Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.Arnold ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; R.G.Bergman ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; N.C.Tomson ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; _publ_contact_author_address ;Department of Chemistry University of California at Berkeley Berkeley, CA 94720-1460 (USA) ; _publ_contact_author_email arnold@berkeley.edu _publ_contact_author_fax (+1)510-666-2504 _publ_contact_author_phone (+1)510-643-5181 _publ_contact_author_name 'Prof. John Arnold' data_n5c69txs _database_code_depnum_ccdc_archive 'CCDC 675085' #TrackingRef '- 2a.cif' _ccdc_journal_manuscript_code 'Dalton Trans.' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H73 B F20 N3 Nb O2' _chemical_formula_sum 'C66 H73 B F20 N3 Nb O2' _chemical_formula_weight 1423.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 '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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.616(3) _cell_length_b 16.444(3) _cell_length_c 17.040(3) _cell_angle_alpha 114.348(2) _cell_angle_beta 102.282(3) _cell_angle_gamma 91.108(3) _cell_volume 3371.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2444 _cell_measurement_theta_min 6.860 _cell_measurement_theta_max 42.695 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.815713 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12998 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 21.72 _reflns_number_total 7758 _reflns_number_gt 5193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _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^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7758 _refine_ls_number_parameters 838 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.005 _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 Nb1 Nb 0.33688(4) 0.61312(3) 0.75609(3) 0.03220(19) Uani 1 1 d . . . C1 C 0.4324(4) 0.5133(4) 0.7684(4) 0.0468(16) Uani 1 1 d . . . H1A H 0.4788 0.5041 0.7311 0.070 Uiso 1 1 calc R . . H1B H 0.3912 0.4578 0.7506 0.070 Uiso 1 1 calc R . . H1C H 0.4697 0.5339 0.8290 0.070 Uiso 1 1 calc R . . C2 C 0.2262(5) 0.5521(4) 0.5512(4) 0.0496(17) Uani 1 1 d . . . C3 C 0.1904(7) 0.4545(5) 0.5067(4) 0.097(3) Uani 1 1 d . . . H3A H 0.1413 0.4416 0.5342 0.146 Uiso 1 1 calc R . . H3B H 0.2467 0.4213 0.5121 0.146 Uiso 1 1 calc R . . H3C H 0.1600 0.4375 0.4451 0.146 Uiso 1 1 calc R . . C4 C 0.1400(6) 0.6092(5) 0.5490(5) 0.081(2) Uani 1 1 d . . . H4A H 0.0904 0.5946 0.5752 0.121 Uiso 1 1 calc R . . H4B H 0.1091 0.5974 0.4886 0.121 Uiso 1 1 calc R . . H4C H 0.1660 0.6717 0.5819 0.121 Uiso 1 1 calc R . . C5 C 0.3036(6) 0.5761(5) 0.5088(4) 0.074(2) Uani 1 1 d . . . H5A H 0.3582 0.5401 0.5090 0.111 Uiso 1 1 calc R . . H5B H 0.3295 0.6386 0.5419 0.111 Uiso 1 1 calc R . . H5C H 0.2716 0.5648 0.4487 0.111 Uiso 1 1 calc R . . C6 C 0.1243(4) 0.6135(4) 0.8045(3) 0.0337(14) Uani 1 1 d . . . C7 C 0.0507(4) 0.6725(4) 0.8057(4) 0.0448(16) Uani 1 1 d . . . C8 C -0.0502(5) 0.6363(5) 0.7787(5) 0.066(2) Uani 1 1 d . . . H8A H -0.1002 0.6738 0.7776 0.079 Uiso 1 1 calc R . . C9 C -0.0780(5) 0.5478(5) 0.7540(5) 0.064(2) Uani 1 1 d . . . H9A H -0.1462 0.5260 0.7377 0.076 Uiso 1 1 calc R . . C10 C -0.0052(5) 0.4901(4) 0.7530(4) 0.0534(18) Uani 1 1 d . . . H10A H -0.0247 0.4294 0.7352 0.064 Uiso 1 1 calc R . . C11 C 0.0972(4) 0.5225(4) 0.7786(4) 0.0419(15) Uani 1 1 d . . . C12 C 0.0772(5) 0.7736(4) 0.8359(5) 0.0552(19) Uani 1 1 d . . . H12A H 0.1511 0.7868 0.8502 0.066 Uiso 1 1 calc R . . C13 C 0.0321(5) 0.8001(4) 0.7615(5) 0.067(2) Uani 1 1 d . . . H13A H 0.0565 0.7657 0.7101 0.100 Uiso 1 1 calc R . . H13B H 0.0515 0.8630 0.7804 0.100 Uiso 1 1 calc R . . H13C H -0.0404 0.7884 0.7471 0.100 Uiso 1 1 calc R . . C14 C 0.0402(6) 0.8301(5) 0.9187(5) 0.081(2) Uani 1 1 d . . . H14A H 0.0699 0.8141 0.9661 0.121 Uiso 1 1 calc R . . H14B H -0.0322 0.8187 0.9056 0.121 Uiso 1 1 calc R . . H14C H 0.0597 0.8927 0.9364 0.121 Uiso 1 1 calc R . . C15 C 0.1756(5) 0.4581(4) 0.7821(6) 0.076(2) Uani 1 1 d . . . H15A H 0.2426 0.4905 0.7954 0.091 Uiso 1 1 calc R . . C16 C 0.1613(6) 0.3765(5) 0.6942(5) 0.086(3) Uani 1 1 d . . . H16A H 0.1650 0.3955 0.6486 0.129 Uiso 1 1 calc R . . H16B H 0.0964 0.3431 0.6798 0.129 Uiso 1 1 calc R . . H16C H 0.2136 0.3391 0.6985 0.129 Uiso 1 1 calc R . . C17 C 0.1752(10) 0.4277(7) 0.8534(6) 0.174(6) Uani 1 1 d . . . H17A H 0.1864 0.4791 0.9097 0.260 Uiso 1 1 calc R . . H17B H 0.2280 0.3901 0.8552 0.260 Uiso 1 1 calc R . . H17C H 0.1109 0.3942 0.8412 0.260 Uiso 1 1 calc R . . C18 C 0.2401(4) 0.6898(4) 0.9876(4) 0.0469(16) Uani 1 1 d . . . H18A H 0.1733 0.6574 0.9641 0.070 Uiso 1 1 calc R . . H18B H 0.2371 0.7505 1.0281 0.070 Uiso 1 1 calc R . . H18C H 0.2833 0.6613 1.0183 0.070 Uiso 1 1 calc R . . C19 C 0.2821(4) 0.6900(3) 0.9125(4) 0.0311(14) Uani 1 1 d . . . C20 C 0.3805(4) 0.7363(3) 0.9360(3) 0.0306(14) Uani 1 1 d . . . H20A H 0.4164 0.7476 0.9931 0.037 Uiso 1 1 calc R . . C21 C 0.4352(4) 0.7688(4) 0.8916(4) 0.0306(14) Uani 1 1 d . . . C22 C 0.5273(4) 0.8352(4) 0.9468(4) 0.0429(16) Uani 1 1 d . . . H22A H 0.5291 0.8824 0.9276 0.064 Uiso 1 1 calc R . . H22B H 0.5870 0.8054 0.9400 0.064 Uiso 1 1 calc R . . H22C H 0.5249 0.8604 1.0080 0.064 Uiso 1 1 calc R . . C23 C 0.4551(4) 0.7864(3) 0.7603(3) 0.0281(13) Uani 1 1 d . . . C24 C 0.4053(4) 0.8517(4) 0.7421(3) 0.0336(14) Uani 1 1 d . . . C25 C 0.4518(5) 0.8958(4) 0.7030(3) 0.0410(15) Uani 1 1 d . . . H25A H 0.4209 0.9407 0.6910 0.049 Uiso 1 1 calc R . . C26 C 0.5435(5) 0.8740(4) 0.6817(4) 0.0473(17) Uani 1 1 d . . . H26A H 0.5744 0.9050 0.6568 0.057 Uiso 1 1 calc R . . C27 C 0.5883(5) 0.8069(4) 0.6974(4) 0.0474(17) Uani 1 1 d . . . H27A H 0.6486 0.7912 0.6810 0.057 Uiso 1 1 calc R . . C28 C 0.5458(4) 0.7617(4) 0.7373(4) 0.0397(15) Uani 1 1 d . . . C29 C 0.3035(4) 0.8763(4) 0.7630(4) 0.0402(15) Uani 1 1 d . . . H29A H 0.2722 0.8265 0.7704 0.048 Uiso 1 1 calc R . . C30 C 0.2310(4) 0.8896(4) 0.6893(4) 0.0504(17) Uani 1 1 d . . . H30A H 0.2213 0.8362 0.6349 0.076 Uiso 1 1 calc R . . H30B H 0.2588 0.9395 0.6821 0.076 Uiso 1 1 calc R . . H30C H 0.1671 0.9016 0.7045 0.076 Uiso 1 1 calc R . . C31 C 0.3186(5) 0.9607(5) 0.8510(4) 0.086(3) Uani 1 1 d . . . H31A H 0.3641 0.9515 0.8972 0.129 Uiso 1 1 calc R . . H31B H 0.2546 0.9723 0.8658 0.129 Uiso 1 1 calc R . . H31C H 0.3467 1.0112 0.8449 0.129 Uiso 1 1 calc R . . C32 C 0.5998(5) 0.6877(5) 0.7525(5) 0.0590(19) Uani 1 1 d . . . H32A H 0.5653 0.6690 0.7884 0.071 Uiso 1 1 calc R . . C33 C 0.7114(5) 0.7213(6) 0.8049(6) 0.101(3) Uani 1 1 d . . . H33A H 0.7138 0.7722 0.8601 0.152 Uiso 1 1 calc R . . H33B H 0.7476 0.7387 0.7706 0.152 Uiso 1 1 calc R . . H33C H 0.7419 0.6741 0.8166 0.152 Uiso 1 1 calc R . . C34 C 0.5915(7) 0.6062(5) 0.6646(6) 0.103(3) Uani 1 1 d . . . H34A H 0.5214 0.5863 0.6345 0.154 Uiso 1 1 calc R . . H34B H 0.6221 0.5586 0.6755 0.154 Uiso 1 1 calc R . . H34C H 0.6256 0.6223 0.6282 0.154 Uiso 1 1 calc R . . C35 C 0.7951(4) 1.0664(3) 0.7922(3) 0.0330(14) Uani 1 1 d . . . C36 C 0.8247(5) 1.0191(4) 0.8423(4) 0.0407(16) Uani 1 1 d . . . C37 C 0.7688(5) 1.0007(4) 0.8935(4) 0.0459(16) Uani 1 1 d . . . C38 C 0.6758(5) 1.0318(4) 0.8945(4) 0.0433(16) Uani 1 1 d . . . C39 C 0.6419(4) 1.0783(4) 0.8484(4) 0.0391(15) Uani 1 1 d . . . C40 C 0.7012(4) 1.0964(4) 0.7991(4) 0.0344(14) Uani 1 1 d . . . C41 C 0.8163(4) 1.1301(3) 0.6697(3) 0.0282(13) Uani 1 1 d . . . C42 C 0.7281(4) 1.0828(4) 0.6051(4) 0.0304(14) Uani 1 1 d . . . C43 C 0.6736(4) 1.1112(4) 0.5458(4) 0.0348(14) Uani 1 1 d . . . C44 C 0.7077(4) 1.1910(4) 0.5474(4) 0.0362(15) Uani 1 1 d . . . C45 C 0.7952(4) 1.2394(4) 0.6068(4) 0.0299(13) Uani 1 1 d . . . C46 C 0.8475(4) 1.2079(4) 0.6646(3) 0.0305(14) Uani 1 1 d . . . C47 C 0.9131(4) 0.9972(4) 0.6703(3) 0.0298(13) Uani 1 1 d . . . C48 C 0.8747(4) 0.9092(4) 0.6402(4) 0.0368(15) Uani 1 1 d . . . C49 C 0.9083(4) 0.8374(4) 0.5777(4) 0.0386(15) Uani 1 1 d . . . C50 C 0.9836(5) 0.8522(4) 0.5426(4) 0.0393(15) Uani 1 1 d . . . C51 C 1.0243(4) 0.9390(4) 0.5692(4) 0.0354(14) Uani 1 1 d . . . C52 C 0.9886(4) 1.0070(4) 0.6301(3) 0.0311(14) Uani 1 1 d . . . C53 C 0.9651(4) 1.1586(4) 0.8208(3) 0.0279(13) Uani 1 1 d . . . C54 C 0.9461(4) 1.2436(4) 0.8743(4) 0.0339(14) Uani 1 1 d . . . C55 C 1.0142(5) 1.3064(4) 0.9453(4) 0.0407(15) Uani 1 1 d . . . C56 C 1.1104(5) 1.2858(4) 0.9692(4) 0.0492(17) Uani 1 1 d . . . C57 C 1.1325(5) 1.2014(5) 0.9200(4) 0.0495(17) Uani 1 1 d . . . C58 C 1.0616(4) 1.1406(4) 0.8494(4) 0.0382(15) Uani 1 1 d . . . C59 C 0.2782(7) 0.5592(6) 1.1599(8) 0.138(4) Uani 1 1 d . . . H59A H 0.2460 0.5767 1.2084 0.207 Uiso 1 1 calc R . . H59B H 0.3023 0.5020 1.1492 0.207 Uiso 1 1 calc R . . H59C H 0.2303 0.5546 1.1076 0.207 Uiso 1 1 calc R . . C60 C 0.3656(7) 0.6283(6) 1.1825(7) 0.110(3) Uani 1 1 d . . . H60A H 0.4147 