#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global #===================================================================== _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Andrew K. Hughes Department of Chemistry Durham University DURHAM DH1 3LE UK ; _publ_contact_author_phone '+44 191 3743111' _publ_contact_author_fax '+44 191 3861127' _publ_contact_author_email A.K.Hughes@durham.ac.uk _publ_requested_journal 'Dalton Transactions' #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ;Synthesis of isomeric B-methylated tantalum carboranes, (Me~2~N)~3~TaC~2~B~9~H~10~Me ; loop_ _publ_author_name _publ_author_address 'Fox, Mark A.' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Howard, Judith A.K.' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Hughes*, Andrew K.' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Malget, John M.' ; Department of Chemistry Durham University Durham DH1 3LE UK ; 'Yufit, Dimitrii S.' ; Department of Chemistry Durham University Durham DH1 3LE UK ; _publ_section_references ; Bruker (1998a). SMART-NT V5.0. Data Collection Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998b). SAINT-NT V5.0. Data Reduction Software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (1998c). SHELXTL-NT. Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1990) Acta Cryst. A46, 467-473 Sheldrick, G.M. (1998). SADABS. Empirical Absorption Correction Program. University of G\"ottingen, Germany. Sheldrick, G.M. (1997) SHELXL-97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. ; #================================================================= data_00srv271 _database_code_CSD 163356 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H31 B9 N3 Ta' _chemical_formula_weight 459.61 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' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 7.614(2) _cell_length_b 18.192(4) _cell_length_c 13.584(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.89(3) _cell_angle_gamma 90.00 _cell_volume 1859.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 5259 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 29.9 _exptl_crystal_description 'rod' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.93 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 5.904 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.0730 _exptl_absorpt_correction_T_max 0.4163 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1994)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(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 CCD' _diffrn_measurement_method '\w-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11038 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 29.92 _reflns_number_total 4708 _reflns_number_gt 4452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(1) _refine_ls_number_reflns 4708 _refine_ls_number_parameters 200 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0510 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.002 _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 Ta4 Ta 0.50089(2) 0.617479(6) 