B5 B9 B12 B11 -0.07(19) . . . . ? B4 B9 B12 B11 -63.86(18) . . . . ? B10 B9 B12 B11 37.02(14) . . . . ? B8 B9 B12 B11 -100.91(15) . . . . ? B5 B9 B12 B7 63.71(18) . . . . ? B4 B9 B12 B7 -0.1(2) . . . . ? B10 B9 B12 B7 100.81(16) . . . . ? B8 B9 B12 B7 -37.12(13) . . . . ? B5 B9 B12 B8 100.84(15) . . . . ? B4 B9 B12 B8 37.05(14) . . . . ? B10 B9 B12 B8 137.93(14) . . . . ? B5 B9 B12 B10 -37.09(14) . . . . ? B4 B9 B12 B10 -100.88(15) . . . . ? B8 B9 B12 B10 -137.93(14) . . . . ? C2 B7 B12 B11 38.92(13) . . . . ? B8 B7 B12 B11 137.95(15) . . . . ? B3 B7 B12 B11 100.80(15) . . . . ? C2 B7 B12 B9 -61.68(18) . . . . ? B8 B7 B12 B9 37.34(14) . . . . ? B11 B7 B12 B9 -100.60(16) . . . . ? B3 B7 B12 B9 0.20(19) . . . . ? C2 B7 B12 B8 -99.02(15) . . . . ? B11 B7 B12 B8 -137.95(15) . . . . ? B3 B7 B12 B8 -37.15(13) . . . . ? C2 B7 B12 B10 1.93(19) . . . . ? B8 B7 B12 B10 100.95(16) . . . . ? B11 B7 B12 B10 -37.00(14) . . . . ? B3 B7 B12 B10 63.80(18) . . . . ? B3 B8 B12 B11 -0.1(2) . . . . ? B4 B8 B12 B11 63.74(18) . . . . ? B7 B8 B12 B11 -37.72(14) . . . . ? B9 B8 B12 B11 100.70(16) . . . . ? B3 B8 B12 B9 -100.78(15) . . . . ? B4 B8 B12 B9 -36.96(13) . . . . ? B7 B8 B12 B9 -138.42(14) . . . . ? B3 B8 B12 B7 37.64(14) . . . . ? B4 B8 B12 B7 101.46(15) . . . . ? B9 B8 B12 B7 138.42(14) . . . . ? B3 B8 B12 B10 -63.08(19) . . . . ? B4 B8 B12 B10 0.74(19) . . . . ? B7 B8 B12 B10 -100.72(16) . . . . ? B9 B8 B12 B10 37.70(14) . . . . ? B5 B10 B12 B11 -101.33(16) . . . . ? B6 B10 B12 B11 -37.75(14) . . . . ? B9 B10 B12 B11 -138.34(15) . . . . ? B11 B10 B12 B9 138.34(15) . . . . ? B5 B10 B12 B9 37.01(14) . . . . ? B6 B10 B12 B9 100.59(16) . . . . ? B11 B10 B12 B7 37.33(14) . . . . ? B5 B10 B12 B7 -64.00(19) . . . . ? B6 B10 B12 B7 -0.4(2) . . . . ? B9 B10 B12 B7 -101.01(16) . . . . ? B11 B10 B12 B8 100.57(15) . . . . ? B5 B10 B12 B8 -0.76(19) . . . . ? B6 B10 B12 B8 62.82(19) . . . . ? B9 B10 B12 B8 -37.77(14) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.396 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.059 _publ_section_references ; Sheldrick G.M. (1998). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. Siemens (1989). P3 and XDISK. Release 4.1. Siemens AXS, Madison, Wisconsin, USA. ; data_posl_3 _database_code_depnum_ccdc_archive 'CCDC 227519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; nido-7,8-(bis(pyridinium)methyl)-7,8-dicarbaundecaboranyl trifluoromethanesulfonate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H24 B9 F3 N2 O3 S' _chemical_formula_weight 466.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 19.400(3) _cell_length_b 8.8993(12) _cell_length_c 12.6404(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2182.