0.6330 1.2351 0.131 Uiso 1 1 calc R . . H60B H 0.3420 0.6866 1.1947 0.131 Uiso 1 1 calc R . . C61 C 0.5063(8) 0.6594(6) 1.1231(7) 0.115(4) Uani 1 1 d . . . H61A H 0.4889 0.7192 1.1326 0.138 Uiso 1 1 calc R . . H61B H 0.5525 0.6641 1.1770 0.138 Uiso 1 1 calc R . . C62 C 0.5565(7) 0.6266(6) 1.0510(6) 0.115(3) Uani 1 1 d . . . H62A H 0.6158 0.6674 1.0652 0.173 Uiso 1 1 calc R . . H62B H 0.5113 0.6225 0.9976 0.173 Uiso 1 1 calc R . . H62C H 0.5758 0.5683 1.0425 0.173 Uiso 1 1 calc R . . C63 C 0.7155(9) 0.8352(8) 1.2727(9) 0.151(5) Uani 1 1 d . . . H63A H 0.7468 0.8871 1.2712 0.226 Uiso 1 1 calc R . . H63B H 0.6539 0.8121 1.2269 0.226 Uiso 1 1 calc R . . H63C H 0.7608 0.7899 1.2633 0.226 Uiso 1 1 calc R . . C64 C 0.6937(12) 0.8591(7) 1.3554(11) 0.190(7) Uani 1 1 d . . . H64A H 0.6488 0.9055 1.3652 0.228 Uiso 1 1 calc R . . H64B H 0.7559 0.8835 1.4017 0.228 Uiso 1 1 calc R . . C65 C 0.6030(13) 0.7851(14) 1.4345(9) 0.243(12) Uani 1 1 d . . . H65A H 0.6558 0.8139 1.4890 0.292 Uiso 1 1 calc R . . H65B H 0.5502 0.8244 1.4393 0.292 Uiso 1 1 calc R . . C66 C 0.5617(14) 0.7052(9) 1.4332(12) 0.216(9) Uani 1 1 d . . . H66A H 0.5363 0.7193 1.4852 0.324 Uiso 1 1 calc R . . H66B H 0.6133 0.6661 1.4325 0.324 Uiso 1 1 calc R . . H66C H 0.5074 0.6758 1.3811 0.324 Uiso 1 1 calc R . . B1 B 0.8730(5) 1.0885(4) 0.7386(4) 0.0318(16) Uani 1 1 d . . . F1 F 0.9172(3) 0.9888(2) 0.8442(2) 0.0504(9) Uani 1 1 d . . . F2 F 0.8044(3) 0.9541(2) 0.9401(2) 0.0666(11) Uani 1 1 d . . . F3 F 0.6181(3) 1.0127(2) 0.9423(2) 0.0681(11) Uani 1 1 d . . . F4 F 0.5499(2) 1.1084(2) 0.8497(2) 0.0537(9) Uani 1 1 d . . . F5 F 0.6598(2) 1.1457(2) 0.7565(2) 0.0430(8) Uani 1 1 d . . . F6 F 0.6900(2) 1.00438(19) 0.60201(19) 0.0404(8) Uani 1 1 d . . . F7 F 0.5877(2) 1.0619(2) 0.4869(2) 0.0500(9) Uani 1 1 d . . . F8 F 0.6549(3) 1.2214(2) 0.4908(2) 0.0545(9) Uani 1 1 d . . . F9 F 0.8292(2) 1.3174(2) 0.6081(2) 0.0461(9) Uani 1 1 d . . . F10 F 0.9357(2) 1.25993(19) 0.71922(19) 0.0375(8) Uani 1 1 d . . . F11 F 0.7978(2) 0.88511(19) 0.6696(2) 0.0456(8) Uani 1 1 d . . . F12 F 0.8664(3) 0.7523(2) 0.5526(2) 0.0595(10) Uani 1 1 d . . . F13 F 1.0194(3) 0.7827(2) 0.4835(2) 0.0579(10) Uani 1 1 d . . . F14 F 1.1000(2) 0.9547(2) 0.5352(2) 0.0483(9) Uani 1 1 d . . . F15 F 1.0308(2) 1.0918(2) 0.65185(19) 0.0400(8) Uani 1 1 d . . . F16 F 0.8522(2) 1.26839(19) 0.85513(18) 0.0375(8) Uani 1 1 d . . . F17 F 0.9904(3) 1.3896(2) 0.9925(2) 0.0559(9) Uani 1 1 d . . . F18 F 1.1803(3) 1.3470(2) 1.0380(2) 0.0733(11) Uani 1 1 d . . . F19 F 1.2269(3) 1.1797(3) 0.9438(2) 0.0738(12) Uani 1 1 d . . . F20 F 1.0925(2) 1.0590(2) 0.8074(2) 0.0511(9) Uani 1 1 d . . . N1 N 0.2780(3) 0.5773(3) 0.6445(3) 0.0370(12) Uani 1 1 d . . . N2 N 0.2297(3) 0.6481(3) 0.8276(3) 0.0276(11) Uani 1 1 d . . . N3 N 0.4078(3) 0.7399(3) 0.8023(3) 0.0287(11) Uani 1 1 d . . . O1 O 0.4139(5) 0.6004(4) 1.1053(4) 0.112(2) Uani 1 1 d . . . O2 O 0.6469(5) 0.7833(5) 1.3608(5) 0.130(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0320(3) 0.0307(3) 0.0337(3) 0.0121(3) 0.0106(2) 0.0048(2) C1 0.053(4) 0.044(4) 0.051(4) 0.024(3) 0.022(3) 0.013(3) C2 0.069(5) 0.051(4) 0.028(4) 0.019(3) 0.007(3) 0.009(4) C3 0.165(9) 0.055(5) 0.043(5) 0.015(4) -0.015(5) -0.031(5) C4 0.079(6) 0.100(6) 0.067(5) 0.040(5) 0.014(4) 0.029(5) C5 0.104(6) 0.081(6) 0.053(5) 0.035(4) 0.036(4) 0.026(5) C6 0.030(4) 0.041(4) 0.025(3) 0.011(3) 0.005(3) 0.003(3) C7 0.033(4) 0.048(4) 0.062(4) 0.031(3) 0.012(3) 0.003(3) C8 0.029(4) 0.057(5) 0.117(6) 0.045(5) 0.008(4) 0.003(4) C9 0.029(4) 0.067(5) 0.088(6) 0.035(4) -0.002(4) -0.008(4) C10 0.052(5) 0.036(4) 0.067(5) 0.018(4) 0.012(4) -0.011(4) C11 0.035(4) 0.035(4) 0.045(4) 0.009(3) 0.006(3) -0.008(3) C12 0.030(4) 0.056(5) 0.101(6) 0.053(4) 0.018(4) 0.013(3) C13 0.084(5) 0.057(5) 0.086(5) 0.043(4) 0.047(5) 0.027(4) C14 0.101(6) 0.061(5) 0.071(5) 0.027(4) 0.006(5) 0.009(5) C15 0.044(5) 0.028(4) 0.143(8) 0.028(5) 0.018(5) 0.000(3) C16 0.116(7) 0.075(6) 0.101(7) 0.051(5) 0.062(6) 0.043(5) C17 0.263(15) 0.107(9) 0.082(7) 0.011(6) -0.042(8) 0.102(9) C18 0.044(4) 0.056(4) 0.037(4) 0.015(3) 0.014(3) -0.009(3) C19 0.032(4) 0.033(3) 0.033(4) 0.016(3) 0.012(3) 0.003(3) C20 0.033(4) 0.034(3) 0.025(3) 0.014(3) 0.005(3) 0.003(3) C21 0.021(3) 0.037(4) 0.030(4) 0.011(3) 0.005(3) 0.003(3) C22 0.030(4) 0.053(4) 0.037(4) 0.016(3) -0.002(3) -0.010(3) C23 0.029(3) 0.030(3) 0.023(3) 0.010(3) 0.005(3) -0.003(3) C24 0.032(4) 0.040(4) 0.024(3) 0.011(3) 0.004(3) -0.002(3) C25 0.045(4) 0.047(4) 0.029(3) 0.018(3) 0.002(3) -0.011(3) C26 0.048(4) 0.059(5) 0.033(4) 0.019(3) 0.008(3) -0.019(4) C27 0.035(4) 0.063(5) 0.037(4) 0.015(4) 0.008(3) -0.003(3) C28 0.028(4) 0.052(4) 0.045(4) 0.023(3) 0.015(3) 0.001(3) C29 0.038(4) 0.047(4) 0.047(4) 0.030(3) 0.013(3) 0.016(3) C30 0.041(4) 0.054(4) 0.057(4) 0.027(4) 0.008(3) 0.005(3) C31 0.072(5) 0.117(7) 0.046(5) 0.013(5) 0.011(4) 0.045(5) C32 0.047(5) 0.072(5) 0.080(5) 0.042(4) 0.041(4) 0.023(4) C33 0.048(5) 0.153(9) 0.141(8) 0.094(7) 0.033(5) 0.038(5) C34 0.153(9) 0.079(6) 0.109(7) 0.047(6) 0.082(7) 0.059(6) C35 0.038(4) 0.029(3) 0.030(3) 0.010(3) 0.009(3) 0.002(3) C36 0.056(4) 0.028(4) 0.035(4) 0.010(3) 0.010(3) 0.011(3) C37 0.073(5) 0.037(4) 0.036(4) 0.021(3) 0.019(4) 0.005(4) C38 0.064(5) 0.033(4) 0.035(4) 0.010(3) 0.027(4) -0.007(3) C39 0.037(4) 0.035(4) 0.038(4) 0.007(3) 0.012(3) -0.008(3) C40 0.040(4) 0.026(3) 0.038(4) 0.014(3) 0.013(3) 0.000(3) C41 0.027(3) 0.025(3) 0.030(3) 0.006(3) 0.015(3) 0.002(3) C42 0.032(4) 0.026(3) 0.034(3) 0.010(3) 0.015(3) -0.001(3) C43 0.029(4) 0.042(4) 0.027(3) 0.014(3) -0.001(3) 0.001(3) C44 0.039(4) 0.044(4) 0.033(4) 0.025(3) 0.006(3) 0.010(3) C45 0.032(4) 0.028(4) 0.034(3) 0.017(3) 0.008(3) -0.001(3) C46 0.021(3) 0.031(4) 0.030(3) 0.006(3) 0.003(3) -0.005(3) C47 0.027(3) 0.034(4) 0.027(3) 0.013(3) 0.004(3) 0.000(3) C48 0.034(4) 0.039(4) 0.040(4) 0.018(3) 0.012(3) 0.002(3) C49 0.046(4) 0.025(4) 0.037(4) 0.006(3) 0.011(3) -0.002(3) C50 0.050(4) 0.031(4) 0.032(4) 0.007(3) 0.011(3) 0.010(3) C51 0.024(3) 0.051(5) 0.036(4) 0.021(3) 0.008(3) 0.010(3) C52 0.035(4) 0.026(4) 0.030(3) 0.012(3) 0.005(3) 0.003(3) C53 0.029(4) 0.034(4) 0.025(3) 0.016(3) 0.008(3) 0.003(3) C54 0.032(4) 0.039(4) 0.029(3) 0.014(3) 0.006(3) 0.003(3) C55 0.054(5) 0.029(4) 0.034(4) 0.006(3) 0.014(3) 0.004(3) C56 0.042(4) 0.050(5) 0.041(4) 0.014(4) -0.005(3) -0.014(4) C57 0.036(4) 0.052(5) 0.052(4) 0.018(4) 0.001(4) 0.004(4) C58 0.038(4) 0.034(4) 0.033(4) 0.008(3) 0.002(3) 0.001(3) C59 0.105(8) 0.079(7) 0.222(12) 0.081(8) -0.010(8) -0.016(6) C60 0.105(8) 0.070(7) 0.142(9) 0.042(6) 0.010(7) 0.029(6) C61 0.104(8) 0.086(7) 0.122(9) 0.041(7) -0.033(7) -0.008(7) C62 0.120(8) 0.123(9) 0.111(8) 0.056(7) 0.030(7) 0.058(7) C63 0.128(10) 0.130(11) 0.203(14) 0.085(11) 0.028(10) 0.028(8) C64 0.227(16) 0.043(7) 0.267(19) 0.008(9) 0.119(14) -0.015(8) C65 0.151(14) 0.34(3) 0.091(10) -0.059(14) 0.033(9) 0.083(17) C66 0.210(18) 0.139(13) 0.240(19) -0.015(13) 0.139(15) 0.001(12) B1 0.035(4) 0.033(4) 0.032(4) 0.015(3) 0.013(3) 0.007(3) F1 0.055(2) 0.057(2) 0.052(2) 0.0335(19) 0.0141(18) 0.0165(19) F2 0.100(3) 0.060(2) 0.061(2) 0.042(2) 0.027(2) 0.010(2) F3 0.089(3) 0.064(3) 0.062(2) 0.027(2) 0.042(2) -0.010(2) F4 0.044(2) 0.057(2) 0.058(2) 0.0152(19) 0.0273(18) -0.0001(18) F5 0.041(2) 0.047(2) 0.048(2) 0.0238(18) 0.0180(16) 0.0111(16) F6 0.0383(19) 0.034(2) 0.044(2) 0.0150(16) 0.0061(15) -0.0075(15) F7 0.040(2) 0.050(2) 0.049(2) 0.0192(18) -0.0080(18) -0.0077(17) F8 0.060(2) 0.054(2) 0.050(2) 0.0298(19) -0.0012(18) 0.0061(18) F9 0.052(2) 0.041(2) 0.048(2) 0.0272(17) 0.0031(17) -0.0066(17) F10 0.035(2) 0.0382(19) 0.0398(19) 0.0199(16) 0.0047(16) -0.0067(16) F11 0.050(2) 0.036(2) 0.052(2) 0.0151(17) 0.0238(18) 0.0003(16) F12 0.069(3) 0.032(2) 0.068(2) 0.0073(18) 0.025(2) 0.0018(18) F13 0.066(2) 0.042(2) 0.057(2) 0.0046(19) 0.030(2) 0.0161(18) F14 0.046(2) 0.059(2) 0.044(2) 0.0206(18) 0.0210(17) 0.0129(17) F15 0.0372(19) 0.040(2) 0.046(2) 0.0181(16) 0.0173(16) 0.0038(16) F16 0.037(2) 0.0357(19) 0.0364(18) 0.0114(15) 0.0110(15) 0.0036(15) F17 0.065(2) 0.039(2) 0.048(2) 0.0036(18) 0.0131(19) -0.0011(18) F18 0.059(3) 0.066(3) 0.058(2) 0.005(2) -0.012(2) -0.011(2) F19 0.040(2) 0.082(3) 0.071(3) 0.018(2) -0.013(2) 0.010(2) F20 0.045(2) 0.047(2) 0.048(2) 0.0125(18) -0.0004(17) 0.0139(18) N1 0.051(3) 0.027(3) 0.034(3) 0.011(2) 0.016(2) -0.001(2) N2 0.021(3) 0.031(3) 0.029(3) 0.014(2) 0.000(2) 0.001(2) N3 0.025(3) 0.036(3) 0.025(3) 0.013(2) 0.005(2) 0.008(2) O1 0.106(5) 0.082(5) 0.104(5) 0.015(4) -0.013(4) 0.017(4) O2 0.091(5) 0.099(5) 0.140(6) 0.003(5) 0.008(5) 0.012(4) _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 Nb1 N1 1.737(4) . ? Nb1 N3 2.036(4) . ? Nb1 N2 2.038(4) . ? Nb1 C1 2.163(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.471(7) . ? C2 C3 1.482(9) . ? C2 C4 