Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Roland Fischer' _publ_contact_author_address ; Department of Chemistry Lehrstuhl fur Anorganische Chemie II - Organometallics and Materials Chemistry Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum Bochum GERMANY ; _publ_contact_author_email ROLAND.FISCHER@RUHR-UNI-BOCHUM.DE _publ_section_title ; Tantalum complexes with all nitrogen coordination sphere: Mixed amido-, imido-, guanidinato complexes of tantalum and their thermal behaviour ; loop_ _publ_author_name 'Roland Fischer' 'Arne Baunemann' 'Christian Gemel' 'Younsoo Kim' 'Andrian Milanov' 'Daniel Rische' ; M.Winter ; data_cvd30 _database_code_depnum_ccdc_archive 'CCDC 266742' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H55 N8 Ta' _chemical_formula_weight 636.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.5129(11) _cell_length_b 18.099(2) _cell_length_c 34.801(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5991.8(12) _cell_formula_units_Z 8 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 4126 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 25.25 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 3.694 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(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 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '1109 images at 1.0 deg in \w and 15 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 92622 _diffrn_reflns_av_R_equivalents 0.1383 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.31 _reflns_number_total 5460 _reflns_number_gt 4424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material SHELXL-97 _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^)+(0.0124P)^2^+15.9941P] 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 calculated _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5460 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_restrained_S_all 1.242 _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 Ta1 Ta 0.46683(2) 0.107114(12) 0.377171(6) 0.01275(8) Uani 1 1 d . . . N1 N 0.5621(5) 0.0090(2) 0.40209(13) 0.0147(11) Uani 1 1 d . . . N2 N 0.6899(4) 0.1101(3) 0.39894(12) 0.0134(10) Uani 1 1 d . . . N3 N 0.5688(5) 0.0796(3) 0.31585(13) 0.0164(12) Uani 1 1 d . . . N4 N 0.4992(5) 0.1915(2) 0.33549(13) 0.0143(11) Uani 1 1 d . . . N5 N 0.2896(5) 0.0584(3) 0.35822(13) 0.0151(11) Uani 1 1 d . . . N6 N 0.3954(5) 0.1560(3) 0.41720(13) 0.0164(11) Uani 1 1 d . . . N7 