0.75073(2) 0.01332(4) Uani 1 1 d . . . N1 N 0.6825(6) 0.6112(2) 0.8736(3) 0.0242(9) Uani 1 1 d . . . N2 N 0.3941(5) 0.7099(2) 0.7877(3) 0.0201(8) Uani 1 1 d . . . N3 N 0.6282(5) 0.6599(2) 0.6468(3) 0.0211(8) Uani 1 1 d . . . C1 C 0.4321(5) 0.5217(2) 0.6212(3) 0.0162(8) Uani 1 1 d . . . H1 H 0.5182 0.5383 0.5651 0.019 Uiso 1 1 calc R . . C2 C 0.2392(6) 0.4853(3) 0.5819(3) 0.0197(9) Uani 1 1 d . . . H2 H 0.1916 0.4790 0.5001 0.024 Uiso 1 1 calc R . . C3 C 0.1797(7) 0.6368(3) 0.5483(4) 0.0260(10) Uani 1 1 d . . . H3A H 0.0783 0.6184 0.5015 0.039 Uiso 1 1 calc R . . H3B H 0.2761 0.6504 0.5117 0.039 Uiso 1 1 calc R . . H3C H 0.1431 0.6800 0.5832 0.039 Uiso 1 1 calc R . . C4 C 0.7445(7) 0.6792(3) 0.9314(4) 0.0290(11) Uani 1 1 d . . . H4A H 0.8331 0.6659 0.9888 0.044 Uiso 1 1 calc R . . H4B H 0.6430 0.7031 0.9547 0.044 Uiso 1 1 calc R . . H4C H 0.7977 0.7132 0.8883 0.044 Uiso 1 1 calc R . . C5 C 0.7744(6) 0.5487(3) 0.9268(4) 0.0294(11) Uani 1 1 d . . . H5A H 0.8557 0.5666 0.9849 0.044 Uiso 1 1 calc R . . H5B H 0.8421 0.5222 0.8822 0.044 Uiso 1 1 calc R . . H5C H 0.6869 0.5155 0.9488 0.044 Uiso 1 1 calc R . . C6 C 0.3620(7) 0.7776(3) 0.7300(4) 0.0322(12) Uani 1 1 d . . . H6A H 0.3061 0.8140 0.7684 0.048 Uiso 1 1 calc R . . H6B H 0.2831 0.7673 0.6674 0.048 Uiso 1 1 calc R . . H6C H 0.4752 0.7970 0.7153 0.048 Uiso 1 1 calc R . . C7 C 0.3134(7) 0.7150(3) 0.8799(4) 0.0304(12) Uani 1 1 d . . . H7A H 0.2702 0.7652 0.8872 0.046 Uiso 1 1 calc R . . H7B H 0.4028 0.7028 0.9375 0.046 Uiso 1 1 calc R . . H7C H 0.2138 0.6805 0.8760 0.046 Uiso 1 1 calc R . . C8 C 0.7867(6) 0.7058(3) 0.6856(4) 0.0270(10) Uani 1 1 d . . . H8A H 0.8410 0.7244 0.6296 0.040 Uiso 1 1 calc R . . H8B H 0.8734 0.6759 0.7290 0.040 Uiso 1 1 calc R . . H8C H 0.7497 0.7473 0.7235 0.040 Uiso 1 1 calc R . . C9 C 0.6172(6) 0.6562(3) 0.5387(4) 0.0246(10) Uani 1 1 d . . . H9A H 0.7102 0.6871 0.5178 0.037 Uiso 1 1 calc R . . H9B H 0.5004 0.6737 0.5071 0.037 Uiso 1 1 calc R . . H9C H 0.6337 0.6052 0.5187 0.037 Uiso 1 1 calc R . . B3 B 0.2475(7) 0.5740(3) 0.6277(4) 0.0186(10) Uani 1 1 d . . . B5 B 0.5250(7) 0.4830(3) 0.7284(3) 0.0166(10) Uani 1 1 d . . . H5 H 0.6712 0.4732 0.7496 0.020 Uiso 1 1 calc R . . B6 B 0.4058(7) 0.4274(3) 0.6333(4) 0.0241(11) Uani 1 1 d . . . H6 H 0.4711 0.3841 0.5929 0.029 Uiso 1 1 calc R . . B7 B 0.0855(7) 0.5070(3) 0.6564(4) 0.0212(11) Uani 1 1 d . . . H7 H -0.0603 0.5151 0.6312 0.025 Uiso 1 1 calc R . . B8 B 0.2038(6) 0.5607(3) 0.7528(4) 0.0187(10) Uani 1 1 d . . . H8 H 0.1290 0.6020 0.7913 0.022 Uiso 1 1 calc R . . B9 B 0.3796(7) 0.5037(3) 0.8165(4) 0.0178(10) Uani 1 1 d . . . H9 H 0.4245 0.5064 0.8989 0.021 Uiso 1 1 calc R . . B10 B 0.3674(8) 0.4156(3) 0.7570(4) 0.0255(11) Uani 1 1 d . . . H10 H 0.4083 0.3640 0.7995 0.031 Uiso 1 1 calc R . . B11 B 0.1839(7) 0.4181(3) 0.6572(4) 0.0258(11) Uani 1 1 d . . . H11 H 0.1023 0.3685 0.6318 0.031 Uiso 1 1 calc R . . B12 B 0.1695(7) 0.4645(3) 0.7708(4) 0.0217(11) Uani 1 1 d . . . H12 H 0.0794 0.4445 0.8229 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta4 0.01506(7) 0.01471(6) 0.01045(7) -0.00074(15) 