1.522(9) . ? C2 C5 1.527(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C11 1.390(7) . ? C6 C7 1.405(7) . ? C6 N2 1.443(7) . ? C7 C8 1.388(8) . ? C7 C12 1.534(8) . ? C8 C9 1.358(8) . ? C8 H8A 0.9300 . ? C9 C10 1.384(8) . ? C9 H9A 0.9300 . ? C10 C11 1.393(8) . ? C10 H10A 0.9300 . ? C11 C15 1.527(8) . ? C12 C13 1.519(8) . ? C12 C14 1.533(9) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C17 1.494(12) . ? C15 C16 1.514(10) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.509(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N2 1.341(6) . ? C19 C20 1.419(7) . ? C20 C21 1.405(7) . ? C20 H20A 0.9300 . ? C21 N3 1.354(6) . ? C21 C22 1.500(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.386(7) . ? C23 C28 1.393(7) . ? C23 N3 1.462(6) . ? C24 C25 1.388(7) . ? C24 C29 1.525(7) . ? C25 C26 1.387(8) . ? C25 H25A 0.9300 . ? C26 C27 1.364(8) . ? C26 H26A 0.9300 . ? C27 C28 1.384(8) . ? C27 H27A 0.9300 . ? C28 C32 1.517(8) . ? C29 C30 1.519(7) . ? C29 C31 1.536(8) . ? C29 H29A 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C34 1.523(10) . ? C32 C33 1.547(10) . ? C32 H32A 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.382(7) . ? C35 C40 1.390(7) . ? C35 B1 1.662(8) . ? C36 F1 1.362(6) . ? C36 C37 1.387(8) . ? C37 F2 1.344(6) . ? C37 C38 1.375(8) . ? C38 C39 1.330(8) . ? C38 F3 1.362(6) . ? C39 F4 1.356(6) . ? C39 C40 1.390(8) . ? C40 F5 1.353(6) . ? C41 C46 1.383(7) . ? C41 C42 1.398(7) . ? C41 B1 1.655(8) . ? C42 F6 1.356(6) . ? C42 C43 1.370(7) . ? C43 F7 1.351(6) . ? C43 C44 1.370(7) . ? C44 F8 1.347(6) . ? C44 C45 1.365(7) . ? C45 F9 1.345(6) . ? C45 C46 1.371(7) . ? C46 F10 1.367(6) . ? C47 C48 1.369(7) . ? C47 C52 1.392(7) . ? C47 B1 1.664(8) . ? C48 F11 1.370(6) . ? C48 C49 1.388(7) . ? C49 C50 1.356(8) . ? C49 F12 1.356(6) . ? C50 F13 1.356(6) . ? C50 C51 1.371(7) . ? C51 F14 1.353(6) . ? C51 C52 1.357(7) . ? C52 F15 1.365(6) . ? C53 C54 1.383(7) . ? C53 C58 1.384(7) . ? C53 B1 1.652(8) . ? C54 C55 1.358(8) . ? C54 F16 1.364(6) . ? C55 F17 1.358(6) . ? C55 C56 1.378(8) . ? C56 F18 1.344(7) . ? C56 C57 1.372(8) . ? C57 C58 1.362(8) . ? C57 F19 1.364(7) . ? C58 F20 1.359(6) . ? C59 C60 1.500(11) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 O1 1.503(11) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.446(12) . ? C61 O1 1.471(11) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.397(15) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 O2 1.434(13) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.41(2) . ? C65 O2 1.491(18) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? 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 N1 Nb1 N3 108.22(18) . . ? N1 Nb1 N2 108.59(19) . . ? N3 Nb1 N2 96.13(16) . . ? N1 Nb1 C1 108.0(2) . . ? N3 Nb1 C1 116.0(2) . . ? N2 Nb1 C1 119.13(19) . . ? Nb1 C1 H1A 109.5 . . ? Nb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Nb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.5(5) . . ? N1 C2 C4 108.4(5) . . ? C3 C2 C4 112.4(7) . . ? N1 C2 C5 106.6(5) . . ? C3 C2 C5 111.4(6) . . ? C4 C2 C5 108.4(5) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.3(5) . . ? C11 C6 N2 119.8(5) . . ? C7 C6 N2 118.8(5) . . ? C8 C7 C6 117.5(6) . . ? C8 C7 C12 119.4(5) . . ? C6 C7 C12 123.1(5) . . ? C9 C8 C7 121.9(6) . . ? C9 C8 H8A 119.0 . . ? C7 C8 H8A 119.0 . . ? C8 C9 C10 120.3(6) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C10 C11 120.3(6) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C6 C11 C10 118.7(5) . . ? C6 C11 C15 122.4(5) . . ? C10 C11 C15 118.9(5) . . ? C13 C12 C14 109.6(5) . . ? C13 C12 C7 110.3(6) . . ? C14 C12 C7 111.9(5) . . ? C13 C12 H12A 108.3 . . ? C14 C12 H12A 108.3 . . ? C7 C12 H12A 108.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 109.0(6) . . ? C17 C15 C11 112.6(7) . . ? C16 C15 C11 112.1(7) . . ? C17 C15 H15A 107.6 . . ? C16 C15 H15A 107.6 . . ? C11 C15 H15A 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C20 121.4(5) . . ? N2 C19 C18 121.9(5) . . ? C20 C19 C18 116.8(5) . . ? C21 C20 C19 133.7(5) . . ? C21 C20 H20A 113.1 . . ? C19 C20 H20A 113.1 . . ? N3 C21 C20 121.7(5) . . ? N3 C21 C22 121.1(5) . . ? C20 C21 C22 117.2(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 122.5(5) . . ? C24 C23 N3 118.2(4) . . ? C28 C23 N3 119.3(5) . . ? C23 C24 C25 117.4(5) . . ? C23 C24 C29 123.0(5) . . ? C25 C24 C29 119.6(5) . . ? C26 C25 C24 121.1(6) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C27 C26 C25 119.9(6) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 121.3(6) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C27 C28 C23 117.8(5) . . ? C27 C28 C32 118.4(5) . . ? C23 C28 C32 123.8(5) . . ? C30 C29 C24 113.0(4) . . ? C30 C29 C31 110.1(5) . . ? C24 C29 C31 110.5(5) . . ? C30 C29 H29A 107.7 . . ? C24 C29 H29A 107.7 . . ? C31 C29 H29A 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 C34 110.5(6) . . ? C28 C32 C33 111.7(6) . . ? C34 C32 C33 111.7(6) . . ? C28 C32 H32A 107.6 . . ? C34 C32 H32A 107.6 . . ? C33 C32 H32A 107.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 112.6(5) . . ? C36 C35 B1 120.2(5) . . ? C40 C35 B1 127.0(5) . . ? F1 C36 C35 118.6(5) . . ? F1 C36 C37 115.9(5) . . ? C35 C36 C37 125.5(6) . . ? F2 C37 C38 121.5(6) . . ? F2 C37 C36 121.0(6) . . ? C38 C37 C36 117.5(6) . . ? C39 C38 F3 120.4(6) . . ? C39 C38 C37 120.8(6) . . ? F3 C38 C37 118.8(6) . . ? C38 C39 F4 120.2(5) . . ? C38 C39 C40 119.8(6) . . ? F4 C39 C40 120.0(5) . . ? F5 C40 C35 121.7(5) . . ? F5 C40 C39 114.5(5) . . ? C35 C40 C39 123.9(5) . . ? C46 C41 C42 112.7(5) . . ? C46 C41 B1 127.7(5) . . ? C42 C41 B1 119.6(5) . . ? F6 C42 C43 116.4(5) . . ? F6 C42 C41 118.7(5) . . ? C43 C42 C41 124.9(5) . . ? F7 C43 C42 120.8(5) . . ? F7 C43 C44 120.5(5) . . ? C42 C43 C44 118.7(5) . . ? F8 C44 C45 120.3(5) . . ? F8 C44 C43 120.1(5) . . ? C45 C44 C43 119.6(5) . . ? F9 C45 C44 119.7(5) . . ? F9 C45 C46 120.7(5) . . ? C44 C45 C46 119.6(5) . . ? F10 C46 C45 114.9(5) . . ? F10 C46 C41 120.7(5) . . ? C45 C46 C41 124.4(5) . . ? C48 C47 C52 112.4(5) . . ? C48 C47 B1 128.0(5) . . ? C52 C47 B1 119.3(5) . . ? C47 C48 F11 121.7(5) . . ? C47 C48 C49 124.0(5) . . ? F11 C48 C49 114.3(5) . . ? C50 C49 F12 120.0(5) . . ? C50 C49 C48 120.2(5) . . ? F12 C49 C48 119.8(5) . . ? C49 C50 F13 121.0(5) . . ? C49 C50 C51 118.7(5) . . ? F13 C50 C51 120.4(5) . . ? F14 C51 C52 121.6(5) . . ? F14 C51 C50 119.3(5) . . ? C52 C51 C50 119.0(5) . . ? C51 C52 F15 115.9(5) . . ? C51 C52 C47 125.7(5) . . ? F15 C52 C47 118.4(5) . . ? C54 C53 C58 112.9(5) . . ? C54 C53 B1 119.6(5) . . ? C58 C53 B1 127.3(5) . . ? C55 C54 F16 116.0(5) . . ? C55 C54 C53 125.4(5) . . ? F16 C54 C53 118.6(5) . . ? C54 C55 F17 121.6(5) . . ? C54 C55 C56 119.3(5) . . ? F17 C55 C56 119.1(5) . . ? F18 C56 C57 121.3(6) . . ? F18 C56 C55 120.9(6) . . ? C57 C56 C55 117.8(6) . . ? C58 C57 F19 120.8(6) . . ? C58 C57 C56 120.8(6) . . ? F19 C57 C56 118.4(6) . . ? F20 C58 C57 114.9(5) . . ? F20 C58 C53 121.3(5) . . ? C57 C58 C53 123.8(5) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C59 C60 O1 108.6(9) . . ? C59 C60 H60A 110.0 . . ? O1 C60 H60A 110.0 . . ? C59 C60 H60B 110.0 . . ? O1 C60 H60B 110.0 . . ? H60A C60 H60B 108.3 . . ? C62 C61 O1 112.3(9) . . ? C62 C61 H61A 109.1 . . ? O1 C61 H61A 109.1 . . ? C62 C61 H61B 109.1 . . ? O1 C61 H61B 109.1 . . ? H61A C61 H61B 107.9 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C63 C64 O2 111.5(10) . . ? C63 C64 H64A 109.3 . . ? O2 C64 H64A 109.3 . . ? C63 C64 H64B 109.3 . . ? O2 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? C66 C65 O2 121.0(14) . . ? C66 C65 H65A 107.1 . . ? O2 C65 H65A 107.1 . . ? C66 C65 H65B 107.1 . . ? O2 C65 H65B 107.1 . . ? H65A C65 H65B 106.8 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C53 B1 C41 114.1(5) . . ? C53 B1 C35 102.4(4) . . ? C41 B1 C35 112.3(4) . . ? C53 B1 C47 113.2(4) . . ? C41 B1 C47 101.8(4) . . ? C35 B1 C47 113.5(4) . . ? C2 N1 Nb1 176.7(4) . . ? C19 N2 C6 121.3(4) . . ? C19 N2 Nb1 104.9(3) . . ? C6 N2 Nb1 130.7(3) . . ? C21 N3 C23 119.9(4) . . ? C21 N3 Nb1 104.5(3) . . ? C23 N3 Nb1 132.7(3) . . ? C61 O1 C60 113.3(7) . . ? C64 O2 C65 126.5(12) . . ? 