# Electronic 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 _publ_contact_author 'Patricia Horrillo-Martinez' _publ_contact_author_email horrillo@chem.ubc.ca _publ_section_title ; Oxygen Extrusion from Amidate Ligands to Generate Terminal Ta=O Units Under Reducing Conditions. How to Successfully Use Amidate Ligands in Dinitrogen Coordination Chemistry ; _publ_contact_author_name 'Patricia Horrillo-Martinez' loop_ _publ_author_name P.Horrillo-Martinez B.Patrick L.Schafer M.Fryzuk #END data_twin4 #TrackingRef '- 3a_mf768_twin4_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trichlorido(eta5-pentamethylcyclopendienyl)(eta3-N-isopropyl(tert-butyl)amidate) tantalum ; _chemical_name_common ; Trichlorido(eta5-pentamethylcyclopendienyl)(eta3-N- isopropyl(tert-butyl)amidate) tantalum ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H31 Cl3 N O Ta' _chemical_formula_sum 'C18 H31 Cl3 N O Ta' _chemical_formula_weight 564.74 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0873(6) _cell_length_b 20.5258(11) _cell_length_c 10.5215(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.685(2) _cell_angle_gamma 90.00 _cell_volume 2163.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6258 _cell_measurement_theta_min 2.187 _cell_measurement_theta_max 27.427 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 5.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.548 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; Crystals are non-merohedrally twinned. Both twin domains are related by a 180o rotation about the (1 0 1) crystal axis.Data were integrated for both twin components, including both overlapped and non-overlapped reflections. In total 34875 reflections were integrated (15898 from component one only, 15745 from component two only, 3232 overlapped). The linear absorption coefficient, mu, for Mo-Kalpha radiation is 54.56 cm-1. Data were corrected for absorption effects using the multi-scan technique (TWINABS) (Bruker Nonius scaling and absorption for twinned crystals - V2008/2, Bruker AXS Inc., Madison, Wisconsin, USA (2007)), with minimum and maximum transmission coefficients of 0.419 and 0.549, respectively. The data were corrected for Lorentz and polarization effects.The structure was solved by direct methods (SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119) using non-over lapped data from the major twin component. Subsequent refinements were carried out using an HKLF 5 format data set containing complete data from both component 1 and component 2. The material crystallizes disordered about a pseudo-mirror plane passing through the Ta atom. The batch scale refinement showed a roughly 59:41 ratio between the major and minor twin components. The final cycle of full-matrix least-squares refinement on F2 was based on 9240 reflections and 434 variable parameters and converged (largest parameter shift was 0.00 times its esd) with unweighted and weighted agreement factors of: R1 = sum ||Fo| - |Fc|| / sum |Fo| = 0.044 wR2 = [ sum ( w (Fo2 - Fc2)2 )/ sum w(Fo2)2]1/2 = 0.068 The standard deviation of an observation of unit weight was 1.12. The weighting scheme was based on counting statistics. The maximum and minimum peaks on the final difference Fourier map corresponded to 1.42 and - 1.71 e /\%A3, respectively. Neutral atom scattering factors were taken from Cromer and Waber (Cromer, D. T. & Waber, J. T.; "International Tables for X-ray Crystallography", Vol. IV, The Kynoch Press, Birmingham, England, Table 2.2 A (1974)). Anomalous dispersion effects were included in Fcalc;(Ibers, J. A. & Hamilton, W. C.; Acta Crystallogr., 17, 781 (1964)) the values for deltaf' and deltaf" were those of Creagh and McAuley. (Creagh, D. C. & McAuley, W.J .; "International Tables for Crystallography", Vol C, (A.J.C. Wilson, ed.), Kluwer Academic Publishers, Boston, Table 4.2.6.8, pages 219-222 (1992)). The values for the mass attenuation coefficients are those of Creagh and Hubbell (Creagh, D. C. & Hubbell, J.H..; "International Tables for Crystallography", Vol C, (A.J.C. Wilson, ed.), Kluwer Academic Publishers, Boston, Table 4.2.4.3, pages 200-206 (1992)). All refinements were performed using the SHELXTL crystallographic software package of Bruker-AXS (SHELXTL Version 5.1. Bruker AXS Inc., Madision, Wisconsin, USA. (1997)). ; _diffrn_ambient_temperature 100(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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9240 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9240 _reflns_number_gt 7565 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; SYMM 1/2 - X, 1/2 + Y, 1/2 - Z EADP C2A C2B EADP C3A C3B 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^ > 2\s(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^)+(0.0070P)^2^+5.7358P] 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 9240 _refine_ls_number_parameters 434 _refine_ls_number_restraints 690 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0630 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.152 _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 0.738152(14) 0.086030(7) 0.262583(13) 0.01213(4) Uani 1 1 d U . . C1A C 0.6808(8) -0.0288(4) 0.2320(7) 0.0179(16) Uani 0.50 1 d PU A 1 C2A C 0.557(2) 0.0123(11) 0.2041(16) 0.0141(18) Uani 0.50 1 d PU A 1 C3A C 0.5660(7) 0.0486(4) 0.1030(7) 0.0118(11) Uani 0.50 1 d PU A 1 C4A C 0.6889(7) 0.0346(4) 0.0520(7) 0.0162(17) Uani 0.50 1 d PU A 1 C5A C 0.7564(8) -0.0133(4) 0.1321(8) 0.0186(17) Uani 0.50 1 d PU A 1 C6A C 0.7057(12) -0.0838(7) 0.3210(12) 0.024(3) Uani 0.50 1 d PU A 1 H6A1 H 0.6703 -0.1239 0.2794 0.036 Uiso 0.50 1 calc PR A 1 H6A2 H 0.6615 -0.0757 0.3977 0.036 Uiso 0.50 1 calc PR A 1 H6A3 H 0.8020 -0.0885 0.3454 0.036 Uiso 0.50 1 calc PR A 1 C7A C 0.4472(8) 0.0039(5) 0.2901(8) 0.0240(19) Uani 0.50 1 d PU A 1 H7A1 H 0.4020 0.0457 0.2984 0.036 Uiso 0.50 1 calc PR A 1 H7A2 H 0.4861 -0.0110 0.3748 0.036 Uiso 0.50 1 calc PR A 1 H7A3 H 0.3826 -0.0284 0.2524 0.036 Uiso 0.50 1 calc PR A 1 C8A C 0.4540(7) 0.0920(4) 0.0483(7) 0.0207(17) Uani 0.50 1 d PU A 1 H8A1 H 0.3749 0.0655 0.0213 0.031 Uiso 0.50 1 calc PR A 1 H8A2 H 0.4807 0.1156 -0.0257 0.031 Uiso 0.50 1 calc PR A 1 H8A3 H 0.4332 0.1233 0.1135 0.031 Uiso 0.50 1 calc PR A 1 C9A C 0.7335(8) 0.0600(4) -0.0690(7) 0.0219(18) Uani 0.50 1 d PU A 1 H9A1 H 0.8219 0.0800 -0.0504 0.033 Uiso 0.50 1 calc PR A 1 H9A2 H 0.6697 0.0926 -0.1067 0.033 Uiso 0.50 1 calc PR A 1 H9A3 H 0.7384 0.0239 -0.1295 0.033 Uiso 0.50 1 calc PR A 1 C10A C 0.8833(8) -0.0468(4) 0.1039(8) 0.0255(18) Uani 0.50 1 d PU A 1 H10A H 0.9113 -0.0781 0.1721 0.038 Uiso 0.50 1 calc PR A 1 H10B H 0.9537 -0.0142 0.0995 0.038 Uiso 0.50 1 calc PR A 1 H10C H 0.8672 -0.0698 0.0219 0.038 Uiso 0.50 1 calc PR A 1 C11A C 0.6481(7) 0.1766(4) 0.4011(7) 0.0156(15) Uani 0.50 1 d PU A 1 C12A C 0.5666(7) 0.2215(4) 0.4775(7) 0.0167(15) Uani 0.50 1 d PU A 1 C13A C 0.6099(9) 0.2074(5) 0.6216(8) 0.027(2) Uani 0.50 1 d PU A 1 H13A H 0.5596 0.2356 0.6739 0.040 Uiso 0.50 1 calc PR A 1 H13B H 0.7055 0.2161 0.6417 0.040 Uiso 0.50 1 calc PR A 1 H13C H 0.5917 0.1617 0.6401 0.040 Uiso 0.50 1 calc PR A 1 C14A C 0.5885(9) 0.2941(4) 0.4471(8) 0.0277(19) Uani 0.50 1 d PU A 1 H14A H 0.5764 0.3006 0.3542 0.042 Uiso 0.50 1 calc PR A 1 H14B H 0.6792 0.3069 0.4814 0.042 Uiso 0.50 1 calc PR A 1 H14C H 0.5238 0.3207 0.4865 0.042 Uiso 0.50 1 calc PR A 1 C15A C 0.4193(9) 0.2066(5) 0.4462(10) 0.028(2) Uani 0.50 1 d PU A 1 H15A H 0.3909 0.2171 0.3563 0.041 Uiso 0.50 1 calc PR A 1 H15B H 0.3680 0.2327 0.5012 0.041 Uiso 0.50 1 calc PR A 1 H15C H 0.4037 0.1602 0.4610 0.041 Uiso 0.50 1 calc PR A 1 C16A C 0.8799(7) 0.2163(4) 0.4555(7) 0.0143(15) Uani 0.50 1 d PU A 1 H16A H 0.8379 0.2493 0.5081 0.017 Uiso 0.50 1 calc PR A 1 C17A C 0.9761(9) 0.1746(4) 0.5445(8) 0.026(2) Uani 0.50 1 d PU A 1 H17A H 0.9259 0.1506 0.6038 0.040 Uiso 0.50 1 calc PR A 1 H17B H 1.0420 0.2028 0.5932 0.040 Uiso 0.50 1 calc PR A 1 H17C H 1.0218 0.1437 0.4936 0.040 Uiso 0.50 1 calc PR A 1 C18A C 0.9490(7) 0.2514(4) 0.3562(7) 0.0207(17) Uani 0.50 1 d PU A 1 H18A H 0.9819 0.2196 0.2979 0.031 Uiso 0.50 1 calc PR A 1 H18B H 1.0242 0.2765 0.3985 0.031 Uiso 0.50 1 calc PR A 1 H18C H 0.8858 0.2810 0.3076 0.031 Uiso 0.50 1 calc PR A 1 N1A N 0.7752(7) 0.1741(3) 0.3929(6) 0.0147(14) Uani 0.50 1 d PU A 1 O1A O 0.5827(6) 0.1311(3) 0.3311(6) 0.0154(12) Uani 0.50 1 d PU A 1 Cl1A Cl 0.7296(2) 0.17893(10) 0.11573(17) 0.0173(4) Uani 0.50 1 d PU B 1 Cl2A Cl 0.97523(17) 0.08475(12) 0.24628(19) 0.0231(4) Uani 0.50 1 d PU A 1 Cl3A Cl 0.7880(3) 0.03876(13) 0.4707(2) 0.0256(6) Uani 0.50 1 d PU A 1 C1B C 0.8161(8) -0.0259(4) 0.3333(7) 0.0159(16) Uani 0.50 1 d PU A 2 C2B C 0.7920(10) 0.0115(5) 0.4400(8) 0.0141(18) Uani 0.50 1 d PU A 2 C3B C 0.8902(7) 0.0641(4) 0.4529(7) 0.0118(11) Uani 0.50 1 d PU A 2 C4B C 0.9691(8) 0.0572(4) 0.3482(7) 0.0202(17) Uani 0.50 1 d PU A 2 C5B C 0.9217(7) 0.0020(4) 0.2759(7) 0.0175(18) Uani 0.50 1 d PU A 2 C6B C 0.7502(11) -0.0902(7) 0.2946(12) 0.025(3) Uani 0.50 1 d PU A 2 H6B1 H 0.7417 -0.0945 0.2013 0.038 Uiso 0.50 1 calc PR A 2 H6B2 H 0.6614 -0.0917 0.3237 0.038 Uiso 0.50 1 calc PR A 2 H6B3 H 0.8047 -0.1260 0.3339 0.038 Uiso 0.50 1 calc PR A 2 C7B C 0.7001(8) -0.0029(4) 0.5372(7) 0.0207(18) Uani 0.50 1 d PU A 2 H7B1 H 0.6254 -0.0295 0.4982 0.031 Uiso 0.50 1 calc PR A 2 H7B2 H 0.6658 0.0380 0.5686 0.031 Uiso 0.50 1 calc PR A 2 H7B3 H 0.7484 -0.0268 0.6088 0.031 Uiso 0.50 1 calc PR A 2 C8B C 0.9068(8) 0.1114(4) 0.5603(8) 0.0240(19) Uani 0.50 1 d PU A 2 H8B1 H 0.9705 0.1452 0.5422 0.036 Uiso 0.50 1 calc PR A 2 H8B2 H 0.9403 0.0887 0.6395 0.036 Uiso 