# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '[(C5Me5Ta)2B5H10(C4H3S)] cif file for CCDC.txt' #================================================================ _audit_creation_method SHELXL-97 # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #================================================================ # SUBMISSION DETAILS _publ_contact_author_name 'Sundargopal Ghosh' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Madras Chennai - 600 036 India. ; _publ_contact_author_email sghosh@iitm.ac.in _publ_contact_author_fax 91(44)22574202 _publ_contact_author_phone 91(44)22574230 #================================================================= # TITLE AND AUTHOR LIST _publ_section_title ; C-H Activation of Arenes and Heteroarenes by Tantalaborane Cluster. ; loop_ _publ_author_name _publ_author_address 'Shubhankar Kumar Bose' ; Department of Chemistry Indian Institute of Technology Madras Chennai - 600 036 India. ; 'K. Geetharani' ; Department of Chemistry Indian Institute of Technology Madras Chennai - 600 036 India. ; 'Sundargopal Ghosh' ; Department of Chemistry Indian Institute of Technology Madras Chennai - 600 036 India. ; #=============================================================== data_shelxl _database_code_depnum_ccdc_archive 'CCDC 814964' #TrackingRef '[(C5Me5Ta)2B5H10(C4H3S)] cif file for CCDC.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H43 B5 S Ta2' _chemical_formula_weight 779.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.7674(8) _cell_length_b 17.0966(14) _cell_length_c 10.1063(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.068(5) _cell_angle_gamma 90.00 _cell_volume 2843.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1667 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 24.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 7.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.321 _exptl_absorpt_correction_T_max 0.463 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford diffraction Xcalibur-S CCD diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15722 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 32.76 _reflns_number_total 4870 _reflns_number_gt 2916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4870 _refine_ls_number_parameters 165 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.863 _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 Ta1 Ta 0.078147(9) 0.166904(11) 0.205271(15) 0.04781(7) Uani 1 1 d . . . B1 B 0.0000 0.2697(4) 0.2500 0.0479(15) Uani 1 2 d S . . B2 B -0.0427(3) 0.2208(4) 0.1011(5) 0.0567(14) Uani 1 1 d D . . B3 B -0.0411(4) 0.1139(4) 0.0892(6) 0.0657(16) Uani 1 1 d D . . C1 C 0.0000 0.3605(4) 0.2500 0.0611(16) Uani 1 2 d S . . C3 C 0.1905(3) 0.1161(3) 0.1186(5) 0.0616(12) Uani 1 1 d . . . C4 C 0.2218(3) 0.1696(4) 0.2202(5) 0.0706(16) Uani 1 1 d . . . C5 C 0.1919(4) 0.2441(4) 0.1761(7) 0.086(2) Uani 1 1 d . . . C6 C 0.1424(3) 0.2347(4) 0.0457(7) 0.0839(19) Uani 1 1 d . . . C7 C 0.1415(3) 0.1549(4) 0.0148(5) 0.0677(15) Uani 1 1 d . . . C8 C 0.2121(4) 0.0304(4) 0.1208(9) 0.124(3) Uani 1 1 d . . . H8C H 0.2642 0.0238 0.0918 0.186 Uiso 1 1 calc R . . H8A H 0.1697 0.0017 0.0595 0.186 Uiso 1 1 calc R . . H8B H 0.2165 0.0100 0.2125 0.186 Uiso 1 1 calc R . . C9 C 0.2828(4) 0.1515(7) 0.3438(7) 0.158(5) Uani 1 1 d . . . H9A H 0.2718 0.0996 0.3773 0.237 Uiso 1 1 calc R . . H9B H 0.2796 0.1908 0.4131 0.237 Uiso 1 1 calc R . . H9C H 0.3374 0.1522 0.3223 0.237 Uiso 1 1 calc R . . C10 C 0.2163(6) 0.3196(5) 0.2470(12) 0.189(6) Uani 1 1 d . . . H10A H 0.1707 0.3403 0.2842 0.284 Uiso 1 1 calc R . . H10B H 0.2313 0.3573 0.1829 0.284 Uiso 1 1 calc R . . H10C H 0.2629 0.3107 0.3203 0.284 Uiso 1 1 calc R . . C11 C 0.1070(6) 0.3007(7) -0.0413(13) 0.237(8) Uani 1 1 d . . . H11B H 0.1347 0.3052 -0.1181 0.356 Uiso 1 1 calc R . . H11C H 0.1140 0.3493 0.0109 0.356 Uiso 1 1 calc R . . H11A H 0.0490 0.2911 -0.0744 0.356 Uiso 1 1 calc R . . C12 C 0.0993(4) 0.1176(7) -0.1167(6) 0.142(4) Uani 1 1 d . . . H12A H 0.0529 0.0866 -0.1006 0.213 Uiso 1 1 calc R . . H12B H 0.1376 0.0835 -0.1513 0.213 Uiso 1 1 calc R . . H12C H 0.0801 0.1586 -0.1829 0.213 Uiso 1 1 calc R . . S1 S 0.0441(3) 0.4137(4) 0.3744(4) 0.1058(12) Uiso 0.50 1 d P A 1 C13 C 0.0263(13) 0.4241(15) 0.3619(7) 0.1058(12) Uiso 0.50 1 d PD A 2 C14 C 0.0230(4) 0.5018(5) 0.3142(5) 0.115(2) Uiso 1 1 d D . . H2A H -0.1009(16) 0.205(3) 0.129(5) 0.080(16) Uiso 1 1 d D . . H2B H -0.055(3) 0.251(3) 0.003(3) 0.092(17) Uiso 1 1 d D . . H3B H -0.077(2) 0.090(3) -0.005(3) 0.074(14) Uiso 1 1 d D . . H3A H 0.018(2) 0.084(4) 0.124(6) 0.16(3) Uiso 1 1 d D . . H3C H -0.076(3) 0.088(3) 0.160(4) 0.089(16) Uiso 1 1 d 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 Ta1 0.03987(9) 0.05245(12) 0.05446(11) -0.00195(8) 0.01743(7) -0.00060(8) B1 0.046(3) 0.050(4) 0.051(3) 0.000 0.016(3) 0.000 B2 0.043(2) 0.082(4) 0.046(2) 0.004(2) 0.011(2) -0.004(2) B3 0.061(3) 0.069(4) 0.073(4) -0.024(3) 0.028(3) -0.019(3) C1 0.058(4) 0.057(4) 0.074(4) 0.000 0.027(3) 0.000 C3 0.039(2) 0.067(3) 0.083(3) -0.009(3) 0.025(2) 0.001(2) C4 0.042(2) 0.114(5) 0.060(3) -0.017(3) 0.0188(19) -0.017(3) C5 0.083(4) 0.066(4) 0.130(5) -0.032(4) 0.075(4) -0.029(3) C6 0.065(3) 0.091(5) 0.113(5) 0.047(4) 0.059(3) 0.020(3) C7 0.040(2) 0.108(5) 0.058(3) -0.007(3) 0.0171(18) -0.008(2) C8 0.091(5) 0.078(5) 0.223(9) 0.001(5) 0.078(5) 0.019(4) C9 0.048(3) 0.343(16) 0.081(4) 0.014(6) 0.007(3) -0.016(5) C10 0.182(9) 0.141(8) 0.300(13) -0.143(9) 0.186(10) -0.114(7) C11 0.168(9) 0.229(12) 0.373(17) 0.240(13) 0.199(11) 0.118(9) C12 0.086(4) 0.281(12) 0.065(4) -0.042(5) 0.030(3) -0.043(6) _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 Ta1 B1 2.289(6) . ? Ta1 B2 2.290(5) . ? Ta1 B3 2.301(6) . ? Ta1 B2 2.340(5) 2 ? Ta1 C7 2.380(4) . ? Ta1 C5 2.384(5) . ? Ta1 C4 2.384(4) . ? Ta1 C3 2.388(4) . ? Ta1 C6 2.403(5) . ? Ta1 B3 2.454(5) 2 ? Ta1 Ta1 2.9318(3) 2 ? Ta1 H3A 1.84(8) . ? B1 C1 1.551(11) . ? B1 B2 1.750(6) . ? B1 B2 1.750(6) 2 ? B1 Ta1 2.289(6) 2 ? B2 B3 1.832(9) . ? B2 Ta1 2.340(5) 2 ? B2 H2A 1.097(10) . ? B2 H2B 1.098(10) . ? B3 Ta1 2.454(5) 2 ? B3 H3B 1.100(10) . ? B3 H3A 1.102(10) . ? B3 H3C 1.105(10) . ? C1 C13 1.571(19) . ? C1 C13 1.571(19) 2 ? C1 S1 1.613(7) . ? C1 S1 1.613(7) 2 ? C3 C7 1.373(7) . ? C3 C4 1.401(7) . ? C3 C8 1.508(8) . ? C4 C5 1.409(8) . ? C4 C9 1.487(8) . ? C5 C6 1.425(9) . ? C5 C10 1.495(8) . ? C6 C7 1.400(8) . ? C6 C11 1.481(9) . ? C7 C12 1.521(8) . ? C8 H8C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11A 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? S1 C14 1.636(11) . ? C13 C14 1.41(2) . ? C14 C14 1.377(8) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 Ta1 B2 44.95(15) . . ? B1 Ta1 B3 85.94(18) . . ? B2 Ta1 B3 47.0(2) . . ? B1 Ta1 B2 44.42(14) . 2 ? B2 Ta1 B2 83.2(2) . 2 ? B3 Ta1 B2 104.26(18) . 2 ? B1 Ta1 C7 125.98(17) . . ? B2 Ta1 C7 98.99(18) . . ? B3 Ta1 C7 91.88(18) . . ? B2 Ta1 C7 159.2(2) 2 . ? B1 Ta1 C5 95.81(19) . . ? B2 Ta1 C5 112.3(3) . . ? B3 Ta1 C5 142.4(2) . . ? B2 Ta1 C5 102.90(19) 2 . ? C7 Ta1 C5 57.00(18) . . ? B1 Ta1 C4 125.59(19) . . ? B2 Ta1 C4 144.6(2) . . ? B3 Ta1 C4 143.91(19) . . ? B2 Ta1 C4 110.78(17) 2 . ? C7 Ta1 C4 56.66(16) . . ? C5 Ta1 C4 34.4(2) . . ? B1 Ta1 C3 150.88(18) . . ? B2 Ta1 C3 131.95(17) . . ? B3 Ta1 C3 109.80(19) . . ? B2 Ta1 C3 142.62(17) 2 . ? C7 Ta1 C3 33.46(18) . . ? C5 Ta1 C3 56.63(19) . . ? C4 Ta1 C3 34.13(17) . . ? B1 Ta1 C6 96.26(19) . . ? B2 Ta1 C6 88.20(19) . . ? B3 Ta1 C6 107.8(2) . . ? B2 Ta1 C6 126.1(3) 2 . ? C7 Ta1 C6 34.0(2) . . ? C5 Ta1 C6 34.6(2) . . ? C4 Ta1 C6 57.03(19) . . ? C3 Ta1 C6 56.14(19) . . ? B1 Ta1 B3 82.48(17) . 2 ? B2 Ta1 B3 101.08(18) . 2 ? B3 Ta1 B3 87.1(3) . 2 ? B2 Ta1 B3 44.9(2) 2 2 ? C7 Ta1 B3 151.4(2) . 2 ? C5 Ta1 B3 130.4(3) . 2 ? C4 Ta1 B3 111.73(19) . 2 ? C3 Ta1 B3 121.44(19) . 2 ? C6 Ta1 B3 165.0(3) . 2 ? B1 Ta1 Ta1 50.18(12) . 2 ? B2 Ta1 Ta1 51.47(12) . 2 ? B3 Ta1 Ta1 54.31(13) . 2 ? B2 Ta1 Ta1 49.96(13) 2 2 ? C7 Ta1 Ta1 144.49(11) . 2 ? C5 Ta1 Ta1 145.29(14) . 2 ? C4 Ta1 Ta1 158.79(11) . 2 ? C3 Ta1 Ta1 158.08(13) . 2 ? C6 Ta1 Ta1 138.53(13) . 2 ? B3 Ta1 Ta1 49.63(13) 2 2 ? B1 Ta1 H3A 113.0(8) . . ? B2 Ta1 H3A 74.9(7) . . ? B3 Ta1 H3A 28.1(6) . . ? B2 Ta1 H3A 118.0(17) 2 . ? C7 Ta1 H3A 82.3(18) . . ? C5 Ta1 H3A 139.1(17) . . ? C4 Ta1 H3A 120.5(10) . . ? C3 Ta1 H3A 87.9(12) . . ? C6 Ta1 H3A 110.5(19) . . ? B3 Ta1 H3A 83.5(19) 2 . ? Ta1 Ta1 H3A 71.9(14) 2 . ? C1 B1 B2 118.6(3) . . ? C1 B1 B2 118.6(3) . 2 ? B2 B1 B2 122.8(6) . 2 ? C1 B1 Ta1 140.18(12) . . ? B2 B1 Ta1 67.6(3) . . ? B2 B1 Ta1 69.3(3) 2 . ? C1 B1 Ta1 140.18(12) . 2 ? B2 B1 Ta1 69.3(3) . 2 ? B2 B1 Ta1 67.6(3) 2 2 ? Ta1 B1 Ta1 79.6(2) . 2 ? B1 B2 B3 121.7(4) . . ? B1 B2 Ta1 67.5(2) . . ? B3 B2 Ta1 66.8(3) . . ? B1 B2 Ta1 66.3(2) . 2 ? B3 B2 Ta1 70.9(3) . 2 ? Ta1 B2 Ta1 78.57(16) . 2 ? B1 B2 H2A 97(3) . . ? B3 B2 H2A 79(3) . . ? Ta1 B2 H2A 122(3) . . ? Ta1 B2 H2A 46(3) 2 . ? B1 B2 H2B 122(3) . . ? B3 B2 H2B 114(3) . . ? Ta1 B2 H2B 127(3) . . ? Ta1 B2 H2B 155(3) 2 . ? H2A B2 H2B 109(4) . . ? B2 B3 Ta1 66.1(2) . . ? B2 B3 Ta1 64.3(2) . 2 ? Ta1 B3 Ta1 76.05(17) . 2 ? B2 B3 H3B 114(3) . . ? Ta1 B3 H3B 150(2) . . ? Ta1 B3 H3B 133(2) 2 . ? B2 B3 H3A 117(4) . . ? Ta1 B3 H3A 52(4) . . ? Ta1 B3 H3A 105(3) 2 . ? H3B B3 H3A 115(4) . . ? B2 B3 H3C 110(3) . . ? Ta1 B3 H3C 111(3) . . ? Ta1 B3 H3C 50(3) 2 . ? H3B B3 H3C 98(3) . . ? H3A B3 H3C 100(4) . . ? B1 C1 C13 133.8(7) . . ? B1 C1 C13 133.8(7) . 2 ? C13 C1 C13 92.3(14) . 2 ? B1 C1 S1 124.4(3) . . ? C13 C1 S1 12.5(9) . . ? C13 C1 S1 101.2(7) 2 . ? B1 C1 S1 124.4(3) . 2 ? C13 C1 S1 101.2(7) . 2 ? C13 C1 S1 12.5(9) 2 2 ? S1 C1 S1 111.2(6) . 2 ? C7 C3 C4 109.2(5) . . ? C7 C3 C8 126.0(6) . . ? C4 C3 C8 124.7(6) . . ? C7 C3 Ta1 72.9(3) . . ? C4 C3 Ta1 72.8(3) . . ? C8 C3 Ta1 123.6(4) . . ? C3 C4 C5 107.3(5) . . ? C3 C4 C9 125.5(7) . . ? C5 C4 C9 126.9(7) . . ? C3 C4 Ta1 73.1(2) . . ? C5 C4 Ta1 72.8(3) . . ? C9 C4 Ta1 125.0(4) . . ? C4 C5 C6 107.5(5) . . ? C4 C5 C10 125.5(8) . . ? C6 C5 C10 126.7(9) . . ? C4 C5 Ta1 72.8(3) . . ? C6 C5 Ta1 73.4(3) . . ? C10 C5 Ta1 124.8(4) . . ? C7 C6 C5 107.1(5) . . ? C7 C6 C11 128.6(9) . . ? C5 C6 C11 124.0(9) . . ? C7 C6 Ta1 72.1(3) . . ? C5 C6 Ta1 71.9(3) . . ? C11 C6 Ta1 125.9(4) . . ? C3 C7 C6 108.8(5) . . ? C3 C7 C12 125.1(7) . . ? C6 C7 C12 125.9(7) . . ? C3 C7 Ta1 73.6(3) . . ? C6 C7 Ta1 73.9(3) . . ? C12 C7 Ta1 122.5(3) . . ? C3 C8 H8C 109.5 . . ? C3 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 S1 C14 101.3(4) . . ? C14 C13 C1 114.8(6) . . ? C14 C14 C13 107.5(5) 2 . ? C14 C14 S1 113.1(2) 2 . ? C13 C14 S1 10.0(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 B2 Ta1 B1 C1 -108.2(2) . . . . ? B3 Ta1 B1 C1 -134.60(16) . . . . ? B2 Ta1 B1 C1 110.2(2) 2 . . . ? C7 Ta1 B1 C1 -45.23(16) . . . . ? C5 Ta1 B1 C1 7.71(19) . . . . ? C4 Ta1 B1 C1 26.38(16) . . . . ? C3 Ta1 B1 C1 -9.8(3) . . . . ? C6 Ta1 B1 C1 -27.13(19) . . . . ? B3 Ta1 B1 C1 137.78(17) 2 . . . ? Ta1 Ta1 B1 C1 180.0 2 . . . ? B3 Ta1 B1 B2 -26.4(3) . . . . ? B2 Ta1 B1 B2 -141.5(4) 2 . . . ? C7 Ta1 B1 B2 63.0(3) . . . . ? C5 Ta1 B1 B2 115.9(3) . . . . ? C4 Ta1 B1 B2 134.6(3) . . . . ? C3 Ta1 B1 B2 98.4(3) . . . . ? C6 Ta1 B1 B2 81.1(3) . . . . ? B3 Ta1 B1 B2 -114.0(3) 2 . . . ? Ta1 Ta1 B1 B2 -71.8(2) 2 . . . ? B2 Ta1 B1 B2 141.5(4) . . . 