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 C6 C7 C8 -1.0(9) . . . . ? N2 C6 C7 C8 176.7(5) . . . . ? C11 C6 C7 C12 178.5(5) . . . . ? N2 C6 C7 C12 -3.8(8) . . . . ? C6 C7 C8 C9 1.6(10) . . . . ? C12 C7 C8 C9 -177.9(6) . . . . ? C7 C8 C9 C10 -1.6(11) . . . . ? C8 C9 C10 C11 0.9(10) . . . . ? C7 C6 C11 C10 0.4(8) . . . . ? N2 C6 C11 C10 -177.3(5) . . . . ? C7 C6 C11 C15 -176.1(6) . . . . ? N2 C6 C11 C15 6.2(9) . . . . ? C9 C10 C11 C6 -0.3(9) . . . . ? C9 C10 C11 C15 176.3(7) . . . . ? C8 C7 C12 C13 -59.5(8) . . . . ? C6 C7 C12 C13 121.0(6) . . . . ? C8 C7 C12 C14 62.8(8) . . . . ? C6 C7 C12 C14 -116.7(6) . . . . ? C6 C11 C15 C17 109.4(8) . . . . ? C10 C11 C15 C17 -67.1(9) . . . . ? C6 C11 C15 C16 -127.3(6) . . . . ? C10 C11 C15 C16 56.2(9) . . . . ? N2 C19 C20 C21 17.3(9) . . . . ? C18 C19 C20 C21 -163.2(6) . . . . ? C19 C20 C21 N3 -17.1(9) . . . . ? C19 C20 C21 C22 164.5(5) . . . . ? C28 C23 C24 C25 -3.0(8) . . . . ? N3 C23 C24 C25 179.4(5) . . . . ? C28 C23 C24 C29 177.1(5) . . . . ? N3 C23 C24 C29 -0.6(7) . . . . ? C23 C24 C25 C26 1.2(8) . . . . ? C29 C24 C25 C26 -178.9(5) . . . . ? C24 C25 C26 C27 1.4(9) . . . . ? C25 C26 C27 C28 -2.3(9) . . . . ? C26 C27 C28 C23 0.6(9) . . . . ? C26 C27 C28 C32 179.9(6) . . . . ? C24 C23 C28 C27 2.1(8) . . . . ? N3 C23 C28 C27 179.8(5) . . . . ? C24 C23 C28 C32 -177.1(5) . . . . ? N3 C23 C28 C32 0.5(8) . . . . ? C23 C24 C29 C30 -138.0(5) . . . . ? C25 C24 C29 C30 42.1(7) . . . . ? C23 C24 C29 C31 98.2(6) . . . . ? C25 C24 C29 C31 -81.7(6) . . . . ? C27 C28 C32 C34 -70.7(8) . . . . ? C23 C28 C32 C34 108.6(7) . . . . ? C27 C28 C32 C33 54.3(8) . . . . ? C23 C28 C32 C33 -126.4(6) . . . . ? C40 C35 C36 F1 -177.5(5) . . . . ? B1 C35 C36 F1 -2.2(8) . . . . ? C40 C35 C36 C37 1.1(8) . . . . ? B1 C35 C36 C37 176.4(5) . . . . ? F1 C36 C37 F2 -1.3(8) . . . . ? C35 C36 C37 F2 -180.0(5) . . . . ? F1 C36 C37 C38 178.7(5) . . . . ? C35 C36 C37 C38 0.1(9) . . . . ? F2 C37 C38 C39 179.7(5) . . . . ? C36 C37 C38 C39 -0.4(9) . . . . ? F2 C37 C38 F3 -1.6(9) . . . . ? C36 C37 C38 F3 178.3(5) . . . . ? F3 C38 C39 F4 1.1(8) . . . . ? C37 C38 C39 F4 179.8(5) . . . . ? F3 C38 C39 C40 -179.3(5) . . . . ? C37 C38 C39 C40 -0.6(9) . . . . ? C36 C35 C40 F5 178.5(5) . . . . ? B1 C35 C40 F5 3.6(9) . . . . ? C36 C35 C40 C39 -2.1(8) . . . . ? B1 C35 C40 C39 -177.1(5) . . . . ? C38 C39 C40 F5 -178.6(5) . . . . ? F4 C39 C40 F5 1.0(7) . . . . ? C38 C39 C40 C35 2.0(9) . . . . ? F4 C39 C40 C35 -178.4(5) . . . . ? C46 C41 C42 F6 179.1(4) . . . . ? B1 C41 C42 F6 1.3(7) . . . . ? C46 C41 C42 C43 -3.5(7) . . . . ? B1 C41 C42 C43 178.7(5) . . . . ? F6 C42 C43 F7 -1.0(7) . . . . ? C41 C42 C43 F7 -178.4(5) . . . . ? F6 C42 C43 C44 178.6(5) . . . . ? C41 C42 C43 C44 1.2(8) . . . . ? F7 C43 C44 F8 0.7(8) . . . . ? C42 C43 C44 F8 -179.0(5) . . . . ? F7 C43 C44 C45 -179.4(5) . . . . ? C42 C43 C44 C45 1.0(8) . . . . ? F8 C44 C45 F9 -0.6(8) . . . . ? C43 C44 C45 F9 179.4(5) . . . . ? F8 C44 C45 C46 179.4(5) . . . . ? C43 C44 C45 C46 -0.5(8) . . . . ? F9 C45 C46 F10 -2.0(7) . . . . ? C44 C45 C46 F10 177.9(5) . . . . ? F9 C45 C46 C41 177.8(5) . . . . ? C44 C45 C46 C41 -2.2(8) . . . . ? C42 C41 C46 F10 -176.1(4) . . . . ? B1 C41 C46 F10 1.4(8) . . . . ? C42 C41 C46 C45 4.0(7) . . . . ? B1 C41 C46 C45 -178.4(5) . . . . ? C52 C47 C48 F11 -178.3(4) . . . . ? B1 C47 C48 F11 -4.5(8) . . . . ? C52 C47 C48 C49 1.1(8) . . . . ? B1 C47 C48 C49 174.9(5) . . . . ? C47 C48 C49 C50 0.0(9) . . . . ? F11 C48 C49 C50 179.4(5) . . . . ? C47 C48 C49 F12 179.3(5) . . . . ? F11 C48 C49 F12 -1.3(7) . . . . ? F12 C49 C50 F13 -1.2(8) . . . . ? C48 C49 C50 F13 178.1(5) . . . . ? F12 C49 C50 C51 179.8(5) . . . . ? C48 C49 C50 C51 -0.9(8) . . . . ? C49 C50 C51 F14 179.5(5) . . . . ? F13 C50 C51 F14 0.5(8) . . . . ? C49 C50 C51 C52 0.6(8) . . . . ? F13 C50 C51 C52 -178.4(5) . . . . ? F14 C51 C52 F15 2.7(7) . . . . ? C50 C51 C52 F15 -178.4(4) . . . . ? F14 C51 C52 C47 -178.3(5) . . . . ? C50 C51 C52 C47 0.6(8) . . . . ? C48 C47 C52 C51 -1.4(8) . . . . ? B1 C47 C52 C51 -175.8(5) . . . . ? C48 C47 C52 F15 177.6(4) . . . . ? B1 C47 C52 F15 3.2(7) . . . . ? C58 C53 C54 C55 3.2(8) . . . . ? B1 C53 C54 C55 178.1(5) . . . . ? C58 C53 C54 F16 -177.6(5) . . . . ? B1 C53 C54 F16 -2.7(7) . . . . ? F16 C54 C55 F17 -1.6(8) . . . . ? C53 C54 C55 F17 177.6(5) . . . . ? F16 C54 C55 C56 179.4(5) . . . . ? C53 C54 C55 C56 -1.3(9) . . . . ? C54 C55 C56 F18 178.8(5) . . . . ? F17 C55 C56 F18 -0.2(9) . . . . ? C54 C55 C56 C57 -0.7(9) . . . . ? F17 C55 C56 C57 -179.7(5) . . . . ? F18 C56 C57 C58 -178.8(6) . . . . ? C55 C56 C57 C58 0.7(10) . . . . ? F18 C56 C57 F19 1.5(9) . . . . ? C55 C56 C57 F19 -179.0(5) . . . . ? F19 C57 C58 F20 0.9(8) . . . . ? C56 C57 C58 F20 -178.8(5) . . . . ? F19 C57 C58 C53 -178.9(5) . . . . ? C56 C57 C58 C53 1.4(10) . . . . ? C54 C53 C58 F20 177.0(5) . . . . ? B1 C53 C58 F20 2.6(8) . . . . ? C54 C53 C58 C57 -3.2(8) . . . . ? B1 C53 C58 C57 -177.6(6) . . . . ? C54 C53 B1 C41 53.8(6) . . . . ? C58 C53 B1 C41 -132.2(5) . . . . ? C54 C53 B1 C35 -67.8(6) . . . . ? C58 C53 B1 C35 106.2(6) . . . . ? C54 C53 B1 C47 169.6(5) . . . . ? C58 C53 B1 C47 -16.3(8) . . . . ? C46 C41 B1 C53 11.8(7) . . . . ? C42 C41 B1 C53 -170.8(4) . . . . ? C46 C41 B1 C35 127.8(5) . . . . ? C42 C41 B1 C35 -54.8(6) . . . . ? C46 C41 B1 C47 -110.5(6) . . . . ? C42 C41 B1 C47 66.9(6) . . . . ? C36 C35 B1 C53 -66.8(6) . . . . ? C40 C35 B1 C53 107.8(6) . . . . ? C36 C35 B1 C41 170.3(5) . . . . ? C40 C35 B1 C41 -15.0(8) . . . . ? C36 C35 B1 C47 55.6(7) . . . . ? C40 C35 B1 C47 -129.8(6) . . . . ? C48 C47 B1 C53 131.0(6) . . . . ? C52 C47 B1 C53 -55.6(6) . . . . ? C48 C47 B1 C41 -106.0(6) . . . . ? C52 C47 B1 C41 67.4(6) . . . . ? C48 C47 B1 C35 14.8(8) . . . . ? C52 C47 B1 C35 -171.7(5) . . . . ? C3 C2 N1 Nb1 -151(7) . . . . ? C4 C2 N1 Nb1 -28(7) . . . . ? C5 C2 N1 Nb1 89(7) . . . . ? N3 Nb1 N1 C2 -42(7) . . . . ? N2 Nb1 N1 C2 61(7) . . . . ? C1 Nb1 N1 C2 -168(7) . . . . ? C20 C19 N2 C6 -170.0(5) . . . . ? C18 C19 N2 C6 10.5(7) . . . . ? C20 C19 N2 Nb1 27.9(5) . . . . ? C18 C19 N2 Nb1 -151.6(4) . . . . ? C11 C6 N2 C19 -99.5(6) . . . . ? C7 C6 N2 C19 82.8(6) . . . . ? C11 C6 N2 Nb1 57.5(6) . . . . ? C7 C6 N2 Nb1 -120.2(5) . . . . ? N1 Nb1 N2 C19 -169.0(3) . . . . ? N3 Nb1 N2 C19 -57.4(3) . . . . ? C1 Nb1 N2 C19 67.0(4) . . . . ? N1 Nb1 N2 C6 31.3(5) . . . . ? N3 Nb1 N2 C6 142.9(4) . . . . ? C1 Nb1 N2 C6 -92.8(5) . . . . ? C20 C21 N3 C23 169.1(5) . . . . ? C22 C21 N3 C23 -12.6(7) . . . . ? C20 C21 N3 Nb1 -28.0(5) . . . . ? C22 C21 N3 Nb1 150.3(4) . . . . ? C24 C23 N3 C21 -95.7(6) . . . . ? C28 C23 N3 C21 86.5(6) . . . . ? C24 C23 N3 Nb1 107.1(5) . . . . ? C28 C23 N3 Nb1 -70.6(6) . . . . ? N1 Nb1 N3 C21 169.1(3) . . . . ? N2 Nb1 N3 C21 57.2(3) . . . . ? C1 Nb1 N3 C21 -69.5(4) . . . . ? N1 Nb1 N3 C23 -31.2(5) . . . . ? N2 Nb1 N3 C23 -143.1(4) . . . . ? C1 Nb1 N3 C23 90.2(5) . . . . ? C62 C61 O1 C60 174.6(7) . . . . ? C59 C60 O1 C61 -175.0(7) . . . . ? C63 C64 O2 C65 -172.8(12) . . . . ? C66 C65 O2 C64 -178.0(17) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 21.72 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.885 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.064 data_n5c145txs _database_code_depnum_ccdc_archive 'CCDC 808678' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C41H62Cl2N4Ta _chemical_formula_sum 'C41 H62 Cl2 N4 Ta' _chemical_formula_weight 862.80 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' Cl Cl 0.1484 0.1585 '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 10.4181(10) _cell_length_b 12.5964(12) _cell_length_c 16.7145(16) _cell_angle_alpha 84.9620(10) _cell_angle_beta 76.5520(10) _cell_angle_gamma 74.7490(10) _cell_volume 2057.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 134(2) _cell_measurement_reflns_used 7696 _cell_measurement_theta_min 6.770 _cell_measurement_theta_max 52.715 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 2.833 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.840323 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 134(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11261 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7455 _reflns_number_gt 6827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker-AXS XP v.6' _computing_publication_material 'Bruker-AXS XP v.6' _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^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7455 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_restrained_S_all 1.267 _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 0.110899(12) 0.826378(9) 0.244403(7) 0.01803(5) Uani 1 1 d . . . Cl1 Cl 0.24304(7) 0.85861(6) 0.33653(4) 0.02329(16) Uani 1 1 d . . . Cl2 Cl -0.05556(8) 0.85793(6) 0.16129(5) 0.02464(16) Uani 1 1 d . . . N1 N 0.0724(2) 0.7124(2) 0.30785(14) 0.0201(5) Uani 1 1 d . . . N2 N 0.2687(2) 0.74092(19) 0.15157(14) 0.0180(5) Uani 1 1 d . . . N3 N 0.1666(2) 0.98582(19) 0.17102(14) 0.0185(5) Uani 1 1 d . . . N4 N -0.0653(2) 0.9399(2) 0.33763(15) 0.0208(5) Uani 1 1 d . . . C1 C 0.0479(3) 0.6348(3) 0.37640(19) 0.0251(7) Uani 1 1 d . . . C2 C 0.0491(4) 0.6870(3) 0.4561(2) 0.0410(9) Uani 1 1 d . . . H2A H 0.1372 0.7040 0.4510 0.062 Uiso 1 1 calc R . . H2B H 0.0348 0.6352 0.5027 0.062 Uiso 1 1 calc R . . H2C H -0.0240 0.7548 0.4654 0.062 Uiso 1 1 calc R . . C3 C -0.0899(4) 0.6089(3) 0.3833(2) 0.0392(9) Uani 1 1 d . . . H3A H -0.1627 0.6769 0.3929 0.059 Uiso 1 1 calc R . . H3B H -0.1048 0.5565 0.4293 0.059 Uiso 