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 854 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.63 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker SMART 1000 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 16511 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.00 _reflns_number_total 5764 _reflns_number_gt 4434 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0605P)^2^] 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 refall _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 0.05(7) _refine_ls_number_reflns 5764 _refine_ls_number_parameters 394 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 S1 S 0.35659(3) 0.73592(6) 0.22102(5) 0.02186(13) Uani 1 1 d . . . O1 O 0.32641(10) 0.76270(19) 0.11844(14) 0.0287(4) Uani 1 1 d . . . O2 O 0.30821(10) 0.7223(2) 0.30592(16) 0.0330(4) Uani 1 1 d . . . O3 O 0.41187(9) 0.62780(18) 0.22108(16) 0.0304(4) Uani 1 1 d . . . C1S C 0.40101(13) 0.9121(3) 0.2482(2) 0.0291(6) Uani 1 1 d . . . F1 F 0.44335(11) 0.9494(2) 0.17137(17) 0.0584(6) Uani 1 1 d . . . F2 F 0.43873(9) 0.90259(19) 0.33644(15) 0.0491(5) Uani 1 1 d . . . F3 F 0.35738(8) 1.02552(17) 0.26310(15) 0.0422(4) Uani 1 1 d . . . B1 B 0.25079(15) 1.3308(3) 0.1812(2) 0.0224(6) Uani 1 1 d . . . B2 B 0.23074(15) 1.1706(3) 0.0963(2) 0.0235(6) Uani 1 1 d . . . B3 B 0.19614(15) 1.0377(3) 0.1937(2) 0.0226(6) Uani 1 1 d . . . B4 B 0.17077(14) 1.4041(3) 0.2283(2) 0.0224(5) Uani 1 1 d . . . B5 B 0.17476(16) 1.3271(3) 0.1014(2) 0.0242(6) Uani 1 1 d . . . B6 B 0.14077(15) 1.1382(3) 0.1094(2) 0.0228(6) Uani 1 1 d . . . B7 B 0.11620(14) 1.1089(3) 0.2406(2) 0.0223(6) Uani 1 1 d . . . B8 B 0.13652(14) 1.2698(3) 0.3160(2) 0.0195(5) Uani 1 1 d . . . B9 B 0.10324(15) 1.2873(3) 0.1865(2) 0.0236(6) Uani 1 1 d . . . C1 C 0.22520(12) 1.2893(2) 0.29972(19) 0.0199(5) Uani 1 1 d . . . C2 C 0.19447(12) 1.1238(2) 0.30658(19) 0.0194(5) Uani 1 1 d . . . C3 C 0.20886(13) 1.0350(3) 0.4067(2) 0.0213(5) Uani 1 1 d . . . N1 N 0.15098(10) 0.9320(2) 0.43499(15) 0.0195(4) Uani 1 1 d . . . C4 C 0.10184(13) 0.9819(3) 0.50048(19) 0.0244(5) Uani 1 1 d . . . C5 C 0.04706(14) 0.8920(3) 0.5266(2) 0.0281(6) Uani 1 1 d . . . C6 C 0.04261(15) 0.7501(3) 0.4832(2) 0.0291(6) Uani 1 1 d . . . C7 C 0.09366(15) 0.7005(3) 0.4162(2) 0.0309(6) Uani 1 1 d . . . C8 C 0.14826(13) 0.7928(3) 0.3937(2) 0.0241(5) Uani 1 1 d . . . C3' C 0.25663(13) 1.3635(3) 0.39612(19) 0.0218(5) Uani 1 1 d . . . N1' N 0.32780(10) 1.3096(2) 0.42441(16) 0.0215(4) Uani 1 1 d . . . C4' C 0.33866(14) 1.2387(3) 0.5176(2) 0.0237(5) Uani 1 1 d . . . C5' C 0.40371(15) 1.1970(3) 0.5464(2) 0.0286(6) Uani 1 1 d . . . C6' C 0.45854(15) 1.2276(3) 0.4812(2) 0.0299(6) Uani 1 1 d . . . C7' C 0.44646(14) 1.3024(3) 0.3864(2) 0.0312(6) Uani 1 1 d . . . C8' C 0.38104(13) 1.3426(3) 0.3605(2) 0.0270(5) Uani 1 1 d . . . H3AA H 0.2447(16) 0.976(3) 0.397(2) 0.026(7) Uiso 1 1 d . . . H3AB H 0.2175(14) 1.098(3) 0.461(2) 0.019(7) Uiso 1 1 d . . . H4 H 0.1059(12) 1.079(3) 0.524(2) 0.014(6) Uiso 1 1 d . . . H5 H 0.0145(16) 0.926(3) 0.573(2) 0.034(8) Uiso 1 1 d . . . H6 H 0.0016(17) 0.679(4) 0.503(3) 0.047(9) Uiso 1 1 d . . . H7 H 0.0944(15) 0.607(4) 0.385(3) 0.034(8) Uiso 1 1 d . . . H8 H 0.1842(12) 0.762(2) 0.3494(19) 0.006(5) Uiso 1 1 d . . . H3A' H 0.2279(12) 1.355(2) 0.4558(18) 0.002(5) Uiso 1 1 d . . . H3B' H 0.2636(14) 1.458(3) 0.379(2) 0.025(7) Uiso 1 1 d . . . H4' H 0.3026(14) 1.226(3) 0.559(2) 0.011(6) Uiso 1 1 d . . . H5' H 0.4090(16) 1.155(4) 0.604(3) 0.038(9) Uiso 1 1 d . . . H6' H 0.5044(16) 1.195(3) 