2 ? B3 Ta1 B1 B2 115.2(3) . . . 2 ? C7 Ta1 B1 B2 -155.5(3) . . . 2 ? C5 Ta1 B1 B2 -102.5(3) . . . 2 ? C4 Ta1 B1 B2 -83.9(3) . . . 2 ? C3 Ta1 B1 B2 -120.1(3) . . . 2 ? C6 Ta1 B1 B2 -137.4(3) . . . 2 ? B3 Ta1 B1 B2 27.5(3) 2 . . 2 ? Ta1 Ta1 B1 B2 69.8(2) 2 . . 2 ? B2 Ta1 B1 Ta1 71.8(2) . . . 2 ? B3 Ta1 B1 Ta1 45.40(16) . . . 2 ? B2 Ta1 B1 Ta1 -69.8(2) 2 . . 2 ? C7 Ta1 B1 Ta1 134.77(16) . . . 2 ? C5 Ta1 B1 Ta1 -172.29(19) . . . 2 ? C4 Ta1 B1 Ta1 -153.62(16) . . . 2 ? C3 Ta1 B1 Ta1 170.2(3) . . . 2 ? C6 Ta1 B1 Ta1 152.87(19) . . . 2 ? B3 Ta1 B1 Ta1 -42.22(17) 2 . . 2 ? C1 B1 B2 B3 177.0(3) . . . . ? B2 B1 B2 B3 -3.0(3) 2 . . . ? Ta1 B1 B2 B3 40.8(3) . . . . ? Ta1 B1 B2 B3 -46.2(3) 2 . . . ? C1 B1 B2 Ta1 136.16(9) . . . . ? B2 B1 B2 Ta1 -43.84(9) 2 . . . ? Ta1 B1 B2 Ta1 -87.01(17) 2 . . . ? C1 B1 B2 Ta1 -136.82(9) . . . 2 ? B2 B1 B2 Ta1 43.18(9) 2 . . 2 ? Ta1 B1 B2 Ta1 87.01(17) . . . 2 ? B3 Ta1 B2 B1 142.7(3) . . . . ? B2 Ta1 B2 B1 26.0(3) 2 . . . ? C7 Ta1 B2 B1 -133.1(2) . . . . ? C5 Ta1 B2 B1 -75.2(3) . . . . ? C4 Ta1 B2 B1 -90.7(3) . . . . ? C3 Ta1 B2 B1 -139.7(3) . . . . ? C6 Ta1 B2 B1 -100.7(3) . . . . ? B3 Ta1 B2 B1 67.4(3) 2 . . . ? Ta1 Ta1 B2 B1 68.8(2) 2 . . . ? B1 Ta1 B2 B3 -142.7(3) . . . . ? B2 Ta1 B2 B3 -116.7(3) 2 . . . ? C7 Ta1 B2 B3 84.1(3) . . . . ? C5 Ta1 B2 B3 142.1(2) . . . . ? C4 Ta1 B2 B3 126.6(3) . . . . ? C3 Ta1 B2 B3 77.6(3) . . . . ? C6 Ta1 B2 B3 116.5(3) . . . . ? B3 Ta1 B2 B3 -75.4(3) 2 . . . ? Ta1 Ta1 B2 B3 -73.9(2) 2 . . . ? B1 Ta1 B2 Ta1 -68.8(2) . . . 2 ? B3 Ta1 B2 Ta1 73.9(2) . . . 2 ? B2 Ta1 B2 Ta1 -42.8(2) 2 . . 2 ? C7 Ta1 B2 Ta1 158.04(17) . . . 2 ? C5 Ta1 B2 Ta1 -144.04(17) . . . 2 ? C4 Ta1 B2 Ta1 -159.5(2) . . . 2 ? C3 Ta1 B2 Ta1 151.49(18) . . . 2 ? C6 Ta1 B2 Ta1 -169.6(2) . . . 2 ? B3 Ta1 B2 Ta1 -1.5(2) 2 . . 2 ? B1 B2 B3 Ta1 -41.1(3) . . . . ? Ta1 B2 B3 Ta1 -85.44(14) 2 . . . ? B1 B2 B3 Ta1 44.3(3) . . . 2 ? Ta1 B2 B3 Ta1 85.44(14) . . . 2 ? B1 Ta1 B3 B2 25.4(2) . . . . ? B2 Ta1 B3 B2 66.2(3) 2 . . . ? C7 Ta1 B3 B2 -100.6(2) . . . . ? C5 Ta1 B3 B2 -68.9(4) . . . . ? C4 Ta1 B3 B2 -127.9(4) . . . . ? C3 Ta1 B3 B2 -129.5(2) . . . . ? C6 Ta1 B3 B2 -69.9(3) . . . . ? B3 Ta1 B3 B2 108.1(3) 2 . . . ? Ta1 Ta1 B3 B2 67.7(2) 2 . . . ? B1 Ta1 B3 Ta1 -42.32(15) . . . 2 ? B2 Ta1 B3 Ta1 -67.7(2) . . . 2 ? B2 Ta1 B3 Ta1 -1.5(2) 2 . . 2 ? C7 Ta1 B3 Ta1 -168.26(19) . . . 2 ? C5 Ta1 B3 Ta1 -136.6(3) . . . 2 ? C4 Ta1 B3 Ta1 164.4(3) . . . 2 ? C3 Ta1 B3 Ta1 162.82(16) . . . 2 ? C6 Ta1 B3 Ta1 -137.60(19) . . . 2 ? B3 Ta1 B3 Ta1 40.3(3) 2 . . 2 ? B2 B1 C1 C13 175.3(12) . . . . ? B2 B1 C1 C13 -4.7(12) 2 . . . ? Ta1 B1 C1 C13 -96.2(12) . . . . ? Ta1 B1 C1 C13 83.8(12) 2 . . . ? B2 B1 C1 C13 -4.7(12) . . . 2 ? B2 B1 C1 C13 175.3(12) 2 . . 2 ? Ta1 B1 C1 C13 83.8(12) . . . 2 ? Ta1 B1 C1 C13 -96.2(12) 2 . . 2 ? B2 B1 C1 S1 -174.2(3) . . . . ? B2 B1 C1 S1 5.8(3) 2 . . . ? Ta1 B1 C1 S1 -85.6(3) . . . . ? Ta1 B1 C1 S1 94.4(3) 2 . . . ? B2 B1 C1 S1 5.8(3) . . . 2 ? B2 B1 C1 S1 -174.2(3) 2 . . 2 ? Ta1 B1 C1 S1 94.4(3) . . . 2 ? Ta1 B1 C1 S1 -85.6(3) 2 . . 2 ? B1 Ta1 C3 C7 -58.2(4) . . . . ? B2 Ta1 C3 C7 11.8(4) . . . . ? B3 Ta1 C3 C7 61.2(4) . . . . ? B2 Ta1 C3 C7 -144.3(4) 2 . . . ? C5 Ta1 C3 C7 -79.3(4) . . . . ? C4 Ta1 C3 C7 -117.1(5) . . . . ? C6 Ta1 C3 C7 -37.4(3) . . . . ? B3 Ta1 C3 C7 160.3(3) 2 . . . ? Ta1 Ta1 C3 C7 101.2(4) 2 . . . ? B1 Ta1 C3 C4 58.9(5) . . . . ? B2 Ta1 C3 C4 128.9(4) . . . . ? B3 Ta1 C3 C4 178.3(4) . . . . ? B2 Ta1 C3 C4 -27.2(5) 2 . . . ? C7 Ta1 C3 C4 117.1(5) . . . . ? C5 Ta1 C3 C4 37.8(3) . . . . ? C6 Ta1 C3 C4 79.7(4) . . . . ? B3 Ta1 C3 C4 -82.6(4) 2 . . . ? Ta1 Ta1 C3 C4 -141.7(3) 2 . . . ? B1 Ta1 C3 C8 179.5(4) . . . . ? B2 Ta1 C3 C8 -110.5(6) . . . . ? B3 Ta1 C3 C8 -61.1(6) . . . . ? B2 Ta1 C3 C8 93.4(6) 2 . . . ? C7 Ta1 C3 C8 -122.3(7) . . . . ? C5 Ta1 C3 C8 158.4(6) . . . . ? C4 Ta1 C3 C8 120.6(7) . . . . ? C6 Ta1 C3 C8 -159.7(6) . . . . ? B3 Ta1 C3 C8 38.0(6) 2 . . . ? Ta1 Ta1 C3 C8 -21.1(8) 2 . . . ? C7 C3 C4 C5 -0.9(5) . . . . ? C8 C3 C4 C5 175.5(5) . . . . ? Ta1 C3 C4 C5 -65.2(3) . . . . ? C7 C3 C4 C9 -174.4(5) . . . . ? C8 C3 C4 C9 2.0(8) . . . . ? Ta1 C3 C4 C9 121.3(5) . . . . ? C7 C3 C4 Ta1 64.3(3) . . . . ? C8 C3 C4 Ta1 -119.3(5) . . . . ? B1 Ta1 C4 C3 -149.2(3) . . . . ? B2 Ta1 C4 C3 -88.9(5) . . . . ? B3 Ta1 C4 C3 -2.7(6) . . . . ? B2 Ta1 C4 C3 162.7(3) 2 . . . ? C7 Ta1 C4 C3 -36.0(3) . . . . ? C5 Ta1 C4 C3 -114.9(5) . . . . ? C6 Ta1 C4 C3 -76.9(4) . . . . ? B3 Ta1 C4 C3 114.4(4) 2 . . . ? Ta1 Ta1 C4 C3 140.2(3) 2 . . . ? B1 Ta1 C4 C5 -34.3(4) . . . . ? B2 Ta1 C4 C5 26.0(5) . . . . ? B3 Ta1 C4 C5 112.2(5) . . . . ? B2 Ta1 C4 C5 -82.4(4) 2 . . . ? C7 Ta1 C4 C5 78.9(4) . . . . ? C3 Ta1 C4 C5 114.9(5) . . . . ? C6 Ta1 C4 C5 38.0(3) . . . . ? B3 Ta1 C4 C5 -130.8(4) 2 . . . ? Ta1 Ta1 C4 C5 -104.9(5) 2 . . . ? B1 Ta1 C4 C9 89.0(7) . . . . ? B2 Ta1 C4 C9 149.3(6) . . . . ? B3 Ta1 C4 C9 -124.5(7) . . . . ? B2 Ta1 C4 C9 40.9(7) 2 . . . ? C7 Ta1 C4 C9 -157.8(8) . . . . ? C5 Ta1 C4 C9 123.3(8) . . . . ? C3 Ta1 C4 C9 -121.8(8) . . . . ? C6 Ta1 C4 C9 161.3(8) . . . . ? B3 Ta1 C4 C9 -7.4(7) 2 . . . ? Ta1 Ta1 C4 C9 18.4(10) 2 . . . ? C3 C4 C5 C6 -0.3(5) . . . . ? C9 C4 C5 C6 173.0(5) . . . . ? Ta1 C4 C5 C6 -65.8(3) . . . . ? C3 C4 C5 C10 -173.7(5) . . . . ? C9 C4 C5 C10 -0.3(8) . . . . ? Ta1 C4 C5 C10 120.9(5) . . . . ? C3 C4 C5 Ta1 65.4(3) . . . . ? C9 C4 C5 Ta1 -121.2(5) . . . . ? B1 Ta1 C5 C4 152.5(3) . . . . ? B2 Ta1 C5 C4 -164.1(3) . . . . ? B3 Ta1 C5 C4 -116.6(5) . . . . ? B2 Ta1 C5 C4 108.0(3) 2 . . . ? C7 Ta1 C5 C4 -77.8(3) . . . . ? C3 Ta1 C5 C4 -37.6(3) . . . . ? C6 Ta1 C5 C4 -114.8(5) . . . . ? B3 Ta1 C5 C4 67.5(4) 2 . . . ? Ta1 Ta1 C5 C4 142.1(2) 2 . . . ? B1 Ta1 C5 C6 -92.6(4) . . . . ? B2 Ta1 C5 C6 -49.3(4) . . . . ? B3 Ta1 C5 C6 -1.7(6) . . . . ? B2 Ta1 C5 C6 -137.1(4) 2 . . . ? C7 Ta1 C5 C6 37.0(3) . . . . ? C4 Ta1 C5 C6 114.8(5) . . . . ? C3 Ta1 C5 C6 77.3(4) . . . . ? B3 Ta1 C5 C6 -177.7(3) 2 . . . ? Ta1 Ta1 C5 C6 -103.0(4) 2 . . . ? B1 Ta1 C5 C10 30.9(9) . . . . ? B2 Ta1 C5 C10 74.2(9) . . . . ? B3 Ta1 C5 C10 121.8(9) . . . . ? B2 Ta1 C5 C10 -13.6(9) 2 . . . ? C7 Ta1 C5 C10 160.5(10) . . . . ? C4 Ta1 C5 C10 -121.7(10) . . . . ? C3 Ta1 C5 C10 -159.3(10) . . . . ? C6 Ta1 C5 C10 123.5(11) . . . . ? B3 Ta1 C5 C10 -54.2(10) 2 . . . ? Ta1 Ta1 C5 C10 20.4(11) 2 . . . ? C4 C5 C6 C7 1.4(5) . . . . ? C10 C5 C6 C7 174.7(5) . . . . ? Ta1 C5 C6 C7 -64.0(3) . . . . ? C4 C5 C6 C11 -173.1(5) . . . . ? C10 C5 C6 C11 0.2(8) . . . . ? Ta1 C5 C6 C11 121.6(5) . . . . ? C4 C5 C6 Ta1 65.4(3) . . . . ? C10 C5 C6 Ta1 -121.4(5) . . . . ? B1 Ta1 C6 C7 -153.3(3) . . . . ? B2 Ta1 C6 C7 -109.0(4) . . . . ? B3 Ta1 C6 C7 -65.6(4) . . . . ? B2 Ta1 C6 C7 170.7(3) 2 . . . ? C5 Ta1 C6 C7 115.5(5) . . . . ? C4 Ta1 C6 C7 77.9(3) . . . . ? C3 Ta1 C6 C7 36.7(3) . . . . ? B3 Ta1 C6 C7 122.4(8) 2 . . . ? Ta1 Ta1 C6 C7 -121.4(3) 2 . . . ? B1 Ta1 C6 C5 91.2(4) . . . . ? B2 Ta1 C6 C5 135.5(4) . . . . ? B3 Ta1 C6 C5 178.9(4) . . . . ? B2 Ta1 C6 C5 55.2(4) 2 . . . ? C7 Ta1 C6 C5 -115.5(5) . . . . ? C4 Ta1 C6 C5 -37.6(3) . . . . ? C3 Ta1 C6 C5 -78.8(4) . . . . ? B3 Ta1 C6 C5 6.8(10) 2 . . . ? Ta1 Ta1 C6 C5 123.1(3) 2 . . . ? B1 Ta1 C6 C11 -28.2(10) . . . . ? B2 Ta1 C6 C11 16.1(10) . . . . ? B3 Ta1 C6 C11 59.5(10) . . . . ? B2 Ta1 C6 C11 -64.1(10) 2 . . . ? C7 Ta1 C6 C11 125.1(11) . . . . ? C5 Ta1 C6 C11 -119.4(11) . . . . ? C4 Ta1 C6 C11 -157.0(11) . . . . ? C3 Ta1 C6 C11 161.8(11) . . . . ? B3 Ta1 C6 C11 -112.5(10) 2 . . . ? Ta1 Ta1 C6 C11 3.7(11) 2 . . . ? C4 C3 C7 C6 1.8(5) . . . . ? C8 C3 C7 C6 -174.5(5) . . . . ? Ta1 C3 C7 C6 66.1(3) . . . . ? C4 C3 C7 C12 177.2(5) . . . . ? C8 C3 C7 C12 0.9(8) . . . . ? Ta1 C3 C7 C12 -118.5(5) . . . . ? C4 C3 C7 Ta1 -64.2(3) . . . . ? C8 C3 C7 Ta1 119.5(5) . . . . ? C5 C6 C7 C3 -2.0(5) . . . . ? C11 C6 C7 C3 172.2(5) . . . . ? Ta1 C6 C7 C3 -65.9(3) . . . . ? C5 C6 C7 C12 -177.4(5) . . . . ? C11 C6 C7 C12 -3.2(8) . . . . ? Ta1 C6 C7 C12 118.8(5) . . . . ? C5 C6 C7 Ta1 63.9(3) . . . . ? C11 C6 C7 Ta1 -122.0(6) . . . . ? B1 Ta1 C7 C3 149.3(3) . . . . ? B2 Ta1 C7 C3 -171.1(3) . . . . ? B3 Ta1 C7 C3 -124.4(4) . . . . ? B2 Ta1 C7 C3 94.3(6) 2 . . . ? C5 Ta1 C7 C3 78.1(4) . . . . ? C4 Ta1 C7 C3 36.7(3) . . . . ? C6 Ta1 C7 C3 115.8(4) . . . . ? B3 Ta1 C7 C3 -37.0(6) 2 . . . ? Ta1 Ta1 C7 C3 -140.9(2) 2 . . . ? B1 Ta1 C7 C6 33.5(4) . . . . ? B2 Ta1 C7 C6 73.1(4) . . . . ? B3 Ta1 C7 C6 119.8(4) . . . . ? B2 Ta1 C7 C6 -21.5(7) 2 . . . ? C5 Ta1 C7 C6 -37.7(3) . . . . ? C4 Ta1 C7 C6 -79.1(4) . . . . ? C3 Ta1 C7 C6 -115.8(4) . . . . ? B3 Ta1 C7 C6 -152.8(5) 2 . . . ? Ta1 Ta1 C7 C6 103.3(3) 2 . . . ? B1 Ta1 C7 C12 -89.2(7) . . . . ? B2 Ta1 C7 C12 -49.6(7) . . . . ? B3 Ta1 C7 C12 -2.9(7) . . . . ? B2 Ta1 C7 C12 -144.2(7) 2 . . . ? C5 Ta1 C7 C12 -160.4(8) . . . . ? C4 Ta1 C7 C12 158.3(7) . . . . ? C3 Ta1 C7 C12 121.5(8) . . . . ? C6 Ta1 C7 C12 -122.7(8) . . . . ? B3 Ta1 C7 C12 84.6(7) 2 . . . ? Ta1 Ta1 C7 C12 -19.4(8) 2 . . . ? B1 C1 S1 C14 179.9(3) . . . . ? C13 C1 S1 C14 -38(4) . . . . ? C13 C1 S1 C14 7.7(11) 2 . . . ? S1 C1 S1 C14 -0.1(3) 2 . . . ? B1 C1 C13 C14 174.2(7) . . . . ? C13 C1 C13 C14 -5.8(7) 2 . . . ? S1 C1 C13 C14 130(6) . . . . ? S1 C1 C13 C14 -14.6(18) 2 . . . ? C1 C13 C14 C14 15.5(19) . . . 2 ? C1 C13 C14 S1 -110(5) . . . . ? C1 S1 C14 C14 0.3(9) . . . 2 ? C1 S1 C14 C13 58(4) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.812 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.115 # Attachment '[(C5Me5Ta)2B5H10(C4H4N)] cif file for CCDC.txt' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 814965' #TrackingRef '[(C5Me5Ta)2B5H10(C4H4N)] cif file for CCDC.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H43 B5 N Ta2' _chemical_formula_weight 761.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5841(4) _cell_length_b 10.1872(6) _cell_length_c 17.2208(10) _cell_angle_alpha 98.965(5) _cell_angle_beta 104.066(5) _cell_angle_gamma 106.012(5) _cell_volume 1363.39(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4526 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 24.8 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 730 _exptl_absorpt_coefficient_mu 8.