N 0.5890(6) 0.1807(3) 0.27127(13) 0.0230(12) Uani 1 1 d . . . N8 N 0.7893(6) 0.0076(3) 0.43275(15) 0.0213(13) Uani 1 1 d . . . C1 C 0.6840(6) 0.0420(3) 0.41148(16) 0.0126(13) Uani 1 1 d . . . C2 C 0.5534(6) 0.1498(3) 0.30652(16) 0.0149(13) Uani 1 1 d . . . C3 C 0.8536(7) 0.0415(4) 0.46597(17) 0.0263(16) Uani 1 1 d . . . H3A H 0.9537 0.0499 0.4609 0.039 Uiso 1 1 calc R . . H3B H 0.8432 0.0088 0.4882 0.039 Uiso 1 1 calc R . . H3C H 0.8075 0.0889 0.4713 0.039 Uiso 1 1 calc R . . C4 C 0.8358(7) -0.0670(3) 0.42442(18) 0.0248(15) Uani 1 1 d . . . H4A H 0.7899 -0.0845 0.4009 0.037 Uiso 1 1 calc R . . H4B H 0.8109 -0.0995 0.4459 0.037 Uiso 1 1 calc R . . H4C H 0.9380 -0.0673 0.4208 0.037 Uiso 1 1 calc R . . C5 C 0.8128(6) 0.1577(3) 0.39955(17) 0.0171(14) Uani 1 1 d . . . H5 H 0.8960 0.1276 0.4076 0.021 Uiso 1 1 calc R . . C6 C 0.7938(7) 0.2208(3) 0.42805(17) 0.0222(15) Uani 1 1 d . . . H6A H 0.7174 0.2530 0.4194 0.033 Uiso 1 1 calc R . . H6B H 0.8811 0.2494 0.4297 0.033 Uiso 1 1 calc R . . H6C H 0.7708 0.2006 0.4534 0.033 Uiso 1 1 calc R . . C7 C 0.8420(7) 0.1904(3) 0.36012(17) 0.0221(15) Uani 1 1 d . . . H7A H 0.8417 0.1509 0.3408 0.033 Uiso 1 1 calc R . . H7B H 0.9340 0.2147 0.3603 0.033 Uiso 1 1 calc R . . H7C H 0.7690 0.2267 0.3538 0.033 Uiso 1 1 calc R . . C8 C 0.7730(7) -0.0039(4) 0.32125(18) 0.0256(17) Uani 1 1 d . . . H8A H 0.8230 0.0349 0.3353 0.038 Uiso 1 1 calc R . . H8B H 0.8404 -0.0330 0.3063 0.038 Uiso 1 1 calc R . . H8C H 0.7243 -0.0362 0.3395 0.038 Uiso 1 1 calc R . . C9 C 0.6657(7) 0.0314(3) 0.29417(17) 0.0213(15) Uani 1 1 d . . . H9 H 0.7171 0.0621 0.2749 0.026 Uiso 1 1 calc R . . C10 C 0.5886(8) -0.0307(4) 0.2729(2) 0.0342(18) Uani 1 1 d . . . H10A H 0.5455 -0.0642 0.2917 0.051 Uiso 1 1 calc R . . H10B H 0.6557 -0.0583 0.2571 0.051 Uiso 1 1 calc R . . H10C H 0.5154 -0.0095 0.2565 0.051 Uiso 1 1 calc R . . C11 C 0.5479(8) 0.1455(4) 0.23584(16) 0.0280(16) Uani 1 1 d . . . H11A H 0.6312 0.1248 0.2232 0.042 Uiso 1 1 calc R . . H11B H 0.5038 0.1819 0.2189 0.042 Uiso 1 1 calc R . . H11C H 0.4810 0.1057 0.2413 0.042 Uiso 1 1 calc R . . C12 C 0.6669(8) 0.2486(3) 0.26785(18) 0.0254(17) Uani 1 1 d . . . H12A H 0.6898 0.2672 0.2935 0.038 Uiso 1 1 calc R . . H12B H 0.6101 0.2852 0.2541 0.038 Uiso 1 1 calc R . . H12C H 0.7540 0.2395 0.2536 0.038 Uiso 1 1 calc R . . C13 C 0.4975(7) 0.3241(3) 0.35068(17) 0.0253(17) Uani 1 1 d . . . H13A H 0.4914 0.3133 0.3782 0.038 Uiso 1 1 calc R . . H13B H 0.4494 0.3708 