0.50 1 calc PR A 2 H8B3 H 0.8205 0.1315 0.5702 0.036 Uiso 0.50 1 calc PR A 2 C9B C 1.0923(7) 0.0954(5) 0.3301(8) 0.028(2) Uani 0.50 1 d PU A 2 H9B1 H 1.1714 0.0686 0.3557 0.042 Uiso 0.50 1 calc PR A 2 H9B2 H 1.0956 0.1348 0.3829 0.042 Uiso 0.50 1 calc PR A 2 H9B3 H 1.0904 0.1076 0.2398 0.042 Uiso 0.50 1 calc PR A 2 C10B C 0.9873(9) -0.0261(4) 0.1691(7) 0.027(2) Uani 0.50 1 d PU A 2 H10D H 1.0522 -0.0592 0.2028 0.041 Uiso 0.50 1 calc PR A 2 H10E H 1.0331 0.0085 0.1272 0.041 Uiso 0.50 1 calc PR A 2 H10F H 0.9197 -0.0463 0.1069 0.041 Uiso 0.50 1 calc PR A 2 C11B C 0.5591(8) 0.1654(5) 0.3251(8) 0.0142(17) Uani 0.50 1 d PU A 2 C12B C 0.4699(9) 0.2117(4) 0.3929(8) 0.0166(17) Uani 0.50 1 d PU A 2 C13B C 0.3241(8) 0.1974(5) 0.3517(10) 0.032(2) Uani 0.50 1 d PU A 2 H13D H 0.3052 0.1518 0.3705 0.047 Uiso 0.50 1 calc PR A 2 H13E H 0.3040 0.2053 0.2596 0.047 Uiso 0.50 1 calc PR A 2 H13F H 0.2686 0.2259 0.3984 0.047 Uiso 0.50 1 calc PR A 2 C14B C 0.5038(9) 0.2830(4) 0.3624(8) 0.028(2) Uani 0.50 1 d PU A 2 H14D H 0.4822 0.2909 0.2705 0.042 Uiso 0.50 1 calc PR A 2 H14E H 0.5992 0.2907 0.3871 0.042 Uiso 0.50 1 calc PR A 2 H14F H 0.4516 0.3125 0.4104 0.042 Uiso 0.50 1 calc PR A 2 C15B C 0.5013(10) 0.2028(4) 0.5379(8) 0.032(2) Uani 0.50 1 d PU A 2 H15D H 0.4405 0.2297 0.5818 0.048 Uiso 0.50 1 calc PR A 2 H15E H 0.5936 0.2161 0.5648 0.048 Uiso 0.50 1 calc PR A 2 H15F H 0.4898 0.1569 0.5599 0.048 Uiso 0.50 1 calc PR A 2 C16B C 0.5003(7) 0.1894(4) 0.0972(7) 0.0167(16) Uani 0.50 1 d PU A 2 H16B H 0.4391 0.2224 0.1291 0.020 Uiso 0.50 1 calc PR A 2 C17B C 0.4156(9) 0.1402(4) 0.0171(8) 0.028(2) Uani 0.50 1 d PU A 2 H17D H 0.4731 0.1061 -0.0120 0.042 Uiso 0.50 1 calc PR A 2 H17E H 0.3674 0.1620 -0.0572 0.042 Uiso 0.50 1 calc PR A 2 H17F H 0.3514 0.1205 0.0688 0.042 Uiso 0.50 1 calc PR A 2 C18B C 0.5939(8) 0.2245(4) 0.0209(7) 0.0223(18) Uani 0.50 1 d PU A 2 H18D H 0.6367 0.2603 0.0719 0.033 Uiso 0.50 1 calc PR A 2 H18E H 0.5442 0.2420 -0.0572 0.033 Uiso 0.50 1 calc PR A 2 H18F H 0.6624 0.1942 -0.0019 0.033 Uiso 0.50 1 calc PR A 2 N2B N 0.5732(6) 0.1565(3) 0.2099(6) 0.0152(14) Uani 0.50 1 d PU A 2 O1B O 0.6428(5) 0.1288(3) 0.4017(5) 0.0149(10) Uani 0.50 1 d PU A 2 Cl1B Cl 0.7603(2) 0.06873(10) 0.04256(17) 0.0215(5) Uani 0.50 1 d PU A 2 Cl2B Cl 0.85412(19) 0.18642(10) 0.25261(19) 0.0217(4) Uani 0.50 1 d PU A 2 Cl3B Cl 0.5381(4) 0.0175(3) 0.2313(3) 0.0186(9) Uani 0.50 1 d PU C 2 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 0.01203(6) 0.01331(7) 0.01092(6) 0.00096(7) 0.00086(4) 0.00177(7) C1A 0.024(4) 0.012(4) 0.018(4) 0.000(3) 0.004(3) -0.007(3) C2A 0.025(4) 0.013(4) 0.006(4) -0.001(3) 0.005(3) -0.008(3) C3A 0.013(2) 0.010(3) 0.010(2) 0.0022(19) -0.0075(19) 0.000(2) C4A 0.010(3) 0.021(5) 0.019(4) -0.003(3) 0.008(3) -0.008(3) C5A 0.018(4) 0.008(4) 0.030(4) -0.005(3) 0.001(3) -0.005(3) C6A 0.029(7) 0.020(5) 0.024(5) 0.002(5) 0.002(4) 0.006(5) C7A 0.020(4) 0.026(5) 0.027(4) -0.002(4) 0.005(4) -0.008(4) C8A 0.022(4) 0.017(5) 0.022(4) -0.003(4) -0.002(3) -0.002(4) C9A 0.019(4) 0.023(5) 0.023(4) 0.004(3) 0.001(3) -0.009(3) C10A 0.018(4) 0.023(5) 0.035(5) -0.009(4) 0.004(4) -0.002(3) C11A 0.015(4) 0.016(4) 0.017(4) 0.006(3) 0.007(3) 0.001(3) C12A 0.017(4) 0.015(4) 0.018(4) 0.002(3) 0.005(3) 0.005(3) C13A 0.031(5) 0.031(6) 0.018(4) 0.002(4) 0.003(4) 0.011(4) C14A 0.036(5) 0.020(4) 0.030(5) -0.001(4) 0.011(4) 0.001(4) C15A 0.018(5) 0.025(6) 0.041(6) -0.002(4) 0.009(5) 0.006(4) C16A 0.011(3) 0.010(4) 0.021(4) -0.007(3) -0.001(3) 0.000(3) C17A 0.032(5) 0.022(5) 0.023(4) -0.002(3) -0.011(4) -0.008(4) C18A 0.016(3) 0.021(5) 0.024(4) -0.008(3) -0.003(3) 0.004(3) N1A 0.017(3) 0.016(4) 0.011(3) 0.001(3) 0.000(3) 0.001(3) O1A 0.016(3) 0.015(4) 0.015(3) 0.001(3) 0.003(3) 0.004(3) Cl1A 0.0240(10) 0.0148(10) 0.0117(8) 0.0047(7) -0.0032(8) -0.0047(8) Cl2A 0.0126(7) 0.0241(11) 0.0324(10) -0.0076(10) 0.0012(8) 0.0006(9) Cl3A 0.0376(13) 0.0179(14) 0.0188(12) 0.0046(10) -0.0073(11) -0.0021(12) C1B 0.020(4) 0.007(4) 0.018(4) -0.001(3) -0.006(3) 0.003(3) C2B 0.025(4) 0.013(4) 0.006(4) -0.001(3) 0.005(3) -0.008(3) C3B 0.013(2) 0.010(3) 0.010(2) 0.0022(19) -0.0075(19) 0.000(2) C4B 0.015(4) 0.028(5) 0.018(4) 0.001(3) 0.007(3) 0.005(3) C5B 0.012(3) 0.027(5) 0.013(3) 0.005(3) 0.002(3) 0.012(3) C6B 0.026(7) 0.018(5) 0.029(6) -0.011(5) -0.009(5) 0.001(5) C7B 0.019(4) 0.028(5) 0.015(4) 0.004(3) 0.005(3) -0.001(3) C8B 0.025(4) 0.022(5) 0.023(4) -0.004(3) -0.002(4) 0.003(3) C9B 0.013(3) 0.038(6) 0.034(4) 0.018(4) 0.005(3) 0.007(4) C10B 0.038(5) 0.031(5) 0.014(4) 0.008(3) 0.003(4) 0.019(4) C11B 0.011(4) 0.009(4) 0.024(4) 0.005(4) 0.010(3) 0.002(3) C12B 0.018(4) 0.012(4) 0.020(4) -0.002(3) 0.004(4) 0.004(3) C13B 0.022(4) 0.027(6) 0.048(6) 0.000(4) 0.013(4) 0.005(4) C14B 0.028(4) 0.024(5) 0.032(5) -0.005(4) 0.007(4) 0.002(4) C15B 0.046(6) 0.028(5) 0.024(5) -0.005(4) 0.007(5) 0.019(4) C16B 0.017(3) 0.009(4) 0.023(4) -0.003(3) -0.004(3) 0.005(3) C17B 0.031(5) 0.023(5) 0.026(4) 0.002(4) -0.010(4) 0.002(4) C18B 0.024(4) 0.023(5) 0.019(4) -0.001(3) -0.002(4) 0.010(3) N2B 0.013(3) 0.018(4) 0.015(3) 0.001(3) 0.002(3) 0.004(3) O1B 0.019(3) 0.011(3) 0.016(3) 0.001(2) 0.005(2) 0.004(2) Cl1B 0.0269(10) 0.0265(13) 0.0111(8) 0.0015(7) 0.0025(8) 0.0093(9) Cl2B 0.0175(8) 0.0165(10) 0.0308(10) 0.0071(8) 0.0012(8) -0.0018(8) Cl3B 0.0184(16) 0.0202(15) 0.0168(18) -0.0011(14) 0.0003(13) -0.0069(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1A 2.025(6) . ? Ta1 O1B 2.042(5) . ? Ta1 N2B 2.226(6) . ? Ta1 N1A 2.274(7) . ? Ta1 Cl2B 2.3778(19) . ? Ta1 Cl1B 2.3782(19) . ? Ta1 Cl3B 2.4512(19) . ? Ta1 Cl3A 2.394(2) . ? Ta1 Cl1A 2.449(19) . ? Ta1 C2A 2.39(2) . ? Ta1 C3A 2.397(7) . ? Ta1 Cl2A 2.4176(18) . ? Ta1 C3B 2.419(6) . ? Ta1 C2B 2.426(10) . ? C1A C5A 1.406(11) . ? C1A C6A 1.470(16) . ? C1A C2A 1.51(2) . ? C2A C3A 1.31(2) . ? C2A C7A 1.52(2) . ? C3A C4A 1.436(11) . ? C3A C8A 1.500(10) . ? C4A C5A 1.417(11) . ? C4A C9A 1.493(11) . ? C5A C10A 1.512(10) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A N1A 1.296(10) . ? C11A O1A 1.318(10) . ? C11A C12A 1.523(10) . ? C12A C15A 1.516(11) . ? C12A C14A 1.545(11) . ? C12A C13A 1.556(10) . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A N1A 1.462(9) . ? C16A C18A 1.505(11) . ? C16A C17A 1.529(11) . ? C16A H16A 1.0000 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C1B C2B 1.404(12) . ? C1B C5B 1.407(11) . ? C1B C6B 1.512(16) . ? C2B C3B 1.462(12) . ? C2B C7B 1.488(12) . ? C3B C4B 1.439(11) . ? C3B C8B 1.485(11) . ? C4B C5B 1.415(12) . ? C4B C9B 1.500(11) . ? C5B C10B 1.486(11) . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B N2B 1.250(11) . ? C11B O1B 1.329(10) . ? C11B C12B 1.541(12) . ? C12B C13B 1.513(11) . ? C12B C15B 1.533(11) . ? C12B C14B 1.544(12) . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B N2B 1.483(9) . ? C16B C18B 1.493(12) . ? C16B C17B 1.515(11) . ? C16B H16B 1.0000 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 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 O1A Ta1 O1B 25.70(19) . . ? O1A Ta1 N2B 37.2(2) . . ? O1B Ta1 N2B 59.9(2) . . ? O1A Ta1 N1A 60.1(2) . . ? O1B Ta1 N1A 44.2(2) . . ? N2B Ta1 N1A 72.5(2) . . ? O1A Ta1 Cl2B 91.43(18) . . ? O1B Ta1 Cl2B 86.23(16) . . ? N2B Ta1 Cl2B 77.49(18) . . ? N1A Ta1 Cl2B 44.79(18) . . ? O1A Ta1 Cl1B 125.40(19) . . ? O1B Ta1 Cl1B 150.21(17) . . ? N2B Ta1 Cl1B 90.40(17) . . ? N1A Ta1 Cl1B 132.70(18) . . ? Cl2B Ta1 Cl1B 89.08(7) . . ? O1A Ta1 Cl3A 87.1(2) . . ? O1B Ta1 Cl3A 65.46(17) . . ? N2B Ta1 Cl3A 124.23(18) . . ? N1A Ta1 Cl3A 76.61(18) . . ? Cl2B Ta1 Cl3A 109.85(8) . . ? Cl1B Ta1 Cl3A 142.77(9) . . ? O1A Ta1 C2A 77.4(5) . . ? O1B Ta1 C2A 92.7(4) . . ? N2B Ta1 C2A 79.7(5) . . ? N1A Ta1 C2A 136.4(5) . . ? Cl2B Ta1 C2A 154.2(5) . . ? Cl1B Ta1 C2A 79.1(4) . . ? Cl3A Ta1 C2A 92.9(5) . . ? O1A Ta1 C3A 82.4(3) . . ? O1B Ta1 C3A 106.1(3) . . ? N2B Ta1 C3A 64.8(2) . . ? N1A Ta1 C3A 137.1(2) . . ? Cl2B Ta1 C3A 124.53(18) . . ? Cl1B Ta1 C3A 54.05(19) . . ? Cl3A Ta1 C3A 124.66(19) . . ? C2A Ta1 C3A 31.7(5) . . ? O1A Ta1 Cl2A 147.56(18) . . ? O1B Ta1 Cl2A 127.46(18) . . ? N2B Ta1 Cl2A 134.96(18) . . ? N1A Ta1 Cl2A 87.52(18) . . ? Cl2B Ta1 Cl2A 60.69(7) . . ? Cl1B Ta1 Cl2A 73.94(7) . . ? Cl3A Ta1 Cl2A 87.49(8) . . ? C2A Ta1 Cl2A 134.8(5) . . ? C3A Ta1 Cl2A 126.07(19) . . ? O1A Ta1 C3B 103.5(3) . . ? O1B Ta1 C3B 78.0(2) . . ? N2B Ta1 C3B 135.3(2) . . ? N1A Ta1 C3B 66.7(2) . . ? Cl2B Ta1 C3B 85.98(18) . . ? Cl1B Ta1 C3B 130.97(19) . . ? Cl3A Ta1 C3B 28.60(19) . . ? C2A Ta1 C3B 119.1(5) . . ? C3A Ta1 C3B 149.1(2) . . ? Cl2A Ta1 C3B 61.28(19) . . ? O1A Ta1 C2B 97.3(3) . . ? O1B Ta1 C2B 78.5(3) . . ? N2B Ta1 C2B 134.1(3) . . ? N1A Ta1 C2B 91.8(3) . . ? Cl2B Ta1 C2B 120.9(2) . . ? Cl1B Ta1 C2B 128.1(2) . . ? Cl3A Ta1 C2B 15.5(2) . . ? C2A Ta1 C2B 83.9(5) . . ? C3A Ta1 C2B 114.6(3) . . ? Cl2A Ta1 C2B 85.0(2) . . ? C3B Ta1 C2B 35.1(3) . . ? C5A C1A C6A 125.7(8) . . ? C5A C1A C2A 103.7(9) . . ? C6A C1A C2A 129.2(11) . . ? C5A C1A Ta1 74.8(4) . . ? C6A C1A Ta1 129.6(7) . . ? C2A C1A Ta1 70.2(9) . . ? C3A C2A C1A 110.2(14) . . ? C3A C2A C7A 132.0(17) . . ? C1A C2A C7A 117.7(15) . . ? C3A C2A Ta1 74.2(11) . . ? C1A C2A Ta1 73.5(9) . . ? C7A C2A Ta1 120.4(10) . . ? C2A C3A C4A 109.4(11) . . ? C2A C3A C8A 122.1(11) . . ? C4A C3A C8A 128.3(7) . . ? C2A C3A Ta1 74.0(10) . . ? C4A C3A Ta1 74.9(4) . . ? C8A C3A Ta1 122.0(5) . . ? C5A C4A C3A 107.1(7) . . ? C5A C4A C9A 125.2(7) . . ? C3A C4A C9A 127.5(7) . . ? C5A C4A Ta1 74.3(4) . . ? C3A C4A Ta1 70.7(4) . . ? C9A C4A Ta1 124.8(6) . . ? C1A C5A C4A 109.7(7) . . ? C1A C5A C10A 126.1(8) . . ? C4A C5A C10A 124.0(8) . . ? C1A C5A Ta1 71.9(4) . . ? C4A C5A Ta1 72.3(5) . . ? C10A C5A