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.367 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8713 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4794 _reflns_number_gt 4018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.1362P)^2^+30.5261P] 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 costr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4794 _refine_ls_number_parameters 299 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2284 _refine_ls_wR_factor_gt 0.2192 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.111 _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 Ta1 Ta 0.30931(7) 0.11897(6) 0.78125(4) 0.0282(3) Uani 1 1 d . . . Ta2 Ta 0.35730(7) 0.23323(6) 0.64040(3) 0.0260(3) Uani 1 1 d . . . N1 N 0.8663(16) 0.3631(16) 0.8149(9) 0.039(3) Uani 1 1 d . . . B1 B 0.144(2) 0.240(3) 0.7015(14) 0.047(5) Uani 1 1 d U . . B2 B 0.367(2) 0.350(2) 0.7679(9) 0.028(3) Uani 1 1 d U . . B3 B 0.538(2) 0.2880(18) 0.7719(11) 0.028(3) Uani 1 1 d U . . B4 B 0.518(2) 0.1183(19) 0.7165(11) 0.031(4) Uani 1 1 d U . . B5 B 0.297(3) -0.0060(17) 0.6572(13) 0.039(4) Uani 1 1 d U . . C1 C 0.7227(19) 0.3871(16) 0.8229(10) 0.030(3) Uani 1 1 d . . . C2 C 0.777(2) 0.5103(19) 0.8834(11) 0.041(4) Uani 1 1 d . . . H2 H 0.7056 0.5546 0.9035 0.050 Uiso 1 1 calc R . . C3 C 0.956(2) 0.558(2) 0.9099(12) 0.056(6) Uani 1 1 d . . . H3 H 1.0264 0.6408 0.9512 0.067 Uiso 1 1 calc R . . C4 C 1.006(2) 0.471(2) 0.8683(16) 0.061(6) Uani 1 1 d . . . H4 H 1.1217 0.4796 0.8735 0.074 Uiso 1 1 calc R . . C5 C 0.470(2) 0.058(2) 0.8948(11) 0.044(4) Uani 1 1 d U . . C6 C 0.325(3) -0.0692(19) 0.8469(11) 0.045(4) Uani 1 1 d U . . C7 C 0.179(2) -0.032(2) 0.8551(11) 0.043(4) Uani 1 1 d U . . C8 C 0.241(3) 0.1050(19) 0.9049(12) 0.049(5) Uani 1 1 d U . . C9 C 0.407(3) 0.157(2) 0.9296(10) 0.045(4) Uani 1 1 d U . . C10 C 0.656(3) 0.070(4) 0.9138(16) 0.097(11) Uani 1 1 d . . . H10A H 0.6880 0.0644 0.8628 0.145 Uiso 1 1 calc R . . H10B H 0.6749 -0.0069 0.9385 0.145 Uiso 1 1 calc R . . H10C H 0.7259 0.1603 0.9526 0.145 Uiso 1 1 calc R . . C11 C 0.334(7) -0.203(3) 0.803(2) 0.15(2) Uani 1 1 d . . . H11A H 0.3325 -0.2683 0.8387 0.224 Uiso 1 1 calc R . . H11B H 0.4396 -0.1835 0.7875 0.224 Uiso 1 1 calc R . . H11C H 0.2365 -0.2440 0.7529 0.224 Uiso 1 1 calc R . . C12 C -0.004(3) -0.131(4) 0.817(2) 0.105(12) Uani 1 1 d . . . H12A H -0.0466 -0.1677 0.8596 0.158 Uiso 1 1 calc R . . H12B H -0.0079 -0.2090 0.7745 0.158 Uiso 1 1 calc R . . H12C H -0.0758 -0.0792 0.7916 0.158 Uiso 1 1 calc R . . C13 C 0.121(4) 0.173(3) 0.9361(18) 0.085(9) Uani 1 1 d . . . H13A H 0.1627 0.2744 0.9418 0.127 Uiso 1 1 calc R . . H13B H 0.1170 0.1535 0.9898 0.127 Uiso 1 1 calc R . . H13C H 0.0064 0.1328 0.8967 0.127 Uiso 1 1 calc R . . C14 C 0.520(4) 0.297(3) 0.9860(15) 0.091(10) Uani 1 1 d . . . H14A H 0.5000 0.3726 0.9607 0.136 Uiso 1 1 calc R . . H14B H 0.6392 0.3020 0.9953 0.136 Uiso 1 1 calc R . . H14C H 0.4953 0.3064 1.0388 0.136 Uiso 1 1 calc R . . C15 C 0.271(2) 0.3095(17) 0.5202(9) 0.029(3) Uani 1 1 d . . . C16 C 0.393(2) 0.2530(17) 0.5122(10) 0.037(4) Uani 1 1 d . . . C17 C 0.551(2) 0.340(2) 0.5716(12) 0.043(4) Uani 1 1 d . . . C18 C 0.519(2) 0.4513(17) 0.6175(11) 0.046(5) Uani 1 1 d . . . C19 C 0.341(2) 0.4318(18) 0.5844(10) 0.033(3) Uani 1 1 d . . . C20 C 0.086(2) 0.257(3) 0.4627(14) 0.060(6) Uani 1 1 d . . . H20A H 0.0870 0.2466 0.4053 0.089 Uiso 1 1 calc R . . H20B H 0.0295 0.3248 0.4758 0.089 Uiso 1 1 calc R . . H20C H 0.0254 0.1656 0.4706 0.089 Uiso 1 1 calc R . . C21 C 0.383(5) 0.127(3) 0.4436(16) 0.090(10) Uani 1 1 d . . . H21A H 0.2820 0.0464 0.4369 0.135 Uiso 1 1 calc R . . H21B H 0.4849 0.1000 0.4597 0.135 Uiso 1 1 calc R . . H21C H 0.3743 0.1551 0.3913 0.135 Uiso 1 1 calc R . . C22 C 0.727(3) 0.326(4) 0.579(2) 0.093(11) Uani 1 1 d . . . H22A H 0.7991 0.4086 0.5676 0.140 Uiso 1 1 calc R . . H22B H 0.7155 0.2410 0.5396 0.140 Uiso 1 1 calc R . . H22C H 0.7780 0.3193 0.6353 0.140 Uiso 1 1 calc R . . C23 C 0.647(3) 0.576(3) 0.6789(14) 0.085(10) Uani 1 1 d . . . H23A H 0.7192 0.5462 0.7209 0.127 Uiso 1 1 calc R . . H23B H 0.5896 0.6328 0.7050 0.127 Uiso 1 1 calc R . . H23C H 0.7176 0.6333 0.6512 0.127 Uiso 1 1 calc R . . C24 C 0.254(4) 0.529(2) 0.6103(15) 0.065(6) Uani 1 1 d . . . H24A H 0.2636 0.6017 0.5786 0.097 Uiso 1 1 calc R . . H24B H 0.3071 0.5742 0.6692 0.097 Uiso 1 1 calc R . . H24C H 0.1337 0.4773 0.6004 0.097 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 Ta1 0.0235(4) 0.0318(4) 0.0250(4) 0.0054(3) 0.0055(3) 0.0049(3) Ta2 0.0226(4) 0.0306(4) 0.0225(4) 0.0040(3) 0.0055(3) 0.0075(3) N1 0.020(6) 0.049(8) 0.043(8) -0.003(6) 0.015(6) 0.004(6) B1 0.017(7) 0.073(15) 0.042(11) 0.007(10) 0.008(7) 0.008(8) B2 0.023(7) 0.053(10) 0.009(7) 0.003(6) 0.010(6) 0.014(7) B3 0.024(7) 0.027(7) 0.025(8) 0.001(6) 0.002(6) 0.005(6) B4 0.033(8) 0.032(8) 0.024(8) 0.000(6) 0.012(7) 0.005(6) B5 0.049(10) 0.012(7) 0.044(11) 0.004(7) 0.000(8) 0.006(6) C1 0.022(7) 0.036(8) 0.036(8) 0.016(7) 0.006(6) 0.014(6) C2 0.029(8) 0.041(9) 0.042(10) -0.002(8) -0.002(7) 0.010(7) C3 0.030(10) 0.056(12) 0.045(11) -0.008(9) -0.011(8) -0.011(9) C4 0.017(8) 0.050(12) 0.097(17) -0.004(11) 0.005(9) 0.004(8) C5 0.043(9) 0.078(12) 0.030(8) 0.030(8) 0.025(7) 0.029(9) C6 0.074(8) 0.038(7) 0.033(7) 0.024(6) 0.019(6) 0.025(6) C7 0.049(10) 0.054(10) 0.029(8) 0.013(7) 0.013(7) 0.019(8) C8 0.066(11) 0.035(9) 0.048(10) 0.017(7) -0.007(9) 0.035(8) C9 0.052(10) 0.062(11) 0.023(8) 0.012(7) 0.023(7) 0.009(9) C10 0.048(13) 0.21(4) 0.058(15) 0.069(19) 0.022(11) 0.063(19) C11 0.34(7) 0.055(16) 0.08(2) 0.023(15) 0.05(3) 0.11(3) C12 0.055(15) 0.12(3) 0.10(2) 0.05(2) -0.001(15) -0.024(16) C13 0.084(18) 0.13(3) 0.082(18) 0.033(17) 0.048(15) 0.071(19) C14 0.11(2) 0.071(17) 0.043(13) -0.014(12) -0.002(14) 0.000(16) C15 0.032(8) 0.038(8) 0.019(7) 0.014(6) 0.004(6) 0.014(7) C16 0.042(9) 0.029(8) 0.033(9) 0.012(7) -0.007(7) 0.012(7) C17 0.024(8) 0.068(12) 0.057(11) 0.042(10) 0.017(8) 0.026(8) C18 0.044(10) 0.024(8) 0.044(10) 0.016(7) -0.001(8) -0.020(7) C19 0.035(8) 0.039(9) 0.033(8) 0.017(7) 0.010(7) 0.017(7) C20 0.028(9) 0.074(14) 0.055(12) 0.012(10) -0.008(9) 0.002(9) C21 0.17(3) 0.066(15) 0.059(15) 0.013(12) 0.038(17) 0.08(2) C22 0.055(14) 0.14(3) 0.14(3) 0.12(2) 0.046(16) 0.067(17) C23 0.078(17) 0.085(18) 0.037(12) 0.017(11) -0.011(11) -0.032(14) C24 0.098(18) 0.054(13) 0.062(14) 0.011(10) 0.042(13) 0.042(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 B5 2.27(2) . ? Ta1 B3 2.285(18) . ? Ta1 B4 2.330(18) . ? Ta1 B2 2.33(2) . ? Ta1 C8 2.36(2) . ? Ta1 C7 2.361(19) . ? Ta1 C5 2.377(17) . ? Ta1 C6 2.390(16) . ? Ta1 C9 2.419(17) . ? Ta1 B1 2.44(2) . ? Ta1 Ta2 2.9171(9) . ? Ta2 B3 2.296(17) . ? Ta2 B2 2.298(15) . ? Ta2 B1 2.33(2) . ? Ta2 C16 2.332(18) . ? Ta2 B4 2.34(2) . ? Ta2 C15 2.347(14) . ? Ta2 C17 2.391(17) . ? Ta2 C19 2.397(16) . ? Ta2 C18 2.419(15) . ? Ta2 B5 2.426(17) . ? N1 C1 1.36(2) . ? N1 C4 1.39(2) . ? B1 B2 1.89(3) . ? B2 B3 1.74(2) . ? B3 C1 1.57(2) . ? B3 B4 1.78(2) . ? B4 B5 1.89(3) . ? C1 C2 1.38(2) . ? C2 C3 1.41(2) . ? C2 H2 0.9500 . ? C3 C4 1.29(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C9 1.40(3) . ? C5 C6 1.48(3) . ? C5 C10 1.52(3) . ? C6 C7 1.44(3) . ? C6 C11 1.48(3) . ? C7 C8 1.40(3) . ? C7 C12 1.53(3) . ? C8 C9 1.31(3) . ? C8 C13 1.54(3) . ? C9 C14 1.50(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.35(2) . ? C15 C19 1.40(2) . ? C15 C20 1.54(2) . ? C16 C17 1.43(2) . ? C16 C21 1.57(3) . ? C17 C18 1.41(3) . ? C17 C22 1.53(3) . ? C18 C19 1.44(3) . ? C18 C23 1.48(3) . ? C19 C24 1.47(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B5 Ta1 B3 87.3(7) . . ? B5 Ta1 B4 48.5(7) . . ? B3 Ta1 B4 45.4(6) . . ? B5 Ta1 B2 104.5(6) . . ? B3 Ta1 B2 44.3(6) . . ? B4 Ta1 B2 83.5(6) . . ? B5 Ta1 C8 145.1(7) . . ? B3 Ta1 C8 123.8(7) . . ? B4 Ta1 C8 144.4(6) . . ? B2 Ta1 C8 109.1(5) . . ? B5 Ta1 C7 110.6(7) . . ? B3 Ta1 C7 150.8(6) . . ? B4 Ta1 C7 133.3(7) . . ? B2 Ta1 C7 140.9(6) . . ? C8 Ta1 C7 34.5(6) . . ? B5 Ta1 C5 113.1(7) . . ? B3 Ta1 C5 94.3(6) . . ? B4 Ta1 C5 89.8(6) . . ? B2 Ta1 C5 122.0(7) . . ? C8 Ta1 C5 55.1(6) . . ? C7 Ta1 C5 57.9(6) . . ? B5 Ta1 C6 93.3(6) . . ? B3 Ta1 C6 125.0(7) . . ? B4 Ta1 C6 98.8(7) . . ? B2 Ta1 C6 157.5(6) . . ? C8 Ta1 C6 57.2(6) . . ? C7 Ta1 C6 35.2(7) . . ? C5 Ta1 C6 36.2(7) . . ? B5 Ta1 C9 146.9(7) . . ? B3 Ta1 C9 95.9(6) . . ? B4 Ta1 C9 114.8(7) . . ? B2 Ta1 C9 100.6(6) . . ? C8 Ta1 C9 31.7(6) . . ? C7 Ta1 C9 56.4(6) . . ? C5 Ta1 C9 33.9(7) . . ? C6 Ta1 C9 58.0(7) . . ? B5 Ta1 B1 85.7(7) . . ? B3 Ta1 B1 84.1(7) . . ? B4 Ta1 B1 102.2(7) . . ? B2 Ta1 B1 46.6(7) . . ? C8 Ta1 B1 110.6(6) . . ? C7 Ta1 B1 118.9(7) . . ? C5 Ta1 B1 161.1(7) . . ? C6 Ta1 B1 150.8(7) . . ? C9 Ta1 B1 127.4(7) . . ? B5 Ta1 Ta2 54.0(5) . . ? B3 Ta1 Ta2 50.6(4) . . ? B4 Ta1 Ta2 51.5(5) . . ? B2 Ta1 Ta2 50.4(4) . . ? C8 Ta1 Ta2 157.8(4) . . ? C7 Ta1 Ta2 158.2(4) . . ? C5 Ta1 Ta2 139.1(4) . . ? C6 Ta1 Ta2 145.0(5) . . ? C9 Ta1 Ta2 145.2(5) . . ? B1 Ta1 Ta2 50.6(5) . . ? B3 Ta2 B2 44.5(6) . . ? B3 Ta2 B1 86.5(7) . . ? B2 Ta2 B1 48.3(7) . . ? B3 Ta2 C16 134.7(6) . . ? B2 Ta2 C16 146.3(6) . . ? B1 Ta2 C16 134.8(7) . . ? B3 Ta2 B4 45.2(6) . . ? B2 Ta2 B4 83.9(6) . . ? B1 Ta2 B4 105.3(7) . . ? C16 Ta2 B4 117.1(6) . . ? B3 Ta2 C15 147.2(6) . . ? B2 Ta2 C15 122.5(6) . . ? B1 Ta2 C15 102.6(7) . . ? C16 Ta2 C15 33.5(6) . . ? B4 Ta2 C15 150.6(6) . . ? B3 Ta2 C17 100.1(6) . . ? B2 Ta2 C17 120.0(7) . . ? B1 Ta2 C17 149.7(8) . . ? C16 Ta2 C17 35.3(6) . . ? B4 Ta2 C17 100.0(6) . . ? C15 Ta2 C17 57.2(6) . . ? B3 Ta2 C19 114.8(6) . . ? B2 Ta2 C19 91.4(6) . . ? B1 Ta2 C19 93.0(8) . . ? C16 Ta2 C19 56.9(6) . . ? B4 Ta2 C19 150.2(6) . . ? C15 Ta2 C19 34.4(6) . . ? C17 Ta2 C19 57.3(6) . . ? B3 Ta2 C18 90.3(6) . . ? B2 Ta2 C18 90.2(7) . . ? B1 Ta2 C18 117.2(8) . . ? C16 Ta2 C18 57.6(6) . . ? B4 Ta2 C18 115.5(7) . . ? C15 Ta2 C18 57.4(6) . . ? C17 Ta2 C18 34.2(7) . . ? C19 Ta2 C18 34.8(6) . . ? B3 Ta2 B5 83.6(6) . . ? B2 Ta2 B5 100.7(7) . . ? B1 Ta2 B5 84.9(9) . . ? C16 Ta2 B5 112.9(7) . . ? B4 Ta2 B5 46.7(7) . . ? C15 Ta2 B5 128.2(6) . . ? C17 Ta2 B5 125.1(7) . . ? C19 Ta2 B5 161.4(6) . . ? C18 Ta2 B5 156.8(8) . . ? B3 Ta2 Ta1 50.3(5) . . ? B2 Ta2 Ta1 51.4(5) . . ? B1 Ta2 Ta1 54.1(6) . . ? C16 Ta2 Ta1 162.0(4) . . ? B4 Ta2 Ta1 51.2(4) . . ? C15 Ta2 Ta1 155.0(4) . . ? C17 Ta2 Ta1 147.6(4) . . ? C19 Ta2 Ta1 140.6(4) . . ? C18 Ta2 Ta1 137.3(4) . . ? B5 Ta2 Ta1 49.3(5) . . ? C1 N1 C4 109.2(15) . . ? B2 B1 Ta2 64.9(7) . . ? B2 B1 Ta1 63.5(9) . . ? Ta2 B1 Ta1 75.2(6) . . ? B3 B2 B1 121.5(14) . . ? B3 B2 Ta2 67.7(8) . . ? B1 B2 Ta2 66.8(8) . . ? B3 B2 Ta1 66.5(9) . . ? B1 B2 Ta1 69.9(10) . . ? Ta2 B2 Ta1 78.1(6) . . ? C1 B3 B2 119.5(13) . . ? C1 B3 B4 116.8(13) . . ? B2 B3 B4 123.6(13) . . ? C1 B3 Ta1 142.4(12) . . ? B2 B3 Ta1 69.3(9) . . ? B4 B3 Ta1 68.6(8) . . ? C1 B3 Ta2 138.5(12) . . ? B2 B3 Ta2 67.8(7) . . ? B4 B3 Ta2 68.8(8) . . ? Ta1 B3 Ta2 79.1(5) . . ? B3 B4 B5 118.0(13) . . ? B3 B4 Ta1 66.0(8) . . ? B5 B4 Ta1 64.2(9) . . ? B3 B4 Ta2 66.1(8) . . ? B5 B4 Ta2 69.0(8) . . ? Ta1 B4 Ta2 77.3(6) . . ? B4 B5 Ta1 67.3(8) . . ? B4 B5 Ta2 64.3(8) . . ? Ta1 B5 Ta2 76.7(5) . . ? N1 C1 C2 105.6(14) . . ? N1 C1 B3 124.1(14) . . ? C2 C1 B3 130.3(14) . . ? C1 C2 C3 107.9(16) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? C4 C3 C2 108.1(17) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? C3 C4 N1 109.2(16) . . ? C3 C4 H4 125.4 . . ? N1 C4 H4 125.4 . . ? C9 C5 C6 108.2(16) . . ? C9 C5 C10 125(2) . . ? C6 C5 C10 126(2) . . ? C9 C5 Ta1 74.7(11) . . ? C6 C5 Ta1 72.4(9) . . ? C10 C5 Ta1 126.1(14) . . ? C7 C6 C5 103.7(15) . . ? C7 C6 C11 130(3) . . ? C5 C6 C11 126(3) . . ? C7 C6 Ta1 71.3(10) . . ? C5 C6 Ta1 71.4(9) . . ? C11 C6 Ta1 121.7(16) . . ? C8 C7 C6 106.7(17) . . ? C8 C7 C12 130(2) . . ? C6 C7 C12 124(2) . . ? C8 C7 Ta1 72.6(12) . . ? C6 C7 Ta1 73.5(10) . . ? C12 C7 Ta1 120.6(15) . . ? C9 C8 C7 113.3(18) . . ? C9 C8 C13 125(2) . . ? C7 C8 C13 121(2) . . ? C9 C8 Ta1 76.8(13) . . ? C7 C8 Ta1 73.0(12) . . ? C13 C8 Ta1 125.8(14) . . ? C8 C9 C5 108.1(18) . . ? C8 C9 C14 129(2) . . ? C5 C9 C14 123(2) . . ? C8 C9 Ta1 71.5(12) . . ? C5 C9 Ta1 71.4(10) . . ? C14 C9 Ta1 123.2(15) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C19 109.9(14) . . ? C16 C15 C20 125.5(16) . . ? C19 C15 C20 124.4(16) . . ? C16 C15 Ta2 72.7(9) . . ? C19 C15 Ta2 74.8(9) . . ? C20 C15 Ta2 123.7(13) . . ? C15 C16 C17 109.0(15) . . ? C15 C16 C21 128.9(18) . . ? C17 C16 C21 122(2) . . ? C15 C16 Ta2 73.8(10) . . ? C17 C16 