0.00279(4) -0.00252(15) N1 0.021(2) 0.030(2) 0.021(2) 0.0018(17) 0.0012(16) -0.0013(17) N2 0.0211(18) 0.0187(18) 0.022(2) 0.0012(15) 0.0081(15) 0.0013(15) N3 0.0212(18) 0.0186(19) 0.024(2) 0.0045(15) 0.0053(15) -0.0033(14) C1 0.018(2) 0.022(2) 0.009(2) -0.0005(16) 0.0018(15) -0.0013(16) C2 0.022(2) 0.024(2) 0.013(2) 0.0007(17) 0.0037(16) -0.0062(18) C3 0.026(2) 0.035(3) 0.018(2) 0.010(2) 0.0044(19) 0.002(2) C4 0.029(3) 0.034(3) 0.023(3) -0.002(2) 0.002(2) -0.009(2) C5 0.023(2) 0.041(3) 0.021(3) 0.005(2) -0.007(2) 0.003(2) C6 0.036(3) 0.021(2) 0.043(3) 0.006(2) 0.015(2) 0.003(2) C7 0.034(3) 0.038(3) 0.022(3) -0.013(2) 0.014(2) -0.004(2) C8 0.027(2) 0.026(2) 0.029(3) -0.006(2) 0.008(2) -0.0067(19) C9 0.025(2) 0.029(3) 0.023(2) 0.003(2) 0.0115(18) -0.0028(19) B3 0.017(2) 0.022(3) 0.016(3) 0.000(2) 0.002(2) -0.005(2) B5 0.028(3) 0.012(2) 0.009(3) -0.0013(15) 0.000(2) 0.0004(18) B6 0.031(3) 0.021(3) 0.021(3) -0.004(2) 0.008(2) -0.002(2) B7 0.025(3) 0.028(3) 0.012(3) -0.003(2) 0.006(2) -0.010(2) B8 0.018(2) 0.026(3) 0.013(2) -0.0005(19) 0.0027(17) -0.0043(18) B9 0.024(2) 0.016(2) 0.014(3) 0.0018(18) 0.006(2) -0.0018(18) B10 0.040(3) 0.019(2) 0.019(3) 0.000(2) 0.007(2) -0.008(2) B11 0.033(3) 0.024(3) 0.020(3) -0.002(2) 0.005(2) -0.010(2) B12 0.028(3) 0.024(3) 0.014(3) 0.0009(19) 0.006(2) -0.011(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 Ta4 N2 1.967(4) . ? Ta4 N3 1.988(4) . ? Ta4 N1 2.000(5) . ? Ta4 C1 2.475(4) . ? Ta4 B5 2.475(5) . ? Ta4 B3 2.479(6) . ? Ta4 B9 2.488(5) . ? Ta4 B8 2.491(5) . ? N1 C5 1.466(7) . ? N1 C4 1.502(7) . ? N2 C6 1.460(6) . ? N2 C7 1.480(6) . ? N3 C9 1.459(6) . ? N3 C8 1.494(6) . ? C1 C2 1.625(6) . ? C1 B5 1.673(6) . ? C1 B3 1.712(7) . ? C1 B6 1.737(7) . ? C2 B11 1.688(7) . ? C2 B7 1.708(7) . ? C2 B6 1.712(7) . ? C2 B3 1.729(8) . ? C3 B3 1.600(7) . ? B3 B8 1.798(7) . ? B3 B7 1.819(8) . ? B5 B6 1.775(7) . ? B5 B9 1.792(7) . ? B5 B10 1.800(7) . ? B6 B10 1.762(8) . ? B6 B11 1.777(8) . ? B7 B12 1.764(8) . ? B7 B8 1.765(7) . ? B7 B11 1.781(8) . ? B8 B12 1.792(7) . ? B8 B9 1.804(7) . ? B9 B12 1.774(7) . ? B9 B10 1.792(8) . ? B10 B12 1.784(8) . ? B10 B11 1.790(8) . ? B11 B12 1.777(8) . ? 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 N2 Ta4 N3 96.63(16) . . ? N2 Ta4 N1 95.46(18) . . ? N3 Ta4 N1 105.35(16) . . ? N2 Ta4 C1 137.19(15) . . ? N3 Ta4 C1 80.87(15) . . ? N1 Ta4 C1 126.62(16) . . ? N2 Ta4 B5 156.62(16) . . ? N3 Ta4 B5 104.08(16) . . ? N1 Ta4 B5 89.48(18) . . ? C1 Ta4 B5 39.51(15) . . ? N2 Ta4 B3 97.79(17) . . ? N3 Ta4 B3 93.41(17) . . ? N1 Ta4 B3 155.57(18) . . ? C1 Ta4 B3 40.44(16) . . ? B5 Ta4 B3 70.56(18) . . ? N2 Ta4 B9 115.37(16) . . ? N3 Ta4 B9 145.80(16) . . ? N1 Ta4 B9 84.25(17) . . ? C1 Ta4 B9 67.68(15) . . ? B5 Ta4 B9 42.33(16) . . ? B3 Ta4 B9 71.54(17) . . ? N2 Ta4 B8 86.56(16) . . ? N3 Ta4 B8 135.45(16) . . ? N1 Ta4 B8 118.60(16) . . ? C1 Ta4 B8 67.87(15) . . ? B5 Ta4 B8 71.11(17) . . ? B3 Ta4 B8 42.42(17) . . ? B9 Ta4 B8 42.49(17) . . ? C5 N1 C4 107.1(4) . . ? C5 N1 Ta4 132.2(4) . . ? C4 N1 Ta4 120.7(3) . . ? C6 N2 C7 110.2(4) . . ? C6 N2 Ta4 128.7(3) . . ? C7 N2 Ta4 