Ta1 127.0(5) . . ? N1A C11A O1A 111.7(7) . . ? N1A C11A C12A 131.1(7) . . ? O1A C11A C12A 117.2(6) . . ? N1A C11A Ta1 61.3(4) . . ? O1A C11A Ta1 50.4(4) . . ? C12A C11A Ta1 167.4(5) . . ? C15A C12A C11A 109.8(7) . . ? C15A C12A C14A 108.0(7) . . ? C11A C12A C14A 112.0(6) . . ? C15A C12A C13A 109.3(7) . . ? C11A C12A C13A 107.2(6) . . ? C14A C12A C13A 110.5(7) . . ? N1A C16A C18A 109.8(6) . . ? N1A C16A C17A 108.5(7) . . ? C18A C16A C17A 112.4(6) . . ? N1A C16A H16A 108.7 . . ? C18A C16A H16A 108.7 . . ? C17A C16A H16A 108.7 . . ? C11A N1A C16A 127.9(7) . . ? C11A N1A Ta1 88.7(5) . . ? C16A N1A Ta1 143.4(5) . . ? C11A O1A Ta1 99.5(5) . . ? C2B C1B C5B 109.3(7) . . ? C2B C1B C6B 125.4(8) . . ? C5B C1B C6B 124.9(8) . . ? C2B C1B Ta1 70.1(5) . . ? C5B C1B Ta1 74.1(5) . . ? C6B C1B Ta1 127.3(6) . . ? C1B C2B C3B 107.4(8) . . ? C1B C2B C7B 128.4(9) . . ? C3B C2B C7B 123.6(8) . . ? C1B C2B Ta1 76.9(5) . . ? C3B C2B Ta1 72.2(5) . . ? C7B C2B Ta1 123.5(6) . . ? C4B C3B C2B 106.6(7) . . ? C4B C3B C8B 128.6(7) . . ? C2B C3B C8B 124.7(7) . . ? C4B C3B Ta1 74.8(4) . . ? C2B C3B Ta1 72.7(4) . . ? C8B C3B Ta1 120.8(5) . . ? C5B C4B C3B 108.0(7) . . ? C5B C4B C9B 125.6(8) . . ? C3B C4B C9B 125.8(8) . . ? C5B C4B Ta1 75.6(4) . . ? C3B C4B Ta1 71.0(4) . . ? C9B C4B Ta1 126.1(6) . . ? C1B C5B C4B 108.7(7) . . ? C1B C5B C10B 126.3(8) . . ? C4B C5B C10B 124.4(8) . . ? C1B C5B Ta1 73.4(4) . . ? C4B C5B Ta1 71.5(5) . . ? C10B C5B Ta1 127.8(5) . . ? C1B C6B H6B1 109.5 . . ? C1B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C1B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2B C7B H7B1 109.5 . . ? C2B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C2B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C3B C8B H8B1 109.5 . . ? C3B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C3B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C4B C9B H9B1 109.5 . . ? C4B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C4B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C5B C10B H10D 109.5 . . ? C5B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C5B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? N2B C11B O1B 111.7(8) . . ? N2B C11B C12B 132.6(8) . . ? O1B C11B C12B 115.6(7) . . ? N2B C11B Ta1 59.9(5) . . ? O1B C11B Ta1 51.9(4) . . ? C12B C11B Ta1 167.0(6) . . ? C13B C12B C15B 110.1(9) . . ? C13B C12B C11B 110.4(7) . . ? C15B C12B C11B 108.8(7) . . ? C13B C12B C14B 110.9(7) . . ? C15B C12B C14B 107.1(7) . . ? C11B C12B C14B 109.5(8) . . ? C12B C13B H13D 109.5 . . ? C12B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C12B C15B H15D 109.5 . . ? C12B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C12B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N2B C16B C18B 111.3(6) . . ? N2B C16B C17B 109.6(7) . . ? C18B C16B C17B 111.9(7) . . ? N2B C16B H16B 107.9 . . ? C18B C16B H16B 107.9 . . ? C17B C16B H16B 107.9 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C16B C18B H18D 109.5 . . ? C16B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C16B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C11B N2B C16B 127.4(7) . . ? C11B N2B Ta1 91.1(5) . . ? C16B N2B Ta1 141.4(5) . . ? C11B O1B Ta1 97.3(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.344 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.165 #END data_ls219_0m #TrackingRef '- 3b_ls219_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trichlorido(eta5-pentamethylcyclopendienyl) (eta3-N-2,6-dimethylphenyl(tert-butyl)amidate)tantalum ; _chemical_name_common ; Trichlorido(eta5-pentamethylcyclopendienyl) (eta3-N-2,6- dimethylphenyl(tert-butyl)amidate)tantalum ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H33 Cl3 N O Ta' _chemical_formula_sum 'C23 H33 Cl3 N O Ta' _chemical_formula_weight 626.80 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.665(2) _cell_length_b 15.049(3) _cell_length_c 28.516(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.859(10) _cell_angle_gamma 90.00 _cell_volume 4916.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 9761 _cell_measurement_theta_min 2.476 _cell_measurement_theta_max 29.967 _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 4.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.152 _exptl_absorpt_correction_T_max 0.236 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 87918 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.04 _reflns_number_total 14191 _reflns_number_gt 12220 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The four largest residual electron density peaks are found adjacent (within 0.80 A) to the two Ta atoms. C4 has very low thermal parameters when anisotropic ISOR 0.20 0.40 C4 SIMU C3 C4 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^ > 2\s(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^)+(0.0000P)^2^+164.1585P] 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 14191 _refine_ls_number_parameters 542 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_restrained_S_all 1.267 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1796(7) 0.3776(6) 0.6181(3) 0.0128(16) Uani 1 1 d . . . C2 C 0.8405(8) 0.2510(6) 0.8993(3) 0.0162(17) Uani 1 1 d . . . C3 C 0.1963(8) 0.4771(6) 0.6128(3) 0.0159(17) Uani 1 1 d U . . C4 C 0.2845(9) 0.5045(6) 0.6578(4) 0.022(2) Uani 1 1 d U . . H4A H 0.2534 0.4887 0.6863 0.033 Uiso 1 1 calc R . . H4B H 0.2975 0.5688 0.6573 0.033 Uiso 1 1 calc R . . H4C H 0.3585 0.4734 0.6584 0.033 Uiso 1 1 calc R . . C5 C 0.2499(9) 0.4976(6) 0.5686(4) 0.0199(19) Uani 1 1 d . . . H5A H 0.3219 0.4633 0.5702 0.030 Uiso 1 1 calc R . . H5B H 0.2675 0.5612 0.5678 0.030 Uiso 1 1 calc R . . H5C H 0.1943 0.4813 0.5396 0.030 Uiso 1 1 calc R . . C6 C 0.0833(8) 0.5315(6) 0.6115(4) 0.0195(18) Uani 1 1 d . . . H6A H 0.0269 0.5168 0.5825 0.029 Uiso 1 1 calc R . . H6B H 0.1015 0.5951 0.6116 0.029 Uiso 1 1 calc R . . H6C H 0.0499 0.5170 0.6397 0.029 Uiso 1 1 calc R . . C7 C -0.0330(7) 0.3508(5) 0.6111(3) 0.0112(15) Uani 1 1 d . . . C8 C -0.0998(8) 0.3566(6) 0.6471(3) 0.0145(16) Uani 1 1 d . . . C9 C -0.2208(9) 0.3627(6) 0.6336(4) 0.0193(18) Uani 1 1 d . . . H9 H -0.2670 0.3642 0.6577 0.023 Uiso 1 1 calc R . . C10 C -0.2762(8) 0.3668(7) 0.5858(4) 0.0207(19) Uani 1 1 d . . . H10 H -0.3588 0.3708 0.5773 0.025 Uiso 1 1 calc R . . C11 C -0.2076(8) 0.3650(6) 0.5512(3) 0.0158(17) Uani 1 1 d . . . H11 H -0.2444 0.3691 0.5186 0.019 Uiso 1 1 calc R . . C12 C -0.0851(8) 0.3574(6) 0.5625(3) 0.0140(16) Uani 1 1 d . . . C13 C -0.0458(8) 0.3577(7) 0.6988(3) 0.0181(18) Uani 1 1 d . . . H13A H -0.1060 0.3698 0.7177 0.027 Uiso 1 1 calc R . . H13B H 0.0140 0.4041 0.7048 0.027 Uiso 1 1 calc R . . H13C H -0.0099 0.2998 0.7080 0.027 Uiso 1 1 calc R . . C14 C -0.0184(9) 0.3596(7) 0.5225(3) 0.0202(19) Uani 1 1 d . . . H14A H -0.0114 0.4212 0.5122 0.030 Uiso 1 1 calc R . . H14B H -0.0597 0.3244 0.4956 0.030 Uiso 1 1 calc R . . H14C H 0.0597 0.3347 0.5334 0.030 Uiso 1 1 calc R . . C15 C 0.3108(8) 0.0667(6) 0.6717(4) 0.0162(17) Uani 1 1 d . . . C16 C 0.3749(8) 0.1340(6) 0.7000(3) 0.0166(17) Uani 1 1 d . . . C17 C 0.4232(7) 0.1923(6) 0.6695(3) 0.0134(16) Uani 1 1 d . . . C18 C 0.3891(7) 0.1593(6) 0.6218(3) 0.0146(16) Uani 1 1 d . . . C19 C 0.3206(8) 0.0808(6) 0.6235(3) 0.0167(17) Uani 1 1 d . . . C21 C 0.3997(10) 0.1335(7) 0.7537(4) 0.024(2) Uani 1 1 d . . . H21A H 0.3259 0.1324 0.7654 0.036 Uiso 1 1 calc R . . H21B H 0.4435 0.1871 0.7655 0.036 Uiso 1 1 calc R . . H21C H 0.4458 0.0808 0.7653 0.036 Uiso 1 1 calc R . . C22 C 0.5001(9) 0.2702(7) 0.6850(4) 0.024(2) Uani 1 1 d . . . H22A H 0.4575 0.3138 0.7006 0.035 Uiso 1 1 calc R . . H22B H 0.5236 0.2975 0.6571 0.035 Uiso 1 1 calc R . . H22C H 0.5696 0.2505 0.7074 0.035 Uiso 1 1 calc R . . C23 C 0.4271(9) 0.1957(7) 0.5786(4) 0.024(2) Uani 1 1 d . . . H23A H 0.4984 0.1653 0.5739 0.036 Uiso 1 1 calc R . . H23B H 0.4424 0.2595 0.5829 0.036 Uiso 1 1 calc R . . H23C H 0.3653 0.1862 0.5506 0.036 Uiso 1 1 calc R . . C24 C 0.2846(10) 0.0156(7) 0.5843(4) 0.027(2) Uani 1 1 d . . . H24A H 0.3403 -0.0338 0.5879 0.040 Uiso 1 1 calc R . . H24B H 0.2833 0.0448 0.5535 0.040 Uiso 1 1 calc R . . H24C H 0.2066 -0.0071 0.5856 0.040 Uiso 1 1 calc R . . C25 C 0.2557(9) -0.0117(6) 0.6901(4) 0.026(2) Uani 1 1 d . . . H25A H 0.3069 -0.0634 0.6906 0.039 Uiso 1 1 calc R . . H25B H 0.1804 -0.0239 0.6693 0.039 Uiso 1 1 calc R . . H25C H 0.2434 0.0006 0.7225 0.039 Uiso 1 1 calc R . . C26 C 0.8303(9) 0.1543(7) 0.9135(4) 0.025(2) Uani 1 1 d . . . C27 C 0.9431(10) 0.1023(7) 0.9197(5) 0.034(3) Uani 1 1 d . . . H27A H 0.9727 0.1030 0.8897 0.051 Uiso 1 1 calc R . . H27B H 0.9289 0.0408 0.9283 0.051 Uiso 1 1 calc R . . H27C H 1.0009 0.1294 0.9450 0.051 Uiso 1 1 calc R . . C28 C 0.7778(11) 0.1501(8) 0.9593(5) 0.035(3) Uani 1 1 d . . . H28A H 0.7612 0.0881 0.9662 0.052 Uiso 1 1 calc R . . H28B H 0.7053 0.1846 0.9547 0.052 Uiso 1 1 calc R . . H28C H 0.8336 0.1749 0.9861 0.052 Uiso 1 1 calc R . . C29 C 0.7409(11) 0.1147(8) 0.8725(5) 0.039(3) Uani 1 1 d . . . H29A H 0.7725 0.1163 0.8430 0.059 Uiso 1 1 calc R . . H29B H 0.6687 0.1495 0.8682 0.059 Uiso 1 1 calc R . . H29C H 0.7244 0.0531 0.8800 0.059 Uiso 1 1 calc R . . C30 C 1.0465(7) 0.2792(6) 0.8944(3) 0.0148(16) Uani 1 1 d . . . C31 C 1.1115(8) 0.2879(6) 0.9410(3) 0.0153(16) Uani 1 1 d . . . C32 C 1.2347(8) 0.2833(6) 0.9475(4) 0.0192(18) Uani 1 1 d . . . H32 H 1.2801 0.2904 0.9786 0.023 Uiso 1 1 calc R . . C33 C 1.2902(9) 0.2685(6) 0.9094(4) 0.0195(18) Uani 1 1 d . . . H33 H 1.3730 0.2677 0.9142 0.023 Uiso 1 1 calc R . . C34 C 1.2234(8) 0.2548(6) 0.8638(3) 0.0177(17) Uani 1 1 d . . . H34 H 1.2612 0.2414 0.8379 0.021 Uiso 1 1 calc R . . C35 C 1.1027(8) 