Ta2 74.6(10) . . ? C21 C16 Ta2 124.4(14) . . ? C18 C17 C16 107.0(15) . . ? C18 C17 C22 125(2) . . ? C16 C17 C22 127(2) . . ? C18 C17 Ta2 74.0(10) . . ? C16 C17 Ta2 70.1(10) . . ? C22 C17 Ta2 126.0(13) . . ? C17 C18 C19 107.0(14) . . ? C17 C18 C23 126(2) . . ? C19 C18 C23 126(2) . . ? C17 C18 Ta2 71.8(9) . . ? C19 C18 Ta2 71.7(9) . . ? C23 C18 Ta2 128.7(14) . . ? C15 C19 C18 107.1(15) . . ? C15 C19 C24 127.4(17) . . ? C18 C19 C24 125.3(18) . . ? C15 C19 Ta2 70.9(9) . . ? C18 C19 Ta2 73.4(9) . . ? C24 C19 Ta2 124.3(14) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B5 Ta1 Ta2 B3 -121.4(9) . . . . ? B4 Ta1 Ta2 B3 -59.4(8) . . . . ? B2 Ta1 Ta2 B3 58.5(8) . . . . ? C8 Ta1 Ta2 B3 84.0(14) . . . . ? C7 Ta1 Ta2 B3 -171.5(13) . . . . ? C5 Ta1 Ta2 B3 -37.1(10) . . . . ? C6 Ta1 Ta2 B3 -97.0(11) . . . . ? C9 Ta1 Ta2 B3 18.8(11) . . . . ? B1 Ta1 Ta2 B3 120.1(9) . . . . ? B5 Ta1 Ta2 B2 -179.9(8) . . . . ? B3 Ta1 Ta2 B2 -58.5(8) . . . . ? B4 Ta1 Ta2 B2 -117.9(8) . . . . ? C8 Ta1 Ta2 B2 25.5(14) . . . . ? C7 Ta1 Ta2 B2 130.1(13) . . . . ? C5 Ta1 Ta2 B2 -95.5(9) . . . . ? C6 Ta1 Ta2 B2 -155.5(11) . . . . ? C9 Ta1 Ta2 B2 -39.7(10) . . . . ? B1 Ta1 Ta2 B2 61.7(9) . . . . ? B5 Ta1 Ta2 B1 118.4(10) . . . . ? B3 Ta1 Ta2 B1 -120.1(9) . . . . ? B4 Ta1 Ta2 B1 -179.6(8) . . . . ? B2 Ta1 Ta2 B1 -61.7(9) . . . . ? C8 Ta1 Ta2 B1 -36.2(15) . . . . ? C7 Ta1 Ta2 B1 68.4(14) . . . . ? C5 Ta1 Ta2 B1 -157.2(11) . . . . ? C6 Ta1 Ta2 B1 142.9(11) . . . . ? C9 Ta1 Ta2 B1 -101.4(11) . . . . ? B5 Ta1 Ta2 C16 -7.8(15) . . . . ? B3 Ta1 Ta2 C16 113.6(15) . . . . ? B4 Ta1 Ta2 C16 54.2(15) . . . . ? B2 Ta1 Ta2 C16 172.1(15) . . . . ? C8 Ta1 Ta2 C16 -162.4(18) . . . . ? C7 Ta1 Ta2 C16 -57.8(19) . . . . ? C5 Ta1 Ta2 C16 76.6(16) . . . . ? C6 Ta1 Ta2 C16 16.6(17) . . . . ? C9 Ta1 Ta2 C16 132.4(16) . . . . ? B1 Ta1 Ta2 C16 -126.2(15) . . . . ? B5 Ta1 Ta2 B4 -62.0(9) . . . . ? B3 Ta1 Ta2 B4 59.4(8) . . . . ? B2 Ta1 Ta2 B4 117.9(8) . . . . ? C8 Ta1 Ta2 B4 143.4(14) . . . . ? C7 Ta1 Ta2 B4 -112.0(13) . . . . ? C5 Ta1 Ta2 B4 22.4(10) . . . . ? C6 Ta1 Ta2 B4 -37.5(11) . . . . ? C9 Ta1 Ta2 B4 78.2(10) . . . . ? B1 Ta1 Ta2 B4 179.6(8) . . . . ? B5 Ta1 Ta2 C15 95.0(11) . . . . ? B3 Ta1 Ta2 C15 -143.6(11) . . . . ? B4 Ta1 Ta2 C15 157.0(11) . . . . ? B2 Ta1 Ta2 C15 -85.1(11) . . . . ? C8 Ta1 Ta2 C15 -59.6(16) . . . . ? C7 Ta1 Ta2 C15 45.0(15) . . . . ? C5 Ta1 Ta2 C15 179.4(12) . . . . ? C6 Ta1 Ta2 C15 119.4(13) . . . . ? C9 Ta1 Ta2 C15 -124.8(13) . . . . ? B1 Ta1 Ta2 C15 -23.4(11) . . . . ? B5 Ta1 Ta2 C17 -93.5(12) . . . . ? B3 Ta1 Ta2 C17 28.0(11) . . . . ? B4 Ta1 Ta2 C17 -31.5(11) . . . . ? B2 Ta1 Ta2 C17 86.4(11) . . . . ? C8 Ta1 Ta2 C17 111.9(16) . . . . ? C7 Ta1 Ta2 C17 -143.5(16) . . . . ? C5 Ta1 Ta2 C17 -9.1(12) . . . . ? C6 Ta1 Ta2 C17 -69.0(13) . . . . ? C9 Ta1 Ta2 C17 46.8(13) . . . . ? B1 Ta1 Ta2 C17 148.1(12) . . . . ? B5 Ta1 Ta2 C19 157.2(9) . . . . ? B3 Ta1 Ta2 C19 -81.3(9) . . . . ? B4 Ta1 Ta2 C19 -140.8(8) . . . . ? B2 Ta1 Ta2 C19 -22.8(9) . . . . ? C8 Ta1 Ta2 C19 2.7(15) . . . . ? C7 Ta1 Ta2 C19 107.2(14) . . . . ? C5 Ta1 Ta2 C19 -118.4(10) . . . . ? C6 Ta1 Ta2 C19 -178.3(10) . . . . ? C9 Ta1 Ta2 C19 -62.5(11) . . . . ? B1 Ta1 Ta2 C19 38.8(9) . . . . ? B5 Ta1 Ta2 C18 -148.8(10) . . . . ? B3 Ta1 Ta2 C18 -27.3(10) . . . . ? B4 Ta1 Ta2 C18 -86.8(10) . . . . ? B2 Ta1 Ta2 C18 31.2(10) . . . . ? C8 Ta1 Ta2 C18 56.7(15) . . . . ? C7 Ta1 Ta2 C18 161.2(14) . . . . ? C5 Ta1 Ta2 C18 -64.4(11) . . . . ? C6 Ta1 Ta2 C18 -124.3(12) . . . . ? C9 Ta1 Ta2 C18 -8.5(12) . . . . ? B1 Ta1 Ta2 C18 92.8(10) . . . . ? B3 Ta1 Ta2 B5 121.4(9) . . . . ? B4 Ta1 Ta2 B5 62.0(9) . . . . ? B2 Ta1 Ta2 B5 179.9(8) . . . . ? C8 Ta1 Ta2 B5 -154.6(15) . . . . ? C7 Ta1 Ta2 B5 -50.0(14) . . . . ? C5 Ta1 Ta2 B5 84.4(10) . . . . ? C6 Ta1 Ta2 B5 24.5(11) . . . . ? C9 Ta1 Ta2 B5 140.2(11) . . . . ? B1 Ta1 Ta2 B5 -118.4(10) . . . . ? B3 Ta2 B1 B2 25.5(10) . . . . ? C16 Ta2 B1 B2 -133.2(9) . . . . ? B4 Ta2 B1 B2 67.0(10) . . . . ? C15 Ta2 B1 B2 -122.6(9) . . . . ? C17 Ta2 B1 B2 -78.6(16) . . . . ? C19 Ta2 B1 B2 -89.2(10) . . . . ? C18 Ta2 B1 B2 -63.0(11) . . . . ? B5 Ta2 B1 B2 109.3(10) . . . . ? Ta1 Ta2 B1 B2 67.3(8) . . . . ? B3 Ta2 B1 Ta1 -41.8(6) . . . . ? B2 Ta2 B1 Ta1 -67.3(8) . . . . ? C16 Ta2 B1 Ta1 159.5(6) . . . . ? B4 Ta2 B1 Ta1 -0.3(6) . . . . ? C15 Ta2 B1 Ta1 170.1(5) . . . . ? C17 Ta2 B1 Ta1 -145.9(11) . . . . ? C19 Ta2 B1 Ta1 -156.5(6) . . . . ? C18 Ta2 B1 Ta1 -130.4(6) . . . . ? B5 Ta2 B1 Ta1 42.0(6) . . . . ? B5 Ta1 B1 B2 -114.6(9) . . . . ? B3 Ta1 B1 B2 -26.8(8) . . . . ? B4 Ta1 B1 B2 -68.7(8) . . . . ? C8 Ta1 B1 B2 97.2(9) . . . . ? C7 Ta1 B1 B2 134.2(8) . . . . ? C5 Ta1 B1 B2 59(2) . . . . ? C6 Ta1 B1 B2 156.3(12) . . . . ? C9 Ta1 B1 B2 66.2(10) . . . . ? Ta2 Ta1 B1 B2 -69.0(7) . . . . ? B5 Ta1 B1 Ta2 -45.6(7) . . . . ? B3 Ta1 B1 Ta2 42.2(6) . . . . ? B4 Ta1 B1 Ta2 0.3(6) . . . . ? B2 Ta1 B1 Ta2 69.0(7) . . . . ? C8 Ta1 B1 Ta2 166.2(6) . . . . ? C7 Ta1 B1 Ta2 -156.8(5) . . . . ? C5 Ta1 B1 Ta2 128.4(19) . . . . ? C6 Ta1 B1 Ta2 -134.7(12) . . . . ? C9 Ta1 B1 Ta2 135.2(7) . . . . ? Ta2 B1 B2 B3 -41.7(13) . . . . ? Ta1 B1 B2 B3 43.7(13) . . . . ? Ta1 B1 B2 Ta2 85.3(5) . . . . ? Ta2 B1 B2 Ta1 -85.3(5) . . . . ? B1 Ta2 B2 B3 142.2(14) . . . . ? C16 Ta2 B2 B3 -106.4(12) . . . . ? B4 Ta2 B2 B3 25.4(9) . . . . ? C15 Ta2 B2 B3 -140.7(9) . . . . ? C17 Ta2 B2 B3 -72.6(10) . . . . ? C19 Ta2 B2 B3 -125.0(9) . . . . ? C18 Ta2 B2 B3 -90.2(10) . . . . ? B5 Ta2 B2 B3 69.2(9) . . . . ? Ta1 Ta2 B2 B3 69.2(8) . . . . ? B3 Ta2 B2 B1 -142.2(14) . . . . ? C16 Ta2 B2 B1 111.4(13) . . . . ? B4 Ta2 B2 B1 -116.8(11) . . . . ? C15 Ta2 B2 B1 77.1(12) . . . . ? C17 Ta2 B2 B1 145.2(10) . . . . ? C19 Ta2 B2 B1 92.8(11) . . . . ? C18 Ta2 B2 B1 127.6(11) . . . . ? B5 Ta2 B2 B1 -73.0(11) . . . . ? Ta1 Ta2 B2 B1 -73.0(10) . . . . ? B3 Ta2 B2 Ta1 -69.2(8) . . . . ? B1 Ta2 B2 Ta1 73.0(10) . . . . ? C16 Ta2 B2 Ta1 -175.6(8) . . . . ? B4 Ta2 B2 Ta1 -43.8(6) . . . . ? C15 Ta2 B2 Ta1 150.1(5) . . . . ? C17 Ta2 B2 Ta1 -141.9(5) . . . . ? C19 Ta2 B2 Ta1 165.7(5) . . . . ? C18 Ta2 B2 Ta1 -159.4(6) . . . . ? B5 Ta2 B2 Ta1 -0.1(6) . . . . ? B5 Ta1 B2 B3 -70.5(9) . . . . ? B4 Ta1 B2 B3 -26.5(8) . . . . ? C8 Ta1 B2 B3 119.3(9) . . . . ? C7 Ta1 B2 B3 136.1(10) . . . . ? C5 Ta1 B2 B3 59.2(9) . . . . ? C6 Ta1 B2 B3 70.8(18) . . . . ? C9 Ta1 B2 B3 87.6(9) . . . . ? B1 Ta1 B2 B3 -140.0(12) . . . . ? Ta2 Ta1 B2 B3 -70.6(7) . . . . ? B5 Ta1 B2 B1 69.5(9) . . . . ? B3 Ta1 B2 B1 140.0(12) . . . . ? B4 Ta1 B2 B1 113.6(9) . . . . ? C8 Ta1 B2 B1 -100.7(9) . . . . ? C7 Ta1 B2 B1 -83.8(12) . . . . ? C5 Ta1 B2 B1 -160.8(9) . . . . ? C6 Ta1 B2 B1 -149.2(16) . . . . ? C9 Ta1 B2 B1 -132.3(9) . . . . ? Ta2 Ta1 B2 B1 69.4(8) . . . . ? B5 Ta1 B2 Ta2 0.1(6) . . . . ? B3 Ta1 B2 Ta2 70.6(7) . . . . ? B4 Ta1 B2 Ta2 44.1(5) . . . . ? C8 Ta1 B2 Ta2 -170.1(5) . . . . ? C7 Ta1 B2 Ta2 -153.3(7) . . . . ? C5 Ta1 B2 Ta2 129.8(5) . . . . ? C6 Ta1 B2 Ta2 141.4(15) . . . . ? C9 Ta1 B2 Ta2 158.2(6) . . . . ? B1 Ta1 B2 Ta2 -69.4(8) . . . . ? B1 B2 B3 C1 175.7(15) . . . . ? Ta2 B2 B3 C1 134.3(15) . . . . ? Ta1 B2 B3 C1 -139.3(15) . . . . ? B1 B2 B3 B4 -1(2) . . . . ? Ta2 B2 B3 B4 -42.3(13) . . . . ? Ta1 B2 B3 B4 44.0(13) . . . . ? B1 B2 B3 Ta1 -45.0(14) . . . . ? Ta2 B2 B3 Ta1 -86.3(4) . . . . ? B1 B2 B3 Ta2 41.3(13) . . . . ? Ta1 B2 B3 Ta2 86.3(4) . . . . ? B5 Ta1 B3 C1 -134.2(19) . . . . ? B4 Ta1 B3 C1 -107(2) . . . . ? B2 Ta1 B3 C1 112(2) . . . . ? C8 Ta1 B3 C1 29(2) . . . . ? C7 Ta1 B3 C1 -4(3) . . . . ? C5 Ta1 B3 C1 -21.3(19) . . . . ? C6 Ta1 B3 C1 -42(2) . . . . ? C9 Ta1 B3 C1 12.7(19) . . . . ? B1 Ta1 B3 C1 139.8(19) . . . . ? Ta2 Ta1 B3 C1 -178(2) . . . . ? B5 Ta1 B3 B2 113.9(8) . . . . ? B4 Ta1 B3 B2 141.5(12) . . . . ? C8 Ta1 B3 B2 -82.9(9) . . . . ? C7 Ta1 B3 B2 -116.3(13) . . . . ? C5 Ta1 B3 B2 -133.1(8) . . . . ? C6 Ta1 B3 B2 -153.8(8) . . . . ? C9 Ta1 B3 B2 -99.1(9) . . . . ? B1 Ta1 B3 B2 28.0(9) . . . . ? Ta2 Ta1 B3 B2 70.2(7) . . . . ? B5 Ta1 B3 B4 -27.6(9) . . . . ? B2 Ta1 B3 B4 -141.5(12) . . . . ? C8 Ta1 B3 B4 135.6(9) . . . . ? C7 Ta1 B3 B4 102.2(14) . . . . ? C5 Ta1 B3 B4 85.4(9) . . . . ? C6 Ta1 B3 B4 64.6(11) . . . . ? C9 Ta1 B3 B4 119.3(9) . . . . ? B1 Ta1 B3 B4 -113.5(9) . . . . ? Ta2 Ta1 B3 B4 -71.3(8) . . . . ? B5 Ta1 B3 Ta2 43.7(6) . . . . ? B4 Ta1 B3 Ta2 71.3(8) . . . . ? B2 Ta1 B3 Ta2 -70.2(7) . . . . ? C8 Ta1 B3 Ta2 -153.1(5) . . . . ? C7 Ta1 B3 Ta2 173.5(10) . . . . ? C5 Ta1 B3 Ta2 156.7(6) . . . . ? C6 Ta1 B3 Ta2 135.9(6) . . . . ? C9 Ta1 B3 Ta2 -169.4(6) . . . . ? B1 Ta1 B3 Ta2 -42.2(6) . . . . ? B2 Ta2 B3 C1 -110.0(19) . . . . ? B1 Ta2 B3 C1 -137.3(18) . . . . ? C16 Ta2 B3 C1 22(2) . . . . ? B4 Ta2 B3 C1 107.0(19) . . . . ? C15 Ta2 B3 C1 -29(2) . . . . ? C17 Ta2 B3 C1 12.9(17) . . . . ? C19 Ta2 B3 C1 -45.6(18) . . . . ? C18 Ta2 B3 C1 -20.0(17) . . . . ? B5 Ta2 B3 C1 137.5(18) . . . . ? Ta1 Ta2 B3 C1 178(2) . . . . ? B1 Ta2 B3 B2 -27.3(11) . . . . ? C16 Ta2 B3 B2 131.5(10) . . . . ? B4 Ta2 B3 B2 -143.0(13) . . . . ? C15 Ta2 B3 B2 80.6(14) . . . . ? C17 Ta2 B3 B2 122.9(9) . . . . ? C19 Ta2 B3 B2 64.4(10) . . . . ? C18 Ta2 B3 B2 90.0(10) . . . . ? B5 Ta2 B3 B2 -112.5(10) . . . . ? Ta1 Ta2 B3 B2 -71.9(9) . . . . ? B2 Ta2 B3 B4 143.0(13) . . . . ? B1 Ta2 B3 B4 115.7(10) . . . . ? C16 Ta2 B3 B4 -85.5(11) . . . . ? C15 Ta2 B3 B4 -136.4(11) . . . . ? C17 Ta2 B3 B4 -94.1(9) . . . . ? C19 Ta2 B3 B4 -152.6(8) . . . . ? C18 Ta2 B3 B4 -127.0(10) . . . . ? B5 Ta2 B3 B4 30.5(10) . . . . ? Ta1 Ta2 B3 B4 71.1(8) . . . . ? B2 Ta2 B3 Ta1 71.9(8) . . . . ? B1 Ta2 B3 Ta1 44.6(7) . . . . ? C16 Ta2 B3 Ta1 -156.6(6) . . . . ? B4 Ta2 B3 Ta1 -71.1(8) . . . . ? C15 Ta2 B3 Ta1 152.5(8) . . . . ? C17 Ta2 B3 Ta1 -165.2(6) . . . . ? C19 Ta2 B3 Ta1 136.3(5) . . . . ? C18 Ta2 B3 Ta1 161.9(7) . . . . ? B5 Ta2 B3 Ta1 -40.6(6) . . . . ? C1 B3 B4 B5 178.1(14) . . . . ? B2 B3 B4 B5 -5(2) . . . . ? Ta1 B3 B4 B5 39.0(12) . . . . ? Ta2 B3 B4 B5 -47.2(12) . . . . ? C1 B3 B4 Ta1 139.0(14) . . . . ? B2 B3 B4 Ta1 -44.3(13) . . . . ? Ta2 B3 B4 Ta1 -86.2(5) . . . . ? C1 B3 B4 Ta2 -134.8(14) . . . . ? B2 B3 B4 Ta2 42.0(13) . . . . ? Ta1 B3 B4 Ta2 86.2(5) . . . . ? B5 Ta1 B4 B3 141.8(12) . . . . ? B2 Ta1 B4 B3 25.9(8) . . . . ? C8 Ta1 B4 B3 -88.0(13) . . . . ? C7 Ta1 B4 B3 -139.0(9) . . . . ? C5 Ta1 B4 B3 -96.3(9) . . . . ? C6 Ta1 B4 B3 -131.5(9) . . . . ? C9 Ta1 B4 B3 -72.8(10) . . . . ? B1 Ta1 B4 B3 68.9(9) . . . . ? Ta2 Ta1 B4 B3 69.2(8) . . . . ? B3 Ta1 B4 B5 -141.8(12) . . . . ? B2 Ta1 B4 B5 -115.9(8) . . . . ? C8 Ta1 B4 B5 130.1(11) . . . . ? C7 Ta1 B4 B5 79.1(11) . . . . ? C5 Ta1 B4 B5 121.8(9) . . . . ? C6 Ta1 B4 B5 86.7(9) . . . . ? C9 Ta1 B4 B5 145.4(9) . . . . ? B1 Ta1 B4 B5 -73.0(9) . . . . ? Ta2 Ta1 B4 B5 -72.6(8) . . . . ? B5 Ta1 B4 Ta2 72.6(8) . . . . ? B3 Ta1 B4 Ta2 -69.2(8) . . . . ? B2 Ta1 B4 Ta2 -43.3(5) . . . . ? C8 Ta1 B4 Ta2 -157.2(8) . . . . ? C7 Ta1 B4 Ta2 151.8(6) . . . . ? C5 Ta1 B4 Ta2 -165.6(6) . . . . ? C6 Ta1 B4 Ta2 159.3(6) . . . . ? C9 Ta1 B4 Ta2 -142.0(6) . . . . ? B1 Ta1 B4 Ta2 -0.3(6) . . . . ? B2 Ta2 B4 B3 -25.1(9) . . . . ? B1 Ta2 B4 B3 -68.8(10) . . . . ? C16 Ta2 B4 B3 127.2(9) . . . . ? C15 Ta2 B4 B3 130.5(12) . . . . ? C17 Ta2 B4 B3 94.4(10) . . . . ? C19 Ta2 B4 B3 57.1(15) . . . . ? C18 Ta2 B4 B3 62.2(10) . . . . ? B5 Ta2 B4 B3 -136.1(13) . . . . ? Ta1 Ta2 B4 B3 -69.1(8) . . . . ? B3 Ta2 