0.500(2) 0.029(7) Uiso 1 1 d . . . H7' H 0.4811(16) 1.325(3) 0.335(2) 0.036(8) Uiso 1 1 d . . . H8' H 0.3682(16) 1.397(3) 0.301(3) 0.039(9) Uiso 1 1 d . . . H1B H 0.2888(14) 1.412(3) 0.170(2) 0.025(7) Uiso 1 1 d . . . H2BA H 0.2556(14) 1.135(3) 0.024(2) 0.021(6) Uiso 1 1 d . . . H2BB H 0.2649(15) 1.150(3) 0.160(3) 0.037(8) Uiso 1 1 d . . . H3B H 0.2026(13) 0.923(3) 0.1927(19) 0.016(6) Uiso 1 1 d . . . H4B H 0.1664(14) 1.522(3) 0.247(2) 0.025(7) Uiso 1 1 d . . . H5B H 0.1709(14) 1.394(3) 0.029(2) 0.029(7) Uiso 1 1 d . . . H6B H 0.1130(11) 1.090(2) 0.0429(17) 0.004(5) Uiso 1 1 d . . . H7B H 0.0778(15) 1.035(3) 0.274(2) 0.029(7) Uiso 1 1 d . . . H8B H 0.1112(12) 1.301(3) 0.391(2) 0.021(7) Uiso 1 1 d . . . H9B H 0.0519(12) 1.330(3) 0.172(2) 0.013(6) 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 0.0237(3) 0.0215(3) 0.0204(3) -0.0008(3) -0.0013(3) -0.0002(2) O1 0.0340(11) 0.0319(10) 0.0203(9) -0.0045(7) -0.0058(8) 0.0039(8) O2 0.0354(11) 0.0378(10) 0.0258(9) 0.0020(8) 0.0059(8) -0.0042(8) O3 0.0313(9) 0.0244(8) 0.0353(9) -0.0042(9) -0.0043(9) 0.0061(7) C1S 0.0251(13) 0.0265(13) 0.0356(15) 0.0001(10) -0.0045(11) 0.0004(10) F1 0.0597(13) 0.0488(11) 0.0667(13) -0.0032(10) 0.0249(11) -0.0230(10) F2 0.0450(11) 0.0426(10) 0.0595(12) -0.0111(9) -0.0301(10) 0.0026(8) F3 0.0362(9) 0.0243(8) 0.0661(12) -0.0115(7) -0.0137(8) 0.0052(7) B1 0.0310(16) 0.0168(12) 0.0193(12) -0.0024(10) 0.0038(11) -0.0013(11) B2 0.0259(14) 0.0241(13) 0.0204(13) -0.0040(11) 0.0015(11) 0.0013(11) B3 0.0252(14) 0.0175(13) 0.0250(14) -0.0032(10) -0.0028(11) -0.0008(10) B4 0.0240(13) 0.0185(12) 0.0247(13) -0.0033(12) -0.0002(12) 0.0010(10) B5 0.0311(16) 0.0197(13) 0.0218(13) 0.0015(11) 0.0018(12) 0.0023(11) B6 0.0231(14) 0.0219(13) 0.0233(13) -0.0012(11) 0.0003(11) 0.0009(10) B7 0.0196(13) 0.0221(12) 0.0252(15) 0.0010(10) -0.0029(11) -0.0008(10) B8 0.0182(13) 0.0216(12) 0.0188(13) -0.0019(10) 0.0002(10) -0.0011(10) B9 0.0216(14) 0.0307(14) 0.0183(13) -0.0037(10) 0.0007(11) 0.0030(11) C1 0.0230(12) 0.0181(10) 0.0185(11) -0.0015(9) 0.0010(10) -0.0012(9) C2 0.0193(11) 0.0172(10) 0.0218(11) -0.0027(9) -0.0017(9) -0.0007(8) C3 0.0228(12) 0.0199(11) 0.0213(12) 0.0009(9) -0.0031(10) -0.0015(10) N1 0.0202(10) 0.0200(9) 0.0184(9) 0.0017(8) -0.0031(8) -0.0013(7) C4 0.0297(14) 0.0226(12) 0.0210(12) -0.0013(9) -0.0024(10) 0.0009(10) C5 0.0246(13) 0.0361(15) 0.0235(12) -0.0033(11) 0.0016(11) -0.0020(11) C6 0.0271(14) 0.0347(14) 0.0253(13) -0.0026(11) 0.0051(11) -0.0108(11) C7 0.0392(16) 0.0203(12) 0.0331(14) -0.0050(11) 0.0051(12) -0.0085(11) C8 0.0270(13) 0.0205(12) 0.0247(12) 0.0005(10) 0.0043(11) 0.0019(10) C3' 0.0224(12) 0.0203(12) 0.0228(12) -0.0012(9) -0.0011(10) -0.0014(9) N1' 0.0217(10) 0.0200(9) 0.0228(10) -0.0032(8) -0.0005(8) -0.0047(8) C4' 0.0235(12) 0.0253(12) 0.0224(12) -0.0019(9) 0.0035(11) -0.0068(10) C5' 0.0323(15) 0.0299(14) 0.0236(14) 0.0042(11) -0.0015(11) -0.0052(11) C6' 0.0212(13) 0.0307(14) 0.0377(15) 0.0024(11) -0.0069(12) -0.0006(11) C7' 0.0239(13) 0.0356(14) 0.0340(15) 0.0020(12) 0.0075(12) -0.0025(11) C8' 0.0286(14) 0.0246(13) 0.0278(14) -0.0002(11) 