0.2605(6) 0.8560(3) 0.0139(16) Uani 1 1 d . . . C36 C 1.0579(9) 0.3015(7) 0.9842(3) 0.0203(19) Uani 1 1 d . . . H36A H 1.0792 0.3604 0.9977 0.030 Uiso 1 1 calc R . . H36B H 1.0867 0.2558 1.0080 0.030 Uiso 1 1 calc R . . H36C H 0.9728 0.2972 0.9751 0.030 Uiso 1 1 calc R . . C37 C 1.0329(9) 0.2420(7) 0.8067(3) 0.0206(19) Uani 1 1 d . . . H37A H 1.0857 0.2240 0.7855 0.031 Uiso 1 1 calc R . . H37B H 0.9907 0.2958 0.7941 0.031 Uiso 1 1 calc R . . H37C H 0.9769 0.1941 0.8086 0.031 Uiso 1 1 calc R . . C38 C 0.6296(8) 0.4820(6) 0.8060(4) 0.0185(18) Uani 1 1 d . . . C39 C 0.6935(8) 0.5517(6) 0.8332(4) 0.0178(18) Uani 1 1 d . . . C40 C 0.6804(8) 0.5408(6) 0.8812(4) 0.0188(18) Uani 1 1 d . . . C41 C 0.6153(8) 0.4615(7) 0.8849(4) 0.0199(19) Uani 1 1 d . . . C42 C 0.5042(9) 0.3459(7) 0.8243(4) 0.023(2) Uani 1 1 d . . . H42A H 0.4533 0.3382 0.8477 0.035 Uiso 1 1 calc R . . H42B H 0.5519 0.2925 0.8237 0.035 Uiso 1 1 calc R . . H42C H 0.4564 0.3557 0.7926 0.035 Uiso 1 1 calc R . . C43 C 0.6070(10) 0.4790(7) 0.7527(4) 0.026(2) Uani 1 1 d . . . H43A H 0.5476 0.5232 0.7400 0.039 Uiso 1 1 calc R . . H43B H 0.5792 0.4196 0.7419 0.039 Uiso 1 1 calc R . . H43C H 0.6793 0.4921 0.7413 0.039 Uiso 1 1 calc R . . C44 C 0.7458(10) 0.6312(7) 0.8135(5) 0.029(2) Uani 1 1 d . . . H44A H 0.6844 0.6747 0.8021 0.043 Uiso 1 1 calc R . . H44B H 0.7827 0.6128 0.7869 0.043 Uiso 1 1 calc R . . H44C H 0.8046 0.6581 0.8386 0.043 Uiso 1 1 calc R . . C45 C 0.7119(9) 0.6079(7) 0.9202(4) 0.026(2) Uani 1 1 d . . . H45A H 0.7802 0.6419 0.9151 0.040 Uiso 1 1 calc R . . H45B H 0.7301 0.5775 0.9511 0.040 Uiso 1 1 calc R . . H45C H 0.6461 0.6485 0.9200 0.040 Uiso 1 1 calc R . . C46 C 0.5810(10) 0.4269(8) 0.9296(4) 0.028(2) Uani 1 1 d . . . H46A H 0.6453 0.4360 0.9567 0.043 Uiso 1 1 calc R . . H46B H 0.5634 0.3633 0.9260 0.043 Uiso 1 1 calc R . . H46C H 0.5117 0.4588 0.9353 0.043 Uiso 1 1 calc R . . C47 C 0.5826(8) 0.4249(6) 0.8381(4) 0.0161(17) Uani 1 1 d . . . N1 N 0.0891(6) 0.3313(5) 0.6243(3) 0.0116(13) Uani 1 1 d . . . N2 N 0.9230(7) 0.2954(5) 0.8852(3) 0.0141(14) Uani 1 1 d . . . O1 O 0.2748(5) 0.3287(4) 0.6215(2) 0.0128(12) Uani 1 1 d . . . O2 O 0.7420(5) 0.2996(4) 0.8945(2) 0.0154(12) Uani 1 1 d . . . Cl1 Cl 0.1161(2) 0.17530(16) 0.56683(8) 0.0203(4) Uani 1 1 d . . . Cl2 Cl 0.06117(19) 0.13929(15) 0.67504(9) 0.0191(4) Uani 1 1 d . . . Cl3 Cl 0.24076(19) 0.29716(15) 0.72071(7) 0.0157(4) Uani 1 1 d . . . Cl4 Cl 0.7537(2) 0.30762(15) 0.79146(8) 0.0182(4) Uani 1 1 d . . . Cl5 Cl 0.9345(2) 0.47295(16) 0.82118(9) 0.0200(4) Uani 1 1 d . . . Cl6 Cl 0.9011(2) 0.46460(16) 0.93397(8) 0.0201(4) Uani 1 1 d . . . Ta01 Ta 0.21320(3) 0.21278(2) 0.646178(12) 0.01022(8) Uani 1 1 d . . . Ta02 Ta 0.79281(3) 0.40857(2) 0.860147(13) 0.01196(8) 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 C1 0.009(4) 0.010(4) 0.021(4) 0.000(3) 0.008(3) 0.001(3) C2 0.014(4) 0.015(4) 0.019(4) 0.002(3) 0.003(3) 0.003(3) C3 0.010(4) 0.016(4) 0.022(4) -0.005(3) 0.004(3) -0.006(3) C4 0.020(4) 0.005(4) 0.039(6) -0.002(4) 0.000(4) -0.009(3) C5 0.022(5) 0.013(4) 0.027(5) 0.004(4) 0.010(4) -0.006(4) C6 0.015(4) 0.012(4) 0.031(5) 0.001(4) 0.006(4) 0.005(3) C7 0.010(4) 0.002(3) 0.022(4) 0.001(3) 0.002(3) -0.002(3) C8 0.012(4) 0.015(4) 0.017(4) 0.002(3) 0.002(3) -0.002(3) C9 0.022(5) 0.011(4) 0.028(5) -0.001(3) 0.012(4) 0.000(3) C10 0.007(4) 0.018(4) 0.035(5) -0.003(4) 0.001(4) -0.005(3) C11 0.013(4) 0.011(4) 0.021(4) -0.001(3) -0.003(3) 0.002(3) C12 0.012(4) 0.007(4) 0.022(4) 0.001(3) 0.001(3) -0.003(3) C13 0.016(4) 0.020(5) 0.019(4) 0.002(3) 0.006(3) 0.005(3) C14 0.023(5) 0.022(5) 0.015(4) 0.003(3) 0.001(3) 0.003(4) C15 0.009(4) 0.011(4) 0.028(5) 0.003(3) 0.004(3) 0.006(3) C16 0.018(4) 0.013(4) 0.020(4) 0.002(3) 0.006(3) 0.004(3) C17 0.010(4) 0.011(4) 0.018(4) 0.000(3) 0.002(3) 0.001(3) C18 0.009(4) 0.016(4) 0.020(4) 0.000(3) 0.006(3) 0.001(3) C19 0.012(4) 0.015(4) 0.023(4) -0.003(3) 0.003(3) 0.003(3) C21 0.034(6) 0.017(5) 0.020(5) 0.004(4) 0.001(4) 0.010(4) C22 0.020(5) 0.015(5) 0.035(5) -0.001(4) 0.003(4) 0.000(4) C23 0.023(5) 0.027(5) 0.025(5) 0.007(4) 0.011(4) 0.003(4) C24 0.023(5) 0.021(5) 0.036(6) -0.016(4) 0.000(4) 0.007(4) C25 0.019(5) 0.008(4) 0.051(7) 0.003(4) 0.010(4) -0.004(4) C26 0.021(5) 0.020(5) 0.034(6) 0.006(4) 0.006(4) 0.005(4) C27 0.019(5) 0.013(5) 0.072(9) 0.014(5) 0.014(5) 0.006(4) C28 0.038(7) 0.024(6) 0.048(7) 0.010(5) 0.024(6) -0.006(5) C29 0.034(7) 0.021(6) 0.057(8) -0.007(5) -0.004(6) 0.010(5) C30 0.008(4) 0.013(4) 0.025(4) 0.002(3) 0.007(3) 0.002(3) C31 0.015(4) 0.012(4) 0.020(4) 0.002(3) 0.005(3) 0.002(3) C32 0.018(4) 0.014(4) 0.024(4) 0.003(4) -0.002(3) 0.000(3) C33 0.016(4) 0.012(4) 0.031(5) 0.003(4) 0.005(4) 0.002(3) C34 0.019(4) 0.013(4) 0.022(4) 0.004(3) 0.007(3) 0.005(3) C35 0.017(4) 0.009(4) 0.016(4) 0.000(3) 0.004(3) 0.002(3) C36 0.018(4) 0.023(5) 0.020(4) 0.001(4) 0.006(3) -0.003(4) C37 0.019(4) 0.026(5) 0.018(4) -0.001(4) 0.005(3) 0.003(4) C38 0.014(4) 0.013(4) 0.027(5) -0.002(3) -0.001(3) -0.001(3) C39 0.010(4) 0.007(4) 0.036(5) -0.002(3) 0.002(3) 0.002(3) C40 0.017(4) 0.007(4) 0.031(5) -0.004(3) 0.001(4) 0.004(3) C41 0.008(4) 0.023(5) 0.029(5) -0.002(4) 0.004(3) 0.007(3) C42 0.016(4) 0.017(5) 0.034(5) -0.004(4) 0.000(4) -0.005(4) C43 0.031(6) 0.020(5) 0.023(5) -0.001(4) -0.002(4) 0.001(4) C44 0.025(5) 0.017(5) 0.047(7) 0.004(4) 0.014(5) 0.004(4) C45 0.018(5) 0.020(5) 0.038(6) -0.012(4) -0.004(4) 0.005(4) C46 0.024(5) 0.031(6) 0.032(6) -0.001(4) 0.012(4) 0.010(4) C47 0.009(4) 0.010(4) 0.028(5) -0.002(3) -0.001(3) 0.000(3) N1 0.012(3) 0.010(3) 0.014(3) -0.002(3) 0.003(3) 0.002(3) N2 0.013(3) 0.014(3) 0.017(3) -0.001(3) 0.006(3) -0.002(3) O1 0.011(3) 0.008(3) 0.020(3) 0.003(2) 0.006(2) 0.000(2) O2 0.012(3) 0.010(3) 0.024(3) 0.002(2) 0.004(2) 0.003(2) Cl1 0.0216(11) 0.0166(10) 0.0200(10) -0.0058(8) -0.0033(8) 0.0032(8) Cl2 0.0120(9) 0.0143(10) 0.0325(12) 0.0028(8) 0.0078(8) -0.0020(8) Cl3 0.0168(9) 0.0143(9) 0.0160(9) -0.0023(7) 0.0030(7) 0.0010(8) Cl4 0.0175(10) 0.0148(10) 0.0210(10) -0.0057(8) 0.0006(8) 0.0012(8) Cl5 0.0152(10) 0.0178(10) 0.0282(11) 0.0031(9) 0.0074(8) -0.0025(8) Cl6 0.0157(10) 0.0184(10) 0.0233(11) -0.0063(8) -0.0034(8) 0.0037(8) Ta01 0.00858(14) 0.00828(15) 0.01380(15) -0.00026(12) 0.00214(11) -0.00067(12) Ta02 0.00863(15) 0.01012(15) 0.01688(16) -0.00157(12) 0.00174(11) -0.00039(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.305(11) . ? C1 O1 1.320(10) . ? C1 C3 1.521(13) . ? C1 Ta01 2.613(9) . ? C2 N2 1.295(12) . ? C2 O2 1.346(11) . ? C2 C26 1.521(14) . ? C2 Ta02 2.635(9) . ? C3 C5 1.539(13) . ? C3 C4 1.542(13) . ? C3 C6 1.546(13) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.402(12) . ? C7 C12 1.408(12) . ? C7 N1 1.434(11) . ? C8 C9 1.395(13) . ? C8 C13 1.492(13) . ? C9 C10 1.393(14) . ? C9 H9 0.9500 . ? C10 C11 1.383(14) . ? C10 H10 0.9500 . ? C11 C12 1.409(12) . ? C11 H11 0.9500 . ? C12 C14 1.499(13) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.417(13) . ? C15 C19 1.417(13) . ? C15 C25 1.485(13) . ? C15 Ta01 2.519(9) . ? C16 C17 1.425(13) . ? C16 C21 1.504(13) . ? C16 Ta01 2.497(9) . ? C17 C18 1.431(12) . ? C17 C22 1.492(13) . ? C17 Ta01 2.433(9) . ? C18 C19 1.433(13) . ? C18 C23 1.490(13) . ? C18 Ta01 2.424(8) . ? C19 C24 1.487(13) . ? C19 Ta01 2.498(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.513(14) . ? C26 C29 1.533(17) . ? C26 C28 1.546(16) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.405(13) . ? C30 C35 1.408(12) . ? C30 N2 1.435(11) . ? C31 C32 1.415(13) . ? C31 C36 1.498(13) . ? C32 C33 1.383(14) . ? C32 H32 0.9500 . ? C33 C34 1.400(14) . ? C33 H33 0.9500 . ? C34 C35 1.386(13) . ? C34 H34 0.9500 . ? C35 C37 1.511(13) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.428(13) . ? C38 C47 1.436(14) . ? C38 C43 1.493(14) . ? C38 Ta02 2.474(9) . ? C39 C40 1.415(15) . ? C39 C44 1.500(14) . ? C39 Ta02 2.497(9) . ? C40 C41 1.429(14) . ? C40 C45 1.497(14) . ? C40 Ta02 2.517(9) . ? C41 C47 1.429(14) . ? C41 C46 1.499(15) . ? C41 Ta02 2.443(9) . ? C42 C47 1.505(13) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 Ta02 2.426(9) . ? N1 Ta01 2.308(7) . ? N2 Ta02 2.305(8) . ? O1 Ta01 2.061(6) . ? O2 Ta02 2.054(6) . ? Cl1 Ta01 2.399(2) . ? Cl2 Ta01 2.365(2) . ? Cl3 Ta01 2.445(2) . ? Cl4 Ta02 2.453(2) . ? Cl5 Ta02 2.366(2) . ? Cl6 Ta02 2.395(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 O1 112.5(8) . . ? N1 C1 C3 131.4(8) . . ? O1 C1 C3 115.7(7) . . ? N1 C1 Ta01 62.0(5) . . ? O1 C1 Ta01 51.2(4) . . ? C3 C1 Ta01 161.9(6) . . ? N2 C2 O2 111.0(8) . . ? N2 C2 C26 132.4(9) . . ? O2 C2 C26 116.0(8) . . ? N2 C2 Ta02 61.0(5) . . ? O2 C2 Ta02 50.3(4) . . ? C26 C2 Ta02 162.3(7) . . ? C1 C3 C5 111.0(8) . . ? C1 C3 C4 104.9(8) . . ? C5 C3 C4 108.5(8) . . ? C1 C3 C6 113.5(7) . . ? C5 C3 C6 110.6(8) . . ? C4 C3 C6 108.0(8) . . ? 