120.8(3) . . ? C9 N3 C8 107.4(4) . . ? C9 N3 Ta4 137.5(3) . . ? C8 N3 Ta4 115.0(3) . . ? C2 C1 B5 110.7(3) . . ? C2 C1 B3 62.3(3) . . ? B5 C1 B3 115.4(3) . . ? C2 C1 B6 61.1(3) . . ? B5 C1 B6 62.7(3) . . ? B3 C1 B6 115.9(3) . . ? C2 C1 Ta4 127.0(3) . . ? B5 C1 Ta4 70.3(2) . . ? B3 C1 Ta4 69.9(3) . . ? B6 C1 Ta4 130.0(3) . . ? C1 C2 B11 113.2(4) . . ? C1 C2 B7 112.2(3) . . ? B11 C2 B7 63.3(3) . . ? C1 C2 B6 62.7(3) . . ? B11 C2 B6 63.0(3) . . ? B7 C2 B6 115.6(4) . . ? C1 C2 B3 61.3(3) . . ? B11 C2 B3 117.2(4) . . ? B7 C2 B3 63.9(3) . . ? B6 C2 B3 116.3(4) . . ? C3 B3 C1 123.0(4) . . ? C3 B3 C2 115.7(5) . . ? C1 B3 C2 56.4(3) . . ? C3 B3 B8 130.2(4) . . ? C1 B3 B8 104.3(4) . . ? C2 B3 B8 102.3(4) . . ? C3 B3 B7 117.7(4) . . ? C1 B3 B7 103.1(4) . . ? C2 B3 B7 57.5(3) . . ? B8 B3 B7 58.4(3) . . ? C3 B3 Ta4 111.3(4) . . ? C1 B3 Ta4 69.7(2) . . ? C2 B3 Ta4 121.5(3) . . ? B8 B3 Ta4 69.2(3) . . ? B7 B3 Ta4 123.5(3) . . ? C1 B5 B6 60.4(3) . . ? C1 B5 B9 105.7(4) . . ? B6 B5 B9 107.8(4) . . ? C1 B5 B10 105.5(4) . . ? B6 B5 B10 59.0(3) . . ? B9 B5 B10 59.8(3) . . ? C1 B5 Ta4 70.2(2) . . ? B6 B5 Ta4 127.8(3) . . ? B9 B5 Ta4 69.2(2) . . ? B10 B5 Ta4 125.6(3) . . ? C2 B6 C1 56.2(3) . . ? C2 B6 B10 104.0(4) . . ? C1 B6 B10 104.5(4) . . ? C2 B6 B5 102.2(4) . . ? C1 B6 B5 56.9(3) . . ? B10 B6 B5 61.2(3) . . ? C2 B6 B11 57.8(3) . . ? C1 B6 B11 103.8(4) . . ? B10 B6 B11 60.8(3) . . ? B5 B6 B11 108.4(4) . . ? C2 B7 B12 103.4(4) . . ? C2 B7 B8 104.5(3) . . ? B12 B7 B8 61.0(3) . . ? C2 B7 B11 57.8(3) . . ? B12 B7 B11 60.1(3) . . ? B8 B7 B11 109.4(4) . . ? C2 B7 B3 58.6(3) . . ? B12 B7 B3 108.5(4) . . ? B8 B7 B3 60.2(3) . . ? B11 B7 B3 108.1(4) . . ? B7 B8 B12 59.5(3) . . ? B7 B8 B3 61.4(3) . . ? B12 B8 B3 108.2(4) . . ? B7 B8 B9 107.1(4) . . ? B12 B8 B9 59.1(3) . . ? B3 B8 B9 107.4(3) . . ? B7 B8 Ta4 125.5(3) . . ? B12 B8 Ta4 124.0(3) . . ? B3 B8 Ta4 68.4(2) . . ? B9 B8 Ta4 68.7(2) . . ? B12 B9 B5 107.4(4) . . ? B12 B9 B10 60.0(3) . . ? B5 B9 B10 60.3(3) . . ? B12 B9 B8 60.1(3) . . ? B5 B9 B8 106.8(3) . . ? B10 B9 B8 108.3(4) . . ? B12 B9 Ta4 125.0(3) . . ? B5 B9 Ta4 68.5(2) . . ? B10 B9 Ta4 125.3(3) . . ? B8 B9 Ta4 68.8(2) . . ? B6 B10 B12 107.9(4) . . ? B6 B10 B11 60.0(3) . . ? B12 B10 B11 59.6(3) . . ? B6 B10 B9 108.4(4) . . ? B12 B10 B9 59.5(3) . . ? B11 B10 B9 107.4(4) . . ? B6 B10 B5 59.8(3) . . ? B12 B10 B5 106.6(4) . . ? B11 B10 B5 106.7(4) . . ? B9 B10 B5 59.8(3) . . ? C2 B11 B12 103.7(4) . . ? C2 B11 B6 59.2(3) . . ? B12 B11 B6 107.5(4) . . ? C2 B11 B7 58.9(3) . . ? B12 B11 B7 59.4(3) . . ? B6 B11 B7 108.8(4) . . ? C2 B11 B10 103.8(4) . . ? B12 B11 B10 60.0(3) . . ? B6 B11 B10 59.2(3) . . ? B7 B11 B10 107.8(4) . . ? B7 B12 B9 108.5(3) . . ? B7 B12 B11 60.4(3) . . ? B9 B12 B11 108.8(4) . . ? B7 B12 B10 108.8(4) . . ? B9 B12 B10 60.5(3) . . ? B11 B12 B10 60.4(3) . . ? B7 B12 B8 59.5(3) . . ? B9 B12 B8 60.8(3) . . ? B11 B12 B8 108.4(4) . . ? B10 B12 B8 109.2(4) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 29.92 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.282 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.123