0.3452 0.038 Uiso 1 1 calc R . . H13C H 0.5965 0.3281 0.3431 0.038 Uiso 1 1 calc R . . C14 C 0.4278(7) 0.2618(3) 0.32803(18) 0.0206(15) Uani 1 1 d . . . H14 H 0.4369 0.2733 0.3000 0.025 Uiso 1 1 calc R . . C15 C 0.2716(7) 0.2567(3) 0.33777(17) 0.0225(16) Uani 1 1 d . . . H15A H 0.2300 0.2146 0.3242 0.034 Uiso 1 1 calc R . . H15B H 0.2243 0.3023 0.3298 0.034 Uiso 1 1 calc R . . H15C H 0.2603 0.2500 0.3655 0.034 Uiso 1 1 calc R . . C16 C 0.2808(7) 0.0026(4) 0.32817(19) 0.0250(16) Uani 1 1 d . . . H16A H 0.2351 -0.0417 0.3384 0.037 Uiso 1 1 calc R . . H16B H 0.3756 -0.0099 0.3193 0.037 Uiso 1 1 calc R . . H16C H 0.2258 0.0220 0.3066 0.037 Uiso 1 1 calc R . . C17 C 0.1483(6) 0.0720(4) 0.37326(19) 0.0265(15) Uani 1 1 d . . . H17A H 0.0870 0.0887 0.3524 0.040 Uiso 1 1 calc R . . H17B H 0.1527 0.1101 0.3932 0.040 Uiso 1 1 calc R . . H17C H 0.1107 0.0263 0.3843 0.040 Uiso 1 1 calc R . . C18 C 0.3579(6) 0.1917(3) 0.45288(16) 0.0185(14) Uani 1 1 d . . . C19 C 0.3767(8) 0.2755(4) 0.45033(18) 0.0280(17) Uani 1 1 d . . . H19A H 0.4752 0.2870 0.4446 0.042 Uiso 1 1 calc R . . H19B H 0.3503 0.2981 0.4749 0.042 Uiso 1 1 calc R . . H19C H 0.3166 0.2951 0.4299 0.042 Uiso 1 1 calc R . . C20 C 0.4539(7) 0.1614(3) 0.48458(16) 0.0245(15) Uani 1 1 d . . . H20A H 0.4405 0.1079 0.4868 0.037 Uiso 1 1 calc R . . H20B H 0.4305 0.1851 0.5091 0.037 Uiso 1 1 calc R . . H20C H 0.5522 0.1719 0.4781 0.037 Uiso 1 1 calc R . . C21 C 0.2048(7) 0.1745(4) 0.46295(19) 0.0306(17) Uani 1 1 d . . . H21A H 0.1430 0.1945 0.4429 0.046 Uiso 1 1 calc R . . H21B H 0.1813 0.1972 0.4877 0.046 Uiso 1 1 calc R . . H21C H 0.1920 0.1209 0.4646 0.046 Uiso 1 1 calc R . . C22 C 0.5091(6) -0.0570(3) 0.42133(16) 0.0178(14) Uani 1 1 d . . . H22 H 0.5822 -0.0744 0.4399 0.021 Uiso 1 1 calc R . . C23 C 0.3754(7) -0.0402(4) 0.4437(2) 0.0308(17) Uani 1 1 d . . . H23A H 0.3954 -0.0030 0.4634 0.046 Uiso 1 1 calc R . . H23B H 0.3411 -0.0855 0.4559 0.046 Uiso 1 1 calc R . . H23C H 0.3036 -0.0211 0.4261 0.046 Uiso 1 1 calc R . . C24 C 0.4814(8) -0.1184(3) 0.39262(19) 0.0299(16) Uani 1 1 d . . . H24A H 0.4124 -0.1016 0.3736 0.045 Uiso 1 1 calc R . . H24B H 0.4447 -0.1618 0.4061 0.045 Uiso 1 1 calc R . . H24C H 0.5692 -0.1314 0.3796 0.045 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 0.01201(11) 0.01568(11) 0.01058(12) -0.00002(12) 0.00005(11) 0.00017(11) N1 0.017(3) 0.014(2) 0.013(3) 0.003(2) 0.000(2) -0.001(2) N2 0.005(2) 0.021(3) 0.014(2) 0.002(2) -0.0003(18) -0.002(2) N3 