B4 B5 136.1(13) . . . . ? B2 Ta2 B4 B5 111.0(10) . . . . ? B1 Ta2 B4 B5 67.3(10) . . . . ? C16 Ta2 B4 B5 -96.7(10) . . . . ? C15 Ta2 B4 B5 -93.4(14) . . . . ? C17 Ta2 B4 B5 -129.5(10) . . . . ? C19 Ta2 B4 B5 -166.8(12) . . . . ? C18 Ta2 B4 B5 -161.7(10) . . . . ? Ta1 Ta2 B4 B5 67.0(9) . . . . ? B3 Ta2 B4 Ta1 69.1(8) . . . . ? B2 Ta2 B4 Ta1 44.0(6) . . . . ? B1 Ta2 B4 Ta1 0.3(7) . . . . ? C16 Ta2 B4 Ta1 -163.7(5) . . . . ? C15 Ta2 B4 Ta1 -160.4(9) . . . . ? C17 Ta2 B4 Ta1 163.5(6) . . . . ? C19 Ta2 B4 Ta1 126.2(10) . . . . ? C18 Ta2 B4 Ta1 131.4(6) . . . . ? B5 Ta2 B4 Ta1 -67.0(9) . . . . ? B3 B4 B5 Ta1 -39.7(12) . . . . ? Ta2 B4 B5 Ta1 -85.6(5) . . . . ? B3 B4 B5 Ta2 45.9(12) . . . . ? Ta1 B4 B5 Ta2 85.6(5) . . . . ? B3 Ta1 B5 B4 26.1(9) . . . . ? B2 Ta1 B5 B4 67.4(9) . . . . ? C8 Ta1 B5 B4 -129.0(12) . . . . ? C7 Ta1 B5 B4 -130.3(9) . . . . ? C5 Ta1 B5 B4 -67.5(10) . . . . ? C6 Ta1 B5 B4 -98.8(9) . . . . ? C9 Ta1 B5 B4 -70.7(15) . . . . ? B1 Ta1 B5 B4 110.4(9) . . . . ? Ta2 Ta1 B5 B4 67.4(8) . . . . ? B3 Ta1 B5 Ta2 -41.3(6) . . . . ? B4 Ta1 B5 Ta2 -67.4(8) . . . . ? B2 Ta1 B5 Ta2 -0.1(6) . . . . ? C8 Ta1 B5 Ta2 163.6(9) . . . . ? C7 Ta1 B5 Ta2 162.3(5) . . . . ? C5 Ta1 B5 Ta2 -134.9(6) . . . . ? C6 Ta1 B5 Ta2 -166.2(7) . . . . ? C9 Ta1 B5 Ta2 -138.1(10) . . . . ? B1 Ta1 B5 Ta2 43.0(6) . . . . ? B3 Ta2 B5 B4 -29.7(9) . . . . ? B2 Ta2 B5 B4 -70.9(9) . . . . ? B1 Ta2 B5 B4 -116.7(9) . . . . ? C16 Ta2 B5 B4 106.4(9) . . . . ? C15 Ta2 B5 B4 141.4(8) . . . . ? C17 Ta2 B5 B4 68.2(11) . . . . ? C19 Ta2 B5 B4 159.2(18) . . . . ? C18 Ta2 B5 B4 45.9(19) . . . . ? Ta1 Ta2 B5 B4 -71.0(8) . . . . ? B3 Ta2 B5 Ta1 41.3(6) . . . . ? B2 Ta2 B5 Ta1 0.1(6) . . . . ? B1 Ta2 B5 Ta1 -45.7(7) . . . . ? C16 Ta2 B5 Ta1 177.4(5) . . . . ? B4 Ta2 B5 Ta1 71.0(8) . . . . ? C15 Ta2 B5 Ta1 -147.7(5) . . . . ? C17 Ta2 B5 Ta1 139.2(6) . . . . ? C19 Ta2 B5 Ta1 -129.8(19) . . . . ? C18 Ta2 B5 Ta1 116.9(15) . . . . ? C4 N1 C1 C2 -1(2) . . . . ? C4 N1 C1 B3 179.5(18) . . . . ? B2 B3 C1 N1 -163.6(15) . . . . ? B4 B3 C1 N1 13(2) . . . . ? Ta1 B3 C1 N1 102(2) . . . . ? Ta2 B3 C1 N1 -74(2) . . . . ? B2 B3 C1 C2 17(3) . . . . ? B4 B3 C1 C2 -165.9(17) . . . . ? Ta1 B3 C1 C2 -77(3) . . . . ? Ta2 B3 C1 C2 106(2) . . . . ? N1 C1 C2 C3 1(2) . . . . ? B3 C1 C2 C3 179.9(18) . . . . ? C1 C2 C3 C4 0(3) . . . . ? C2 C3 C4 N1 -1(3) . . . . ? C1 N1 C4 C3 1(3) . . . . ? B5 Ta1 C5 C9 -176.9(11) . . . . ? B3 Ta1 C5 C9 94.2(12) . . . . ? B4 Ta1 C5 C9 139.4(12) . . . . ? B2 Ta1 C5 C9 57.2(13) . . . . ? C8 Ta1 C5 C9 -34.7(11) . . . . ? C7 Ta1 C5 C9 -76.2(12) . . . . ? C6 Ta1 C5 C9 -115.3(15) . . . . ? B1 Ta1 C5 C9 10(3) . . . . ? Ta2 Ta1 C5 C9 122.0(10) . . . . ? B5 Ta1 C5 C6 -61.6(12) . . . . ? B3 Ta1 C5 C6 -150.6(11) . . . . ? B4 Ta1 C5 C6 -105.4(11) . . . . ? B2 Ta1 C5 C6 172.5(10) . . . . ? C8 Ta1 C5 C6 80.5(12) . . . . ? C7 Ta1 C5 C6 39.0(10) . . . . ? C9 Ta1 C5 C6 115.3(15) . . . . ? B1 Ta1 C5 C6 125(2) . . . . ? Ta2 Ta1 C5 C6 -122.7(10) . . . . ? B5 Ta1 C5 C10 60(3) . . . . ? B3 Ta1 C5 C10 -29(2) . . . . ? B4 Ta1 C5 C10 16(2) . . . . ? B2 Ta1 C5 C10 -66(2) . . . . ? C8 Ta1 C5 C10 -158(3) . . . . ? C7 Ta1 C5 C10 161(3) . . . . ? C6 Ta1 C5 C10 122(3) . . . . ? C9 Ta1 C5 C10 -123(3) . . . . ? B1 Ta1 C5 C10 -113(3) . . . . ? Ta2 Ta1 C5 C10 -1(3) . . . . ? C9 C5 C6 C7 2.2(18) . . . . ? C10 C5 C6 C7 173.2(18) . . . . ? Ta1 C5 C6 C7 -64.6(11) . . . . ? C9 C5 C6 C11 -177(2) . . . . ? C10 C5 C6 C11 -6(3) . . . . ? Ta1 C5 C6 C11 116(2) . . . . ? C9 C5 C6 Ta1 66.7(13) . . . . ? C10 C5 C6 Ta1 -122.2(18) . . . . ? B5 Ta1 C6 C7 -122.0(12) . . . . ? B3 Ta1 C6 C7 148.9(10) . . . . ? B4 Ta1 C6 C7 -170.5(11) . . . . ? B2 Ta1 C6 C7 95.3(19) . . . . ? C8 Ta1 C6 C7 37.9(11) . . . . ? C5 Ta1 C6 C7 112.1(15) . . . . ? C9 Ta1 C6 C7 75.7(11) . . . . ? B1 Ta1 C6 C7 -34.9(19) . . . . ? Ta2 Ta1 C6 C7 -141.6(9) . . . . ? B5 Ta1 C6 C5 125.8(11) . . . . ? B3 Ta1 C6 C5 36.8(13) . . . . ? B4 Ta1 C6 C5 77.4(11) . . . . ? B2 Ta1 C6 C5 -17(2) . . . . ? C8 Ta1 C6 C5 -74.2(11) . . . . ? C7 Ta1 C6 C5 -112.1(15) . . . . ? C9 Ta1 C6 C5 -36.5(10) . . . . ? B1 Ta1 C6 C5 -147.0(14) . . . . ? Ta2 Ta1 C6 C5 106.2(10) . . . . ? B5 Ta1 C6 C11 4(3) . . . . ? B3 Ta1 C6 C11 -85(3) . . . . ? B4 Ta1 C6 C11 -45(3) . . . . ? B2 Ta1 C6 C11 -139(3) . . . . ? C8 Ta1 C6 C11 164(3) . . . . ? C7 Ta1 C6 C11 126(3) . . . . ? C5 Ta1 C6 C11 -122(3) . . . . ? C9 Ta1 C6 C11 -158(3) . . . . ? B1 Ta1 C6 C11 91(3) . . . . ? Ta2 Ta1 C6 C11 -16(3) . . . . ? C5 C6 C7 C8 -0.9(19) . . . . ? C11 C6 C7 C8 178(2) . . . . ? Ta1 C6 C7 C8 -65.5(13) . . . . ? C5 C6 C7 C12 -179(2) . . . . ? C11 C6 C7 C12 0(3) . . . . ? Ta1 C6 C7 C12 116(2) . . . . ? C5 C6 C7 Ta1 64.6(10) . . . . ? C11 C6 C7 Ta1 -116(2) . . . . ? B5 Ta1 C7 C8 178.7(11) . . . . ? B3 Ta1 C7 C8 53.8(18) . . . . ? B4 Ta1 C7 C8 126.9(11) . . . . ? B2 Ta1 C7 C8 -28.9(15) . . . . ? C5 Ta1 C7 C8 73.8(11) . . . . ? C6 Ta1 C7 C8 114.0(15) . . . . ? C9 Ta1 C7 C8 33.2(11) . . . . ? B1 Ta1 C7 C8 -84.6(12) . . . . ? Ta2 Ta1 C7 C8 -139.8(11) . . . . ? B5 Ta1 C7 C6 64.8(12) . . . . ? B3 Ta1 C7 C6 -60.1(17) . . . . ? B4 Ta1 C7 C6 13.0(15) . . . . ? B2 Ta1 C7 C6 -142.9(11) . . . . ? C8 Ta1 C7 C6 -114.0(15) . . . . ? C5 Ta1 C7 C6 -40.2(11) . . . . ? C9 Ta1 C7 C6 -80.7(12) . . . . ? B1 Ta1 C7 C6 161.5(11) . . . . ? Ta2 Ta1 C7 C6 106.3(14) . . . . ? B5 Ta1 C7 C12 -55(2) . . . . ? B3 Ta1 C7 C12 -180(2) . . . . ? B4 Ta1 C7 C12 -107(2) . . . . ? B2 Ta1 C7 C12 97(2) . . . . ? C8 Ta1 C7 C12 126(3) . . . . ? C5 Ta1 C7 C12 -160(2) . . . . ? C6 Ta1 C7 C12 -120(3) . . . . ? C9 Ta1 C7 C12 159(2) . . . . ? B1 Ta1 C7 C12 42(2) . . . . ? Ta2 Ta1 C7 C12 -14(3) . . . . ? C6 C7 C8 C9 -1(2) . . . . ? C12 C7 C8 C9 177(2) . . . . ? Ta1 C7 C8 C9 -66.9(16) . . . . ? C6 C7 C8 C13 -171.9(19) . . . . ? C12 C7 C8 C13 6(3) . . . . ? Ta1 C7 C8 C13 121.9(19) . . . . ? C6 C7 C8 Ta1 66.1(12) . . . . ? C12 C7 C8 Ta1 -116(2) . . . . ? B5 Ta1 C8 C9 117.7(16) . . . . ? B3 Ta1 C8 C9 -31.9(14) . . . . ? B4 Ta1 C8 C9 27.0(17) . . . . ? B2 Ta1 C8 C9 -79.1(13) . . . . ? C7 Ta1 C8 C9 119.8(16) . . . . ? C5 Ta1 C8 C9 37.2(12) . . . . ? C6 Ta1 C8 C9 81.0(13) . . . . ? B1 Ta1 C8 C9 -128.8(13) . . . . ? Ta2 Ta1 C8 C9 -99.6(16) . . . . ? B5 Ta1 C8 C7 -2.1(18) . . . . ? B3 Ta1 C8 C7 -151.7(10) . . . . ? B4 Ta1 C8 C7 -92.7(15) . . . . ? B2 Ta1 C8 C7 161.1(10) . . . . ? C5 Ta1 C8 C7 -82.6(12) . . . . ? C6 Ta1 C8 C7 -38.8(11) . . . . ? C9 Ta1 C8 C7 -119.8(16) . . . . ? B1 Ta1 C8 C7 111.4(11) . . . . ? Ta2 Ta1 C8 C7 140.6(11) . . . . ? B5 Ta1 C8 C13 -118(2) . . . . ? B3 Ta1 C8 C13 92(2) . . . . ? B4 Ta1 C8 C13 151.1(19) . . . . ? B2 Ta1 C8 C13 45(2) . . . . ? C7 Ta1 C8 C13 -116(3) . . . . ? C5 Ta1 C8 C13 161(2) . . . . ? C6 Ta1 C8 C13 -155(2) . . . . ? C9 Ta1 C8 C13 124(3) . . . . ? B1 Ta1 C8 C13 -5(2) . . . . ? Ta2 Ta1 C8 C13 24(3) . . . . ? C7 C8 C9 C5 2(2) . . . . ? C13 C8 C9 C5 173(2) . . . . ? Ta1 C8 C9 C5 -62.4(13) . . . . ? C7 C8 C9 C14 -177(2) . . . . ? C13 C8 C9 C14 -7(4) . . . . ? Ta1 C8 C9 C14 118(2) . . . . ? C7 C8 C9 Ta1 64.6(16) . . . . ? C13 C8 C9 Ta1 -125(2) . . . . ? C6 C5 C9 C8 -3(2) . . . . ? C10 C5 C9 C8 -174(2) . . . . ? Ta1 C5 C9 C8 62.5(14) . . . . ? C6 C5 C9 C14 176.8(19) . . . . ? C10 C5 C9 C14 6(3) . . . . ? Ta1 C5 C9 C14 -118(2) . . . . ? C6 C5 C9 Ta1 -65.2(11) . . . . ? C10 C5 C9 Ta1 124(2) . . . . ? B5 Ta1 C9 C8 -112.0(15) . . . . ? B3 Ta1 C9 C8 153.8(12) . . . . ? B4 Ta1 C9 C8 -163.1(11) . . . . ? B2 Ta1 C9 C8 109.2(12) . . . . ? C7 Ta1 C9 C8 -36.1(11) . . . . ? C5 Ta1 C9 C8 -117.3(17) . . . . ? C6 Ta1 C9 C8 -78.2(13) . . . . ? B1 Ta1 C9 C8 66.7(14) . . . . ? Ta2 Ta1 C9 C8 139.3(9) . . . . ? B5 Ta1 C9 C5 5.3(19) . . . . ? B3 Ta1 C9 C5 -88.9(12) . . . . ? B4 Ta1 C9 C5 -45.8(13) . . . . ? B2 Ta1 C9 C5 -133.5(12) . . . . ? C8 Ta1 C9 C5 117.3(17) . . . . ? C7 Ta1 C9 C5 81.1(13) . . . . ? C6 Ta1 C9 C5 39.0(12) . . . . ? B1 Ta1 C9 C5 -176.1(11) . . . . ? Ta2 Ta1 C9 C5 -103.4(13) . . . . ? B5 Ta1 C9 C14 123(2) . . . . ? B3 Ta1 C9 C14 28(2) . . . . ? B4 Ta1 C9 C14 71(2) . . . . ? B2 Ta1 C9 C14 -16(2) . . . . ? C8 Ta1 C9 C14 -125(3) . . . . ? C7 Ta1 C9 C14 -162(2) . . . . ? C5 Ta1 C9 C14 117(2) . . . . ? C6 Ta1 C9 C14 156(2) . . . . ? B1 Ta1 C9 C14 -59(2) . . . . ? Ta2 Ta1 C9 C14 14(3) . . . . ? B3 Ta2 C15 C16 90.4(14) . . . . ? B2 Ta2 C15 C16 145.5(10) . . . . ? B1 Ta2 C15 C16 -166.3(11) . . . . ? B4 Ta2 C15 C16 -5.3(17) . . . . ? C17 Ta2 C15 C16 38.4(10) . . . . ? C19 Ta2 C15 C16 117.1(14) . . . . ? C18 Ta2 C15 C16 79.3(11) . . . . ? B5 Ta2 C15 C16 -72.9(12) . . . . ? Ta1 Ta2 C15 C16 -147.0(9) . . . . ? B3 Ta2 C15 C19 -26.6(16) . . . . ? B2 Ta2 C15 C19 28.5(12) . . . . ? B1 Ta2 C15 C19 76.6(11) . . . . ? C16 Ta2 C15 C19 -117.1(14) . . . . ? B4 Ta2 C15 C19 -122.4(13) . . . . ? C17 Ta2 C15 C19 -78.7(11) . . . . ? C18 Ta2 C15 C19 -37.8(10) . . . . ? B5 Ta2 C15 C19 170.0(10) . . . . ? Ta1 Ta2 C15 C19 95.9(12) . . . . ? B3 Ta2 C15 C20 -148.1(15) . . . . ? B2 Ta2 C15 C20 -93.0(16) . . . . ? B1 Ta2 C15 C20 -44.8(16) . . . . ? C16 Ta2 C15 C20 121.5(19) . . . . ? B4 Ta2 C15 C20 116.2(17) . . . . ? C17 Ta2 C15 C20 159.9(17) . . . . ? C19 Ta2 C15 C20 -121.4(19) . . . . ? C18 Ta2 C15 C20 -159.2(18) . . . . ? B5 Ta2 C15 C20 48.6(18) . . . . ? Ta1 Ta2 C15 C20 -26(2) . . . . ? C19 C15 C16 C17 -0.8(19) . . . . ? C20 C15 C16 C17 173.8(17) . . . . ? Ta2 C15 C16 C17 -66.8(12) . . . . ? C19 C15 C16 C21 -173(2) . . . . ? C20 C15 C16 C21 2(3) . . . . ? Ta2 C15 C16 C21 121(2) . . . . ? C19 C15 C16 Ta2 66.0(11) . . . . ? C20 C15 C16 Ta2 -119.4(17) . . . . ? B3 Ta2 C16 C15 -130.4(11) . . . . ? B2 Ta2 C16 C15 -59.3(15) . . . . ? B1 Ta2 C16 C15 19.1(15) . . . . ? B4 Ta2 C16 C15 177.1(10) . . . . ? C17 Ta2 C16 C15 -115.6(14) . . . . ? C19 Ta2 C16 C15 -36.9(9) . . . . ? C18 Ta2 C16 C15 -78.6(11) . . . . ? B5 Ta2 C16 C15 125.4(10) . . . . ? Ta1 Ta2 C16 C15 131.9(12) . . . . ? B3 Ta2 C16 C17 -14.8(14) . . . . ? B2 Ta2 C16 C17 56.3(15) . . . . ? B1 Ta2 C16 C17 134.6(12) . . . . ? B4 Ta2 C16 C17 -67.3(11) . . . . ? C15 Ta2 C16 C17 115.6(14) . . . . ? C19 Ta2 C16 C17 78.7(11) . . . . ? C18 Ta2 C16 C17 37.0(10) . . . . ? B5 Ta2 C16 C17 -119.0(11) . . . . ? Ta1 Ta2 C16 C17 -112.5(14) . . . . ? B3 Ta2 C16 C21 103(2) . . . . ? B2 Ta2 C16 C21 174.2(18) . . . . ? B1 Ta2 C16 C21 -107(2) . . . . ? B4 Ta2 C16 C21 51(2) . . . . ? C15 Ta2 C16 C21 -126(2) . . . . ? C17 Ta2 C16 C21 118(2) . . . . ? C19 Ta2 C16 C21 -163(2) . . . . ? C18 Ta2 C16 C21 155(2) . . . . ? B5 Ta2 C16 C21 -1(2) . . . . ? Ta1 Ta2 C16 C21 5(3) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C21 C16 C17 C18 173.4(18) . . . . ? Ta2 C16 C17 C18 -65.4(12) . . . . ? C15 C16 C17 C22 -172.9(18) . . . . ? C21 C16 C17 C22 0(3) . . . . ? Ta2 C16 C17 C22 120.7(19) . . . . ? C15 C16 C17 Ta2 66.4(13) . . . . ? C21 C16 C17 Ta2 -121.2(18) . . . . ? B3 Ta2 C17 C18 -75.4(11) . . . . ? B2 Ta2 C17 C18 -32.6(12) . . . . ? B1 Ta2 C17 C18 25.1(19) . . . . ? C16 Ta2 C17 C18 115.2(14) . . . . ? B4 Ta2 C17 C18 -121.3(10) . . . . ? C15 Ta2 C17 C18 78.9(11) . . . . ? C19 Ta2 C17 C18 37.7(10) . . . . ? B5 Ta2 C17 C18 -164.6(10) . . . . ? Ta1 Ta2 C17 C18 -96.9(11) . . . . ? B3 Ta2 C17 C16 169.4(10) . . . . ? B2 Ta2 C17 C16 -147.8(10) . . . . ? B1 Ta2 C17 C16 -90.2(17) . . . . ? B4 Ta2 C17 C16 123.5(10) . . . . ? C15 Ta2 C17 C16 -36.4(9) . . . . ? C19 Ta2 C17 C16 -77.5(10) . . . . ? C18 