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 . . ? C8 C7 C12 121.3(8) . . ? C8 C7 N1 118.8(8) . . ? C12 C7 N1 119.7(8) . . ? C9 C8 C7 118.3(8) . . ? C9 C8 C13 119.3(8) . . ? C7 C8 C13 122.3(8) . . ? C10 C9 C8 122.1(9) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C11 C10 C9 118.1(9) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 122.5(9) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C7 C12 C11 117.5(8) . . ? C7 C12 C14 124.2(8) . . ? C11 C12 C14 118.3(8) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 . . ? C16 C15 C19 108.4(8) . . ? C16 C15 C25 125.7(9) . . ? C19 C15 C25 125.4(9) . . ? C16 C15 Ta01 72.7(5) . . ? C19 C15 Ta01 72.8(5) . . ? C25 C15 Ta01 126.4(6) . . ? C15 C16 C17 108.5(8) . . ? C15 C16 C21 123.8(9) . . ? C17 C16 C21 127.1(9) . . ? C15 C16 Ta01 74.5(5) . . ? C17 C16 Ta01 70.8(5) . . ? C21 C16 Ta01 127.3(6) . . ? C16 C17 C18 107.2(8) . . ? C16 C17 C22 126.0(9) . . ? C18 C17 C22 126.7(9) . . ? C16 C17 Ta01 75.7(5) . . ? C18 C17 Ta01 72.5(5) . . ? C22 C17 Ta01 120.0(6) . . ? C17 C18 C19 108.1(8) . . ? C17 C18 C23 125.8(9) . . ? C19 C18 C23 125.8(9) . . ? C17 C18 Ta01 73.2(5) . . ? C19 C18 Ta01 75.9(5) . . ? C23 C18 Ta01 121.0(6) . . ? C15 C19 C18 107.6(8) . . ? C15 C19 C24 124.7(9) . . ? C18 C19 C24 126.8(9) . . ? C15 C19 Ta01 74.4(5) . . ? C18 C19 Ta01 70.3(5) . . ? C24 C19 Ta01 129.4(6) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C2 114.6(9) . . ? C27 C26 C29 109.9(10) . . ? C2 C26 C29 104.2(9) . . ? C27 C26 C28 110.8(10) . . ? C2 C26 C28 109.1(9) . . ? C29 C26 C28 108.0(10) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 120.4(8) . . ? C31 C30 N2 120.1(8) . . ? C35 C30 N2 119.3(8) . . ? C30 C31 C32 118.3(8) . . ? C30 C31 C36 123.7(8) . . ? C32 C31 C36 118.0(8) . . ? C33 C32 C31 121.2(9) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 119.5(9) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 120.7(9) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C30 119.7(8) . . ? C34 C35 C37 119.4(8) . . ? C30 C35 C37 120.8(8) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C47 108.4(9) . . ? C39 C38 C43 123.3(9) . . ? C47 C38 C43 127.9(9) . . ? C39 C38 Ta02 74.2(5) . . ? C47 C38 Ta02 71.2(5) . . ? C43 C38 Ta02 126.1(7) . . ? C40 C39 C38 107.5(9) . . ? C40 C39 C44 125.5(9) . . ? C38 C39 C44 126.1(10) . . ? C40 C39 Ta02 74.4(5) . . ? C38 C39 Ta02 72.4(5) . . ? C44 C39 Ta02 127.3(6) . . ? C39 C40 C41 108.9(8) . . ? C39 C40 C45 125.8(9) . . ? C41 C40 C45 124.7(10) . . ? C39 C40 Ta02 72.8(5) . . ? C41 C40 Ta02 70.4(5) . . ? C45 C40 Ta02 130.2(7) . . ? C47 C41 C40 107.8(9) . . ? C47 C41 C46 126.4(10) . . ? C40 C41 C46 125.7(10) . . ? C47 C41 Ta02 72.3(5) . . ? C40 C41 Ta02 76.1(5) . . ? C46 C41 Ta02 120.6(7) . . ? C47 C42 H42A 109.5 . . ? C47 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C47 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C41 C47 C38 107.3(8) . . ? C41 C47 C42 126.1(9) . . ? C38 C47 C42 126.4(9) . . ? C41 C47 Ta02 73.6(5) . . ? C38 C47 Ta02 74.8(5) . . ? C42 C47 Ta02 121.5(6) . . ? C1 N1 C7 130.1(8) . . ? C1 N1 Ta01 88.1(5) . . ? C7 N1 Ta01 140.5(6) . . ? C2 N2 C30 129.4(8) . . ? C2 N2 Ta02 89.5(6) . . ? C30 N2 Ta02 139.6(6) . . ? C1 O1 Ta01 98.9(5) . . ? C2 O2 Ta02 99.5(5) . . ? O1 Ta01 N1 59.6(3) . . ? O1 Ta01 Cl2 147.90(18) . . ? N1 Ta01 Cl2 88.98(19) . . ? O1 Ta01 Cl1 90.57(19) . . ? N1 Ta01 Cl1 76.46(19) . . ? Cl2 Ta01 Cl1 88.08(9) . . ? O1 Ta01 C18 79.3(3) . . ? N1 Ta01 C18 134.5(3) . . ? Cl2 Ta01 C18 132.4(2) . . ? Cl1 Ta01 C18 85.8(2) . . ? O1 Ta01 C17 78.6(3) . . ? N1 Ta01 C17 136.0(3) . . ? Cl2 Ta01 C17 128.9(2) . . ? Cl1 Ta01 C17 120.0(2) . . ? C18 Ta01 C17 34.3(3) . . ? O1 Ta01 Cl3 81.96(19) . . ? N1 Ta01 Cl3 78.86(18) . . ? Cl2 Ta01 Cl3 85.68(8) . . ? Cl1 Ta01 Cl3 154.63(8) . . ? C18 Ta01 Cl3 116.2(2) . . ? C17 Ta01 Cl3 82.4(2) . . ? O1 Ta01 C16 109.9(3) . . ? N1 Ta01 C16 153.7(3) . . ? Cl2 Ta01 C16 95.3(2) . . ? Cl1 Ta01 C16 129.5(2) . . ? C18 Ta01 C16 55.7(3) . . ? C17 Ta01 C16 33.6(3) . . ? Cl3 Ta01 C16 75.6(2) . . ? O1 Ta01 C19 111.2(3) . . ? N1 Ta01 C19 149.8(3) . . ? Cl2 Ta01 C19 99.4(2) . . ? Cl1 Ta01 C19 74.9(2) . . ? C18 Ta01 C19 33.8(3) . . ? C17 Ta01 C19 56.1(3) . . ? Cl3 Ta01 C19 130.4(2) . . ? C16 Ta01 C19 54.8(3) . . ? O1 Ta01 C15 132.1(3) . . ? N1 Ta01 C15 168.2(3) . . ? Cl2 Ta01 C15 79.6(2) . . ? Cl1 Ta01 C15 100.1(2) . . ? C18 Ta01 C15 55.4(3) . . ? C17 Ta01 C15 55.5(3) . . ? Cl3 Ta01 C15 102.9(2) . . ? C16 Ta01 C15 32.8(3) . . ? C19 Ta01 C15 32.8(3) . . ? O1 Ta01 C1 29.9(2) . . ? N1 Ta01 C1 29.9(3) . . ? Cl2 Ta01 C1 118.13(19) . . ? Cl1 Ta01 C1 85.3(2) . . ? C18 Ta01 C1 108.3(3) . . ? C17 Ta01 C1 106.8(3) . . ? Cl3 Ta01 C1 76.2(2) . . ? C16 Ta01 C1 133.8(3) . . ? C19 Ta01 C1 136.8(3) . . ? C15 Ta01 C1 161.9(3) . . ? O2 Ta02 N2 59.6(3) . . ? O2 Ta02 Cl5 147.22(19) . . ? N2 Ta02 Cl5 88.3(2) . . ? O2 Ta02 Cl6 90.8(2) . . ? N2 Ta02 Cl6 77.3(2) . . ? Cl5 Ta02 Cl6 88.22(9) . . ? O2 Ta02 C47 80.6(3) . . ? N2 Ta02 C47 136.9(3) . . ? Cl5 Ta02 C47 126.7(2) . . ? Cl6 Ta02 C47 122.2(2) . . ? O2 Ta02 C41 77.7(3) . . ? N2 Ta02 C41 134.1(3) . . ? Cl5 Ta02 C41 135.0(3) . . ? Cl6 Ta02 C41 88.1(2) . . ? C47 Ta02 C41 34.1(3) . . ? O2 Ta02 Cl4 81.9(2) . . ? N2 Ta02 Cl4 78.6(2) . . ? Cl5 Ta02 Cl4 85.41(8) . . ? Cl6 Ta02 Cl4 155.22(8) . . ? C47 Ta02 Cl4 80.1(2) . . ? C41 Ta02 Cl4 113.1(3) . . ? O2 Ta02 C38 113.4(3) . . ? N2 Ta02 C38 155.3(3) . . ? Cl5 Ta02 C38 92.7(2) . . ? Cl6 Ta02 C38 127.4(2) . . ? C47 Ta02 C38 34.1(3) . . ? C41 Ta02 C38 56.0(3) . . ? Cl4 Ta02 C38 76.9(2) . . ? O2 Ta02 C39 132.6(3) . . ? N2 Ta02 C39 166.8(3) . . ? Cl5 Ta02 C39 80.0(2) . . ? Cl6 Ta02 C39 96.0(2) . . ? C47 Ta02 C39 56.3(3) . . ? C41 Ta02 C39 55.8(3) . . ? Cl4 Ta02 C39 106.4(2) . . ? C38 Ta02 C39 33.4(3) . . ? O2 Ta02 C40 107.9(3) . . ? N2 Ta02 C40 148.5(3) . . ? Cl5 Ta02 C40 103.3(2) . . ? Cl6 Ta02 C40 74.0(2) . . ? C47 Ta02 C40 55.6(3) . . ? C41 Ta02 C40 33.4(3) . . ? Cl4 Ta02 C40 130.8(2) . . ? C38 Ta02 C40 54.7(3) . . ? C39 Ta02 C40 32.8(3) . . ? O2 Ta02 C2 30.3(3) . . ? N2 Ta02 C2 29.5(3) . . ? Cl5 Ta02 C2 117.2(2) . . ? Cl6 Ta02 C2 84.8(2) . . ? C47 Ta02 C2 108.9(3) . . ? C41 Ta02 C2 107.1(3) . . ? Cl4 Ta02 C2 76.9(2) . . ? C38 Ta02 C2 137.9(3) . . ? C39 Ta02 C2 162.8(3) . . ? C40 Ta02 C2 133.5(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 4.243 _refine_diff_density_min -5.498 _refine_diff_density_rms 0.286 #END data_ls229_0m #TrackingRef '- 3c_ls229_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841451' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trichlorido(eta5-pentamethylcyclopendienyl)(eta3-N-2,6-dimethylphenyl(phenyl) amidate)tantalum ; _chemical_name_common ; Trichlorido(eta5-pentamethylcyclopendienyl)(eta3-N-2,6- dimethylphenyl(phenyl) amidate)tantalum ; _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 Cl3 N O Ta' _chemical_formula_sum 'C25 H29 Cl3 N O Ta' _chemical_formula_weight 646.79 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' O O 0.0106 0.0060 '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 8.776(5) _cell_length_b 12.131(5) _cell_length_c 12.167(5) _cell_angle_alpha 95.859(5) _cell_angle_beta 90.822(5) _cell_angle_gamma 109.198(5) _cell_volume 1215.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.4605 _cell_measurement_theta_max 27.4155 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 4.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 0.614 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19180 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5498 _reflns_number_gt 5011 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The two largest residual electron density peaks are found adjacent (within 0.90 A) to the Ta atom. 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^ > 2\s(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^)+(0.0439P)^2^+0.2630P] 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 5498 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.004 _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 0.233630(15) 0.852565(11) 0.226613(11) 0.01207(5) Uani 1 1 d . . . Cl3 Cl 0.16796(11) 0.86210(8) 0.41825(7) 0.01979(18) Uani 1 1 d . . . Cl1 Cl 0.34998(11) 0.78219(8) 0.06708(7) 0.01863(17) Uani 1 1 d . . . Cl2 Cl 0.50003(10) 0.97329(7) 0.28555(7) 0.01949(18) Uani 1 1 d . . . O1 O 0.0570(3) 0.6906(2) 0.2126(2) 0.0162(5) Uani 1 1 d . . . C2 C 0.0477(4) 0.5080(3) 0.2760(3) 0.0148(7) Uani 1 1 d . . . C5 C -0.1365(4) 0.2829(3) 0.3163(3) 0.0210(8) Uani 1 1 d . . . H5 H -0.1992 0.2058 0.3300 0.025 Uiso 1 1 calc R . . C10 C 0.5564(4) 0.5076(3) 0.2589(3) 0.0194(7) Uani 1 1 d . . . H10 H 0.5775 0.4501 0.2081 0.023 Uiso 1 1 calc R . . C21 C -0.0661(4) 0.7709(3) 0.0187(3) 0.0221(8) Uani 1 1 d . . . H21A H -0.1253 0.7985 -0.0351 0.033 Uiso 1 1 calc R . . H21B H -0.1430 0.7133 0.0595 0.033 Uiso 1 1 calc R . . H21C H 0.0049 0.7341 -0.0202 0.033 Uiso 1 1 calc R . . N1 N 0.2883(3) 0.6914(3) 0.2806(2) 0.0141(6) Uani 1 1 d . . . C11 C 0.6448(4) 0.5432(3) 0.3586(3) 0.0226(8) Uani 1 1 d . . . H11 H 0.7253 0.5102 0.3760 0.027 Uiso 1 1 calc R . . C12 C 0.6155(4) 0.6271(3) 0.4329(3) 0.0202(7) Uani 1 1 d . . . H12 H 0.6756 0.6508 0.5019 0.024 Uiso 1 1 calc R . . C20 C 0.1791(4) 0.9600(3) 0.0748(3) 0.0147(7) Uani 1 1 d . . . C18 C 0.1127(4) 1.0119(3) 0.2504(3) 0.0161(7) Uani 1 1 d . . . C19 C 0.2302(4) 1.0452(3) 0.1694(3) 0.0150(7) Uani 1 1 d . . . C1 C 0.1381(4) 0.6298(3) 0.2567(3) 0.0144(7) Uani 1 1 d . . . C8 C 0.4097(4) 0.6404(3) 0.3073(3) 0.0141(7) Uani 1 1 d . . . C14 C 0.3405(5) 0.5035(3) 0.1229(3) 0.0228(8) Uani 1 1 d . . . H14A H 0.4051 0.4722 0.0714 0.034 Uiso 1 1 calc R . . H14B H 0.3120 0.5655 0.0908 0.034 Uiso 1 1 calc R . . H14C H 0.2416 0.4403 0.1364 0.034 Uiso 1 1 calc R . . C22 C -0.1606(4) 0.8423(3) 0.2614(3) 0.0235(8) Uani 1 1 d . . . H22A H -0.2512 0.8624 0.2315 0.035 Uiso 1 1 calc R . . H22B H -0.1460 0.8663 0.3413 0.035 Uiso 1 1 calc R . . H22C H -0.1834 0.7573 0.2472 0.035 Uiso 1 1 calc R . . C25 C 0.2516(4) 0.9726(3) -0.0359(3) 0.0194(7) Uani 1 1 d . . . H25A H 0.2182 0.8958 -0.0804 0.029 Uiso 1 1 calc R . . H25B H 0.3697 1.0030 -0.0258 0.029 Uiso 1 1 calc R . . H25C H 0.2144 1.0272 -0.0739 0.029 Uiso 1 1 calc R . . C17 C -0.0094(4) 0.9051(3) 0.2064(3) 0.0164(7) Uani 1 1 d . . . C16 C 0.0337(4) 0.8732(3) 0.0983(3) 0.0166(7) Uani 1 1 d . . . C9 C 0.4371(4) 0.5537(3) 0.2307(3) 0.0165(7) Uani 1 1 d . . . C24 C 0.3684(5) 1.1575(3) 0.1779(3) 0.0214(8) Uani 1 1 d . . . H24A H 0.4396 1.1550 0.1170 0.032 Uiso 1 1 calc