0.019(3) 0.019(3) 0.010(3) -0.003(2) 0.001(2) 0.001(2) N4 0.017(3) 0.013(2) 0.012(3) 0.000(2) -0.0005(19) 0.001(2) N5 0.014(3) 0.019(3) 0.012(3) -0.001(2) 0.000(2) 0.001(2) N6 0.014(3) 0.019(3) 0.016(3) 0.003(2) -0.003(2) -0.001(2) N7 0.035(3) 0.023(3) 0.011(3) 0.000(2) 0.003(2) -0.004(3) N8 0.020(3) 0.018(3) 0.026(3) -0.002(2) -0.009(2) 0.006(2) C1 0.013(3) 0.016(3) 0.009(3) -0.004(3) 0.000(2) 0.004(3) C2 0.012(3) 0.022(3) 0.011(3) 0.001(2) -0.001(2) -0.001(3) C3 0.027(4) 0.032(4) 0.020(4) 0.000(3) -0.009(3) 0.000(3) C4 0.023(4) 0.026(4) 0.025(4) 0.002(3) 0.001(3) 0.005(3) C5 0.016(3) 0.017(3) 0.018(4) -0.002(3) 0.001(3) 0.002(3) C6 0.027(4) 0.024(4) 0.016(4) -0.001(3) 0.003(3) -0.007(3) C7 0.022(4) 0.022(3) 0.022(3) 0.001(3) -0.002(3) -0.003(3) C8 0.031(4) 0.027(4) 0.019(4) 0.001(3) 0.010(3) 0.009(3) C9 0.027(4) 0.020(3) 0.017(3) -0.004(3) 0.008(3) 0.000(3) C10 0.040(4) 0.031(4) 0.032(4) -0.011(3) 0.013(3) 0.003(4) C11 0.042(5) 0.031(4) 0.011(3) 0.000(3) -0.001(3) -0.005(3) C12 0.032(4) 0.030(4) 0.015(4) 0.003(3) 0.000(3) -0.004(3) C13 0.039(5) 0.016(3) 0.021(3) 0.000(3) -0.005(3) 0.000(3) C14 0.031(4) 0.016(3) 0.015(3) 0.001(3) 0.001(3) 0.005(3) C15 0.027(4) 0.028(4) 0.013(3) 0.003(3) -0.006(3) 0.007(3) C16 0.020(4) 0.025(4) 0.029(4) -0.006(3) 0.000(3) -0.005(3) C17 0.014(3) 0.043(4) 0.023(4) 0.000(3) 0.001(3) 0.000(3) C18 0.018(3) 0.023(3) 0.014(3) -0.003(3) 0.002(3) 0.002(3) C19 0.043(5) 0.028(4) 0.013(3) -0.006(3) -0.001(3) 0.008(3) C20 0.034(4) 0.026(3) 0.013(3) 0.002(3) 0.001(3) 0.005(3) C21 0.023(4) 0.042(4) 0.026(4) -0.010(3) 0.009(3) 0.000(3) C22 0.023(4) 0.015(3) 0.015(3) 0.005(2) -0.002(2) -0.001(3) C23 0.023(4) 0.028(4) 0.041(4) 0.006(3) 0.009(3) -0.004(3) C24 0.039(4) 0.013(3) 0.038(4) 0.003(3) -0.003(3) -0.006(3) _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 N6 1.785(5) . ? Ta1 N5 2.014(5) . ? Ta1 N4 2.129(4) . ? Ta1 N1 2.174(4) . ? Ta1 N2 2.254(4) . ? Ta1 N3 2.396(5) . ? Ta1 C1 2.661(6) . ? N1 C1 1.345(7) . ? N1 C22 1.459(7) . ? N2 C1 1.309(7) . ? N2 C5 1.452(7) . ? N3 C2 1.320(7) . ? N3 C9 1.477(7) . ? N4 C2 1.361(7) . ? N4 C14 1.466(7) . ? N5 C16 1.456(7) . ? N5 C17 1.463(7) . ? N6 C18 1.444(7) . ? N7 C2 1.390(7) . ? N7 C12 1.440(8) . ? N7 C11 1.442(7) . ? N8 C1 1.393(7) . ? N8 C3 1.444(8) . ? N8 C4 1.450(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.520(8) . ? C5 C6 1.524(8) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.529(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.532(9) . ? C9 H9 1.0000 . ? 