0.0021(11) -0.0025(10) _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 O2 1.431(2) . ? S1 O3 1.4409(17) . ? S1 O1 1.4425(18) . ? S1 C1S 1.822(3) . ? C1S F1 1.315(3) . ? C1S F3 1.330(3) . ? C1S F2 1.336(3) . ? B1 C1 1.621(4) . ? B1 B4 1.786(4) . ? B1 B5 1.787(4) . ? B1 B2 1.826(4) . ? B2 B5 1.767(4) . ? B2 B6 1.777(4) . ? B2 B3 1.834(4) . ? B3 C2 1.620(4) . ? B3 B6 1.758(4) . ? B3 B7 1.777(4) . ? B4 C1 1.724(4) . ? B4 B5 1.747(4) . ? B4 B9 1.753(4) . ? B4 B8 1.760(4) . ? B5 B9 1.791(4) . ? B5 B6 1.808(4) . ? B6 B7 1.745(4) . ? B6 B9 1.801(4) . ? B7 C2 1.738(3) . ? B7 B9 1.747(4) . ? B7 B8 1.765(4) . ? B8 C2 1.722(3) . ? B8 C1 1.741(4) . ? B8 B9 1.766(4) . ? C1 C3' 1.514(3) . ? C1 C2 1.592(3) . ? C2 C3 1.518(3) . ? C3 N1 1.493(3) . ? N1 C4 1.338(3) . ? N1 C8 1.346(3) . ? C4 C5 1.371(4) . ? C5 C6 1.379(4) . ? C6 C7 1.376(4) . ? C7 C8 1.371(4) . ? C3' N1' 1.505(3) . ? N1' C8' 1.344(3) . ? N1' C4' 1.353(3) . ? C4' C5' 1.365(4) . ? C5' C6' 1.373(4) . ? C6' C7' 1.391(4) . ? C7' C8' 1.359(4) . ? 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 O2 S1 O3 115.55(12) . . ? O2 S1 O1 114.97(12) . . ? O3 S1 O1 114.38(12) . . ? O2 S1 C1S 103.98(12) . . ? O3 S1 C1S 102.86(11) . . ? O1 S1 C1S 102.68(11) . . ? F1 C1S F3 108.1(2) . . ? F1 C1S F2 106.9(2) . . ? F3 C1S F2 106.2(2) . . ? F1 C1S S1 111.90(19) . . ? F3 C1S S1 112.24(17) . . ? F2 C1S S1 111.22(18) . . ? C1 B1 B4 60.58(16) . . ? C1 B1 B5 105.4(2) . . ? B4 B1 B5 58.52(16) . . ? C1 B1 B2 107.44(19) . . ? B4 B1 B2 107.2(2) . . ? B5 B1 B2 58.54(16) . . ? B5 B2 B6 61.36(16) . . ? B5 B2 B1 59.64(16) . . ? B6 B2 B1 106.35(19) . . ? B5 B2 B3 105.01(19) . . ? B6 B2 B3 58.23(16) . . ? B1 B2 B3 100.79(18) . . ? C2 B3 B6 106.36(19) . . ? C2 B3 B7 61.34(16) . . ? B6 B3 B7 59.18(16) . . ? C2 B3 B2 107.08(18) . . ? B6 B3 B2 59.27(16) . . ? B7 B3 B2 108.28(19) . . ? C1 B4 B5 102.79(18) . . ? C1 B4 B9 105.32(19) . . ? B5 B4 B9 61.57(16) . . ? C1 B4 B8 59.96(15) . . ? B5 B4 B8 109.19(18) . . ? B9 B4 B8 60.34(16) . . ? C1 B4 B1 54.97(14) . . ? B5 B4 B1 60.79(16) . . ? B9 B4 B1 109.44(19) . . ? B8 B4 B1 106.87(18) . . ? B4 B5 B2 111.7(2) . . ? B4 B5 B1 60.69(16) . . ? B2 B5 B1 61.83(16) . . ? B4 B5 B9 59.40(15) . . ? B2 B5 B9 110.0(2) . . ? B1 B5 B9 107.66(19) . . ? B4 B5 B6 107.28(19) . . ? B2 B5 B6 59.59(16) . . ? B1 B5 B6 106.66(19) . . ? B9 B5 B6 60.03(16) . . ? B7 B6 B3 60.96(16) . . ? B7 B6 B2 112.4(2) . . ? B3 B6 B2 62.50(17) . . ? B7 B6 B9 59.00(16) . . ? B3 B6 B9 107.1(2) . . ? B2 B6 B9 109.1(2) . . ? B7 B6 B5 106.96(19) . . ? B3 B6 B5 106.5(2) . . ? B2 B6 B5 59.05(16) . . ? B9 B6 B5 59.52(16) . . ? C2 B7 B6 101.90(19) . . ? C2 B7 B9 104.13(19) . . ? B6 B7 B9 62.08(16) . . ? C2 B7 B8 58.90(14) . . ? B6 B7 B8 109.32(19) . . ? B9 B7 B8 60.37(16) . . ? C2 B7 B3 54.87(14) . . ? B6 B7 B3 59.86(16) . . ? B9 B7 B3 108.6(2) . . ? B8 B7 B3 105.91(19) . . ? C2 B8 C1 54.71(13) . . ? C2 B8 B4 102.86(18) . . ? C1 B8 B4 59.00(15) . . ? C2 B8 B7 59.77(14) . . ? C1 B8 B7 103.77(18) . . ? B4 B8 B7 107.18(19) . . ? C2 B8 B9 103.97(19) . . ? C1 B8 B9 104.07(19) . . ? B4 B8 B9 59.65(16) . . ? B7 B8 B9 59.31(16) . . ? B7 B9 B4 108.3(2) . . ? B7 