1 1 calc R . . H3C H -0.0903 0.5767 0.3321 0.059 Uiso 1 1 calc R . . C4 C 0.1625(3) 0.5290(3) 0.3627(2) 0.0302(7) Uani 1 1 d . . . H4A H 0.2504 0.5464 0.3580 0.045 Uiso 1 1 calc R . . H4B H 0.1628 0.4954 0.3120 0.045 Uiso 1 1 calc R . . H4C H 0.1478 0.4775 0.4093 0.045 Uiso 1 1 calc R . . C5 C 0.3346(3) 0.6258(2) 0.16731(18) 0.0206(6) Uani 1 1 d . . . C6 C 0.2811(3) 0.5426(2) 0.14679(18) 0.0213(6) Uani 1 1 d . . . C7 C 0.3441(3) 0.4332(3) 0.1645(2) 0.0299(7) Uani 1 1 d . . . H7A H 0.3089 0.3757 0.1523 0.036 Uiso 1 1 calc R . . C8 C 0.4567(3) 0.4076(3) 0.1994(2) 0.0327(8) Uani 1 1 d . . . H8A H 0.4964 0.3331 0.2126 0.039 Uiso 1 1 calc R . . C9 C 0.5113(3) 0.4898(3) 0.2151(2) 0.0329(8) Uani 1 1 d . . . H9A H 0.5912 0.4707 0.2369 0.039 Uiso 1 1 calc R . . C10 C 0.4520(3) 0.6015(3) 0.19973(18) 0.0234(7) Uani 1 1 d . . . C11 C 0.1626(3) 0.5656(3) 0.1028(2) 0.0266(7) Uani 1 1 d . . . H11A H 0.1443 0.6446 0.0837 0.032 Uiso 1 1 calc R . . C12 C 0.0318(3) 0.5471(3) 0.1595(2) 0.0337(8) Uani 1 1 d . . . H12A H 0.0085 0.5922 0.2082 0.051 Uiso 1 1 calc R . . H12B H 0.0456 0.4693 0.1766 0.051 Uiso 1 1 calc R . . H12C H -0.0427 0.5680 0.1301 0.051 Uiso 1 1 calc R . . C13 C 0.1983(4) 0.4934(3) 0.0258(2) 0.0374(8) Uani 1 1 d . . . H13A H 0.2817 0.5051 -0.0111 0.056 Uiso 1 1 calc R . . H13B H 0.1232 0.5139 -0.0031 0.056 Uiso 1 1 calc R . . H13C H 0.2125 0.4156 0.0433 0.056 Uiso 1 1 calc R . . C14 C 0.5190(3) 0.6891(3) 0.2151(2) 0.0311(8) Uani 1 1 d . . . H14A H 0.4503 0.7616 0.2158 0.037 Uiso 1 1 calc R . . C15 C 0.5604(4) 0.6732(3) 0.2975(2) 0.0474(10) Uani 1 1 d . . . H15A H 0.4808 0.6701 0.3416 0.071 Uiso 1 1 calc R . . H15B H 0.5960 0.7350 0.3061 0.071 Uiso 1 1 calc R . . H15C H 0.6310 0.6043 0.2980 0.071 Uiso 1 1 calc R . . C16 C 0.6425(4) 0.6961(4) 0.1453(3) 0.0529(11) Uani 1 1 d . . . H16A H 0.6830 0.7533 0.1571 0.079 Uiso 1 1 calc R . . H16B H 0.6128 0.7144 0.0932 0.079 Uiso 1 1 calc R . . H16C H 0.7102 0.6250 0.1411 0.079 Uiso 1 1 calc R . . C17 C 0.4009(3) 0.6990(3) 0.00853(19) 0.0283(7) Uani 1 1 d . . . H17A H 0.4178 0.7376 -0.0449 0.042 Uiso 1 1 calc R . . H17B H 0.3583 0.6398 0.0040 0.042 Uiso 1 1 calc R . . H17C H 0.4876 0.6678 0.0253 0.042 Uiso 1 1 calc R . . C18 C 0.3068(3) 0.7795(2) 0.07217(18) 0.0212(6) Uani 1 1 d . . . C19 C 0.2682(3) 0.8865(3) 0.04502(18) 0.0239(7) Uani 1 1 d . . . H19A H 0.2807 0.8965 -0.0130 0.029 Uiso 1 1 calc R . . C20 C 0.2120(3) 0.9852(2) 0.09015(18) 0.0219(6) Uani 1 1 d . . . C21 C 0.2126(4) 1.0895(3) 0.03761(19) 0.0293(7) Uani 1 1 d . . . H21A H 0.1765 1.1536 0.0729 0.044 Uiso 1 1 calc R . . H21B H 0.1556 1.0943 -0.0023 0.044 Uiso 1 1 calc R . . H21C H 0.3062 1.0881 0.0083 0.044 Uiso 1 1 calc R . . C22 C 0.1384(3) 1.0892(2) 0.21150(17) 0.0197(6) Uani 1 1 d . . . C23 C 0.0112(3) 1.1658(2) 0.21902(19) 0.0245(7) Uani 1 1 d . . . C24 C -0.0152(4) 1.2556(3) 0.2697(2) 0.0314(8) Uani 1 1 d . . . H24A H -0.1015 1.3073 0.2772 0.038 Uiso 1 1 calc R . . C25 C 0.0808(4) 1.2705(3) 0.3089(2) 0.0361(8) Uani 1 1 d . . . H25A H 0.0590 1.3299 0.3451 0.043 Uiso 1 1 calc R . . C26 C 0.2099(4) 1.1984(3) 0.2956(2) 0.0316(8) Uani 1 1 d . . . H26A H 0.2775 1.2116 0.3203 0.038 Uiso 1 1 calc R . . C27 C 0.2417(3) 1.1069(2) 0.24634(18) 0.0233(6) Uani 1 1 d . . . C28 C -0.0938(3) 1.1604(3) 0.1709(2) 0.0326(8) Uani 1 1 d . . . H28A H -0.0589 1.0915 0.1388 0.039 Uiso 1 1 calc R . . C29 C -0.2327(4) 1.1583(3) 0.2253(3) 0.0446(10) Uani 1 1 d . . . H29A H -0.2225 1.0953 0.2642 0.067 Uiso 1 1 calc R . . H29B H -0.2944 1.1516 0.1908 0.067 Uiso 1 1 calc R . . H29C H -0.2705 1.2266 0.2558 0.067 Uiso 1 1 calc R . . C30 C -0.1121(4) 1.2593(3) 0.1093(2) 0.0420(9) Uani 1 1 d . . . H30A H -0.0235 1.2611 0.0736 0.063 Uiso 1 1 calc R . . H30B H -0.1498 1.3278 0.1396 0.063 Uiso 1 1 calc R . . H30C H -0.1746 1.2519 0.0757 0.063 Uiso 1 1 calc R . . C31 C 0.3872(3) 1.0357(3) 0.22550(19) 0.0282(7) Uani 1 1 d . . . H31A H 0.3828 0.9605 0.2135 0.034 Uiso 1 1 calc R . . C32 C 0.4642(4) 1.0234(3) 0.2942(2) 0.0395(9) Uani 1 1 d . . . H32A H 0.4137 0.9931 0.3439 0.059 Uiso 1 1 calc R . . H32B H 0.4737 1.0956 0.3057 0.059 Uiso 1 1 calc R . . H32C H 0.5548 0.9735 0.2772 0.059 Uiso 1 1 calc R . . C33 C 0.4692(4) 1.0811(3) 0.1472(2) 0.0370(8) Uani 1 1 d . . . H33A H 0.5621 1.0337 0.1341 0.055 Uiso 1 1 calc R . . H33B H 0.4728 1.1559 0.1565 0.055 Uiso 1 1 calc R . . H33C H 0.4250 1.0825 0.1013 0.055 Uiso 1 1 calc R . . C34 C -0.1871(3) 0.9132(3) 0.35761(19) 0.0255(7) Uani 1 1 d . . . H34A H -0.2016 0.8602 0.3259 0.031 Uiso 1 1 calc R . . C35 C -0.2910(3) 0.9599(3) 0.4220(2) 0.0327(8) Uani 1 1 d . . . H35A H -0.3744 0.9382 0.4342 0.039 Uiso 1 1 calc R . . C36 C -0.2733(4) 1.0381(3) 0.4687(2) 0.0363(8) Uani 1 1 d . . . H36A H -0.3433 1.0707 0.5134 0.044 Uiso 1 1 calc R . . C37 C -0.1496(4) 1.0676(3) 0.4482(2) 0.0336(8) Uani 1 1 d . . . H37A H -0.1338 1.1218 0.4782 0.040 Uiso 1 1 calc R . . C38 C -0.0502(3) 1.0166(3) 0.38326(19) 0.0269(7) Uani 1 1 d . . . H38A H 0.0340 1.0371 0.3701 0.032 Uiso 1 1 calc R . . C39 C 0.5400(4) 0.5344(3) 0.5131(2) 0.0405(9) Uani 1 1 d . . . H39B H 0.6113 0.5470 0.4652 0.061 Uiso 1 1 calc R . . H39C H 0.5864 0.4928 0.5558 0.061 Uiso 1 1 calc R . . C40 C 0.4542(4) 0.6456(3) 0.5469(3) 0.0502(11) Uani 1 1 d . . . H40A H 0.3840 0.6335 0.5955 0.060 Uiso 1 1 calc R . . H40B H 0.4066 0.6872 0.5046 0.060 Uiso 1 1 calc R . . C41 C 0.5393(5) 0.7140(3) 0.5713(3) 0.0544(11) Uani 1 1 d . . . H41A H 0.4798 0.7843 0.5927 0.082 Uiso 1 1 calc R . . H41B H 0.6076 0.7277 0.5231 0.082 Uiso 1 1 calc R . . H41C H 0.5852 0.6739 0.6140 0.082 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 0.01825(7) 0.02037(8) 0.01568(7) 0.00017(5) -0.00313(5) -0.00589(5) Cl1 0.0221(4) 0.0309(4) 0.0184(3) 0.0000(3) -0.0052(3) -0.0088(3) Cl2 0.0248(4) 0.0262(4) 0.0258(4) 0.0011(3) -0.0107(3) -0.0073(3) N1 0.0220(13) 0.0187(13) 0.0172(12) -0.0006(10) -0.0027(10) -0.0024(10) N2 0.0199(13) 0.0174(12) 0.0159(12) -0.0014(10) -0.0015(10) -0.0050(10) N3 0.0182(12) 0.0199(13) 0.0184(12) -0.0002(10) -0.0053(10) -0.0056(10) N4 0.0210(13) 0.0199(13) 0.0212(13) 0.0026(10) -0.0047(10) -0.0053(10) C1 0.0334(18) 0.0227(16) 0.0199(15) 0.0043(13) -0.0061(13) -0.0096(13) C2 0.072(3) 0.032(2) 0.0208(17) 0.0037(15) -0.0061(17) -0.0212(18) C3 0.035(2) 0.042(2) 0.040(2) 0.0137(17) -0.0037(16) -0.0170(16) C4 0.0362(19) 0.0239(17) 0.0299(18) 0.0069(14) -0.0096(15) -0.0072(14) C5 0.0203(15) 0.0201(15) 0.0172(14) -0.0013(12) -0.0011(12) 0.0001(12) C6 0.0228(16) 0.0195(15) 0.0175(15) -0.0037(12) -0.0004(12) -0.0008(12) C7 0.0352(19) 0.0247(17) 0.0277(17) -0.0002(14) -0.0049(14) -0.0057(14) C8 0.0349(19) 0.0228(17) 0.0337(19) -0.0008(14) -0.0100(15) 0.0066(14) C9 0.0257(18) 0.0334(19) 0.0360(19) -0.0028(15) -0.0132(15) 0.0049(14) C10 0.0191(15) 0.0268(17) 0.0197(15) -0.0056(12) -0.0021(12) 0.0017(12) C11 0.0300(18) 0.0218(16) 0.0298(17) -0.0019(13) -0.0101(14) -0.0061(13) C12 0.0324(19) 0.0340(19) 0.037(2) -0.0032(15) -0.0070(15) -0.0123(15) C13 0.044(2) 0.035(2) 0.034(2) -0.0068(16) -0.0128(17) -0.0059(16) C14 0.0222(17) 0.0370(19) 0.0333(19) -0.0077(15) -0.0088(14) -0.0015(14) C15 0.052(3) 0.046(2) 0.052(2) -0.0078(19) -0.031(2) -0.0055(19) C16 0.035(2) 0.070(3) 0.059(3) -0.023(2) 0.0024(19) -0.025(2) C17 0.0307(18) 0.0287(18) 0.0201(16) -0.0031(13) 0.0028(13) -0.0045(14) C18 0.0227(16) 0.0225(16) 0.0194(15) -0.0017(12) -0.0036(12) -0.0080(12) C19 0.0304(17) 0.0272(17) 0.0133(14) 0.0006(12) -0.0022(12) -0.0082(13) C20 0.0235(16) 0.0216(15) 0.0224(16) 0.0026(12) -0.0069(12) -0.0084(12) C21 0.041(2) 0.0236(17) 0.0214(16) 0.0051(13) -0.0044(14) -0.0089(14) C22 0.0264(16) 0.0191(15) 0.0152(14) 0.0011(11) -0.0011(12) -0.0116(12) C23 0.0278(17) 0.0193(15) 0.0261(16) 0.0016(13) -0.0031(13) -0.0082(12) C24 0.0341(19) 0.0208(17) 0.0335(19) -0.0014(14) 0.0026(15) -0.0054(14) C25 0.052(2) 0.0265(18) 0.0306(19) -0.0082(14) -0.0005(16) -0.0154(16) C26 0.041(2) 0.038(2) 0.0245(17) -0.0025(14) -0.0070(15) -0.0245(16) C27 0.0314(17) 0.0233(16) 0.0176(15) 0.0056(12) -0.0044(13) -0.0139(13) C28 0.0300(18) 0.0224(17) 0.045(2) 0.0007(15) -0.0143(16) -0.0014(13) C29 0.036(2) 0.033(2) 0.064(3) 0.0155(19) -0.0185(19) -0.0081(16) C30 0.044(2) 0.034(2) 0.047(2) 0.0073(17) -0.0191(18) -0.0023(16) C31 0.0267(17) 0.0347(18) 0.0273(17) 0.0035(14) -0.0077(14) -0.0148(14) C32 0.034(2) 0.055(2) 0.039(2) 0.0057(18) -0.0151(16) -0.0220(17) C33 0.0325(19) 0.045(2) 0.036(2) 0.0012(16) -0.0001(15) -0.0206(16) C34 0.0236(16) 0.0249(16) 0.0266(16) 0.0026(13) -0.0067(13) -0.0036(13) C35 0.0232(17) 0.040(2) 0.0305(18) 0.0023(15) -0.0001(14) -0.0057(14) C36 0.033(2) 0.042(2) 0.0245(17) -0.0019(15) 0.0009(14) 0.0012(16) C37 0.038(2) 0.0354(19) 0.0245(17) -0.0084(14) -0.0046(15) -0.0045(15) C38 0.0287(17) 0.0277(17) 0.0237(16) 0.0019(13) -0.0082(13) -0.0049(13) C39 0.041(2) 0.040(2) 0.042(2) 0.0003(17) -0.0160(18) -0.0085(17) C40 0.054(3) 0.044(2) 0.056(3) -0.010(2) -0.022(2) -0.0070(19) C41 0.069(3) 0.040(2) 0.058(3) -0.005(2) -0.024(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.784(2) . ? Ta1 N2 2.108(2) . ? Ta1 N4 2.350(2) . ? Ta1 N3 2.392(2) . ? Ta1 Cl2 2.3993(7) . ? Ta1 Cl1 2.4128(7) . ? N1 C1 1.460(4) . ? N2 C18 1.378(4) . ? N2 C5 1.462(4) . ? N3 C20 1.324(4) . ? N3 C22 1.449(4) . ? N4 C38 1.345(4) . ? N4 C34 1.357(4) . ? C1 C3 1.531(5) . ? C1 C4 1.531(4) . ? C1 C2 1.540(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? 