R . . H24B H 0.4291 1.1685 0.2487 0.032 Uiso 1 1 calc R . . H24C H 0.3274 1.2231 0.1735 0.032 Uiso 1 1 calc R . . C23 C 0.1106(5) 1.0874(3) 0.3558(3) 0.0246(8) Uani 1 1 d . . . H23A H 0.2099 1.1012 0.4009 0.037 Uiso 1 1 calc R . . H23B H 0.0169 1.0475 0.3969 0.037 Uiso 1 1 calc R . . H23C H 0.1036 1.1627 0.3383 0.037 Uiso 1 1 calc R . . C7 C 0.0823(4) 0.4617(3) 0.3702(3) 0.0166(7) Uani 1 1 d . . . H7 H 0.1699 0.5070 0.4202 0.020 Uiso 1 1 calc R . . C13 C 0.4993(4) 0.6774(3) 0.4085(3) 0.0168(7) Uani 1 1 d . . . C6 C -0.0106(4) 0.3501(3) 0.3906(3) 0.0192(7) Uani 1 1 d . . . H6 H 0.0115 0.3193 0.4554 0.023 Uiso 1 1 calc R . . C4 C -0.1714(4) 0.3280(3) 0.2220(3) 0.0202(8) Uani 1 1 d . . . H4 H -0.2573 0.2816 0.1713 0.024 Uiso 1 1 calc R . . C3 C -0.0803(4) 0.4410(3) 0.2024(3) 0.0183(7) Uani 1 1 d . . . H3 H -0.1050 0.4726 0.1389 0.022 Uiso 1 1 calc R . . C15 C 0.4667(5) 0.7654(4) 0.4931(3) 0.0234(8) Uani 1 1 d . . . H15A H 0.5252 0.7684 0.5632 0.035 Uiso 1 1 calc R . . H15B H 0.3505 0.7419 0.5045 0.035 Uiso 1 1 calc R . . H15C H 0.5031 0.8431 0.4668 0.035 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 0.00984(8) 0.01386(8) 0.01287(8) 0.00300(5) 0.00328(5) 0.00386(5) Cl3 0.0244(4) 0.0248(4) 0.0149(4) 0.0054(3) 0.0066(3) 0.0135(4) Cl1 0.0218(4) 0.0209(4) 0.0164(4) 0.0042(3) 0.0071(3) 0.0105(3) Cl2 0.0129(4) 0.0188(4) 0.0251(5) 0.0024(3) -0.0005(3) 0.0031(3) O1 0.0119(12) 0.0172(12) 0.0206(13) 0.0054(10) 0.0007(10) 0.0053(10) C2 0.0123(16) 0.0159(16) 0.0176(17) 0.0030(13) 0.0066(13) 0.0062(13) C5 0.0176(18) 0.0149(17) 0.030(2) 0.0056(14) 0.0117(15) 0.0041(14) C10 0.0163(17) 0.0177(17) 0.025(2) 0.0024(14) 0.0056(14) 0.0059(14) C21 0.0199(19) 0.0188(18) 0.026(2) 0.0005(15) -0.0059(15) 0.0056(15) N1 0.0115(14) 0.0161(14) 0.0148(14) 0.0027(11) 0.0027(11) 0.0043(11) C11 0.0163(18) 0.0250(19) 0.030(2) 0.0074(16) 0.0029(15) 0.0104(15) C12 0.0118(17) 0.027(2) 0.0208(19) 0.0058(15) -0.0020(14) 0.0051(15) C20 0.0148(16) 0.0164(16) 0.0150(17) 0.0045(13) 0.0032(13) 0.0069(13) C18 0.0185(17) 0.0175(17) 0.0156(17) 0.0044(13) 0.0030(13) 0.0096(14) C19 0.0139(17) 0.0160(16) 0.0177(17) 0.0053(13) 0.0026(13) 0.0071(13) C1 0.0152(17) 0.0154(16) 0.0140(16) 0.0024(13) 0.0048(13) 0.0067(13) C8 0.0094(15) 0.0155(16) 0.0182(17) 0.0050(13) 0.0021(13) 0.0044(13) C14 0.0216(19) 0.0246(19) 0.0216(19) -0.0047(15) -0.0014(15) 0.0092(16) C22 0.0161(18) 0.027(2) 0.030(2) 0.0125(16) 0.0088(15) 0.0081(15) C25 0.0197(18) 0.0248(19) 0.0161(18) 0.0055(14) 0.0051(14) 0.0096(15) C17 0.0114(16) 0.0196(17) 0.0227(18) 0.0092(14) 0.0041(13) 0.0091(14) C16 0.0149(17) 0.0131(16) 0.0227(18) 0.0048(13) -0.0028(14) 0.0052(13) C9 0.0152(17) 0.0154(16) 0.0186(18) 0.0049(13) 0.0048(13) 0.0038(13) C24 0.0187(18) 0.0175(18) 0.025(2) 0.0048(15) 0.0002(15) 0.0015(14) C23 0.035(2) 0.024(2) 0.0209(19) 0.0037(15) 0.0084(16) 0.0164(17) C7 0.0110(16) 0.0177(17) 0.0213(18) 0.0021(14) 0.0023(13) 0.0049(13) C13 0.0134(16) 0.0193(17) 0.0184(18) 0.0052(14) 0.0038(13) 0.0055(14) C6 0.0194(18) 0.0200(18) 0.0219(19) 0.0075(14) 0.0057(14) 0.0099(15) C4 0.0113(16) 0.0219(18) 0.026(2) -0.0019(15) 0.0042(14) 0.0047(14) C3 0.0160(17) 0.0197(17) 0.0201(18) 0.0017(14) 0.0033(14) 0.0072(14) C15 0.0241(19) 0.032(2) 0.0175(18) -0.0011(15) -0.0025(15) 0.0147(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.053(2) . ? Ta1 N1 2.315(3) . ? Ta1 Cl2 2.3687(14) . ? Ta1 Cl3 2.4103(13) . ? Ta1 Cl1 2.4148(11) . ? Ta1 C16 2.423(4) . ? Ta1 C17 2.434(3) . ? Ta1 C18 2.488(3) . ? Ta1 C20 2.494(4) . ? Ta1 C19 2.514(4) . ? Ta1 C1 2.619(4) . ? O1 C1 1.324(4) . ? C2 C3 1.395(5) . ? C2 C7 1.399(5) . ? C2 C1 1.474(5) . ? C5 C6 1.389(5) . ? C5 C4 1.392(6) . ? C5 H5 0.9500 . ? C10 C11 1.380(5) . ? C10 C9 1.393(5) . ? C10 H10 0.9500 . ? C21 C16 1.504(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N1 C1 1.295(5) . ? N1 C8 1.444(4) . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C20 C16 1.417(5) . ? C20 C19 1.426(5) . ? C20 C25 1.498(5) . ? C18 C19 1.426(5) . ? C18 C17 1.429(5) . ? C18 C23 1.501(5) . ? C19 C24 1.490(5) . ? C8 C13 1.401(5) . ? C8 C9 1.416(5) . ? C14 C9 1.509(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C22 C17 1.502(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C17 C16 1.425(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C7 C6 1.381(5) . ? C7 H7 0.9500 . ? C13 C15 1.505(5) . ? C6 H6 0.9500 . ? C4 C3 1.388(5) . ? C4 H4 0.9500 . ? C3 H3 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 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 O1 Ta1 N1 59.47(10) . . ? O1 Ta1 Cl2 149.19(7) . . ? N1 Ta1 Cl2 89.80(8) . . ? O1 Ta1 Cl3 84.49(7) . . ? N1 Ta1 Cl3 78.75(7) . . ? Cl2 Ta1 Cl3 87.46(4) . . ? O1 Ta1 Cl1 87.62(7) . . ? N1 Ta1 Cl1 76.04(7) . . ? Cl2 Ta1 Cl1 86.83(4) . . ? Cl3 Ta1 Cl1 154.15(3) . . ? O1 Ta1 C16 76.74(11) . . ? N1 Ta1 C16 133.04(11) . . ? Cl2 Ta1 C16 133.04(9) . . ? Cl3 Ta1 C16 115.15(9) . . ? Cl1 Ta1 C16 86.70(9) . . ? O1 Ta1 C17 78.54(11) . . ? N1 Ta1 C17 134.85(11) . . ? Cl2 Ta1 C17 129.55(9) . . ? Cl3 Ta1 C17 81.65(9) . . ? Cl1 Ta1 C17 120.78(9) . . ? C16 Ta1 C17 34.12(12) . . ? O1 Ta1 C18 110.73(11) . . ? N1 Ta1 C18 153.42(11) . . ? Cl2 Ta1 C18 95.85(9) . . ? Cl3 Ta1 C18 75.60(8) . . ? Cl1 Ta1 C18 130.08(8) . . ? C16 Ta1 C18 55.89(12) . . ? C17 Ta1 C18 33.73(11) . . ? O1 Ta1 C20 107.51(11) . . ? N1 Ta1 C20 148.97(10) . . ? Cl2 Ta1 C20 100.32(9) . . ? Cl3 Ta1 C20 130.51(8) . . ? Cl1 Ta1 C20 75.34(8) . . ? C16 Ta1 C20 33.47(11) . . ? C17 Ta1 C20 55.77(11) . . ? C18 Ta1 C20 55.08(11) . . ? O1 Ta1 C19 130.74(11) . . ? N1 Ta1 C19 169.37(10) . . ? Cl2 Ta1 C19 80.06(9) . . ? Cl3 Ta1 C19 103.78(8) . . ? Cl1 Ta1 C19 100.02(8) . . ? C16 Ta1 C19 55.54(11) . . ? C17 Ta1 C19 55.67(11) . . ? C18 Ta1 C19 33.12(11) . . ? C20 Ta1 C19 33.07(11) . . ? O1 Ta1 C1 29.91(10) . . ? N1 Ta1 C1 29.62(10) . . ? Cl2 Ta1 C1 119.28(8) . . ? Cl3 Ta1 C1 78.92(8) . . ? Cl1 Ta1 C1 82.00(8) . . ? C16 Ta1 C1 105.70(11) . . ? C17 Ta1 C1 106.66(11) . . ? C18 Ta1 C1 135.17(11) . . ? C20 Ta1 C1 132.85(11) . . ? C19 Ta1 C1 160.65(12) . . ? C1 O1 Ta1 99.4(2) . . ? C3 C2 C7 119.8(3) . . ? C3 C2 C1 119.2(3) . . ? C7 C2 C1 120.9(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C11 C10 C9 121.8(3) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C1 N1 C8 123.3(3) . . ? C1 N1 Ta1 88.3(2) . . ? C8 N1 Ta1 147.2(2) . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 121.1(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C16 C20 C19 108.1(3) . . ? C16 C20 C25 126.1(3) . . ? C19 C20 C25 125.0(3) . . ? C16 C20 Ta1 70.5(2) . . ? C19 C20 Ta1 74.3(2) . . ? C25 C20 Ta1 129.0(2) . . ? C19 C18 C17 108.1(3) . . ? C19 C18 C23 124.1(3) . . ? C17 C18 C23 127.3(3) . . ? C19 C18 Ta1 74.46(19) . . ? C17 C18 Ta1 71.07(19) . . ? C23 C18 Ta1 126.7(2) . . ? C20 C19 C18 107.8(3) . . ? C20 C19 C24 126.6(3) . . ? C18 C19 C24 125.2(3) . . ? C20 C19 Ta1 72.7(2) . . ? C18 C19 Ta1 72.42(19) . . ? C24 C19 Ta1 126.8(2) . . ? N1 C1 O1 112.5(3) . . ? N1 C1 C2 129.7(3) . . ? O1 C1 C2 117.6(3) . . ? N1 C1 Ta1 62.05(19) . . ? O1 C1 Ta1 50.65(16) . . ? C2 C1 Ta1 166.8(2) . . ? C13 C8 C9 120.7(3) . . ? C13 C8 N1 119.7(3) . . ? C9 C8 N1 119.6(3) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C16 C17 C18 107.5(3) . . ? C16 C17 C22 126.3(3) . . ? C18 C17 C22 126.1(3) . . ? C16 C17 Ta1 72.50(19) . . ? C18 C17 Ta1 75.19(19) . . ? C22 C17 Ta1 120.9(2) . . ? C20 C16 C17 108.4(3) . . ? C20 C16 C21 125.7(3) . . ? C17 C16 C21 125.7(3) . . ? C20 C16 Ta1 76.0(2) . . ? C17 C16 Ta1 73.4(2) . . ? C21 C16 Ta1 121.0(2) . . ? C10 C9 C8 117.9(3) . . ? C10 C9 C14 117.6(3) . . ? C8 C9 C14 124.4(3) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C6 C7 C2 120.0(3) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C12 C13 C8 118.9(3) . . ? C12 C13 C15 119.6(3) . . ? C8 C13 C15 121.4(3) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 3.107 _refine_diff_density_min -1.495 _refine_diff_density_rms 0.147 #END data_ls182_0m #TrackingRef '- 4a_ls182_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841452' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta5-pentamethylcyclopendienyl)(oxo)(eta2-N-isopropyl(tert-butyl)iminoacyl) tantalum ; _chemical_name_common ; (eta5-pentamethylcyclopendienyl)(oxo)(eta2-N-isopropyl(tert- butyl)iminoacyl) tantalum ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H31 Cl N O Ta' _chemical_formula_sum 'C18 H31 Cl N O Ta' _chemical_formula_weight 493.84 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9863(4) _cell_length_b 19.3004(9) _cell_length_c 11.7122(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.886(2) _cell_angle_gamma 90.00 _cell_volume 1921.99(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.618 _cell_measurement_theta_max 30.151 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 5.