B9 B8 60.32(16) . . ? B4 B9 B8 60.01(16) . . ? B7 B9 B5 107.6(2) . . ? B4 B9 B5 59.03(16) . . ? B8 B9 B5 106.9(2) . . ? B7 B9 B6 58.91(16) . . ? B4 B9 B6 107.3(2) . . ? B8 B9 B6 106.8(2) . . ? B5 B9 B6 60.46(15) . . ? C3' C1 C2 120.7(2) . . ? C3' C1 B1 121.4(2) . . ? C2 C1 B1 112.09(19) . . ? C3' C1 B4 114.20(19) . . ? C2 C1 B4 110.33(18) . . ? B1 C1 B4 64.45(17) . . ? C3' C1 B8 110.27(19) . . ? C2 C1 B8 62.03(15) . . ? B1 C1 B8 115.7(2) . . ? B4 C1 B8 61.04(15) . . ? C3 C2 C1 117.29(19) . . ? C3 C2 B3 118.99(19) . . ? C1 C2 B3 112.46(19) . . ? C3 C2 B8 117.1(2) . . ? C1 C2 B8 63.26(15) . . ? B3 C2 B8 115.49(19) . . ? C3 C2 B7 121.42(19) . . ? C1 C2 B7 111.83(18) . . ? B3 C2 B7 63.79(16) . . ? B8 C2 B7 61.33(15) . . ? N1 C3 C2 112.39(19) . . ? C4 N1 C8 121.2(2) . . ? C4 N1 C3 118.7(2) . . ? C8 N1 C3 120.1(2) . . ? N1 C4 C5 120.5(2) . . ? C4 C5 C6 119.1(3) . . ? C7 C6 C5 119.6(3) . . ? C8 C7 C6 119.5(3) . . ? N1 C8 C7 120.1(2) . . ? N1' C3' C1 115.0(2) . . ? C8' N1' C4' 120.4(2) . . ? C8' N1' C3' 119.5(2) . . ? C4' N1' C3' 119.9(2) . . ? N1' C4' C5' 120.2(2) . . ? C4' C5' C6' 120.2(3) . . ? C5' C6' C7' 118.8(3) . . ? C8' C7' C6' 119.4(3) . . ? N1' C8' C7' 121.1(3) . . ? 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 O2 S1 C1S F1 -173.94(19) . . . . ? O3 S1 C1S F1 65.2(2) . . . . ? O1 S1 C1S F1 -53.8(2) . . . . ? O2 S1 C1S F3 -52.2(2) . . . . ? O3 S1 C1S F3 -173.06(19) . . . . ? O1 S1 C1S F3 67.9(2) . . . . ? O2 S1 C1S F2 66.6(2) . . . . ? O3 S1 C1S F2 -54.2(2) . . . . ? O1 S1 C1S F2 -173.29(19) . . . . ? C1 B1 B2 B5 97.7(2) . . . . ? B4 B1 B2 B5 33.87(19) . . . . ? C1 B1 B2 B6 56.3(2) . . . . ? B4 B1 B2 B6 -7.5(3) . . . . ? B5 B1 B2 B6 -41.35(19) . . . . ? C1 B1 B2 B3 -3.5(2) . . . . ? B4 B1 B2 B3 -67.3(2) . . . . ? B5 B1 B2 B3 -101.2(2) . . . . ? B5 B2 B3 C2 -57.8(2) . . . . ? B6 B2 B3 C2 -99.2(2) . . . . ? B1 B2 B3 C2 3.4(3) . . . . ? B5 B2 B3 B6 41.44(18) . . . . ? B1 B2 B3 B6 102.7(2) . . . . ? B5 B2 B3 B7 7.0(2) . . . . ? B6 B2 B3 B7 -34.49(18) . . . . ? B1 B2 B3 B7 68.2(2) . . . . ? B5 B1 B4 C1 134.57(19) . . . . ? B2 B1 B4 C1 100.7(2) . . . . ? C1 B1 B4 B5 -134.57(19) . . . . ? B2 B1 B4 B5 -33.88(18) . . . . ? C1 B1 B4 B9 -95.4(2) . . . . ? B5 B1 B4 B9 39.1(2) . . . . ? B2 B1 B4 B9 5.3(3) . . . . ? C1 B1 B4 B8 -31.63(18) . . . . ? B5 B1 B4 B8 102.9(2) . . . . ? B2 B1 B4 B8 69.1(2) . . . . ? C1 B4 B5 B2 -0.4(3) . . . . ? B9 B4 B5 B2 -101.1(2) . . . . ? B8 B4 B5 B2 -62.7(3) . . . . ? B1 B4 B5 B2 36.32(19) . . . . ? C1 B4 B5 B1 -36.74(16) . . . . ? B9 B4 B5 B1 -137.4(2) . . . . ? B8 B4 B5 B1 -99.1(2) . . . . ? C1 B4 B5 B9 100.7(2) . . . . ? B8 B4 B5 B9 38.35(19) . . . . ? B1 B4 B5 B9 137.4(2) . . . . ? C1 B4 B5 B6 63.0(2) . . . . ? B9 B4 B5 B6 -37.64(19) . . . . ? B8 B4 B5 B6 0.7(3) . . . . ? B1 B4 B5 B6 99.8(2) . . . . ? B6 B2 B5 B4 97.9(2) . . . . ? B1 B2 B5 B4 -35.86(19) . . . . ? B3 B2 B5 B4 58.0(2) . . . . ? B6 B2 B5 B1 133.8(2) . . . . ? B3 B2 B5 B1 93.9(2) . . . . ? B6 B2 B5 B9 33.89(19) . . . . ? B1 B2 B5 B9 -99.9(2) . . . . ? B3 B2 B5 B9 -6.0(3) . . . . ? B1 B2 B5 B6 -133.8(2) . . . . ? B3 B2 B5 B6 -39.88(17) . . . . ? C1 