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 C14 1.527(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.527(9) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.530(8) . ? C18 C19 1.530(8) . ? C18 C20 1.533(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C24 1.518(8) . ? C22 C23 1.521(8) . ? C22 H22 1.0000 . ? 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 N6 Ta1 N5 98.8(2) . . ? N6 Ta1 N4 103.35(19) . . ? N5 Ta1 N4 102.23(18) . . ? N6 Ta1 N1 104.64(19) . . ? N5 Ta1 N1 97.00(18) . . ? N4 Ta1 N1 142.91(17) . . ? N6 Ta1 N2 94.84(19) . . ? N5 Ta1 N2 155.36(19) . . ? N4 Ta1 N2 94.35(17) . . ? N1 Ta1 N2 59.56(18) . . ? N6 Ta1 N3 162.19(19) . . ? N5 Ta1 N3 87.50(17) . . ? N4 Ta1 N3 58.92(16) . . ? N1 Ta1 N3 90.96(17) . . ? N2 Ta1 N3 85.60(16) . . ? N6 Ta1 C1 99.52(19) . . ? N5 Ta1 C1 127.09(18) . . ? N4 Ta1 C1 120.74(17) . . ? N1 Ta1 C1 30.22(17) . . ? N2 Ta1 C1 29.42(17) . . ? N3 Ta1 C1 89.61(16) . . ? C1 N1 C22 123.4(5) . . ? C1 N1 Ta1 95.3(3) . . ? C22 N1 Ta1 135.0(4) . . ? C1 N2 C5 126.0(5) . . ? C1 N2 Ta1 92.8(3) . . ? C5 N2 Ta1 141.0(4) . . ? C2 N3 C9 120.8(5) . . ? C2 N3 Ta1 88.5(3) . . ? C9 N3 Ta1 146.2(4) . . ? C2 N4 C14 121.7(5) . . ? C2 N4 Ta1 99.3(3) . . ? C14 N4 Ta1 132.6(4) . . ? C16 N5 C17 108.7(5) . . ? C16 N5 Ta1 125.9(4) . . ? C17 N5 Ta1 125.3(4) . . ? C18 N6 Ta1 170.6(4) . . ? C2 N7 C12 122.8(5) . . ? C2 N7 C11 120.7(5) . . ? C12 N7 C11 116.5(5) . . ? C1 N8 C3 122.7(5) . . ? C1 N8 C4 121.9(5) . . ? C3 N8 C4 115.3(5) . . ? N2 C1 N1 112.0(5) . . ? N2 C1 N8 124.6(5) . . ? N1 C1 N8 123.4(5) . . ? N2 C1 Ta1 57.8(3) . . ? N1 C1 Ta1 54.4(3) . . ? N8 C1 Ta1 174.2(4) . . ? N3 C2 N4 113.2(5) . . ? N3 C2 N7 125.3(5) . . ? N4 C2 N7 121.5(5) . . ? N8 C3 H3A 109.5 . . ? N8 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N8 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N8 C4 H4A 109.5 . . ? N8 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N8 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C7 111.4(5) . . ? N2 C5 C6 111.0(5) . . ? C7 C5 C6 108.5(5) . . ? N2 C5 H5 108.6 . . ? C7 C5 H5 108.6 . . ? C6 C5 H5 108.6 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C8 110.4(5) . . ? N3 C9 C10 112.4(5) . . ? C8 C9 C10 108.1(5) . . ? N3 C9 H9 108.6 . . ? C8 C9 H9 108.6 . . ? C10 C9 H9 108.