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 C10 1.402(4) . ? C5 C6 1.408(4) . ? C6 C7 1.400(4) . ? C6 C11 1.532(4) . ? C7 C8 1.380(5) . ? C7 H7A 0.9500 . ? C8 C9 1.376(5) . ? C8 H8A 0.9500 . ? C9 C10 1.406(4) . ? C9 H9A 0.9500 . ? C10 C14 1.520(5) . ? C11 C12 1.529(5) . ? C11 C13 1.557(4) . ? C11 H11A 1.0000 . ? 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 C15 1.519(5) . ? C14 C16 1.539(5) . ? C14 H14A 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 C18 1.517(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.370(4) . ? C19 C20 1.426(4) . ? C19 H19A 0.9500 . ? C20 C21 1.515(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.405(4) . ? C22 C27 1.410(4) . ? C23 C24 1.403(4) . ? C23 C28 1.518(5) . ? C24 C25 1.375(5) . ? C24 H24A 0.9500 . ? C25 C26 1.392(5) . ? C25 H25A 0.9500 . ? C26 C27 1.399(4) . ? C26 H26A 0.9500 . ? C27 C31 1.522(4) . ? C28 C29 1.525(5) . ? C28 C30 1.546(5) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.522(4) . ? C31 C33 1.541(4) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.383(4) . ? C34 H34A 0.9500 . ? C35 C36 1.382(5) . ? C35 H35A 0.9500 . ? C36 C37 1.393(5) . ? C36 H36A 0.9500 . ? C37 C38 1.383(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C39 1.501(7) 2_666 ? C39 C40 1.525(5) . ? C39 H39B 0.9900 . ? C39 H39C 0.9900 . ? C40 C41 1.526(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 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 N1 Ta1 N2 99.51(10) . . ? N1 Ta1 N4 87.02(10) . . ? N2 Ta1 N4 173.32(8) . . ? N1 Ta1 N3 174.34(9) . . ? N2 Ta1 N3 83.59(9) . . ? N4 Ta1 N3 90.03(8) . . ? N1 Ta1 Cl2 101.07(8) . . ? N2 Ta1 Cl2 93.26(7) . . ? N4 Ta1 Cl2 84.02(6) . . ? N3 Ta1 Cl2 83.40(6) . . ? N1 Ta1 Cl1 90.32(8) . . ? N2 Ta1 Cl1 100.04(7) . . ? N4 Ta1 Cl1 81.23(6) . . ? N3 Ta1 Cl1 84.46(6) . . ? Cl2 Ta1 Cl1 160.85(3) . . ? C1 N1 Ta1 164.9(2) . . ? C18 N2 C5 115.0(2) . . ? C18 N2 Ta1 125.73(19) . . ? C5 N2 Ta1 118.81(18) . . ? C20 N3 C22 117.6(2) . . ? C20 N3 Ta1 120.6(2) . . ? C22 N3 Ta1 121.51(17) . . ? C38 N4 C34 116.5(3) . . ? C38 N4 Ta1 125.5(2) . . ? C34 N4 Ta1 117.0(2) . . ? N1 C1 C3 110.3(3) . . ? N1 C1 C4 109.2(3) . . ? C3 C1 C4 110.0(3) . . ? N1 C1 C2 108.4(3) . . ? C3 C1 C2 109.9(3) . . ? C4 C1 C2 108.9(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 122.0(3) . . ? C10 C5 N2 118.9(3) . . ? C6 C5 N2 119.1(3) . . ? C7 C6 C5 117.9(3) . . ? C7 C6 C11 118.7(3) . . ? C5 C6 C11 123.4(3) . . ? C8 C7 C6 121.1(3) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 121.7(3) . . ? C8 C9 H9A 119.2 . . ? C10 C9 H9A 119.2 . . ? C5 C10 C9 117.2(3) . . ? C5 C10 C14 123.0(3) . . ? C9 C10 C14 119.8(3) . . ? C12 C11 C6 112.3(3) . . ? C12 C11 C13 108.9(3) . . ? C6 C11 C13 111.6(3) . . ? C12 C11 H11A 107.9 . . ? C6 C11 H11A 107.9 . . ? C13 C11 H11A 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C10 113.0(3) . . ? C15 C14 C16 110.1(3) . . ? C10 C14 C16 111.6(3) . . ? C15 C14 H14A 107.3 . . ? C10 C14 H14A 107.3 . . ? C16 C14 H14A 107.3 . . ? 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 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N2 125.3(3) . . ? C19 C18 C17 116.0(3) . . ? N2 C18 C17 118.6(3) . . ? C18 C19 C20 130.2(3) . . ? C18 C19 H19A 114.9 . . ? C20 C19 H19A 114.9 . . ? N3 C20 C19 123.1(3) . . ? N3 C20 C21 122.9(3) . . ? C19 C20 C21 114.0(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 121.6(3) . . ? C23 C22 N3 121.3(3) . . ? C27 C22 N3 117.0(3) . . ? C24 C23 C22 117.6(3) . . ? C24 C23 C28 118.8(3) . . ? C22 C23 C28 123.4(3) . . ? C25 C24 C23 121.6(3) . . ? C25 C24 H24A 119.2 . . ? C23 C24 H24A 119.2 . . ? C24 C25 C26 119.9(3) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C27 121.0(3) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C26 C27 C22 117.9(3) . . ? C26 C27 C31 120.1(3) . . ? C22 C27 C31 121.8(3) . . ? C23 C28 C29 113.5(3) . . ? C23 C28 C30 110.3(3) . . ? C29 C28 C30 108.8(3) . . ? C23 C28 H28A 108.1 . . ? C29 C28 H28A 108.1 . . ? C30 C28 H28A 108.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C27 114.4(3) . . ? C32 C31 C33 108.9(3) . . ? C27 C31 C33 110.5(3) . . ? C32 C31 H31A 107.6 . . ? C27 C31 H31A 107.6 . . ? C33 C31 H31A 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 C35 122.9(3) . . ? N4 C34 H34A 118.5 . . ? C35 C34 H34A 118.5 . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C35 C36 C37 118.0(3) . . ? C35 C36 H36A 121.0 . . ? C37 C36 H36A 121.0 . . ? C38 C37 C36 118.8(3) . . ? C38 C37 H37A 120.6 . . ? C36 C37 H37A 120.6 . . ? N4 C38 C37 124.0(3) . . ? N4 C38 H38A 118.0 . . ? C37 C38 H38A 118.0 . . ? C39 C39 C40 114.1(4) 2_666 . ? C39 C39 H39B 108.7 2_666 . ? C40 C39 H39B 108.7 . . ? C39 C39 H39C 108.7 2_666 . ? C40 C39 H39C 108.7 . . ? H39B C39 H39C 107.6 . . ? C39 C40 C41 112.6(4) . . ? C39 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? C39 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 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 N2 Ta1 N1 C1 124.6(8) . . . . ? N4 Ta1 N1 C1 -56.9(8) . . . . ? N3 Ta1 N1 C1 1.7(16) . . . . ? Cl2 Ta1 N1 C1 -140.2(8) . . . . ? Cl1 Ta1 N1 C1 24.3(8) . . . . ? N1 Ta1 N2 C18 155.7(2) . . . . ? N4 Ta1 N2 C18 -11.8(8) . . . . ? N3 Ta1 N2 C18 -29.1(2) . . . . ? Cl2 Ta1 N2 C18 53.9(2) . . . . ? Cl1 Ta1 N2 C18 -112.3(2) . . . . ? N1 Ta1 N2 C5 -16.3(2) . . . . ? N4 Ta1 N2 C5 176.2(6) . . . . ? N3 Ta1 N2 C5 159.0(2) . . . . ? Cl2 Ta1 N2 C5 -118.1(2) . . . . ? Cl1 Ta1 N2 C5 75.8(2) . . . . ? N1 Ta1 N3 C20 155.4(9) . . . . ? N2 Ta1 N3 C20 31.9(2) . . . . ? N4 Ta1 N3 C20 -146.1(2) . . . . ? Cl2 Ta1 N3 C20 -62.2(2) . . . . ? Cl1 Ta1 N3 C20 132.7(2) . . . . ? N1 Ta1 N3 C22 -31.3(10) . . . . ? N2 Ta1 N3 C22 -154.8(2) . . . . ? N4 Ta1 N3 C22 27.1(2) . . . . ? Cl2 Ta1 N3 C22 111.1(2) . . . . ? Cl1 Ta1 N3 C22 -54.1(2) . . . . ? N1 Ta1 N4 C38 117.9(2) . . . . ? N2 Ta1 N4 C38 -74.3(8) . . . . ? N3 Ta1 N4 C38 -57.2(2) . . . . ? Cl2 Ta1 N4 C38 -140.6(2) . . . . ? Cl1 Ta1 N4 C38 27.2(2) . . . . ? N1 Ta1 N4 C34 -50.0(2) . . . . ? N2 Ta1 N4 C34 117.7(7) . . . . ? N3 Ta1 N4 C34 134.8(2) . . . . ? Cl2 Ta1 N4 C34 51.5(2) . . . . ? Cl1 Ta1 N4 C34 -140.8(2) . . . . ? Ta1 N1 C1 C3 128.6(7) . . . . ? Ta1 N1 C1 C4 -110.4(8) . . . . ? Ta1 N1 C1 C2 8.2(9) . . . . ? C18 N2 C5 C10 94.9(3) . . . . ? Ta1 N2 C5 C10 -92.3(3) . . . . ? C18 N2 C5 C6 -82.8(3) . . . . ? Ta1 N2 C5 C6 90.0(3) . . . . ? C10 C5 C6 C7 3.9(4) . . . . ? N2 C5 C6 C7 -178.4(3) . . . . ? C10 C5 C6 C11 -173.2(3) . . . . ? N2 C5 C6 C11 4.5(4) . . . . ? C5 C6 C7 C8 -1.3(5) . . . . ? C11 C6 C7 C8 175.9(3) . . . . ? C6 C7 C8 C9 -2.0(5) . . . . ? C7 C8 C9 C10 2.8(5) . . . . ? C6 C5 C10 C9 -3.1(4) . . . . ? N2 C5 C10 C9 179.1(3) . . . . ? C6 C5 C10 C14 174.3(3) . . . . ? N2 C5 C10 C14 -3.4(4) . . . . ? C8 C9 C10 C5 -0.2(5) . . . . ? C8 C9 C10 C14 -177.7(3) . . . . ? C7 C6 C11 C12 73.9(4) . . . . ? C5 C6 C11 C12 -109.0(3) . . . . ? C7 C6 C11 C13 -48.7(4) . . . . ? C5 C6 C11 C13 128.3(3) . . . . ? C5 C10 C14 C15 136.0(3) . . . . ? C9 C10 C14 C15 -46.6(4) . . . . ? C5 C10 C14 C16 -99.3(4) . . . . ? C9 C10 C14 C16 78.0(4) . . . . ? C5 N2 C18 C19 -173.9(3) . . . . ? Ta1 N2 C18 C19 13.9(4) . . . . ? C5 N2 C18 C17 5.2(4) . . . . ? Ta1 N2 C18 C17 -167.1(2) . . . . ? N2 C18 C19 C20 17.0(5) . . . . ? C17 C18 C19 C20 -162.1(3) . . . . ? C22 N3 C20 C19 167.5(3) . . . . ? Ta1 N3 C20 C19 -19.0(4) . . . . ? C22 N3 C20 C21 -10.6(4) . . . . ? Ta1 N3 C20 C21 162.9(2) . . . . ? C18 C19 C20 N3 -11.6(5) . . . . ? C18 C19 C20 C21 166.7(3) . . . . ? C20 N3 C22 C23 86.6(3) . . . . ? Ta1 N3 C22 C23 -86.8(3) . . . . ? C20 N3 C22 C27 -96.3(3) . . . . ? Ta1 N3 C22 C27 90.2(3) . . . . ? C27 C22 C23 C24 -6.5(4) . . . . ? N3 C22 C23 C24 170.4(3) . . . . ? C27 C22 C23 C28 169.2(3) . . . . ? N3 C22 C23 C28 -13.9(4) . . . . ? C22 C23 C24 C25 1.9(5) . . . . ? C28 C23 C24 C25 -173.9(3) . . . . ? C23 C24 C25 C26 3.1(5) . . . . ? C24 C25 C26 C27 -3.7(5) . . . . ? C25 C26 C27 C22 -0.8(5) . . . . ? C25 C26 C27 C31 173.8(3) . . . . ? C23 C22 C27 C26 5.9(4) . . . . ? N3 C22 C27 C26 -171.1(3) . . . . ? C23 C22 C27 C31 -168.6(3) . . . . ? N3 C22 C27 C31 14.4(4) . . . . ? C24 C23 C28 C29 -59.8(4) . . . . ? C22 C23 C28 C29 124.6(3) . . . . ? C24 C23 C28 C30 62.5(4) . . . . ? C22 C23 C28 C30 -113.1(3) . . . . ? C26 C27 C31 C32 35.3(4) . . . . ? C22 C27 C31 C32 -150.3(3) . . . . ? C26 C27 C31 C33 -88.0(3) . . . . ? C22 C27 C31 C33 86.3(4) . . . . ? C38 N4 C34 C35 -1.1(4) . . . . ? Ta1 N4 C34 C35 168.0(2) . . . . ? N4 C34 C35 C36 0.7(5) . . . . ? C34 C35 C36 C37 0.4(5) . . . . ? C35 C36 C37 C38 -0.9(5) . . . . ? C34 N4 C38 C37 0.5(4) . . . . ? Ta1 N4 C38 C37 -167.5(2) . . . . ? C36 C37 C38 N4 0.5(5) . . . . ? C39 C39 C40 C41 -179.0(4) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.888 _refine_diff_density_max 2.594 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.087 # Attachment '- 5.cif' data_neils _database_code_depnum_ccdc_archive 'CCDC 808679' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34.86 H55.58 Cl0.14 N3 Ta' _chemical_formula_sum 'C34.86 H55.58 Cl0.14 N3 Ta' _chemical_formula_weight 702.