B1 B5 B4 40.05(17) . . . . ? B2 B1 B5 B4 141.4(2) . . . . ? C1 B1 B5 B2 -101.3(2) . . . . ? B4 B1 B5 B2 -141.4(2) . . . . ? C1 B1 B5 B9 2.4(2) . . . . ? B4 B1 B5 B9 -37.69(18) . . . . ? B2 B1 B5 B9 103.7(2) . . . . ? C1 B1 B5 B6 -60.8(2) . . . . ? B4 B1 B5 B6 -100.8(2) . . . . ? B2 B1 B5 B6 40.56(18) . . . . ? C2 B3 B6 B7 -40.78(19) . . . . ? B2 B3 B6 B7 -141.2(2) . . . . ? C2 B3 B6 B2 100.5(2) . . . . ? B7 B3 B6 B2 141.2(2) . . . . ? C2 B3 B6 B9 -2.6(3) . . . . ? B7 B3 B6 B9 38.13(18) . . . . ? B2 B3 B6 B9 -103.1(2) . . . . ? C2 B3 B6 B5 59.8(2) . . . . ? B7 B3 B6 B5 100.6(2) . . . . ? B2 B3 B6 B5 -40.65(18) . . . . ? B5 B2 B6 B7 -97.0(2) . . . . ? B1 B2 B6 B7 -56.5(3) . . . . ? B3 B2 B6 B7 36.29(19) . . . . ? B5 B2 B6 B3 -133.25(19) . . . . ? B1 B2 B6 B3 -92.7(2) . . . . ? B5 B2 B6 B9 -33.49(19) . . . . ? B1 B2 B6 B9 7.0(3) . . . . ? B3 B2 B6 B9 99.8(2) . . . . ? B1 B2 B6 B5 40.50(18) . . . . ? B3 B2 B6 B5 133.25(19) . . . . ? B4 B5 B6 B7 0.9(3) . . . . ? B2 B5 B6 B7 106.3(2) . . . . ? B1 B5 B6 B7 64.7(2) . . . . ? B9 B5 B6 B7 -36.46(19) . . . . ? B4 B5 B6 B3 -63.1(2) . . . . ? B2 B5 B6 B3 42.36(19) . . . . ? B1 B5 B6 B3 0.7(2) . . . . ? B9 B5 B6 B3 -100.4(2) . . . . ? B4 B5 B6 B2 -105.4(2) . . . . ? B1 B5 B6 B2 -41.65(19) . . . . ? B9 B5 B6 B2 -142.8(2) . . . . ? B4 B5 B6 B9 37.36(19) . . . . ? B2 B5 B6 B9 142.8(2) . . . . ? B1 B5 B6 B9 101.1(2) . . . . ? B3 B6 B7 C2 36.65(16) . . . . ? B2 B6 B7 C2 -0.3(2) . . . . ? B9 B6 B7 C2 -99.8(2) . . . . ? B5 B6 B7 C2 -63.1(2) . . . . ? B3 B6 B7 B9 136.5(2) . . . . ? B2 B6 B7 B9 99.6(2) . . . . ? B5 B6 B7 B9 36.69(19) . . . . ? B3 B6 B7 B8 97.6(2) . . . . ? B2 B6 B7 B8 60.7(2) . . . . ? B9 B6 B7 B8 -38.86(19) . . . . ? B5 B6 B7 B8 -2.2(3) . . . . ? B2 B6 B7 B3 -36.91(19) . . . . ? B9 B6 B7 B3 -136.5(2) . . . . ? B5 B6 B7 B3 -99.8(2) . . . . ? B6 B3 B7 C2 -134.4(2) . . . . ? B2 B3 B7 C2 -99.9(2) . . . . ? C2 B3 B7 B6 134.4(2) . . . . ? B2 B3 B7 B6 34.53(18) . . . . ? C2 B3 B7 B9 94.5(2) . . . . ? B6 B3 B7 B9 -39.95(19) . . . . ? B2 B3 B7 B9 -5.4(3) . . . . ? C2 B3 B7 B8 30.99(17) . . . . ? B6 B3 B7 B8 -103.4(2) . . . . ? B2 B3 B7 B8 -68.9(2) . . . . ? C1 B4 B8 C2 -34.06(15) . . . . ? B5 B4 B8 C2 59.9(2) . . . . ? B9 B4 B8 C2 98.82(19) . . . . ? B1 B4 B8 C2 -4.3(2) . . . . ? B5 B4 B8 C1 94.0(2) . . . . ? B9 B4 B8 C1 132.88(19) . . . . ? B1 B4 B8 C1 29.74(17) . . . . ? C1 B4 B8 B7 -96.02(19) . . . . ? B5 B4 B8 B7 -2.0(3) . . . . ? B9 B4 B8 B7 36.86(18) . . . . ? B1 B4 B8 B7 -66.3(2) . . . . ? C1 B4 B8 B9 -132.88(19) . . . . ? B5 B4 B8 B9 -38.90(19) . . . . ? B1 B4 B8 B9 -103.1(2) . . . . ? B6 B7 B8 C2 -92.5(2) . . . . ? B9 B7 B8 C2 -132.1(2) . . . . ? B3 B7 B8 C2 -29.46(17) . . . . ? C2 B7 B8 C1 33.77(16) . . . . ? B6 B7 B8 C1 -58.7(2) . . . . ? B9 B7 B8 C1 -98.4(2) . . . . ? B3 B7 B8 C1 4.3(2) . . . . ? C2 B7 B8 B4 95.1(2) . . . . ? B6 B7 B8 B4 2.6(3) . . . . ? B9 B7 B8 B4 -37.01(18) . . . . ? B3 B7 B8 B4 65.7(2) . . . . ? C2 B7 B8 B9 132.1(2) . . . . ? B6 B7 B8 B9 39.63(19) . . . . ? B3 B7 B8 B9 102.7(2) . . . . ? C2 B7 B9 B4 -3.5(3) . . . . ? B6 B7 B9 B4 -99.6(2) . . . . ? B8 B7 B9 B4 37.44(19) . . . . ? B3 