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N7 C11 H11A 109.5 . . ? N7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N7 C12 H12A 109.5 . . ? N7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C13 110.4(5) . . ? N4 C14 C15 111.0(5) . . ? C13 C14 C15 110.6(5) . . ? N4 C14 H14 108.2 . . ? C13 C14 H14 108.2 . . ? C15 C14 H14 108.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N6 C18 C21 109.9(5) . . ? N6 C18 C19 111.4(5) . . ? C21 C18 C19 109.0(5) . . ? N6 C18 C20 108.2(5) . . ? C21 C18 C20 109.3(5) . . ? C19 C18 C20 109.0(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C24 110.9(5) . . ? N1 C22 C23 111.1(5) . . ? C24 C22 C23 109.7(5) . . ? N1 C22 H22 108.3 . . ? C24 C22 H22 108.3 . . ? C23 C22 H22 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 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 N6 Ta1 N1 C1 -83.7(4) . . . . ? N5 Ta1 N1 C1 175.2(3) . . . . ? N4 Ta1 N1 C1 54.1(5) . . . . ? N2 Ta1 N1 C1 3.2(3) . . . . ? N3 Ta1 N1 C1 87.6(3) . . . . ? N6 Ta1 N1 C22 67.4(5) . . . . ? N5 Ta1 N1 C22 -33.7(5) . . . . ? N4 Ta1 N1 C22 -154.8(4) . . . . ? N2 Ta1 N1 C22 154.4(6) . . . . ? N3 Ta1 N1 C22 -121.3(5) . . . . ? C1 Ta1 N1 C22 151.2(7) . . . . ? N6 Ta1 N2 C1 100.8(3) . . . . ? N5 Ta1 N2 C1 -22.9(6) . . . . ? N4 Ta1 N2 C1 -155.4(3) . . . . ? N1 Ta1 N2 C1 -3.3(3) . . . . ? N3 Ta1 N2 C1 -97.0(3) . . . . ? N6 Ta1 N2 C5 -84.1(6) . . . . ? N5 Ta1 N2 C5 152.2(6) . . . . ? N4 Ta1 N2 C5 19.7(6) . . . . ? N1 Ta1 N2 C5 171.7(7) . . . . ? N3 Ta1 N2 C5 78.0(6) . . . . ? C1 Ta1 N2 C5 175.1(8) . . . . ? N6 Ta1 N3 C2 -7.3(8) . . . . ? N5 Ta1 N3 C2 104.3(3) . . . . ? N4 Ta1 N3 C2 -1.6(3) . . . . ? N1 Ta1 N3 C2 -158.7(3) . . . . ? N2 Ta1 N3 C2 -99.4(3) . . . . ? C1 Ta1 N3 C2 -128.5(3) . . . . ? N6 Ta1 N3 C9 144.7(7) . . . . ? N5 Ta1 N3 C9 -103.8(7) . . . . ? N4 Ta1 N3 C9 150.3(7) . . . . ? N1 Ta1 N3 C9 -6.8(7) . . . . ? N2 Ta1 N3 C9 52.5(7) . . . . ? C1 Ta1 N3 C9 23.4(7) . . . . ? N6 Ta1 N4 C2 179.8(3) . . . . ? N5 Ta1 N4 C2 -77.9(3) . . . . ? N1 Ta1 N4 C2 41.7(5) . . . . ? N2 Ta1 N4 C2 83.8(3) . . . . ? N3 Ta1 N4 C2 1.6(3) . . . . ? C1 Ta1 N4 C2 70.0(4) . . . . ? N6 Ta1 N4 C14 -29.2(5) . . . . ? N5 Ta1 N4 C14 73.1(5) . . . . ? N1 Ta1 N4 C14 -167.3(4) . . . . ? N2 Ta1 N4 C14 -125.2(5) . . . . ? N3 Ta1 N4 C14 152.6(6) . . . . ? C1 Ta1 N4 C14 -139.0(5) . . . . ? N6 Ta1 N5 C16 -172.0(5) . . . . ? N4 Ta1 N5 C16 82.1(5) . . . . ? N1 Ta1 N5 C16 -66.0(5) . . . . ? N2 Ta1 N5 C16 -49.1(7) . . . . ? N3 Ta1 N5 C16 24.7(5) . . . . ? C1 Ta1 N5 C16 -62.9(5) . . . . ? N6 Ta1 N5 C17 6.2(5) . . . . ? N4 Ta1 N5 