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1535 _exptl_absorpt_correction_T_max 0.3097 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21963 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.15 _reflns_number_total 5671 _reflns_number_gt 4970 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0208P)^2^+1.5622P] 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 5671 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0464 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 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 Ta01 Ta 0.034170(11) 0.129523(4) 0.209790(7) 0.01536(3) Uani 1 1 d . . . Cl1 Cl 0.26032(8) 0.09911(3) 0.15095(6) 0.02716(13) Uani 1 1 d . . . O1 O -0.0966(2) 0.14924(9) 0.06799(14) 0.0213(3) Uani 1 1 d . . . C9 C 0.0120(3) 0.00379(12) 0.2300(2) 0.0226(5) Uani 1 1 d . . . C13 C -0.1378(3) 0.03209(12) 0.2121(2) 0.0203(5) Uani 1 1 d . . . C7 C 0.3485(3) 0.27636(15) 0.2134(2) 0.0293(6) Uani 1 1 d . . . H7A H 0.3535 0.2343 0.1679 0.044 Uiso 1 1 calc R . . H7B H 0.4492 0.3009 0.2341 0.044 Uiso 1 1 calc R . . H7C H 0.2644 0.3065 0.1641 0.044 Uiso 1 1 calc R . . C12 C -0.1284(3) 0.07513(12) 0.3125(2) 0.0211(5) Uani 1 1 d . . . C10 C 0.1141(3) 0.02590(13) 0.3460(2) 0.0259(5) Uani 1 1 d . . . C11 C 0.0281(3) 0.06907(13) 0.3974(2) 0.0246(5) Uani 1 1 d . . . C15 C 0.0541(4) -0.04731(14) 0.1490(3) 0.0335(6) Uani 1 1 d . . . H15A H 0.0613 -0.0938 0.1841 0.050 Uiso 1 1 calc R . . H15B H 0.1557 -0.0346 0.1406 0.050 Uiso 1 1 calc R . . H15C H -0.0271 -0.0469 0.0695 0.050 Uiso 1 1 calc R . . C18 C 0.0871(4) 0.10100(16) 0.5199(2) 0.0356(7) Uani 1 1 d . . . H18A H 0.1023 0.0648 0.5813 0.053 Uiso 1 1 calc R . . H18B H 0.0101 0.1348 0.5287 0.053 Uiso 1 1 calc R . . H18C H 0.1874 0.1244 0.5302 0.053 Uiso 1 1 calc R . . N1 N 0.1680(2) 0.21639(10) 0.29420(16) 0.0176(4) Uani 1 1 d . . . C6 C 0.3151(3) 0.25683(13) 0.3281(2) 0.0213(5) Uani 1 1 d . . . H6 H 0.3014 0.2999 0.3710 0.026 Uiso 1 1 calc R . . C5 C 0.0098(3) 0.35696(13) 0.2774(3) 0.0297(6) Uani 1 1 d . . . H5A H 0.1219 0.3661 0.3179 0.044 Uiso 1 1 calc R . . H5B H -0.0520 0.3968 0.2879 0.044 Uiso 1 1 calc R . . H5C H -0.0089 0.3492 0.1912 0.044 Uiso 1 1 calc R . . C2 C -0.0394(3) 0.29239(12) 0.3325(2) 0.0177(4) Uani 1 1 d . . . C17 C -0.2674(3) 0.10808(15) 0.3331(3) 0.0317(6) Uani 1 1 d . . . H17A H -0.3268 0.1343 0.2611 0.048 Uiso 1 1 calc R . . H17B H -0.2320 0.1395 0.4024 0.048 Uiso 1 1 calc R . . H17C H -0.3350 0.0721 0.3493 0.048 Uiso 1 1 calc R . . C16 C -0.2823(3) 0.02014(14) 0.1070(2) 0.0276(5) Uani 1 1 d . . . H16A H -0.2864 0.0538 0.0434 0.041 Uiso 1 1 calc R . . H16B H -0.3753 0.0256 0.1324 0.041 Uiso 1 1 calc R . . H16C H -0.2801 -0.0269 0.0760 0.041 Uiso 1 1 calc R . . C1 C 0.0298(3) 0.22764(12) 0.29607(19) 0.0165(4) Uani 1 1 d . . . C4 C 0.0169(3) 0.29822(15) 0.4697(2) 0.0320(6) Uani 1 1 d . . . H4A H -0.0157 0.2570 0.5042 0.048 Uiso 1 1 calc R . . H4B H -0.0292 0.3395 0.4935 0.048 Uiso 1 1 calc R . . H4C H 0.1318 0.3019 0.4995 0.048 Uiso 1 1 calc R . . C14 C 0.2812(4) 0.00339(17) 0.4009(3) 0.0419(7) Uani 1 1 d . . . H14A H 0.3355 0.0349 0.4668 0.063 Uiso 1 1 calc R . . H14B H 0.3336 0.0043 0.3394 0.063 Uiso 1 1 calc R . . H14C H 0.2842 -0.0438 0.4326 0.063 Uiso 1 1 calc R . . C8 C 0.4435(3) 0.21276(16) 0.4127(3) 0.0322(6) Uani 1 1 d . . . H8A H 0.4135 0.2000 0.4833 0.048 Uiso 1 1 calc R . . H8B H 0.5420 0.2391 0.4389 0.048 Uiso 1 1 calc R . . H8C H 0.4579 0.1707 0.3706 0.048 Uiso 1 1 calc R . . C3 C -0.2177(3) 0.28752(14) 0.2851(3) 0.0320(6) Uani 1 1 d . . . H3A H -0.2524 0.2795 0.1978 0.048 Uiso 1 1 calc R . . H3B H -0.2632 0.3309 0.3020 0.048 Uiso 1 1 calc R . . H3C H -0.2524 0.2490 0.3249 0.048 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 Ta01 0.01858(5) 0.01519(5) 0.01338(5) -0.00054(3) 0.00666(4) -0.00167(3) Cl1 0.0281(3) 0.0274(3) 0.0317(3) -0.0091(2) 0.0176(3) -0.0020(2) O1 0.0257(9) 0.0221(8) 0.0149(7) 0.0023(6) 0.0050(7) -0.0041(7) C9 0.0340(14) 0.0138(11) 0.0220(11) 0.0032(8) 0.0119(10) 0.0006(9) C13 0.0275(13) 0.0148(10) 0.0211(11) 0.0015(8) 0.0112(10) -0.0048(9) C7 0.0291(14) 0.0350(14) 0.0309(13) -0.0097(11) 0.0194(11) -0.0129(11) C12 0.0288(13) 0.0166(11) 0.0226(11) 0.0015(9) 0.0149(10) -0.0034(9) C10 0.0295(14) 0.0226(12) 0.0237(12) 0.0089(10) 0.0062(10) 0.0007(10) C11 0.0355(14) 0.0229(12) 0.0159(10) 0.0023(9) 0.0090(10) -0.0079(10) C15 0.0471(18) 0.0192(13) 0.0398(15) -0.0014(11) 0.0218(14) 0.0047(12) C18 0.0527(19) 0.0351(15) 0.0188(12) -0.0013(11) 0.0114(12) -0.0128(14) N1 0.0190(10) 0.0210(10) 0.0141(8) -0.0028(7) 0.0071(7) -0.0019(8) C6 0.0181(11) 0.0261(12) 0.0216(11) -0.0087(9) 0.0092(9) -0.0055(9) C5 0.0350(15) 0.0178(12) 0.0428(16) -0.0001(11) 0.0217(13) -0.0013(10) C2 0.0174(11) 0.0180(11) 0.0197(10) -0.0008(8) 0.0085(9) -0.0011(8) C17 0.0360(15) 0.0271(13) 0.0433(16) -0.0027(12) 0.0284(13) -0.0053(12) C16 0.0315(14) 0.0245(13) 0.0251(12) -0.0006(10) 0.0069(11) -0.0078(11) C1 0.0188(11) 0.0194(11) 0.0117(9) 0.0013(8) 0.0054(8) -0.0007(9) C4 0.0364(16) 0.0391(16) 0.0220(12) -0.0033(11) 0.0117(11) 0.0117(12) C14 0.0366(17) 0.0439(18) 0.0381(16) 0.0136(14) 0.0022(13) 0.0083(14) C8 0.0203(13) 0.0416(16) 0.0325(14) -0.0084(12) 0.0056(11) 0.0014(11) C3 0.0177(13) 0.0231(13) 0.0520(18) -0.0009(12) 0.0069(12) 0.0021(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ta01 O1 1.7379(16) . ? Ta01 N1 2.1131(19) . ? Ta01 C1 2.153(2) . ? Ta01 C12 2.413(2) . ? Ta01 Cl1 2.4199(6) . ? Ta01 C13 2.440(2) . ? Ta01 C9 2.452(2) . ? Ta01 C11 2.503(2) . ? Ta01 C10 2.514(2) . ? C9 C13 1.404(4) . ? C9 C10 1.436(3) . ? C9 C15 1.499(4) . ? C13 C12 1.420(3) . ? C13 C16 1.490(3) . ? C7 C6 1.516(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C12 C11 1.441(4) . ? C12 C17 1.489(4) . ? C10 C11 1.398(4) . ? C10 C14 1.494(4) . ? C11 C18 1.493(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N1 C1 1.268(3) . ? N1 C6 1.475(3) . ? C6 C8 1.515(4) . ? C6 H6 1.0000 . ? C5 C2 1.533(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C2 C1 1.517(3) . ? C2 C3 1.519(3) . ? C2 C4 1.524(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 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 O1 Ta01 N1 112.32(8) . . ? O1 Ta01 C1 98.43(8) . . ? N1 Ta01 C1 34.56(8) . . ? O1 Ta01 C12 103.92(8) . . ? N1 Ta01 C12 117.18(8) . . ? C1 Ta01 C12 92.45(8) . . ? O1 Ta01 Cl1 98.70(6) . . ? N1 Ta01 Cl1 85.55(5) . . ? C1 Ta01 Cl1 119.44(6) . . ? C12 Ta01 Cl1 137.42(6) . . ? O1 Ta01 C13 86.82(8) . . ? N1 Ta01 C13 150.82(7) . . ? C1 Ta01 C13 124.41(8) . . ? C12 Ta01 C13 34.03(8) . . ? Cl1 Ta01 C13 114.18(6) . . ? O1 Ta01 C9 104.94(8) . . ? N1 Ta01 C9 142.35(8) . . ? C1 Ta01 C9 144.17(8) . . ? C12 Ta01 C9 55.96(8) . . ? Cl1 Ta01 C9 83.65(6) . . ? C13 Ta01 C9 33.36(8) . . ? O1 Ta01 C11 137.79(8) . . ? N1 Ta01 C11 97.46(8) . . ? C1 Ta01 C11 89.38(8) . . ? C12 Ta01 C11 34.02(8) . . ? Cl1 Ta01 C11 113.30(7) . . ? C13 Ta01 C11 55.77(8) . . ? C9 Ta01 C11 55.16(8) . . ? O1 Ta01 C10 138.30(8) . . ? N1 Ta01 C10 109.38(8) . . ? C1 Ta01 C10 116.55(8) . . ? C12 Ta01 C10 55.41(9) . . ? Cl1 Ta01 C10 83.90(6) . . ? C13 Ta01 C10 55.37(9) . . ? C9 Ta01 C10 33.60(8) . . ? C11 Ta01 C10 32.36(9) . . ? C13 C9 C10 108.3(2) . . ? C13 C9 C15 126.0(2) . . ? C10 C9 C15 125.4(2) . . ? C13 C9 Ta01 72.82(13) . . ? C10 C9 Ta01 75.53(14) . . ? C15 C9 Ta01 123.02(17) . . ? C9 C13 C12 107.9(2) . . ? C9 C13 C16 126.9(2) . . ? C12 C13 C16 125.3(2) . . ? C9 C13 Ta01 73.82(14) . . ? C12 C13 Ta01 71.96(13) . . ? C16 C13 Ta01 119.74(16) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C12 C11 107.9(2) . . ? C13 C12 C17 123.8(2) . . ? C11 C12 C17 127.3(2) . . ? C13 C12 Ta01 74.02(13) . . ? C11 C12 Ta01 76.43(14) . . ? C17 C12 Ta01 124.73(17) . . ? C11 C10 C9 108.1(2) . . ? C11 C10 C14 127.3(3) . . ? C9 C10 C14 124.5(3) . . ? C11 C10 Ta01 73.42(14) . . ? C9 C10 Ta01 70.87(13) . . ? C14 C10 Ta01 123.08(19) . . ? C10 C11 C12 107.7(2) . . ? C10 C11 C18 125.9(3) . . ? C12 C11 C18 126.4(3) . . ? C10 C11 Ta01 74.22(14) . . ? C12 C11 Ta01 69.55(13) . . ? C18 C11 Ta01 123.35(17) . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 N1 C6 134.6(2) . . ? C1 N1 Ta01 74.43(13) . . ? C6 N1 Ta01 150.55(15) . . ? N1 C6 C8 107.8(2) . . ? N1 C6 C7 108.08(19) . . ? C8 C6 C7 113.1(2) . . ? N1 C6 H6 109.3 . . ? C8 C6 H6 109.3 . . ? C7 C6 H6 109.3 . . ? 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 . . ? C1 C2 C3 109.0(2) . . ? C1 C2 C4 109.32(19) . . ? C3 C2 C4 109.9(2) . . ? C1 C2 C5 110.52(19) . . ? C3 C2 C5 108.1(2) . . ? C4 C2 C5 110.0(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C1 C2 129.7(2) . . ? N1 C1 Ta01 71.01(13) . . ? C2 C1 Ta01 158.10(17) . . ? 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 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.540 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.105 #END data_ls206 #TrackingRef '- 4b_ls206_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841453' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta5-pentamethylcyclopendienyl)(eta2-N-2,6-dimethylphenyl(tert-butyl)iminoacyl) (oxo)tantalum ; _chemical_name_common ; (eta5-pentamethylcyclopendienyl)(eta2-N-2,6- dimethylphenyl(tert-butyl)iminoacyl) (oxo)tantalum ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H33 Cl N O Ta, C13 H19 N O' _chemical_formula_sum 'C36 H52 Cl N2 O2 Ta' _chemical_formula_weight 761.20 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' O O 0.0106 0.0060 '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 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 8.4087(8) _cell_length_b 19.2914(17) _cell_length_c 22.039(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.868(3) _cell_angle_gamma 90.00 _cell_volume 3562.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 8026 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 29.96 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 3.