B7 B9 B4 -60.7(2) . . . . ? C2 B7 B9 B8 -40.90(17) . . . . ? B6 B7 B9 B8 -137.1(2) . . . . ? B3 B7 B9 B8 -98.1(2) . . . . ? C2 B7 B9 B5 58.9(2) . . . . ? B6 B7 B9 B5 -37.25(19) . . . . ? B8 B7 B9 B5 99.8(2) . . . . ? B3 B7 B9 B5 1.7(3) . . . . ? C2 B7 B9 B6 96.2(2) . . . . ? B8 B7 B9 B6 137.1(2) . . . . ? B3 B7 B9 B6 38.94(19) . . . . ? C1 B4 B9 B7 3.6(3) . . . . ? B5 B4 B9 B7 100.0(2) . . . . ? B8 B4 B9 B7 -37.57(19) . . . . ? B1 B4 B9 B7 61.2(3) . . . . ? C1 B4 B9 B8 41.13(18) . . . . ? B5 B4 B9 B8 137.6(2) . . . . ? B1 B4 B9 B8 98.8(2) . . . . ? C1 B4 B9 B5 -96.5(2) . . . . ? B8 B4 B9 B5 -137.6(2) . . . . ? B1 B4 B9 B5 -38.78(19) . . . . ? C1 B4 B9 B6 -58.6(2) . . . . ? B5 B4 B9 B6 37.84(19) . . . . ? B8 B4 B9 B6 -99.8(2) . . . . ? B1 B4 B9 B6 -0.9(3) . . . . ? C2 B8 B9 B7 41.31(17) . . . . ? C1 B8 B9 B7 97.85(19) . . . . ? B4 B8 B9 B7 138.2(2) . . . . ? C2 B8 B9 B4 -96.89(19) . . . . ? C1 B8 B9 B4 -40.35(17) . . . . ? B7 B8 B9 B4 -138.2(2) . . . . ? C2 B8 B9 B5 -59.7(2) . . . . ? C1 B8 B9 B5 -3.2(2) . . . . ? B4 B8 B9 B5 37.18(18) . . . . ? B7 B8 B9 B5 -101.0(2) . . . . ? C2 B8 B9 B6 3.8(2) . . . . ? C1 B8 B9 B6 60.3(2) . . . . ? B4 B8 B9 B6 100.7(2) . . . . ? B7 B8 B9 B6 -37.55(18) . . . . ? B4 B5 B9 B7 -101.1(2) . . . . ? B2 B5 B9 B7 2.9(3) . . . . ? B1 B5 B9 B7 -62.8(2) . . . . ? B6 B5 B9 B7 36.58(18) . . . . ? B2 B5 B9 B4 104.0(2) . . . . ? B1 B5 B9 B4 38.27(18) . . . . ? B6 B5 B9 B4 137.7(2) . . . . ? B4 B5 B9 B8 -37.63(18) . . . . ? B2 B5 B9 B8 66.3(2) . . . . ? B1 B5 B9 B8 0.6(3) . . . . ? B6 B5 B9 B8 100.1(2) . . . . ? B4 B5 B9 B6 -137.7(2) . . . . ? B2 B5 B9 B6 -33.72(19) . . . . ? B1 B5 B9 B6 -99.4(2) . . . . ? B3 B6 B9 B7 -39.04(18) . . . . ? B2 B6 B9 B7 -105.2(2) . . . . ? B5 B6 B9 B7 -138.5(2) . . . . ? B7 B6 B9 B4 101.3(2) . . . . ? B3 B6 B9 B4 62.2(2) . . . . ? B2 B6 B9 B4 -3.9(3) . . . . ? B5 B6 B9 B4 -37.20(19) . . . . ? B7 B6 B9 B8 38.19(18) . . . . ? B3 B6 B9 B8 -0.9(3) . . . . ? B2 B6 B9 B8 -67.0(2) . . . . ? B5 B6 B9 B8 -100.3(2) . . . . ? B7 B6 B9 B5 138.5(2) . . . . ? B3 B6 B9 B5 99.4(2) . . . . ? B2 B6 B9 B5 33.30(19) . . . . ? B4 B1 C1 C3' -103.9(2) . . . . ? B5 B1 C1 C3' -143.0(2) . . . . ? B2 B1 C1 C3' 155.8(2) . . . . ? B4 B1 C1 C2 102.8(2) . . . . ? B5 B1 C1 C2 63.7(2) . . . . ? B2 B1 C1 C2 2.5(3) . . . . ? B5 B1 C1 B4 -39.05(17) . . . . ? B2 B1 C1 B4 -100.3(2) . . . . ? B4 B1 C1 B8 34.27(18) . . . . ? B5 B1 C1 B8 -4.8(2) . . . . ? B2 B1 C1 B8 -66.0(2) . . . . ? B5 B4 C1 C3' 154.4(2) . . . . ? B9 B4 C1 C3' -142.0(2) . . . . ? B8 B4 C1 C3' -100.7(2) . . . . ? B1 B4 C1 C3' 114.7(2) . . . . ? B5 B4 C1 C2 -65.9(2) . . . . ? B9 B4 C1 C2 -2.3(2) . . . . ? B8 B4 C1 C2 39.05(18) . . . . ? B1 B4 C1 C2 -105.5(2) . . . . ? B5 B4 C1 B1 39.61(18) . . . . ? B9 B4 C1 B1 103.3(2) . . . . ? B8 B4 C1 B1 144.57(19) . . . . ? B5 B4 C1 B8 -105.0(2) . . . . ? B9 B4 C1 B8 -41.32(18) . . . . ? B1 B4 C1 B8 -144.57(19) . . . . ? C2 B8 C1 C3' -114.8(2) . . . . ? B4 B8 C1 C3' 107.2(2) . . . . ? B7 B8 C1 C3' -150.87(19) . . . . ? B9 B8 C1 C3' 147.84(19) . . . . ? B4 B8 C1 C2 -138.02(19) . . . . ? B7 B8 C1 C2 -36.04(17) . . . . ? B9 