C17 -99.6(5) . . . . ? N1 Ta1 N5 C17 112.3(5) . . . . ? N2 Ta1 N5 C17 129.2(5) . . . . ? N3 Ta1 N5 C17 -157.1(5) . . . . ? C1 Ta1 N5 C17 115.3(5) . . . . ? N5 Ta1 N6 C18 137(3) . . . . ? N4 Ta1 N6 C18 -118(3) . . . . ? N1 Ta1 N6 C18 38(3) . . . . ? N2 Ta1 N6 C18 -22(3) . . . . ? N3 Ta1 N6 C18 -113(2) . . . . ? C1 Ta1 N6 C18 7(3) . . . . ? C5 N2 C1 N1 -171.2(5) . . . . ? Ta1 N2 C1 N1 5.0(5) . . . . ? C5 N2 C1 N8 10.2(9) . . . . ? Ta1 N2 C1 N8 -173.7(5) . . . . ? C5 N2 C1 Ta1 -176.2(6) . . . . ? C22 N1 C1 N2 -161.1(5) . . . . ? Ta1 N1 C1 N2 -5.2(5) . . . . ? C22 N1 C1 N8 17.6(8) . . . . ? Ta1 N1 C1 N8 173.5(5) . . . . ? C22 N1 C1 Ta1 -155.9(6) . . . . ? C3 N8 C1 N2 48.6(9) . . . . ? C4 N8 C1 N2 -135.4(6) . . . . ? C3 N8 C1 N1 -129.9(6) . . . . ? C4 N8 C1 N1 46.1(9) . . . . ? C3 N8 C1 Ta1 -63(4) . . . . ? C4 N8 C1 Ta1 113(4) . . . . ? N6 Ta1 C1 N2 -82.9(3) . . . . ? N5 Ta1 C1 N2 168.3(3) . . . . ? N4 Ta1 C1 N2 28.9(4) . . . . ? N1 Ta1 C1 N2 174.3(5) . . . . ? N3 Ta1 C1 N2 81.7(3) . . . . ? N6 Ta1 C1 N1 102.8(3) . . . . ? N5 Ta1 C1 N1 -6.0(4) . . . . ? N4 Ta1 C1 N1 -145.4(3) . . . . ? N2 Ta1 C1 N1 -174.3(5) . . . . ? N3 Ta1 C1 N1 -92.6(3) . . . . ? N6 Ta1 C1 N8 33(4) . . . . ? N5 Ta1 C1 N8 -76(4) . . . . ? N4 Ta1 C1 N8 144(4) . . . . ? N1 Ta1 C1 N8 -70(4) . . . . ? N2 Ta1 C1 N8 116(4) . . . . ? N3 Ta1 C1 N8 -163(4) . . . . ? C9 N3 C2 N4 -159.9(5) . . . . ? Ta1 N3 C2 N4 2.3(5) . . . . ? C9 N3 C2 N7 19.4(9) . . . . ? Ta1 N3 C2 N7 -178.4(5) . . . . ? C14 N4 C2 N3 -157.9(5) . . . . ? Ta1 N4 C2 N3 -2.7(5) . . . . ? C14 N4 C2 N7 22.8(8) . . . . ? Ta1 N4 C2 N7 178.1(5) . . . . ? C12 N7 C2 N3 -133.4(7) . . . . ? C11 N7 C2 N3 46.8(9) . . . . ? C12 N7 C2 N4 45.8(9) . . . . ? C11 N7 C2 N4 -134.0(6) . . . . ? C1 N2 C5 C7 127.8(6) . . . . ? Ta1 N2 C5 C7 -46.1(8) . . . . ? C1 N2 C5 C6 -111.3(6) . . . . ? Ta1 N2 C5 C6 74.9(7) . . . . ? C2 N3 C9 C8 123.9(6) . . . . ? Ta1 N3 C9 C8 -22.8(9) . . . . ? C2 N3 C9 C10 -115.3(6) . . . . ? Ta1 N3 C9 C10 98.0(7) . . . . ? C2 N4 C14 C13 -123.8(6) . . . . ? Ta1 N4 C14 C13 90.4(6) . . . . ? C2 N4 C14 C15 113.1(6) . . . . ? Ta1 N4 C14 C15 -32.7(7) . . . . ? Ta1 N6 C18 C21 -133(2) . . . . ? Ta1 N6 C18 C19 106(3) . . . . ? Ta1 N6 C18 C20 -13(3) . . . . ? C1 N1 C22 C24 -124.2(6) . . . . ? Ta1 N1 C22 C24 90.9(6) . . . . ? C1 N1 C22 C23 113.4(6) . . . . ? Ta1 N1 C22 C23 -31.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.142 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.119