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4872(15) _cell_length_b 13.1367(19) _cell_length_c 24.997(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.375(2) _cell_angle_gamma 90.00 _cell_volume 3437.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used 9923 _cell_measurement_theta_min 4.499 _cell_measurement_theta_max 56.574 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 3.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4088 _exptl_absorpt_correction_T_max 0.6202 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 147(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 APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 21789 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8300 _reflns_number_gt 6457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material CIFTAB _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^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8300 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.283834(14) 0.312579(12) 0.357787(6) 0.01634(6) Uani 1 1 d . . . N1 N 0.3531(3) 0.3772(2) 0.30408(12) 0.0176(7) Uani 1 1 d . A . N2 N 0.2175(3) 0.4402(2) 0.39988(12) 0.0158(7) Uani 1 1 d . A . N3 N 0.1701(3) 0.2209(2) 0.42000(13) 0.0181(7) Uani 1 1 d . A . C1 C 0.1803(14) 0.2126(12) 0.2999(6) 0.033(4) Uani 0.860(8) 1 d P A 1 H1A H 0.1670 0.2474 0.2663 0.050 Uiso 0.860(8) 1 calc PR A 1 H1B H 0.0992 0.1947 0.3132 0.050 Uiso 0.860(8) 1 calc PR A 1 H1C H 0.2294 0.1520 0.2950 0.050 Uiso 0.860(8) 1 calc PR A 1 Cl1 Cl 0.193(2) 0.189(3) 0.2973(11) 0.046(7) Uani 0.140(8) 1 d P A 2 C2 C 0.4618(4) 0.2522(3) 0.39362(17) 0.0259(10) Uani 1 1 d . A . H2A H 0.5321 0.2788 0.3751 0.039 Uiso 1 1 calc R . . H2B H 0.4611 0.1793 0.3910 0.039 Uiso 1 1 calc R . . H2C H 0.4708 0.2717 0.4306 0.039 Uiso 1 1 calc R . . C3 C 0.4081(4) 0.4104(3) 0.25458(15) 0.0209(9) Uani 1 1 d . . . C4 C 0.3418(5) 0.3553(4) 0.20727(17) 0.0373(12) Uani 1 1 d . A . H4A H 0.3543 0.2832 0.2114 0.056 Uiso 1 1 calc R . . H4B H 0.3772 0.3775 0.1747 0.056 Uiso 1 1 calc R . . H4C H 0.2521 0.3702 0.2058 0.056 Uiso 1 1 calc R . . C5 C 0.5503(4) 0.3849(4) 0.25767(18) 0.0340(11) Uani 1 1 d . A . H5A H 0.5612 0.3127 0.2617 0.051 Uiso 1 1 calc R . . H5B H 0.5918 0.4191 0.2879 0.051 Uiso 1 1 calc R . . H5C H 0.5873 0.4068 0.2254 0.051 Uiso 1 1 calc R . . C6 C 0.3889(5) 0.5256(3) 0.24773(19) 0.0362(12) Uani 1 1 d . A . H6A H 0.4316 0.5605 0.2774 0.054 Uiso 1 1 calc R . . H6B H 0.2993 0.5410 0.2466 0.054 Uiso 1 1 calc R . . H6C H 0.4237 0.5472 0.2149 0.054 Uiso 1 1 calc R . . C7 C 0.2214(4) 0.5391(3) 0.37359(15) 0.0179(8) Uani 1 1 d . . . C8 C 0.1169(4) 0.5678(3) 0.33915(15) 0.0192(8) Uani 1 1 d . A . C9 C 0.1213(4) 0.6626(3) 0.31448(17) 0.0251(10) Uani 1 1 d . . . H9A H 0.0519 0.6838 0.2924 0.030 Uiso 1 1 calc R A . C10 C 0.2254(4) 0.7259(3) 0.32177(18) 0.0272(10) Uani 1 1 d . A . H10A H 0.2272 0.7879 0.3039 0.033 Uiso 1 1 calc R . . C11 C 0.3268(4) 0.6964(3) 0.35583(18) 0.0264(10) Uani 1 1 d . . . H11A H 0.3967 0.7397 0.3609 0.032 Uiso 1 1 calc R A . C12 C 0.3275(4) 0.6031(3) 0.38316(16) 0.0188(8) Uani 1 1 d . A . C13 C 0.0012(4) 0.4998(3) 0.32818(17) 0.0250(9) Uani 1 1 d . . . H13A H 0.0139 0.4383 0.3500 0.030 Uiso 1 1 calc R A . C14 C -0.0120(4) 0.4672(3) 0.26945(18) 0.0348(11) Uani 1 1 d . A . H14A H 0.0652 0.4340 0.2600 0.052 Uiso 1 1 calc R . . H14B H -0.0269 0.5260 0.2472 0.052 Uiso 1 1 calc R . . H14C H -0.0825 0.4209 0.2643 0.052 Uiso 1 1 calc R . . C15 C -0.1219(4) 0.5514(4) 0.3446(2) 0.0418(12) Uani 1 1 d . A . H15A H -0.1929 0.5064 0.3374 0.063 Uiso 1 1 calc R . . H15B H -0.1354 0.6131 0.3245 0.063 Uiso 1 1 calc R . . H15C H -0.1144 0.5670 0.3821 0.063 Uiso 1 1 calc R . . C16 C 0.4401(4) 0.5760(3) 0.42136(17) 0.0238(9) Uani 1 1 d . . . H16A H 0.4156 0.5170 0.4424 0.029 Uiso 1 1 calc R A . C17 C 0.5577(4) 0.5459(3) 0.39091(18) 0.0323(11) Uani 1 1 d . A . H17A H 0.5352 0.4919 0.3663 0.048 Uiso 1 1 calc R . . H17B H 0.6247 0.5235 0.4160 0.048 Uiso 1 1 calc R . . H17C H 0.5866 0.6037 0.3715 0.048 Uiso 1 1 calc R . . C18 C 0.4773(4) 0.6623(3) 0.46068(19) 0.0353(11) Uani 1 1 d . A . H18A H 0.4047 0.6806 0.4803 0.053 Uiso 1 1 calc R . . H18B H 0.5049 0.7204 0.4411 0.053 Uiso 1 1 calc R . . H18C H 0.5454 0.6398 0.4852 0.053 Uiso 1 1 calc R . . C19 C 0.1593(4) 0.5438(3) 0.47777(16) 0.0263(10) Uani 1 1 d . A . H19A H 0.1385 0.5331 0.5142 0.039 Uiso 1 1 calc R . . H19B H 0.0887 0.5761 0.4583 0.039 Uiso 1 1 calc R . . H19C H 0.2334 0.5865 0.4770 0.039 Uiso 1 1 calc R . . C20 C 0.1866(3) 0.4420(3) 0.45203(15) 0.0181(8) Uani 1 1 d . . . C21 C 0.1747(4) 0.3572(3) 0.48398(16) 0.0208(9) Uani 1 1 d . A . H21A H 0.1784 0.3697 0.5207 0.025 Uiso 1 1 calc R . . C22 C 0.1579(4) 0.2548(3) 0.46905(16) 0.0181(8) Uani 1 1 d . . . C23 C 0.1184(5) 0.1848(3) 0.51366(16) 0.0308(10) Uani 1 1 d . A . H23A H 0.1100 0.1165 0.5003 0.046 Uiso 1 1 calc R . . H23B H 0.0381 0.2072 0.5260 0.046 Uiso 1 1 calc R . . H23C H 0.1822 0.1867 0.5428 0.046 Uiso 1 1 calc R . . C24 C 0.1069(4) 0.1241(3) 0.40732(16) 0.0211(9) Uani 1 1 d . . . C25 C -0.0223(4) 0.1283(3) 0.38816(16) 0.0234(9) Uani 1 1 d . A . C26 C -0.0833(4) 0.0374(3) 0.37375(17) 0.0280(10) Uani 1 1 d . . . H26A H -0.1688 0.0384 0.3615 0.034 Uiso 1 1 calc R A . C27 C -0.0188(4) -0.0544(3) 0.37735(17) 0.0313(11) Uani 1 1 d . A . H27A H -0.0603 -0.1143 0.3669 0.038 Uiso 1 1 calc R . . C28 C 0.1054(4) -0.0570(3) 0.39626(17) 0.0308(10) Uani 1 1 d . . . H28A H 0.1477 -0.1193 0.3983 0.037 Uiso 1 1 calc R A . C29 C 0.1713(4) 0.0308(3) 0.41269(16) 0.0252(10) Uani 1 1 d . A . C30 C -0.0954(4) 0.2291(3) 0.38298(18) 0.0283(10) Uani 1 1 d . . . H30A H -0.0325 0.2843 0.3832 0.034 Uiso 1 1 calc R A . C31 C -0.1778(4) 0.2363(4) 0.33071(19) 0.0412(12) Uani 1 1 d . A . H31A H -0.2209 0.3007 0.3290 0.062 Uiso 1 1 calc R . . H31B H -0.2397 0.1824 0.3293 0.062 Uiso 1 1 calc R . . H31C H -0.1246 0.2302 0.3009 0.062 Uiso 1 1 calc R . . C32 C -0.1783(5) 0.2458(4) 0.42960(19) 0.0414(13) Uani 1 1 d . A . H32A H -0.2224 0.3095 0.4252 0.062 Uiso 1 1 calc R . . H32B H -0.1257 0.2469 0.4624 0.062 Uiso 1 1 calc R . . H32C H -0.2393 0.1915 0.4309 0.062 Uiso 1 1 calc R . . C33 C 0.3091(4) 0.0228(3) 0.43517(17) 0.0274(10) Uani 1 1 d . . . H33A H 0.3370 0.0903 0.4478 0.033 Uiso 1 1 calc R A . C34 C 0.3969(5) -0.0117(4) 0.3919(2) 0.0406(12) Uani 1 1 d . A . H34A H 0.3904 0.0352 0.3625 0.061 Uiso 1 1 calc R . . H34B H 0.3719 -0.0784 0.3795 0.061 Uiso 1 1 calc R . . H34C H 0.4835 -0.0137 0.4066 0.061 Uiso 1 1 calc R . . C35 C 0.3201(5) -0.0516(3) 0.4831(2) 0.0403(12) Uani 1 1 d . A . H35A H 0.2644 -0.0297 0.5100 0.060 Uiso 1 1 calc R . . H35B H 0.4066 -0.0524 0.4980 0.060 Uiso 1 1 calc R . . H35C H 0.2962 -0.1187 0.4712 0.060 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 0.01843(8) 0.01724(9) 0.01356(9) -0.00123(7) 0.00269(6) 0.00057(7) N1 0.0193(16) 0.0188(16) 0.0149(17) 0.0031(14) 0.0016(13) 0.0008(14) N2 0.0160(15) 0.0153(16) 0.0158(17) -0.0024(14) -0.0009(13) -0.0019(13) N3 0.0208(17) 0.0174(16) 0.0164(18) -0.0002(14) 0.0027(14) -0.0004(14) C1 0.039(6) 0.040(9) 0.022(5) 0.003(4) 0.015(4) -0.002(5) Cl1 0.045(9) 0.040(12) 0.050(11) 0.006(7) -0.028(9) -0.010(8) C2 0.025(2) 0.028(2) 0.025(2) 0.001(2) 0.0054(18) -0.0043(19) C3 0.022(2) 0.027(2) 0.014(2) 0.0038(17) 0.0062(16) 0.0032(17) C4 0.043(3) 0.048(3) 0.021(3) 0.004(2) 0.007(2) -0.003(2) C5 0.027(2) 0.047(3) 0.029(3) 0.010(2) 0.013(2) 0.010(2) C6 0.045(3) 0.033(3) 0.033(3) 0.013(2) 0.019(2) 0.011(2) C7 0.0216(19) 0.017(2) 0.015(2) -0.0023(16) 0.0041(16) 0.0049(16) C8 0.0205(19) 0.023(2) 0.015(2) -0.0001(18) 0.0041(16) 0.0013(17) C9 0.029(2) 0.023(2) 0.023(2) 0.0034(18) 0.0033(18) 0.0064(18) C10 0.032(2) 0.018(2) 0.032(3) 0.0026(19) 0.008(2) 0.0036(19) C11 0.027(2) 0.018(2) 0.035(3) -0.004(2) 0.0077(19) -0.0018(18) C12 0.0214(19) 0.020(2) 0.016(2) -0.0028(17) 0.0043(16) 0.0041(17) C13 0.021(2) 0.027(2) 0.027(2) 0.008(2) -0.0014(18) -0.0037(18) C14 0.034(3) 0.038(3) 0.033(3) -0.007(2) -0.002(2) -0.002(2) C15 