B8 C1 C2 -97.3(2) . . . . ? C2 B8 C1 B1 102.5(2) . . . . ? B4 B8 C1 B1 -35.50(19) . . . . ? B7 B8 C1 B1 66.5(2) . . . . ? B9 B8 C1 B1 5.2(3) . . . . ? C2 B8 C1 B4 138.02(19) . . . . ? B7 B8 C1 B4 102.0(2) . . . . ? B9 B8 C1 B4 40.68(18) . . . . ? C3' C1 C2 C3 -10.2(3) . . . . ? B1 C1 C2 C3 143.3(2) . . . . ? B4 C1 C2 C3 -146.9(2) . . . . ? B8 C1 C2 C3 -108.3(2) . . . . ? C3' C1 C2 B3 -153.6(2) . . . . ? B1 C1 C2 B3 -0.1(3) . . . . ? B4 C1 C2 B3 69.6(2) . . . . ? B8 C1 C2 B3 108.2(2) . . . . ? C3' C1 C2 B8 98.1(2) . . . . ? B1 C1 C2 B8 -108.4(2) . . . . ? B4 C1 C2 B8 -38.62(18) . . . . ? C3' C1 C2 B7 136.8(2) . . . . ? B1 C1 C2 B7 -69.7(2) . . . . ? B4 C1 C2 B7 0.1(2) . . . . ? B8 C1 C2 B7 38.69(18) . . . . ? B6 B3 C2 C3 152.8(2) . . . . ? B7 B3 C2 C3 113.0(2) . . . . ? B2 B3 C2 C3 -145.1(2) . . . . ? B6 B3 C2 C1 -64.4(2) . . . . ? B7 B3 C2 C1 -104.2(2) . . . . ? B2 B3 C2 C1 -2.3(3) . . . . ? B6 B3 C2 B8 5.5(3) . . . . ? B7 B3 C2 B8 -34.20(19) . . . . ? B2 B3 C2 B8 67.7(3) . . . . ? B6 B3 C2 B7 39.73(18) . . . . ? B2 B3 C2 B7 101.9(2) . . . . ? C1 B8 C2 C3 108.6(2) . . . . ? B4 B8 C2 C3 144.6(2) . . . . ? B7 B8 C2 C3 -112.8(2) . . . . ? B9 B8 C2 C3 -153.9(2) . . . . ? B4 B8 C2 C1 36.02(17) . . . . ? B7 B8 C2 C1 138.59(19) . . . . ? B9 B8 C2 C1 97.5(2) . . . . ? C1 B8 C2 B3 -103.5(2) . . . . ? B4 B8 C2 B3 -67.5(2) . . . . ? B7 B8 C2 B3 35.1(2) . . . . ? B9 B8 C2 B3 -6.0(3) . . . . ? C1 B8 C2 B7 -138.59(19) . . . . ? B4 B8 C2 B7 -102.6(2) . . . . ? B9 B8 C2 B7 -41.08(18) . . . . ? B6 B7 C2 C3 -148.5(2) . . . . ? B9 B7 C2 C3 147.6(2) . . . . ? B8 B7 C2 C3 105.9(2) . . . . ? B3 B7 C2 C3 -109.4(2) . . . . ? B6 B7 C2 C1 66.0(2) . . . . ? B9 B7 C2 C1 2.1(2) . . . . ? B8 B7 C2 C1 -39.51(18) . . . . ? B3 B7 C2 C1 105.2(2) . . . . ? B6 B7 C2 B3 -39.14(17) . . . . ? B9 B7 C2 B3 -103.0(2) . . . . ? B8 B7 C2 B3 -144.7(2) . . . . ? B6 B7 C2 B8 105.5(2) . . . . ? B9 B7 C2 B8 41.66(18) . . . . ? B3 B7 C2 B8 144.7(2) . . . . ? C1 C2 C3 N1 146.9(2) . . . . ? B3 C2 C3 N1 -72.1(3) . . . . ? B8 C2 C3 N1 74.6(3) . . . . ? B7 C2 C3 N1 3.2(3) . . . . ? C2 C3 N1 C4 -92.0(3) . . . . ? C2 C3 N1 C8 87.0(3) . . . . ? C8 N1 C4 C5 -0.4(4) . . . . ? C3 N1 C4 C5 178.6(2) . . . . ? N1 C4 C5 C6 -1.0(4) . . . . ? C4 C5 C6 C7 1.2(4) . . . . ? C5 C6 C7 C8 0.1(4) . . . . ? C4 N1 C8 C7 1.6(4) . . . . ? C3 N1 C8 C7 -177.3(2) . . . . ? C6 C7 C8 N1 -1.5(4) . . . . ? C2 C1 C3' N1' 76.7(3) . . . . ? B1 C1 C3' N1' -74.4(3) . . . . ? B4 C1 C3' N1' -148.1(2) . . . . ? B8 C1 C3' N1' 145.5(2) . . . . ? C1 C3' N1' C8' 68.7(3) . . . . ? C1 C3' N1' C4' -116.5(2) . . . . ? C8' N1' C4' C5' -1.5(4) . . . . ? C3' N1' C4' C5' -176.4(2) . . . . ? N1' C4' C5' C6' 0.4(4) . . . . ? C4' C5' C6' C7' 0.5(4) . . . . ? C5' C6' C7' C8' -0.3(4) . . . . ? C4' N1' C8' C7' 1.8(4) . . . . ? C3' N1' C8' C7' 176.6(2) . . . . ? C6' C7' C8' N1' -0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.684 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.068 _publ_section_references ; Bruker (1998a). SAINTPlus. Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b). SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;