Ta2 C17 C16 -115.2(14) . . . . ? B5 Ta2 C17 C16 80.2(11) . . . . ? Ta1 Ta2 C17 C16 147.9(8) . . . . ? B3 Ta2 C17 C22 47(2) . . . . ? B2 Ta2 C17 C22 90(2) . . . . ? B1 Ta2 C17 C22 147(2) . . . . ? C16 Ta2 C17 C22 -122(3) . . . . ? B4 Ta2 C17 C22 1(2) . . . . ? C15 Ta2 C17 C22 -159(3) . . . . ? C19 Ta2 C17 C22 160(3) . . . . ? C18 Ta2 C17 C22 122(3) . . . . ? B5 Ta2 C17 C22 -42(3) . . . . ? Ta1 Ta2 C17 C22 25(3) . . . . ? C16 C17 C18 C19 -0.8(19) . . . . ? C22 C17 C18 C19 173.3(17) . . . . ? Ta2 C17 C18 C19 -63.5(11) . . . . ? C16 C17 C18 C23 -172.1(19) . . . . ? C22 C17 C18 C23 2(3) . . . . ? Ta2 C17 C18 C23 125.2(19) . . . . ? C16 C17 C18 Ta2 62.8(12) . . . . ? C22 C17 C18 Ta2 -123.2(19) . . . . ? B3 Ta2 C18 C17 107.7(11) . . . . ? B2 Ta2 C18 C17 152.2(11) . . . . ? B1 Ta2 C18 C17 -166.1(10) . . . . ? C16 Ta2 C18 C17 -38.3(10) . . . . ? B4 Ta2 C18 C17 68.8(11) . . . . ? C15 Ta2 C18 C17 -78.3(11) . . . . ? C19 Ta2 C18 C17 -115.7(15) . . . . ? B5 Ta2 C18 C17 33(2) . . . . ? Ta1 Ta2 C18 C17 128.4(9) . . . . ? B3 Ta2 C18 C19 -136.6(11) . . . . ? B2 Ta2 C18 C19 -92.1(11) . . . . ? B1 Ta2 C18 C19 -50.4(12) . . . . ? C16 Ta2 C18 C19 77.3(11) . . . . ? B4 Ta2 C18 C19 -175.5(10) . . . . ? C15 Ta2 C18 C19 37.3(10) . . . . ? C17 Ta2 C18 C19 115.7(15) . . . . ? B5 Ta2 C18 C19 149.1(15) . . . . ? Ta1 Ta2 C18 C19 -116.0(9) . . . . ? B3 Ta2 C18 C23 -15(2) . . . . ? B2 Ta2 C18 C23 30(2) . . . . ? B1 Ta2 C18 C23 71(2) . . . . ? C16 Ta2 C18 C23 -161(3) . . . . ? B4 Ta2 C18 C23 -54(3) . . . . ? C15 Ta2 C18 C23 159(3) . . . . ? C17 Ta2 C18 C23 -123(3) . . . . ? C19 Ta2 C18 C23 122(3) . . . . ? B5 Ta2 C18 C23 -89(3) . . . . ? Ta1 Ta2 C18 C23 6(3) . . . . ? C16 C15 C19 C18 0.3(19) . . . . ? C20 C15 C19 C18 -174.3(17) . . . . ? Ta2 C15 C19 C18 65.0(11) . . . . ? C16 C15 C19 C24 176.2(19) . . . . ? C20 C15 C19 C24 2(3) . . . . ? Ta2 C15 C19 C24 -119.1(19) . . . . ? C16 C15 C19 Ta2 -64.7(12) . . . . ? C20 C15 C19 Ta2 120.7(17) . . . . ? C17 C18 C19 C15 0.3(19) . . . . ? C23 C18 C19 C15 171.6(18) . . . . ? Ta2 C18 C19 C15 -63.3(11) . . . . ? C17 C18 C19 C24 -175.7(18) . . . . ? C23 C18 C19 C24 -4(3) . . . . ? Ta2 C18 C19 C24 120.7(19) . . . . ? C17 C18 C19 Ta2 63.6(12) . . . . ? C23 C18 C19 Ta2 -125(2) . . . . ? B3 Ta2 C19 C15 164.5(10) . . . . ? B2 Ta2 C19 C15 -156.3(10) . . . . ? B1 Ta2 C19 C15 -108.0(10) . . . . ? C16 Ta2 C19 C15 35.9(9) . . . . ? B4 Ta2 C19 C15 123.5(13) . . . . ? C17 Ta2 C19 C15 78.3(11) . . . . ? C18 Ta2 C19 C15 115.3(15) . . . . ? B5 Ta2 C19 C15 -25(3) . . . . ? Ta1 Ta2 C19 C15 -138.6(8) . . . . ? B3 Ta2 C19 C18 49.1(12) . . . . ? B2 Ta2 C19 C18 88.4(11) . . . . ? B1 Ta2 C19 C18 136.7(11) . . . . ? C16 Ta2 C19 C18 -79.4(11) . . . . ? B4 Ta2 C19 C18 8.2(18) . . . . ? C15 Ta2 C19 C18 -115.3(15) . . . . ? C17 Ta2 C19 C18 -37.0(11) . . . . ? B5 Ta2 C19 C18 -141(2) . . . . ? Ta1 Ta2 C19 C18 106.1(11) . . . . ? B3 Ta2 C19 C24 -72.7(18) . . . . ? B2 Ta2 C19 C24 -33.4(17) . . . . ? B1 Ta2 C19 C24 14.8(18) . . . . ? C16 Ta2 C19 C24 158.8(19) . . . . ? B4 Ta2 C19 C24 -113.7(19) . . . . ? C15 Ta2 C19 C24 123(2) . . . . ? C17 Ta2 C19 C24 -159(2) . . . . ? C18 Ta2 C19 C24 -122(2) . . . . ? B5 Ta2 C19 C24 98(3) . . . . ? Ta1 Ta2 C19 C24 -16(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 7.549 _refine_diff_density_min -7.509 _refine_diff_density_rms 0.388 _vrf_PLAT220_shelxl ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.17 Ratio RESPONSE:This is due large libration of the molecule about its axis. This fact can be directly verified from the ORTEP. ; #=============================================================== data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 814966' #TrackingRef '[(C5Me5Ta)2B5H10(C6H5)] cif file for CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H45 B5 Ta2' _chemical_formula_weight 773.57 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' 'Ta' 'Ta' -0.7052 6.5227 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.7619(4) _cell_length_b 17.2045(4) _cell_length_c 10.0036(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.8740(10) _cell_angle_gamma 90.00 _cell_volume 2833.04(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3898 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.5 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 7.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_T_max 0.492 _exptl_absorpt_process_details 'SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10619 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.31 _reflns_number_total 3368 _reflns_number_gt 2517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altornare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+6.5223P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3368 _refine_ls_number_parameters 175 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B -0.0405(4) 0.1120(4) 0.0885(7) 0.0435(15) Uani 1 1 d . . . B2 B 0.0000 0.2683(5) 0.2500 0.0369(19) Uani 1 2 d S . . B3 B -0.0415(3) 0.2179(4) 0.0989(6) 0.0374(13) Uani 1 1 d D . . C6A C 0.2836(8) 0.1403(7) 0.3441(12) 0.123(6) Uani 0.353(3) 1 d PD A 1 H6A1 H 0.2651 0.1523 0.4268 0.184 Uiso 0.353(3) 1 calc PR A 1 H6A2 H 0.3355 0.1643 0.3456 0.184 Uiso 0.353(3) 1 calc PR A 1 H6A3 H 0.2887 0.0850 0.3361 0.184 Uiso 0.353(3) 1 calc PR A 1 C1A C 0.2230(8) 0.1709(7) 0.2235(12) 0.0478(15) Uani 0.353(3) 1 d PRD A 1 C2A C 0.1902(8) 0.1178(7) 0.1188(12) 0.0501(15) Uani 0.353(3) 1 d PRD A 1 C3A C 0.1413(8) 0.1605(7) 0.0124(12) 0.063(2) Uani 0.353(3) 1 d PRD A 1 C4A C 0.1439(8) 0.2400(7) 0.0514(12) 0.075(3) Uani 0.353(3) 1 d PRD A 1 C5A C 0.1944(8) 0.2464(7) 0.1818(12) 0.066(2) Uani 0.353(3) 1 d PRD A 1 C7A C 0.1920(8) 0.0413(7) 0.0465(12) 0.064(3) Uani 0.353(3) 1 d PRD A 1 H7A1 H 0.1558 0.0054 0.0781 0.095 Uiso 0.353(3) 1 calc PR A 1 H7A2 H 0.2462 0.0208 0.0651 0.095 Uiso 0.353(3) 1 calc PR A 1 H7A3 H 0.1752 0.0490 -0.0497 0.095 Uiso 0.353(3) 1 calc PR A 1 C8A C 0.0928(11) 0.1688(14) -0.1332(13) 0.065(3) Uani 0.353(3) 1 d PD A 1 H8A1 H 0.0427 0.1952 -0.1313 0.098 Uiso 0.353(3) 1 calc PR A 1 H8A2 H 0.0816 0.1181 -0.1725 0.098 Uiso 0.353(3) 1 calc PR A 1 H8A3 H 0.1240 0.1981 -0.1869 0.098 Uiso 0.353(3) 1 calc PR A 1 C9A C 0.1267(14) 0.3273(9) 0.019(3) 0.079(4) Uani 0.353(3) 1 d PD A 1 H9A1 H 0.1675 0.3477 -0.0272 0.118 Uiso 0.353(3) 1 calc PR A 1 H9A2 H 0.1278 0.3554 0.1021 0.118 Uiso 0.353(3) 1 calc PR A 1 H9A3 H 0.0742 0.3328 -0.0384 0.118 Uiso 0.353(3) 1 calc PR A 1 C10A C 0.2439(13) 0.300(2) 0.291(4) 0.114(9) Uani 0.353(3) 1 d PD A 1 H10A H 0.2430 0.2800 0.3797 0.171 Uiso 0.353(3) 1 calc PR A 1 H10B H 0.2203 0.3514 0.2826 0.171 Uiso 0.353(3) 1 calc PR A 1 H10C H 0.2990 0.3033 0.2770 0.171 Uiso 0.353(3) 1 calc PR A 1 C6B C 0.2827(4) 0.1678(4) 0.3531(6) 0.123(6) Uani 0.647(3) 1 d PD A 2 H6B1 H 0.3216 0.1265 0.3571 0.184 Uiso 0.647(3) 1 calc PR A 2 H6B2 H 0.2541 0.1626 0.4272 0.184 Uiso 0.647(3) 1 calc PR A 2 H6B3 H 0.3103 0.2169 0.3597 0.184 Uiso 0.647(3) 1 calc PR A 2 C1B C 0.2228(4) 0.1636(4) 0.2194(6) 0.0478(15) Uani 0.647(3) 1 d PRD A 2 C2B C 0.1899(4) 0.1105(4) 0.1146(6) 0.0501(15) Uani 0.647(3) 1 d PRD A 2 C3B C 0.1410(4) 0.1533(4) 0.0082(6) 0.063(2) Uani 0.647(3) 1 d PRD A 2 C4B C 0.1436(4) 0.2327(4) 0.0472(6) 0.075(3) Uani 0.647(3) 1 d PRD A 2 C5B C 0.1942(4) 0.2391(4) 0.1777(6) 0.066(2) Uani 0.647(3) 1 d PRD A 2 C7B C 0.2161(4) 0.0254(4) 0.1328(6) 0.064(3) Uani 0.647(3) 1 d PRD A 2 H7B1 H 0.2204 0.0038 0.0459 0.095 Uiso 0.647(3) 1 calc PR A 2 H7B2 H 0.1766 -0.0032 0.1707 0.095 Uiso 0.647(3) 1 calc PR A 2 H7B3 H 0.2679 0.0223 0.1930 0.095 Uiso 0.647(3) 1 calc PR A 2 C8B C 0.1013(6) 0.1075(7) -0.1178(9) 0.065(3) Uani 0.647(3) 1 d PD A 2 H8B1 H 0.0472 0.1267 -0.1496 0.098 Uiso 0.647(3) 1 calc PR A 2 H8B2 H 0.0989 0.0535 -0.0950 0.098 Uiso 0.647(3) 1 calc PR A 2 H8B3 H 0.1327 0.1137 -0.1881 0.098 Uiso 0.647(3) 1 calc PR A 2 C9B C 0.0996(7) 0.2895(7) -0.0616(12) 0.079(4) Uani 0.647(3) 1 d PD A 2 H9B1 H 0.1377 0.3102 -0.1128 0.118 Uiso 0.647(3) 1 calc PR A 2 H9B2 H 0.0763 0.3312 -0.0179 0.118 Uiso 0.647(3) 1 calc PR A 2 H9B3 H 0.0573 0.2624 -0.1218 0.118 Uiso 0.647(3) 1 calc PR A 2 C10B C 0.2066(7) 0.3234(8) 0.232(2) 0.114(9) Uani 0.647(3) 1 d PD A 2 H10D H 0.1563 0.3514 0.2098 0.171 Uiso 0.647(3) 1 calc PR A 2 H10E H 0.2470 0.3487 0.1912 0.171 Uiso 0.647(3) 1 calc PR A 2 H10F H 0.2242 0.3223 0.3292 0.171 Uiso 0.647(3) 1 calc PR A 2 C11 C 0.0000 0.3596(4) 0.2500 0.0381(17) Uani 1 2 d S . . C12 C 0.0439(3) 0.4034(4) 0.3580(6) 0.0495(14) Uani 1 1 d . . . H12 H 0.0735 0.3773 0.4325 0.059 Uiso 1 1 calc R . . C13 C 0.0447(4) 0.4846(4) 0.3578(7) 0.0651(18) Uani 1 1 d . . . H13 H 0.0753 0.5115 0.4304 0.078 Uiso 1 1 calc R . . C14 C 0.0000 0.5246(6) 0.2500 0.071(3) Uani 1 2 d S . . H14 H 0.0000 0.5786 0.2500 0.085 Uiso 1 2 calc SR . . Ta1 Ta 0.078823(10) 0.165596(12) 0.206179(18) 0.03133(7) Uani 1 1 d . . . H1X H -0.065(4) 0.088(4) -0.012(6) 0.08(2) Uiso 1 1 d . . . H1Z H 0.018(3) 0.077(3) 0.122(5) 0.045(14) Uiso 1 1 d . . . H1Y H -0.074(3) 0.090(3) 0.164(6) 0.067(18) Uiso 1 1 d . . . H3B H -0.058(3) 0.246(3) 0.009(5) 0.043(14) Uiso 1 1 d . . . H3A H -0.1057(11) 0.207(3) 0.104(5) 0.050(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.033(3) 0.057(4) 0.043(4) -0.014(3) 0.014(3) -0.009(3) B2 0.026(3) 0.052(6) 0.033(4) 0.000 0.007(3) 0.000 B3 0.027(3) 0.054(4) 0.032(3) 0.003(3) 0.008(2) 0.003(2) C6A 0.030(3) 0.277(18) 0.059(5) 0.023(7) 0.002(3) -0.010(6) C1A 0.021(2) 0.088(5) 0.037(3) -0.008(3) 0.0113(19) -0.011(3) C2A 0.027(2) 0.060(4) 0.069(4) -0.016(3) 0.026(2) -0.006(3) C3A 0.025(2) 0.133(7) 0.034(3) -0.005(4) 0.013(2) -0.002(3) C4A 0.049(3) 0.104(6) 0.088(5) 0.056(5) 0.053(4) 0.032(4) C5A 0.064(4) 0.055(4) 0.098(5) -0.036(4) 0.066(4) -0.033(3) C7A 0.043(5) 0.052(6) 0.105(9) 0.018(6) 0.039(5) 0.024(4) C8A 0.048(4) 0.112(9) 0.038(4) -0.010(6) 0.012(3) -0.018(7) C9A 0.066(7) 0.076(9) 0.109(12) 0.049(7) 0.056(7) 0.014(6) C10A 0.066(9) 0.086(12) 0.22(2) -0.079(13) 0.100(13) -0.045(9) C6B 0.030(3) 0.277(18) 0.059(5) 0.023(7) 0.002(3) -0.010(6) C1B 0.021(2) 0.088(5) 0.037(3) -0.008(3) 0.0113(19) -0.011(3) C2B 0.027(2) 0.060(4) 0.069(4) -0.016(3) 0.026(2) -0.006(3) C3B 0.025(2) 0.133(7) 0.034(3) -0.005(4) 0.013(2) -0.002(3) C4B 0.049(3) 0.104(6) 0.088(5) 0.056(5) 0.053(4) 0.032(4) C5B 0.064(4) 0.055(4) 0.098(5) -0.036(4) 0.066(4) -0.033(3) C7B 0.043(5) 0.052(6) 0.105(9) 0.018(6) 0.039(5) 0.024(4) C8B 0.048(4) 0.112(9) 0.038(4) -0.010(6) 0.012(3) -0.018(7) C9B 0.066(7) 0.076(9) 0.109(12) 0.049(7) 0.056(7) 0.014(6) C10B 0.066(9) 0.086(12) 0.22(2) -0.079(13) 0.100(13) -0.045(9) C11 0.022(3) 0.054(5) 0.042(4) 0.000 0.014(3) 0.000 C12 0.043(3) 0.053(4) 0.054(4) -0.009(3) 0.014(2) -0.003(3) C13 0.068(4) 0.057(5) 0.076(5) -0.020(3) 0.028(3) -0.012(3) C14 0.071(6) 0.058(7) 0.093(8) 0.000 0.043(6) 0.000 Ta1 0.02256(9) 0.04252(13) 0.03094(12) -0.00079(9) 0.01026(7) 0.00048(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 B3 1.826(9) . ? B1 Ta1 2.313(6) . ? B1 Ta1 2.445(6) 2 ? B1 H1X 1.09(6) . ? B1 H1Z 1.14(5) . ? B1 H1Y 1.09(6) . ? B2 C11 1.570(12) . ? B2 B3 1.767(7) . ? B2 B3 1.767(7) 2 ? B2 Ta1 2.298(7) . ? B2 Ta1 2.298(7) 2 ? B3 Ta1 2.283(6) . ? B3 Ta1 2.338(6) 2 ? B3 H3B 1.01(5) . ? B3 H3A 1.103(10) . ? C6A C1A 1.5162 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C1A C5A 1.4200 . ? C1A C2A 1.4200 . ? C1A Ta1 2.392(13) . ? C2A C3A 1.4200 . ? C2A C7A 1.5041 . ? C2A Ta1 2.354(14) . ? C3A C4A 1.4200 . ? C3A C8A 1.534(9) . ? C3A Ta1 2.372(14) . ? C4A C5A 1.4200 . ? C4A C9A 1.552(9) . ? C4A Ta1 2.421(14) . ? C5A C10A 1.548(10) . ? C5A Ta1 2.434(14) . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C8A H8A1 0.9600 . ? C8A H8A2 0.9600 . ? C8A H8A3 0.9600 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C6B C1B 1.5154 . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C1B C2B 1.4200 . ? C1B C5B 1.4200 . ? C1B Ta1 2.392(7) . ? C2B C3B 1.4200 . ? C2B C7B 1.5297 . ? C2B Ta1 2.418(7) . ? C3B C4B 1.4200 . ? C3B C8B 1.528(8) . ? C3B Ta1 2.415(7) . ? C4B C5B 1.4200 . ? C4B C9B 1.543(8) . ? C4B Ta1 2.387(7) . ? C5B C10B 1.549(8) . ? C5B Ta1 2.372(8) . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? C8B H8B1 0.9600 . ? C8B H8B2 0.9600 . ? C8B H8B3 0.9600 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? C11 C12 1.406(7) 2 ? C11 C12 1.406(7) . ? C12 C13 1.396(8) . ? C12 H12 0.9300 . ? C13 C14 1.376(8) . ? C13 H13 0.9300 . ? C14 C13 1.376(8) 2 ? C14 H14 0.9300 . ? Ta1 B3 2.338(6) 2 ? Ta1 H1Z 1.94(5) . ? 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 B3 B1 Ta1 65.7(3) . . ? B3 B1 Ta1 64.5(3) . 2 ? Ta1 B1 Ta1 76.18(19) . 2 ? B3 B1 H1X 115(3) . . ? Ta1 B1 H1X 139(3) . . ? Ta1 B1 H1X 143(3) 2 . ? B3 B1 H1Z 122(2) . . ? Ta1 B1 H1Z 57(2) . . ? Ta1 B1 H1Z 108(2) 2 . ? H1X B1 H1Z 103(4) . . ? B3 B1 H1Y 107(3) . . ? Ta1 B1 H1Y 107(3) . . ? Ta1 B1 H1Y 45(3) 2 . ? H1X B1 H1Y 111(4) . . ? H1Z B1 H1Y 98(4) . . ? C11 B2 B3 119.4(3) . . ? C11 B2 B3 119.4(3) . 2 ? B3 B2 B3 121.3(7) . 2 ? C11 B2 Ta1 140.27(15) . . ? B3 B2 Ta1 66.9(3) . . ? B3 B2 Ta1 68.8(3) 2 . ? C11 B2 Ta1 140.28(15) . 2 ? B3 B2 Ta1 68.8(3) . 2 ? B3 B2 Ta1 66.9(3) 2 2 ? Ta1 B2 Ta1 79.5(3) . 2 ? B2 B3 B1 122.1(5) . . ? B2 B3 Ta1 67.7(3) . . ? B1 B3 Ta1 67.4(3) . . ? B2 B3 Ta1 66.4(3) . 2 ? B1 B3 Ta1 70.7(3) . 2 ? Ta1 B3 Ta1 78.90(19) . 2 ? B2 B3 H3B 122(3) . . ? B1 B3 H3B 115(3) . . ? Ta1 B3 H3B 133(3) . . ? Ta1 B3 H3B 148(3) 2 . ? B2 B3 H3A 106(3) . . ? B1 B3 H3A 81(3) . . ? Ta1 B3 H3A 134(3) . . ? Ta1 B3 H3A 59(3) 2 . ? H3B B3 H3A 91(4) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C1A C2A 108.0 . . ? C5A C1A C6A 133.5 . . ? C2A C1A C6A 118.2 . . ? C5A C1A Ta1 74.5(3) . . ? C2A C1A Ta1 71.1(3) . . ? C6A C1A Ta1 124.1(3) . . ? C3A C2A C1A 108.0 . . ? C3A C2A C7A 98.8 . . ? C1A C2A C7A 151.2 . . ? C3A C2A Ta1 73.2(2) . . ? C1A C2A Ta1 74.1(3) . . ? C7A C2A Ta1 125.0(3) . . ? C4A C3A C2A 108.0 . . ? C4A C3A C8A 98.9(10) . . ? C2A C3A C8A 152.5(10) . . ? C4A C3A Ta1 74.7(3) . . ? C2A C3A Ta1 71.8(2) . . ? C8A C3A Ta1 122.4(10) . . ? C3A C4A C5A 108.0 . . ? C3A C4A C9A 151.6(11) . . ? C5A C4A C9A 99.9(11) . . ? C3A C4A Ta1 70.9(3) . . ? C5A C4A Ta1 73.5(3) . . ? C9A C4A Ta1 123.9(11) . . ? C1A C5A C4A 108.0 . . ? C1A C5A C10A 103.7(15) . . ? C4A C5A C10A 147.2(17) . . ? C1A C5A Ta1 71.3(3) . . ? C4A C5A Ta1 72.5(3) . . ? C10A C5A Ta1 127.1(15) . . ? C1B C6B H6B1 109.5 . . ? C1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2B C1B C5B 108.0 . . ? C2B C1B C6B 141.5 . . ? C5B C1B C6B 110.3 . . ? C2B C1B Ta1 73.84(17) . . ? C5B C1B Ta1 71.90(15) . . ? C6B C1B Ta1 122.80(16) . . ? C1B C2B C3B 108.0 . . ? C1B C2B C7B 117.7 . . ? C3B C2B C7B 134.2 . . ? C1B C2B Ta1 71.82(16) . . ? C3B C2B Ta1 72.79(13) . . ? C7B C2B Ta1 123.69(16) . . ? C2B C3B C4B 108.0 . . ? C2B C3B C8B 116.9(5) . . ? C4B C3B C8B 135.1(5) . . ? C2B C3B Ta1 73.03(13) . . ? C4B C3B Ta1 71.71(16) . . ? C8B C3B Ta1 122.2(6) . . ? C5B C4B C3B 108.0 . . ? C5B C4B C9B 136.3(6) . . ? C3B C4B C9B 115.5(6) . . ? C5B C4B Ta1 72.08(15) . . ? C3B C4B Ta1 73.89(17) . . ? C9B C4B Ta1 124.0(5) . . ? C4B C5B C1B 108.0 . . ? C4B C5B C10B 114.4(8) . . ? C1B C5B C10B 137.5(8) . . ? C4B C5B Ta1 73.20(14) . . ? C1B C5B Ta1 73.41(14) . . ? C10B C5B Ta1 121.0(6) . . ? C2B C7B H7B1 109.5 . . ? C2B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C2B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C3B C8B H8B1 109.5 . . ? C3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C4B C9B H9B1 109.5 . . ? C4B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C4B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C5B C10B H10D 109.5 . . ? C5B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C5B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C12 C11 C12 115.1(8) 2 . ? C12 C11 B2 122.5(4) 2 . ? C12 C11 B2 122.5(4) . . ? C13 C12 C11 122.7(6) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C14 C13 C12 119.8(7) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C13 120.0(9) . 2 ? C13 C14 H14 120.0 . . ? C13 C14 H14 120.0 2 . ? B3 Ta1 B2 45.38(16) . . ? B3 Ta1 B1 46.8(2) . . ? B2 Ta1 B1 86.0(2) . . ? B3 Ta1 B3 83.6(2) . 2 ? B2 Ta1 B3 44.81(16) . 2 ? B1 Ta1 B3 103.7(2) . 2 ? B3 Ta1 C2A 130.9(3) . . ? B2 Ta1 C2A 149.8(3) . . ? B1 Ta1 C2A 110.0(3) . . ? B3 Ta1 C2A 143.1(3) 2 . ? B3 Ta1 C3A 96.7(3) . . ? B2 Ta1 C3A 122.9(3) . . ? B1 Ta1 C3A 92.4(3) . . ? B3 Ta1 C3A 157.6(4) 2 . ? C2A Ta1 C3A 35.0(2) . . ? B3 Ta1 C5B 113.6(2) . . ? B2 Ta1 C5B 97.1(2) . . ? B1 Ta1 C5B 142.9(2) . . ? B3 Ta1 C5B 104.3(2) 2 . ? C2A Ta1 C5B 54.6(4) . . ? C3A Ta1 C5B 55.0(4) . . ? B3 Ta1 C4B 88.2(2) . . ? B2 Ta1 C4B 96.0(2) . . ? B1 Ta1 C4B 108.2(2) . . ? B3 Ta1 C4B 126.6(2) 2 . ? C2A Ta1 C4B 55.2(3) . . ? C3A Ta1 C4B 31.4(4) . . ? C5B Ta1 C4B 34.72(11) . . ? B3 Ta1 C1B 145.5(2) . . ? B2 Ta1 C1B 127.7(2) . . ? B1 Ta1 C1B 142.1(2) . . ? B3 Ta1 C1B 112.7(2) 2 . ? C2A Ta1 C1B 32.1(4) . . ? C3A Ta1 C1B 56.5(3) . . ? C5B Ta1 C1B 34.68(11) . . ? C4B Ta1 C1B 57.48(18) . . ? B3 Ta1 C1A 144.1(3) . . ? B2 Ta1 C1A 124.5(3) . . ? B1 Ta1 C1A 144.8(4) . . ? B3 Ta1 C1A 110.5(3) 2 . ? C2A Ta1 C1A 34.81(19) . . ? C3A Ta1 C1A 57.7(3) . . ? C5B Ta1 C1A 32.1(4) . . ? C4B Ta1 C1A 56.6(3) . . ? C1B Ta1 C1A 3.1(5) . . ? B3 Ta1 C3B 97.4(2) . . ? B2 Ta1 C3B 125.22(17) . . ? B1 Ta1 C3B 90.8(2) . . ? B3 Ta1 C3B 160.5(2) 2 . ? C2A Ta1 C3B 33.9(3) . . ? C3A Ta1 C3B 3.0(5) . . ? C5B Ta1 C3B 57.36(18) . . ? C4B Ta1 C3B 34.40(10) . . ? C1B Ta1 C3B 57.11(17) . . ? C1A Ta1 C3B 58.4(4) . . ? B3 Ta1 C2B 130.6(2) . . ? B2 Ta1 C2B 152.3(2) . . ? B1 Ta1 C2B 107.8(2) . . ? B3 Ta1 C2B 144.41(19) 2 . ? C2A Ta1 C2B 2.8(5) . . ? C3A Ta1 C2B 35.5(3) . . ? C5B Ta1 C2B 57.32(17) . . ? C4B Ta1 C2B 57.13(17) . . ? C1B Ta1 C2B 34.34(10) . . ? C1A Ta1 C2B 37.1(4) . . ? C3B Ta1 C2B 34.17(10) . . ? B3 Ta1 H1Z 76.0(15) . . ? B2 Ta1 H1Z 114.4(15) . . ? B1 Ta1 H1Z 29.5(15) . . ? B3 Ta1 H1Z 117.7(14) 2 . ? C2A Ta1 H1Z 87.3(15) . . ? C3A Ta1 H1Z 83.8(14) . . ? C5B Ta1 H1Z 137.9(14) . . ? C4B Ta1 H1Z 111.0(14) . . ? C1B Ta1 H1Z 117.2(15) . . ? C1A Ta1 H1Z 120.3(15) . . ? C3B Ta1 H1Z 81.2(14) . . ? C2B Ta1 H1Z 84.7(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 C11 B2 B3 B1 177.7(3) . . . . ? B3 B2 B3 B1 -2.3(3) 2 . . . ? Ta1 B2 B3 B1 41.7(4) . . . . ? Ta1 B2 B3 B1 -45.5(4) 2 . . . ? C11 B2 B3 Ta1 136.00(10) . . . . ? B3 B2 B3 Ta1 -44.00(10) 2 . . . ? Ta1 B2 B3 Ta1 -87.25(19) 2 . . . ? C11 B2 B3 Ta1 -136.75(11) . . . 2 ? B3 B2 B3 Ta1 43.25(11) 2 . . 2 ? Ta1 B2 B3 Ta1 87.25(19) . . . 2 ? Ta1 B1 B3 B2 -41.8(3) . . . . ? Ta1 B1 B3 B2 43.8(3) 2 . . . ? Ta1 B1 B3 Ta1 85.68(16) 2 . . . ? Ta1 B1 B3 Ta1 -85.68(16) . . . 2 ? C5A C1A C2A C3A 0.0 . . . . ? C6A C1A C2A C3A -174.8 . . . . ? Ta1 C1A C2A C3A 65.9(3) . . . . ? C5A C1A C2A C7A 158.0 . . . . ? C6A C1A C2A C7A -16.8 . . . . ? Ta1 C1A C2A C7A -136.1(3) . . . . ? C5A C1A C2A Ta1 -65.9(3) . . . . ? C6A C1A C2A Ta1 119.3(3) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C7A C2A C3A C4A -169.5 . . . . ? Ta1 C2A C3A C4A 66.5(3) . . . . ? C1A C2A C3A C8A 167.3(19) . . . . ? C7A C2A C3A C8A -2.2(19) . . . . ? Ta1 C2A C3A C8A -126(2) . . . . ? C1A C2A C3A Ta1 -66.5(3) . . . . ? C7A C2A C3A Ta1 124.0(3) . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C8A C3A C4A C5A -174.1(9) . . . . ? Ta1 C3A C4A C5A 64.6(3) . . . . ? C2A C3A C4A C9A 169(2) . . . . ? C8A C3A C4A C9A -5.4(19) . . . . ? Ta1 C3A C4A C9A -127(2) . . . . ? C2A C3A C4A Ta1 -64.6(3) . . . . ? C8A C3A C4A Ta1 121.3(10) . . . . ? C2A C1A C5A C4A 0.0 . . . . ? C6A C1A C5A C4A 173.7 . . . . ? Ta1 C1A C5A C4A -63.7(3) . . . . ? C2A C1A C5A C10A -171.3(13) . . . . ? C6A C1A C5A C10A 2.4(13) . . . . ? Ta1 C1A C5A C10A 125.0(14) . . . . ? C2A C1A C5A Ta1 63.7(3) . . . . ? C6A C1A C5A Ta1 -122.6(3) . . . . ? C3A C4A C5A C1A 0.0 . . . . ? C9A C4A C5A C1A -174.6(10) . . . . ? Ta1 C4A C5A C1A 62.9(3) . . . . ? C3A C4A C5A C10A 164(2) . . . . ? C9A C4A C5A C10A -10(2) . . . . ? Ta1 C4A C5A C10A -133(2) . . . . ? C3A C4A C5A Ta1 -62.9(3) . . . . ? C9A C4A C5A Ta1 122.6(11) . . . . ? C5B C1B C2B C3B 0.0 . . . . ? C6B C1B C2B C3B -172.9 . . . . ? Ta1 C1B C2B C3B 64.27(15) . . . . ? C5B C1B C2B C7B 176.6 . . . . ? C6B C1B C2B C7B 3.6 . . . . ? Ta1 C1B C2B C7B -119.14(15) . . . . ? C5B C1B C2B Ta1 -64.27(15) . . . . ? C6B C1B C2B Ta1 122.78(15) . . . . ? C1B C2B C3B C4B 0.0 . . . . ? C7B C2B C3B C4B -175.8 . . . . ? Ta1 C2B C3B C4B 63.63(18) . . . . ? C1B C2B C3B C8B 178.3(5) . . . . ? C7B C2B C3B C8B 2.5(5) . . . . ? Ta1 C2B C3B C8B -118.1(6) . . . . ? C1B C2B C3B Ta1 -63.63(18) . . . . ? C7B C2B C3B Ta1 120.58(18) . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C8B C3B C4B C5B -177.8(7) . . . . ? Ta1 C3B C4B C5B 64.50(14) . . . . ? C2B C3B C4B C9B 175.0(5) . . . . ? C8B C3B C4B C9B -2.8(7) . . . . ? Ta1 C3B C4B C9B -120.5(6) . . . . ? C2B C3B C4B Ta1 -64.50(14) . . . . ? C8B C3B C4B Ta1 117.7(7) . . . . ? C3B C4B C5B C1B 0.0 . . . . ? C9B C4B C5B C1B -173.5(7) . . . . ? Ta1 C4B C5B C1B 65.69(16) . . . . ? C3B C4B C5B C10B 177.3(6) . . . . ? C9B C4B C5B C10B 3.8(8) . . . . ? Ta1 C4B C5B C10B -117.0(7) . . . . ? C3B C4B C5B Ta1 -65.69(16) . . . . ? C9B C4B C5B Ta1 120.8(8) . . . . ? C2B C1B C5B C4B 0.0 . . . . ? C6B C1B C5B C4B 175.3 . . . . ? Ta1 C1B C5B C4B -65.55(17) . . . . ? C2B C1B C5B C10B -176.3(9) . . . . ? C6B C1B C5B C10B -1.0(9) . . . . ? Ta1 C1B C5B C10B 118.1(10) . . . . ? C2B C1B C5B Ta1 65.55(17) . . . . ? C6B C1B C5B Ta1 -119.13(17) . . . . ? B3 B2 C11 C12 11.2(3) . . . 2 ? B3 B2 C11 C12 -168.8(3) 2 . . 2 ? Ta1 B2 C11 C12 99.6(3) . . . 2 ? Ta1 B2 C11 C12 -80.4(3) 2 . . 2 ? B3 B2 C11 C12 -168.8(3) . . . . ? B3 B2 C11 C12 11.2(3) 2 . . . ? Ta1 B2 C11 C12 -80.4(3) . . . . ? Ta1 B2 C11 C12 99.6(3) 2 . . . ? C12 C11 C12 C13 -0.6(4) 2 . . . ? B2 C11 C12 C13 179.4(4) . . . . ? C11 C12 C13 C14 1.3(8) . . . . ? C12 C13 C14 C13 -0.6(4) . . . 2 ? B1 B3 Ta1 B2 -142.4(4) . . . . ? Ta1 B3 Ta1 B2 -68.8(2) 2 . . . ? B2 B3 Ta1 B1 142.4(4) . . . . ? Ta1 B3 Ta1 B1 73.5(3) 2 . . . ? B2 B3 Ta1 B3 26.8(3) . . . 2 ? B1 B3 Ta1 B3 -115.5(3) . . . 2 ? Ta1 B3 Ta1 B3 -42.0(3) 2 . . 2 ? B2 B3 Ta1 C2A -138.7(5) . . . . ? B1 B3 Ta1 C2A 78.9(5) . . . . ? Ta1 B3 Ta1 C2A 152.4(4) 2 . . . ? B2 B3 Ta1 C3A -130.6(4) . . . . ? B1 B3 Ta1 C3A 87.0(4) . . . . ? Ta1 B3 Ta1 C3A 160.5(3) 2 . . . ? B2 B3 Ta1 C5B -76.0(3) . . . . ? B1 B3 Ta1 C5B 141.6(3) . . . . ? Ta1 B3 Ta1 C5B -144.9(2) 2 . . . ? B2 B3 Ta1 C4B -100.3(3) . . . . ? B1 B3 Ta1 C4B 117.3(3) . . . . ? Ta1 B3 Ta1 C4B -169.2(2) 2 . . . ? B2 B3 Ta1 C1B -94.6(4) . . . . ? B1 B3 Ta1 C1B 123.0(4) . . . . ? Ta1 B3 Ta1 C1B -163.4(3) 2 . . . ? B2 B3 Ta1 C1A -89.7(6) . . . . ? B1 B3 Ta1 C1A 127.9(6) . . . . ? Ta1 B3 Ta1 C1A -158.5(6) 2 . . . ? B2 B3 Ta1 C3B -133.5(3) . . . . ? B1 B3 Ta1 C3B 84.1(3) . . . . ? Ta1 B3 Ta1 C3B 157.6(2) 2 . . . ? B2 B3 Ta1 C2B -142.4(3) . . . . ? B1 B3 Ta1 C2B 75.3(4) . . . . ? Ta1 B3 Ta1 C2B 148.8(2) 2 . . . ? C11 B2 Ta1 B3 -108.7(3) . . . . ? B3 B2 Ta1 B3 140.5(4) 2 . . . ? Ta1 B2 Ta1 B3 71.3(3) 2 . . . ? C11 B2 Ta1 B1 -135.17(18) . . . . ? B3 B2 Ta1 B1 -26.5(3) . . . . ? B3 B2 Ta1 B1 114.0(3) 2 . . . ? Ta1 B2 Ta1 B1 44.83(18) 2 . . . ? C11 B2 Ta1 B3 110.9(2) . . . 