0.029(2) 0.056(3) 0.041(3) -0.005(3) 0.007(2) -0.005(2) C16 0.021(2) 0.021(2) 0.029(2) -0.0044(19) -0.0003(18) -0.0030(17) C17 0.020(2) 0.040(3) 0.036(3) -0.009(2) 0.0012(19) 0.004(2) C18 0.030(2) 0.040(3) 0.035(3) -0.011(2) -0.003(2) 0.001(2) C19 0.034(2) 0.027(2) 0.019(2) -0.0051(19) 0.0098(18) -0.0003(19) C20 0.0167(18) 0.0195(19) 0.018(2) -0.0029(18) 0.0030(16) 0.0013(17) C21 0.024(2) 0.026(2) 0.012(2) -0.0030(18) -0.0024(17) -0.0035(18) C22 0.0184(19) 0.022(2) 0.014(2) 0.0034(17) 0.0015(16) 0.0000(17) C23 0.047(3) 0.030(2) 0.016(2) -0.001(2) 0.007(2) -0.005(2) C24 0.030(2) 0.020(2) 0.014(2) -0.0011(17) 0.0050(17) -0.0030(18) C25 0.027(2) 0.025(2) 0.019(2) 0.0002(18) 0.0042(18) -0.0049(18) C26 0.033(2) 0.026(2) 0.026(2) 0.0038(19) 0.0005(19) -0.0094(19) C27 0.048(3) 0.025(2) 0.021(2) -0.002(2) 0.006(2) -0.013(2) C28 0.047(3) 0.022(2) 0.024(2) 0.002(2) 0.008(2) 0.002(2) C29 0.036(2) 0.022(2) 0.018(2) -0.0011(18) 0.0072(19) -0.0046(19) C30 0.023(2) 0.027(2) 0.034(3) 0.001(2) -0.001(2) -0.0045(19) C31 0.039(3) 0.051(3) 0.034(3) 0.006(3) 0.003(2) 0.013(3) C32 0.051(3) 0.045(3) 0.028(3) -0.009(2) 0.001(2) 0.008(3) C33 0.038(3) 0.018(2) 0.027(3) 0.0022(19) 0.005(2) 0.0039(19) C34 0.045(3) 0.035(3) 0.044(3) -0.003(2) 0.017(2) 0.009(2) C35 0.045(3) 0.033(3) 0.043(3) 0.011(2) -0.002(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.779(3) . ? Ta1 N2 2.119(3) . ? Ta1 C2 2.172(4) . ? Ta1 C1 2.193(14) . ? Ta1 N3 2.347(3) . ? Ta1 Cl1 2.38(3) . ? N1 C3 1.462(5) . ? N2 C20 1.362(5) . ? N2 C7 1.458(5) . ? N3 C22 1.317(5) . ? N3 C24 1.461(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.520(6) . ? C3 C5 1.526(5) . ? C3 C6 1.534(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C12 1.403(5) . ? C7 C8 1.405(5) . ? C8 C9 1.391(5) . ? C8 C13 1.518(5) . ? C9 C10 1.375(6) . ? C9 H9A 0.9300 . ? C10 C11 1.378(6) . ? C10 H10A 0.9300 . ? C11 C12 1.404(5) . ? C11 H11A 0.9300 . ? C12 C16 1.516(5) . ? C13 C14 1.528(6) . ? C13 C15 1.535(6) . ? C13 H13A 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C18 1.535(6) . ? C16 C17 1.539(5) . ? C16 H16A 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.518(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.381(5) . ? C21 C22 1.405(5) . ? C21 H21A 0.9300 . ? C22 C23 1.521(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C29 1.402(5) . ? C24 C25 1.411(5) . ? C25 C26 1.392(5) . ? C25 C30 1.532(6) . ? C26 C27 1.383(6) . ? C26 H26A 0.9300 . ? C27 C28 1.360(6) . ? C27 H27A 0.9300 . ? C28 C29 1.395(6) . ? C28 H28A 0.9300 . ? C29 C33 1.522(6) . ? C30 C32 1.510(6) . ? C30 C31 1.526(6) . ? C30 H30A 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.530(6) . ? C33 C35 1.546(6) . ? C33 H33A 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? 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 N1 Ta1 N2 99.09(13) . . ? N1 Ta1 C2 96.11(15) . . ? N2 Ta1 C2 112.57(14) . . ? N1 Ta1 C1 89.8(4) . . ? N2 Ta1 C1 129.6(4) . . ? C2 Ta1 C1 115.7(4) . . ? N1 Ta1 N3 172.17(12) . . ? N2 Ta1 N3 83.24(11) . . ? C2 Ta1 N3 89.84(14) . . ? C1 Ta1 N3 83.0(4) . . ? N1 Ta1 Cl1 90.7(7) . . ? N2 Ta1 Cl1 136.3(8) . . ? C2 Ta1 Cl1 108.4(8) . . ? C1 Ta1 Cl1 7.2(11) . . ? N3 Ta1 Cl1 82.5(7) . . ? C3 N1 Ta1 168.5(3) . . ? C20 N2 C7 115.5(3) . . ? C20 N2 Ta1 126.4(3) . . ? C7 N2 Ta1 117.5(2) . . ? C22 N3 C24 115.4(3) . . ? C22 N3 Ta1 121.6(3) . . ? C24 N3 Ta1 123.0(2) . . ? Ta1 C1 H1A 109.5 . . ? Ta1 C1 H1B 109.5 . . ? Ta1 C1 H1C 109.5 . . ? Ta1 C2 H2A 109.5 . . ? Ta1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Ta1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.3(3) . . ? N1 C3 C5 108.9(3) . . ? C4 C3 C5 109.6(4) . . ? N1 C3 C6 109.5(3) . . ? C4 C3 C6 109.4(4) . . ? C5 C3 C6 110.1(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 121.7(4) . . ? C12 C7 N2 120.0(3) . . ? C8 C7 N2 118.3(3) . . ? C9 C8 C7 117.8(4) . . ? C9 C8 C13 119.6(4) . . ? C7 C8 C13 122.6(4) . . ? C10 C9 C8 122.0(4) . . ? C10 C9 H9A 119.0 . . ? C8 C9 H9A 119.0 . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C10 C11 C12 121.8(4) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C7 C12 C11 117.3(4) . . ? C7 C12 C16 123.2(4) . . ? C11 C12 C16 119.5(4) . . ? C8 C13 C14 111.4(3) . . ? C8 C13 C15 111.6(4) . . ? C14 C13 C15 110.5(4) . . ? C8 C13 H13A 107.7 . . ? C14 C13 H13A 107.7 . . ? C15 C13 H13A 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C18 112.9(3) . . ? C12 C16 C17 111.5(3) . . ? C18 C16 C17 109.0(3) . . ? C12 C16 H16A 107.8 . . ? C18 C16 H16A 107.8 . . ? C17 C16 H16A 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C21 125.0(4) . . ? N2 C20 C19 118.9(3) . . ? C21 C20 C19 116.1(3) . . ? C20 C21 C22 129.3(4) . . ? C20 C21 H21A 115.3 . . ? C22 C21 H21A 115.3 . . ? N3 C22 C21 123.6(4) . . ? N3 C22 C23 121.6(4) . . ? C21 C22 C23 114.8(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 . . ? C29 C24 C25 121.0(4) . . ? C29 C24 N3 122.0(4) . . ? C25 C24 N3 117.0(3) . . ? C26 C25 C24 118.2(4) . . ? C26 C25 C30 120.0(4) . . ? C24 C25 C30 121.9(4) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 122.0(4) . . ? C27 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C28 C29 C24 117.8(4) . . ? C28 C29 C33 119.6(4) . . ? C24 C29 C33 122.6(4) . . ? C32 C30 C31 109.2(4) . . ? C32 C30 C25 111.6(4) . . ? C31 C30 C25 112.4(4) . . ? C32 C30 H30A 107.8 . . ? C31 C30 H30A 107.8 . . ? C25 C30 H30A 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C34 110.9(4) . . ? C29 C33 C35 110.9(4) . . ? C34 C33 C35 109.9(4) . . ? C29 C33 H33A 108.4 . . ? C34 C33 H33A 108.4 . . ? C35 C33 H33A 108.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 N2 Ta1 N1 C3 -161.2(13) . . . . ? C2 Ta1 N1 C3 84.8(13) . . . . ? C1 Ta1 N1 C3 -31.0(14) . . . . ? N3 Ta1 N1 C3 -54.5(19) . . . . ? Cl1 Ta1 N1 C3 -23.9(15) . . . . ? N1 Ta1 N2 C20 -160.8(3) . . . . ? C2 Ta1 N2 C20 -60.2(3) . . . . ? C1 Ta1 N2 C20 101.9(6) . . . . ? N3 Ta1 N2 C20 26.8(3) . . . . ? Cl1 Ta1 N2 C20 98.5(11) . . . . ? N1 Ta1 N2 C7 10.0(3) . . . . ? C2 Ta1 N2 C7 110.6(3) . . . . ? C1 Ta1 N2 C7 -87.3(6) . . . . ? N3 Ta1 N2 C7 -162.4(3) . . . . ? Cl1 Ta1 N2 C7 -90.7(11) . . . . ? N1 Ta1 N3 C22 -139.3(9) . . . . ? N2 Ta1 N3 C22 -31.6(3) . . . . ? C2 Ta1 N3 C22 81.1(3) . . . . ? C1 Ta1 N3 C22 -163.0(5) . . . . ? Cl1 Ta1 N3 C22 -170.2(8) . . . . ? N1 Ta1 N3 C24 39.9(10) . . . . ? N2 Ta1 N3 C24 147.6(3) . . . . ? C2 Ta1 N3 C24 -99.7(3) . . . . ? C1 Ta1 N3 C24 16.2(5) . . . . ? Cl1 Ta1 N3 C24 9.0(8) . . . . ? Ta1 N1 C3 C4 35.7(15) . . . . ? Ta1 N1 C3 C5 -84.0(14) . . . . ? Ta1 N1 C3 C6 155.5(12) . . . . ? C20 N2 C7 C12 78.3(5) . . . . ? Ta1 N2 C7 C12 -93.5(4) . . . . ? C20 N2 C7 C8 -101.4(4) . . . . ? Ta1 N2 C7 C8 86.8(4) . . . . ? C12 C7 C8 C9 0.0(6) . . . . ? N2 C7 C8 C9 179.7(3) . . . . ? C12 C7 C8 C13 180.0(4) . . . . ? N2 C7 C8 C13 -0.4(6) . . . . ? C7 C8 C9 C10 1.9(6) . . . . ? C13 C8 C9 C10 -178.1(4) . . . . ? C8 C9 C10 C11 -2.1(7) . . . . ? C9 C10 C11 C12 0.4(7) . . . . ? C8 C7 C12 C11 -1.5(6) . . . . ? N2 C7 C12 C11 178.8(3) . . . . ? C8 C7 C12 C16 178.0(4) . . . . ? N2 C7 C12 C16 -1.7(6) . . . . ? C10 C11 C12 C7 1.3(6) . . . . ? C10 C11 C12 C16 -178.3(4) . . . . ? C9 C8 C13 C14 64.3(5) . . . . ? C7 C8 C13 C14 -115.7(4) . . . . ? C9 C8 C13 C15 -59.8(5) . . . . ? C7 C8 C13 C15 120.3(4) . . . . ? C7 C12 C16 C18 -131.1(4) . . . . ? C11 C12 C16 C18 48.5(5) . . . . ? C7 C12 C16 C17 105.8(4) . . . . ? C11 C12 C16 C17 -74.6(5) . . . . ? C7 N2 C20 C21 178.5(3) . . . . ? Ta1 N2 C20 C21 -10.5(5) . . . . ? C7 N2 C20 C19 0.2(5) . . . . ? Ta1 N2 C20 C19 171.1(3) . . . . ? N2 C20 C21 C22 -18.2(7) . . . . ? C19 C20 C21 C22 160.1(4) . . . . ? C24 N3 C22 C21 -159.1(4) . . . . ? Ta1 N3 C22 C21 20.1(5) . . . . ? C24 N3 C22 C23 18.2(5) . . . . ? Ta1 N3 C22 C23 -162.5(3) . . . . ? C20 C21 C22 N3 10.8(7) . . . . ? C20 C21 C22 C23 -166.7(4) . . . . ? C22 N3 C24 C29 -93.8(5) . . . . ? Ta1 N3 C24 C29 86.9(4) . . . . ? C22 N3 C24 C25 87.5(4) . . . . ? Ta1 N3 C24 C25 -91.8(4) . . . . ? C29 C24 C25 C26 -1.2(6) . . . . ? N3 C24 C25 C26 177.5(4) . . . . ? C29 C24 C25 C30 178.8(4) . . . . ? N3 C24 C25 C30 -2.5(6) . . . . ? C24 C25 C26 C27 -0.9(6) . . . . ? C30 C25 C26 C27 179.1(4) . . . . ? C25 C26 C27 C28 1.4(7) . . . . ? C26 C27 C28 C29 0.3(7) . . . . ? C27 C28 C29 C24 -2.4(6) . . . . ? C27 C28 C29 C33 178.1(4) . . . . ? C25 C24 C29 C28 2.8(6) . . . . ? N3 C24 C29 C28 -175.8(4) . . . . ? C25 C24 C29 C33 -177.6(4) . . . . ? N3 C24 C29 C33 3.7(6) . . . . ? C26 C25 C30 C32 80.3(5) . . . . ? C24 C25 C30 C32 -99.8(5) . . . . ? C26 C25 C30 C31 -42.8(5) . . . . ? C24 C25 C30 C31 137.1(4) . . . . ? C28 C29 C33 C34 66.7(5) . . . . ? C24 C29 C33 C34 -112.9(4) . . . . ? C28 C29 C33 C35 -55.7(5) . . . . ? C24 C29 C33 C35 124.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.406 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.134