2 ? B3 B2 Ta1 B3 -140.5(4) . . . 2 ? Ta1 B2 Ta1 B3 -69.1(2) 2 . . 2 ? C11 B2 Ta1 C2A -11.0(5) . . . . ? B3 B2 Ta1 C2A 97.7(6) . . . . ? B3 B2 Ta1 C2A -121.8(6) 2 . . . ? Ta1 B2 Ta1 C2A 169.0(5) 2 . . . ? C11 B2 Ta1 C3A -44.9(4) . . . . ? B3 B2 Ta1 C3A 63.8(5) . . . . ? B3 B2 Ta1 C3A -155.7(4) 2 . . . ? Ta1 B2 Ta1 C3A 135.1(4) 2 . . . ? C11 B2 Ta1 C5B 7.68(15) . . . . ? B3 B2 Ta1 C5B 116.4(3) . . . . ? B3 B2 Ta1 C5B -103.2(3) 2 . . . ? Ta1 B2 Ta1 C5B -172.31(15) 2 . . . ? C11 B2 Ta1 C4B -27.26(15) . . . . ? B3 B2 Ta1 C4B 81.4(3) . . . . ? B3 B2 Ta1 C4B -138.1(3) 2 . . . ? Ta1 B2 Ta1 C4B 152.74(15) 2 . . . ? C11 B2 Ta1 C1B 25.8(2) . . . . ? B3 B2 Ta1 C1B 134.5(3) . . . . ? B3 B2 Ta1 C1B -85.1(3) 2 . . . ? Ta1 B2 Ta1 C1B -154.2(2) 2 . . . ? C11 B2 Ta1 C1A 25.9(3) . . . . ? B3 B2 Ta1 C1A 134.6(4) . . . . ? B3 B2 Ta1 C1A -84.9(4) 2 . . . ? Ta1 B2 Ta1 C1A -154.1(3) 2 . . . ? C11 B2 Ta1 C3B -47.1(2) . . . . ? B3 B2 Ta1 C3B 61.6(4) . . . . ? B3 B2 Ta1 C3B -157.9(3) 2 . . . ? Ta1 B2 Ta1 C3B 132.9(2) 2 . . . ? C11 B2 Ta1 C2B -13.5(3) . . . . ? B3 B2 Ta1 C2B 95.1(4) . . . . ? B3 B2 Ta1 C2B -124.4(4) 2 . . . ? Ta1 B2 Ta1 C2B 166.5(3) 2 . . . ? Ta1 B1 Ta1 B3 -67.9(3) 2 . . . ? B3 B1 Ta1 B2 25.8(3) . . . . ? Ta1 B1 Ta1 B2 -42.13(16) 2 . . . ? B3 B1 Ta1 B3 67.3(3) . . . 2 ? Ta1 B1 Ta1 B3 -0.6(3) 2 . . 2 ? B3 B1 Ta1 C2A -127.9(4) . . . . ? Ta1 B1 Ta1 C2A 164.1(3) 2 . . . ? B3 B1 Ta1 C3A -97.0(4) . . . . ? Ta1 B1 Ta1 C3A -164.9(3) 2 . . . ? B3 B1 Ta1 C5B -70.7(4) . . . . ? Ta1 B1 Ta1 C5B -138.6(3) 2 . . . ? B3 B1 Ta1 C4B -69.2(3) . . . . ? Ta1 B1 Ta1 C4B -137.18(19) 2 . . . ? B3 B1 Ta1 C1B -129.3(4) . . . . ? Ta1 B1 Ta1 C1B 162.7(3) 2 . . . ? B3 B1 Ta1 C1A -126.6(6) . . . . ? Ta1 B1 Ta1 C1A 165.5(5) 2 . . . ? B3 B1 Ta1 C3B -99.4(3) . . . . ? Ta1 B1 Ta1 C3B -167.38(19) 2 . . . ? B3 B1 Ta1 C2B -129.6(3) . . . . ? Ta1 B1 Ta1 C2B 162.45(17) 2 . . . ? C3A C2A Ta1 B3 14.2(3) . . . . ? C1A C2A Ta1 B3 129.1(4) . . . . ? C7A C2A Ta1 B3 -75.0(4) . . . . ? C3A C2A Ta1 B2 -54.9(4) . . . . ? C1A C2A Ta1 B2 60.1(5) . . . . ? C7A C2A Ta1 B2 -144.0(4) . . . . ? C3A C2A Ta1 B1 63.7(2) . . . . ? C1A C2A Ta1 B1 178.7(3) . . . . ? C7A C2A Ta1 B1 -25.4(3) . . . . ? C3A C2A Ta1 B3 -141.5(6) . . . 2 ? C1A C2A Ta1 B3 -26.5(4) . . . 2 ? C7A C2A Ta1 B3 129.4(4) . . . 2 ? C1A C2A Ta1 C3A 114.94(16) . . . . ? C7A C2A Ta1 C3A -89.1(2) . . . . ? C3A C2A Ta1 C5B -77.8(4) . . . . ? C1A C2A Ta1 C5B 37.2(4) . . . . ? C7A C2A Ta1 C5B -166.9(5) . . . . ? C3A C2A Ta1 C4B -35.0(5) . . . . ? C1A C2A Ta1 C4B 79.9(4) . . . . ? C7A C2A Ta1 C4B -124.1(5) . . . . ? C3A C2A Ta1 C1B -117.9(6) . . . . ? C1A C2A Ta1 C1B -3.0(8) . . . . ? C7A C2A Ta1 C1B 153.0(8) . . . . ? C3A C2A Ta1 C1A -114.94(16) . . . . ? C7A C2A Ta1 C1A 155.94(11) . . . . ? C3A C2A Ta1 C3B 4.9(9) . . . . ? C1A C2A Ta1 C3B 119.8(7) . . . . ? C7A C2A Ta1 C3B -84.2(8) . . . . ? C3A C2A Ta1 C2B 99(7) . . . . ? C1A C2A Ta1 C2B -146(7) . . . . ? C7A C2A Ta1 C2B 10(7) . . . . ? C4A C3A Ta1 B3 75.43(18) . . . . ? C2A C3A Ta1 B3 -169.3(2) . . . . ? C8A C3A Ta1 B3 -15.5(13) . . . . ? C4A C3A Ta1 B2 35.40(19) . . . . ? C2A C3A Ta1 B2 150.7(3) . . . . ? C8A C3A Ta1 B2 -55.5(14) . . . . ? C4A C3A Ta1 B1 122.2(2) . . . . ? C2A C3A Ta1 B1 -122.5(2) . . . . ? C8A C3A Ta1 B1 31.3(13) . . . . ? C4A C3A Ta1 B3 -14.1(6) . . . 2 ? C2A C3A Ta1 B3 101.2(7) . . . 2 ? C8A C3A Ta1 B3 -105.0(15) . . . 2 ? C4A C3A Ta1 C2A -115.29(16) . . . . ? C8A C3A Ta1 C2A 153.8(12) . . . . ? C4A C3A Ta1 C5B -38.8(4) . . . . ? C2A C3A Ta1 C5B 76.5(4) . . . . ? C8A C3A Ta1 C5B -129.7(14) . . . . ? C4A C3A Ta1 C4B 0.1(7) . . . . ? C2A C3A Ta1 C4B 115.4(6) . . . . ? C8A C3A Ta1 C4B -90.8(13) . . . . ? C4A C3A Ta1 C1B -81.0(4) . . . . ? C2A C3A Ta1 C1B 34.3(5) . . . . ? C8A C3A Ta1 C1B -172.0(15) . . . . ? C4A C3A Ta1 C1A -77.51(18) . . . . ? C2A C3A Ta1 C1A 37.78(9) . . . . ? C8A C3A Ta1 C1A -168.5(12) . . . . ? C2A C3A Ta1 C3B -66(7) . . . . ? C8A C3A Ta1 C3B 88(7) . . . . ? C4A C3A Ta1 C2B -120.0(7) . . . . ? C2A C3A Ta1 C2B -4.7(8) . . . . ? C8A C3A Ta1 C2B 149.1(18) . . . . ? C4B C5B Ta1 B3 -46.24(17) . . . . ? C1B C5B Ta1 B3 -161.5(2) . . . . ? C10B C5B Ta1 B3 62.5(10) . . . . ? C4B C5B Ta1 B2 -90.36(5) . . . . ? C1B C5B Ta1 B2 154.38(7) . . . . ? C10B C5B Ta1 B2 18.4(10) . . . . ? C4B C5B Ta1 B1 2.4(3) . . . . ? C1B C5B Ta1 B1 -112.8(4) . . . . ? C10B C5B Ta1 B1 111.2(11) . . . . ? C4B C5B Ta1 B3 -135.45(17) . . . 2 ? C1B C5B Ta1 B3 109.29(17) . . . 2 ? C10B C5B Ta1 B3 -26.7(10) . . . 2 ? C4B C5B Ta1 C2A 78.3(4) . . . . ? C1B C5B Ta1 C2A -37.0(4) . . . . ? C10B C5B Ta1 C2A -173.0(11) . . . . ? C4B C5B Ta1 C3A 35.1(4) . . . . ? C1B C5B Ta1 C3A -80.2(4) . . . . ? C10B C5B Ta1 C3A 143.9(11) . . . . ? C1B C5B Ta1 C4B -115.26(9) . . . . ? C10B C5B Ta1 C4B 108.8(10) . . . . ? C4B C5B Ta1 C1B 115.26(9) . . . . ? C10B C5B Ta1 C1B -136.0(10) . . . . ? C4B C5B Ta1 C1A 118.7(8) . . . . ? C1B C5B Ta1 C1A 3.4(9) . . . . ? C10B C5B Ta1 C1A -132.6(14) . . . . ? C4B C5B Ta1 C3B 37.2 . . . . ? C1B C5B Ta1 C3B -78.01(8) . . . . ? C10B C5B Ta1 C3B 146.0(10) . . . . ? C4B C5B Ta1 C2B 78.10(9) . . . . ? C1B C5B Ta1 C2B -37.2 . . . . ? C10B C5B Ta1 C2B -173.1(10) . . . . ? C5B C4B Ta1 B3 138.54(17) . . . . ? C3B C4B Ta1 B3 -105.90(16) . . . . ? C9B C4B Ta1 B3 4.3(8) . . . . ? C5B C4B Ta1 B2 93.77(9) . . . . ? C3B C4B Ta1 B2 -150.67(9) . . . . ? C9B C4B Ta1 B2 -40.5(8) . . . . ? C5B C4B Ta1 B1 -178.5(2) . . . . ? C3B C4B Ta1 B1 -62.90(19) . . . . ? C9B C4B Ta1 B1 47.3(9) . . . . ? C5B C4B Ta1 B3 57.89(19) . . . 2 ? C3B C4B Ta1 B3 173.4(2) . . . 2 ? C9B C4B Ta1 B3 -76.4(8) . . . 2 ? C5B C4B Ta1 C2A -76.3(5) . . . . ? C3B C4B Ta1 C2A 39.2(5) . . . . ? C9B C4B Ta1 C2A 149.4(11) . . . . ? C5B C4B Ta1 C3A -115.4(7) . . . . ? C3B C4B Ta1 C3A 0.1(7) . . . . ? C9B C4B Ta1 C3A 110.3(11) . . . . ? C3B C4B Ta1 C5B 115.56(7) . . . . ? C9B C4B Ta1 C5B -134.3(8) . . . . ? C5B C4B Ta1 C1B -37.61(6) . . . . ? C3B C4B Ta1 C1B 77.95(9) . . . . ? C9B C4B Ta1 C1B -171.9(8) . . . . ? C5B C4B Ta1 C1A -34.0(5) . . . . ? C3B C4B Ta1 C1A 81.5(5) . . . . ? C9B C4B Ta1 C1A -168.3(11) . . . . ? C5B C4B Ta1 C3B -115.56(7) . . . . ? C9B C4B Ta1 C3B 110.2(8) . . . . ? C5B C4B Ta1 C2B -78.68(8) . . . . ? C3B C4B Ta1 C2B 36.88(6) . . . . ? C9B C4B Ta1 C2B 147.1(8) . . . . ? C2B C1B Ta1 B3 -84.8(4) . . . . ? C5B C1B Ta1 B3 30.9(3) . . . . ? C6B C1B Ta1 B3 133.7(3) . . . . ? C2B C1B Ta1 B2 -148.48(17) . . . . ? C5B C1B Ta1 B2 -32.82(11) . . . . ? C6B C1B Ta1 B2 70.06(19) . . . . ? C2B C1B Ta1 B1 -0.5(3) . . . . ? C5B C1B Ta1 B1 115.2(4) . . . . ? C6B C1B Ta1 B1 -141.9(3) . . . . ? C2B C1B Ta1 B3 162.0(2) . . . 2 ? C5B C1B Ta1 B3 -82.37(19) . . . 2 ? C6B C1B Ta1 B3 20.5(2) . . . 2 ? C2B C1B Ta1 C2A -3.0(8) . . . . ? C5B C1B Ta1 C2A 112.7(7) . . . . ? C6B C1B Ta1 C2A -144.4(8) . . . . ? C2B C1B Ta1 C3A -40.4(5) . . . . ? C5B C1B Ta1 C3A 75.3(5) . . . . ? C6B C1B Ta1 C3A 178.2(5) . . . . ? C2B C1B Ta1 C5B -115.67(8) . . . . ? C6B C1B Ta1 C5B 102.88(10) . . . . ? C2B C1B Ta1 C4B -78.01(9) . . . . ? C5B C1B Ta1 C4B 37.65(6) . . . . ? C6B C1B Ta1 C4B 140.54(6) . . . . ? C2B C1B Ta1 C1A -151(7) . . . . ? C5B C1B Ta1 C1A -35(7) . . . . ? C6B C1B Ta1 C1A 68(7) . . . . ? C2B C1B Ta1 C3B -36.87(6) . . . . ? C5B C1B Ta1 C3B 78.80(8) . . . . ? C6B C1B Ta1 C3B -178.318(18) . . . . ? C5B C1B Ta1 C2B 115.67(8) . . . . ? C6B C1B Ta1 C2B -141.45(7) . . . . ? C5A C1A Ta1 B3 27.4(5) . . . . ? C2A C1A Ta1 B3 -88.3(5) . . . . ? C6A C1A Ta1 B3 159.9(4) . . . . ? C5A C1A Ta1 B2 -32.36(15) . . . . ? C2A C1A Ta1 B2 -148.1(3) . . . . ? C6A C1A Ta1 B2 100.1(3) . . . . ? C5A C1A Ta1 B1 113.6(5) . . . . ? C2A C1A Ta1 B1 -2.2(4) . . . . ? C6A C1A Ta1 B1 -114.0(5) . . . . ? C5A C1A Ta1 B3 -80.9(2) . . . 2 ? C2A C1A Ta1 B3 163.4(3) . . . 2 ? C6A C1A Ta1 B3 51.6(3) . . . 2 ? C5A C1A Ta1 C2A 115.71(14) . . . . ? C6A C1A Ta1 C2A -111.8(2) . . . . ? C5A C1A Ta1 C3A 77.75(16) . . . . ? C2A C1A Ta1 C3A -37.96(12) . . . . ? C6A C1A Ta1 C3A -149.75(10) . . . . ? C5A C1A Ta1 C5B 3.4(8) . . . . ? C2A C1A Ta1 C5B -112.3(7) . . . . ? C6A C1A Ta1 C5B 135.9(9) . . . . ? C5A C1A Ta1 C4B 40.2(5) . . . . ? C2A C1A Ta1 C4B -75.6(4) . . . . ? C6A C1A Ta1 C4B 172.7(6) . . . . ? C5A C1A Ta1 C1B 146(7) . . . . ? C2A C1A Ta1 C1B 30(7) . . . . ? C6A C1A Ta1 C1B -82(7) . . . . ? C5A C1A Ta1 C3B 81.1(4) . . . . ? C2A C1A Ta1 C3B -34.6(4) . . . . ? C6A C1A Ta1 C3B -146.4(5) . . . . ? C5A C1A Ta1 C2B 118.3(5) . . . . ? C2A C1A Ta1 C2B 2.6(6) . . . . ? C6A C1A Ta1 C2B -109.2(7) . . . . ? C2B C3B Ta1 B3 -168.06(18) . . . . ? C4B C3B Ta1 B3 75.77(17) . . . . ? C8B C3B Ta1 B3 -56.5(7) . . . . ? C2B C3B Ta1 B2 152.8(2) . . . . ? C4B C3B Ta1 B2 36.60(16) . . . . ? C8B C3B Ta1 B2 -95.7(7) . . . . ? C2B C3B Ta1 B1 -121.57(19) . . . . ? C4B C3B Ta1 B1 122.25(19) . . . . ? C8B C3B Ta1 B1 -10.1(7) . . . . ? C2B C3B Ta1 B3 100.2(6) . . . 2 ? C4B C3B Ta1 B3 -15.9(5) . . . 2 ? C8B C3B Ta1 B3 -148.3(7) . . . 2 ? C2B C3B Ta1 C2A 4.9(9) . . . . ? C4B C3B Ta1 C2A -111.3(8) . . . . ? C8B C3B Ta1 C2A 116.4(12) . . . . ? C2B C3B Ta1 C3A 115(7) . . . . ? C4B C3B Ta1 C3A -1(7) . . . . ? C8B C3B Ta1 C3A -134(7) . . . . ? C2B C3B Ta1 C5B 78.57(8) . . . . ? C4B C3B Ta1 C5B -37.61(5) . . . . ? C8B C3B Ta1 C5B -169.9(6) . . . . ? C2B C3B Ta1 C4B 116.17(9) . . . . ? C8B C3B Ta1 C4B -132.3(7) . . . . ? C2B C3B Ta1 C1B 37.0 . . . . ? C4B C3B Ta1 C1B -79.12(10) . . . . ? C8B C3B Ta1 C1B 148.6(6) . . . . ? C2B C3B Ta1 C1A 40.4(5) . . . . ? C4B C3B Ta1 C1A -75.7(4) . . . . ? C8B C3B Ta1 C1A 151.9(9) . . . . ? C4B C3B Ta1 C2B -116.17(9) . . . . ? C8B C3B Ta1 C2B 111.5(7) . . . . ? C1B C2B Ta1 B3 131.9(3) . . . . ? C3B C2B Ta1 B3 15.7(2) . . . . ? C7B C2B Ta1 B3 -116.4(2) . . . . ? C1B C2B Ta1 B2 62.8(3) . . . . ? C3B C2B Ta1 B2 -53.4(3) . . . . ? C7B C2B Ta1 B2 174.48(19) . . . . ? C1B C2B Ta1 B1 179.7(2) . . . . ? C3B C2B Ta1 B1 63.5(2) . . . . ? C7B C2B Ta1 B1 -68.6(2) . . . . ? C1B C2B Ta1 B3 -29.4(3) . . . 2 ? C3B C2B Ta1 B3 -145.6(4) . . . 2 ? C7B C2B Ta1 B3 82.3(4) . . . 2 ? C1B C2B Ta1 C2A 35(7) . . . . ? C3B C2B Ta1 C2A -81(7) . . . . ? C7B C2B Ta1 C2A 146(8) . . . . ? C1B C2B Ta1 C3A 111.6(8) . . . . ? C3B C2B Ta1 C3A -4.7(8) . . . . ? C7B C2B Ta1 C3A -136.7(9) . . . . ? C1B C2B Ta1 C5B 37.54(5) . . . . ? C3B C2B Ta1 C5B -78.70(8) . . . . ? C7B C2B Ta1 C5B 149.22(6) . . . . ? C1B C2B Ta1 C4B 79.12(10) . . . . ? C3B C2B Ta1 C4B -37.1 . . . . ? C7B C2B Ta1 C4B -169.2 . . . . ? C3B C2B Ta1 C1B -116.25(9) . . . . ? C7B C2B Ta1 C1B 111.68(10) . . . . ? C1B C2B Ta1 C1A 2.6(6) . . . . ? C3B C2B Ta1 C1A -113.7(6) . . . . ? C7B C2B Ta1 C1A 114.2(6) . . . . ? C1B C2B Ta1 C3B 116.25(9) . . . . ? C7B C2B Ta1 C3B -132.08(7) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.924 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.123