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_T_max 0.528 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39833 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 29.96 _reflns_number_total 10316 _reflns_number_gt 8920 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0113P)^2^+1.7372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10316 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0496 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.004 _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 C14 C 0.6068(3) 0.85379(11) -0.17339(9) 0.0230(4) Uani 1 1 d . . . C15 C 0.7740(3) 0.84507(10) -0.16718(9) 0.0205(4) Uani 1 1 d . . . C16 C 0.8185(2) 0.80723(10) -0.21812(8) 0.0166(4) Uani 1 1 d . . . C17 C 0.6774(2) 0.79583(10) -0.25803(8) 0.0155(4) Uani 1 1 d . . . C18 C 0.5484(2) 0.82441(11) -0.23063(9) 0.0208(4) Uani 1 1 d . . . C19 C 0.5088(4) 0.89404(13) -0.13168(12) 0.0434(7) Uani 1 1 d . . . H19A H 0.5658 0.8965 -0.0911 0.065 Uiso 1 1 calc R . . H19B H 0.4059 0.8708 -0.1290 0.065 Uiso 1 1 calc R . . H19C H 0.4907 0.9410 -0.1477 0.065 Uiso 1 1 calc R . . C20 C 0.8891(3) 0.87181(13) -0.11690(10) 0.0400(7) Uani 1 1 d . . . H20A H 0.9523 0.9096 -0.1324 0.060 Uiso 1 1 calc R . . H20B H 0.9604 0.8342 -0.1019 0.060 Uiso 1 1 calc R . . H20C H 0.8299 0.8891 -0.0836 0.060 Uiso 1 1 calc R . . C21 C 0.9878(2) 0.79677(12) -0.23220(11) 0.0290(5) Uani 1 1 d . . . H21A H 1.0381 0.8419 -0.2377 0.044 Uiso 1 1 calc R . . H21B H 0.9900 0.7696 -0.2697 0.044 Uiso 1 1 calc R . . H21C H 1.0463 0.7720 -0.1985 0.044 Uiso 1 1 calc R . . C22 C 0.6707(3) 0.76452(12) -0.32088(10) 0.0273(5) Uani 1 1 d . . . H22A H 0.5839 0.7305 -0.3255 0.041 Uiso 1 1 calc R . . H22B H 0.7723 0.7415 -0.3265 0.041 Uiso 1 1 calc R . . H22C H 0.6516 0.8012 -0.3514 0.041 Uiso 1 1 calc R . . C23 C 0.3799(3) 0.82890(15) -0.25823(12) 0.0406(7) Uani 1 1 d . . . H23A H 0.3654 0.8720 -0.2816 0.061 Uiso 1 1 calc R . . H23B H 0.3069 0.8284 -0.2258 0.061 Uiso 1 1 calc R . . H23C H 0.3569 0.7892 -0.2853 0.061 Uiso 1 1 calc R . . C1 C 0.7507(2) 0.63871(10) -0.20298(8) 0.0152(4) Uani 1 1 d . . . C2 C 0.8813(2) 0.59133(10) -0.22132(9) 0.0195(4) Uani 1 1 d . . . C5 C 0.9330(3) 0.61293(12) -0.28342(10) 0.0316(5) Uani 1 1 d . . . H5A H 0.8418 0.6096 -0.3140 0.047 Uiso 1 1 calc R . . H5B H 1.0185 0.5822 -0.2947 0.047 Uiso 1 1 calc R . . H5C H 0.9719 0.6608 -0.2813 0.047 Uiso 1 1 calc R . . C3 C 1.0196(3) 0.60179(12) -0.17144(10) 0.0293(5) Uani 1 1 d . . . H3A H 1.0499 0.6508 -0.1696 0.044 Uiso 1 1 calc R . . H3B H 1.1115 0.5739 -0.1811 0.044 Uiso 1 1 calc R . . H3C H 0.9853 0.5873 -0.1320 0.044 Uiso 1 1 calc R . . C4 C 0.8324(3) 0.51475(11) -0.22388(11) 0.0284(5) Uani 1 1 d . . . H4A H 0.7999 0.5004 -0.1841 0.043 Uiso 1 1 calc R . . H4B H 0.9231 0.4865 -0.2342 0.043 Uiso 1 1 calc R . . H4C H 0.7431 0.5084 -0.2549 0.043 Uiso 1 1 calc R . . C6 C 0.5070(2) 0.56672(10) -0.18984(9) 0.0181(4) Uani 1 1 d . . . C11 C 0.4961(3) 0.53187(11) -0.13479(9) 0.0222(4) Uani 1 1 d . . . C10 C 0.3932(3) 0.47539(11) -0.13500(11) 0.0274(5) Uani 1 1 d . . . H10 H 0.3850 0.4500 -0.0984 0.033 Uiso 1 1 calc R . . C9 C 0.3027(3) 0.45543(11) -0.18728(11) 0.0287(5) Uani 1 1 d . . . H9 H 0.2331 0.4167 -0.1865 0.034 Uiso 1 1 calc R . . C8 C 0.3135(2) 0.49188(11) -0.24082(11) 0.0258(5) Uani 1 1 d . . . H8 H 0.2507 0.4778 -0.2765 0.031 Uiso 1 1 calc R . . C7 C 0.4143(2) 0.54875(11) -0.24347(9) 0.0215(4) Uani 1 1 d . . . C13 C 0.5932(3) 0.55465(12) -0.07788(10) 0.0295(5) Uani 1 1 d . . . H13A H 0.7068 0.5537 -0.0847 0.044 Uiso 1 1 calc R . . H13B H 0.5736 0.5232 -0.0444 0.044 Uiso 1 1 calc R . . H13C H 0.5624 0.6019 -0.0674 0.044 Uiso 1 1 calc R . . C12 C 0.4217(3) 0.59021(12) -0.30073(10) 0.0286(5) Uani 1 1 d . . . H12A H 0.3483 0.5703 -0.3330 0.043 Uiso 1 1 calc R . . H12B H 0.5307 0.5892 -0.3133 0.043 Uiso 1 1 calc R . . H12C H 0.3908 0.6383 -0.2933 0.043 Uiso 1 1 calc R . . C24 C 1.0071(2) 0.73209(10) 0.06712(9) 0.0193(4) Uani 1 1 d . . . C25 C 1.0629(3) 0.66230(11) 0.04352(9) 0.0224(4) Uani 1 1 d . . . C26 C 0.9199(3) 0.61409(13) 0.03148(13) 0.0402(6) Uani 1 1 d . . . H26A H 0.8678 0.6076 0.0692 0.060 Uiso 1 1 calc R . . H26B H 0.9562 0.5692 0.0172 0.060 Uiso 1 1 calc R . . H26C H 0.8439 0.6346 0.0004 0.060 Uiso 1 1 calc R . . C27 C 1.1449(3) 0.67342(13) -0.01565(10) 0.0333(5) Uani 1 1 d . . . H27A H 1.0669 0.6912 -0.0475 0.050 Uiso 1 1 calc R . . H27B H 1.1880 0.6292 -0.0289 0.050 Uiso 1 1 calc R . . H27C H 1.2320 0.7069 -0.0083 0.050 Uiso 1 1 calc R . . C28 C 1.1825(3) 0.63077(14) 0.09162(11) 0.0429(7) Uani 1 1 d . . . H28A H 1.2738 0.6621 0.0992 0.064 Uiso 1 1 calc R . . H28B H 1.2194 0.5860 0.0771 0.064 Uiso 1 1 calc R . . H28C H 1.1312 0.6239 0.1295 0.064 Uiso 1 1 calc R . . C29 C 0.8426(3) 0.83492(11) 0.03984(8) 0.0197(4) Uani 1 1 d . . . C30 C 0.9467(3) 0.89141(12) 0.04828(9) 0.0253(5) Uani 1 1 d . . . C31 C 0.8816(3) 0.95661(12) 0.05697(10) 0.0340(6) Uani 1 1 d . . . H31 H 0.9503 0.9955 0.0634 0.041 Uiso 1 1 calc R . . C32 C 0.7181(3) 0.96550(14) 0.05632(10) 0.0391(6) Uani 1 1 d . . . H32 H 0.6753 1.0104 0.0619 0.047 Uiso 1 1 calc R . . C33 C 0.6174(3) 0.90961(14) 0.04769(10) 0.0341(6) Uani 1 1 d . . . H33 H 0.5055 0.9164 0.0477 0.041 Uiso 1 1 calc R . . C34 C 0.6766(3) 0.84317(12) 0.03896(9) 0.0247(5) Uani 1 1 d . . . C35 C 1.1243(3) 0.88339(13) 0.04646(11) 0.0315(5) Uani 1 1 d . . . H35A H 1.1736 0.9293 0.0442 0.047 Uiso 1 1 calc R . . H35B H 1.1465 0.8562 0.0106 0.047 Uiso 1 1 calc R . . H35C H 1.1685 0.8595 0.0834 0.047 Uiso 1 1 calc R . . C36 C 0.5645(3) 0.78332(13) 0.02734(10) 0.0307(5) Uani 1 1 d . . . H36A H 0.4628 0.7938 0.0440 0.046 Uiso 1 1 calc R . . H36B H 0.6113 0.7416 0.0470 0.046 Uiso 1 1 calc R . . H36C H 0.5461 0.7754 -0.0166 0.046 Uiso 1 1 calc R . . N1 N 0.60907(19) 0.62628(8) -0.19021(7) 0.0161(3) Uani 1 1 d . . . N2 N 0.9044(2) 0.76790(9) 0.02761(8) 0.0189(4) Uani 1 1 d . . . O1 O 0.76476(17) 0.72461(7) -0.09056(6) 0.0182(3) Uani 1 1 d . . . O2 O 1.05084(19) 0.75422(8) 0.11794(6) 0.0255(3) Uani 1 1 d . . . Cl1 Cl 0.38644(6) 0.72480(3) -0.13364(2) 0.02332(11) Uani 1 1 d . . . Ta1 Ta 0.656420(8) 0.729749(4) -0.161808(3) 0.01190(3) Uani 1 1 d . . . HN2 H 0.867(3) 0.7522(13) -0.0039(11) 0.025(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C14 0.0341(12) 0.0139(10) 0.0224(10) 0.0047(8) 0.0112(9) 0.0055(9) C15 0.0319(11) 0.0135(9) 0.0157(9) 0.0035(7) -0.0005(8) -0.0074(9) C16 0.0146(9) 0.0149(9) 0.0205(9) 0.0054(8) 0.0013(7) -0.0025(8) C17 0.0168(9) 0.0164(9) 0.0131(9) 0.0031(7) 0.0006(7) -0.0018(7) C18 0.0161(9) 0.0234(11) 0.0228(10) 0.0102(8) 0.0015(8) 0.0028(8) C19 0.0691(19) 0.0243(12) 0.0418(15) 0.0047(11) 0.0335(13) 0.0163(13) C20 0.0610(18) 0.0332(13) 0.0235(12) 0.0015(10) -0.0092(11) -0.0268(13) C21 0.0150(10) 0.0263(12) 0.0461(14) 0.0109(10) 0.0046(9) -0.0005(9) C22 0.0372(13) 0.0277(12) 0.0168(10) -0.0012(9) 0.0011(9) -0.0080(10) C23 0.0183(11) 0.0606(18) 0.0423(14) 0.0264(13) -0.0002(10) 0.0060(11) C1 0.0181(9) 0.0166(9) 0.0106(8) 0.0001(7) -0.0002(7) -0.0013(8) C2 0.0197(10) 0.0169(10) 0.0224(10) -0.0028(8) 0.0041(8) 0.0021(8) C5 0.0364(13) 0.0295(12) 0.0307(12) -0.0002(10) 0.0139(10) 0.0091(10) C3 0.0214(11) 0.0299(12) 0.0358(13) -0.0077(10) -0.0022(9) 0.0073(9) C4 0.0281(12) 0.0175(10) 0.0399(13) -0.0047(9) 0.0047(10) 0.0032(9) C6 0.0164(9) 0.0136(9) 0.0245(10) -0.0045(8) 0.0037(8) -0.0026(8) C11 0.0236(10) 0.0172(10) 0.0265(11) -0.0018(8) 0.0057(8) -0.0030(8) C10 0.0289(12) 0.0164(10) 0.0385(13) 0.0017(9) 0.0116(10) -0.0030(9) C9 0.0207(11) 0.0162(10) 0.0502(15) -0.0085(10) 0.0091(10) -0.0059(9) C8 0.0180(10) 0.0216(11) 0.0378(13) -0.0145(9) 0.0029(9) -0.0010(9) C7 0.0175(10) 0.0201(10) 0.0271(11) -0.0095(8) 0.0026(8) 0.0004(8) C13 0.0391(13) 0.0254(11) 0.0239(11) 0.0046(9) 0.0026(10) -0.0072(10) C12 0.0281(12) 0.0333(13) 0.0235(11) -0.0062(9) -0.0030(9) -0.0036(10) C24 0.0198(10) 0.0228(10) 0.0152(9) 0.0027(8) 0.0016(7) -0.0021(8) C25 0.0245(11) 0.0218(10) 0.0202(10) 0.0015(8) -0.0020(8) 0.0008(9) C26 0.0429(15) 0.0226(12) 0.0548(17) 0.0028(11) 0.0031(12) -0.0079(11) C27 0.0352(13) 0.0364(14) 0.0290(12) -0.0031(10) 0.0074(10) 0.0057(11) C28 0.0566(18) 0.0369(14) 0.0328(14) 0.0015(11) -0.0108(12) 0.0197(13) C29 0.0255(10) 0.0220(10) 0.0114(9) -0.0014(7) 0.0003(8) 0.0029(8) C30 0.0334(12) 0.0265(11) 0.0155(10) -0.0018(8) -0.0017(8) -0.0018(10) C31 0.0539(16) 0.0238(12) 0.0240(12) -0.0050(9) 0.0022(11) -0.0013(11) C32 0.0595(18) 0.0321(14) 0.0266(12) -0.0024(10) 0.0100(12) 0.0183(13) C33 0.0365(13) 0.0446(15) 0.0217(11) 0.0010(10) 0.0059(10) 0.0168(12) C34 0.0261(11) 0.0356(13) 0.0123(9) 0.0013(8) 0.0005(8) 0.0046(10) C35 0.0304(12) 0.0306(13) 0.0321(13) 0.0008(10) -0.0047(10) -0.0081(10) C36 0.0213(11) 0.0488(15) 0.0220(11) 0.0005(10) 0.0022(9) -0.0015(10) N1 0.0190(8) 0.0143(8) 0.0150(8) -0.0015(6) 0.0008(6) -0.0032(6) N2 0.0202(9) 0.0216(9) 0.0141(8) -0.0026(7) -0.0031(7) 0.0006(7) O1 0.0214(7) 0.0170(7) 0.0159(7) -0.0001(5) 0.0002(5) -0.0009(6) O2 0.0291(8) 0.0315(8) 0.0151(7) -0.0016(6) -0.0025(6) 0.0014(7) Cl1 0.0161(2) 0.0273(3) 0.0274(3) -0.0012(2) 0.00652(19) -0.0023(2) Ta1 0.01148(4) 0.01226(4) 0.01184(4) -0.00025(3) 0.00032(3) -0.00097(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C14 C15 1.411(3) . ? C14 C18 1.431(3) . ? C14 C19 1.502(3) . ? C14 Ta1 2.439(2) . ? C15 C16 1.416(3) . ? C15 C20 1.500(3) . ? C15 Ta1 2.4414(19) . ? C16 C17 1.433(3) . ? C16 C21 1.497(3) . ? C16 Ta1 2.4327(19) . ? C17 C18 1.399(3) . ? C17 C22 1.508(3) . ? C17 Ta1 2.4933(18) . ? C18 C23 1.497(3) . ? C18 Ta1 2.4953(19) . ? 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 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C1 N1 1.270(2) . ? C1 C2 1.510(3) . ? C1 Ta1 2.1585(19) . ? C2 C5 1.529(3) . ? C2 C4 1.533(3) . ? C2 C3 1.544(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 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 . ? C6 C11 1.397(3) . ? C6 C7 1.403(3) . ? C6 N1 1.435(2) . ? C11 C10 1.391(3) . ? C11 C13 1.503(3) . ? C10 C9 1.381(3) . ? C10 H10 0.9500 . ? C9 C8 1.383(3) . ? C9 H9 0.9500 . ? C8 C7 1.391(3) . ? C8 H8 0.9500 . ? C7 C12 1.500(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C24 O2 1.226(2) . ? C24 N2 1.361(3) . ? C24 C25 1.531(3) . ? C25 C28 1.525(3) . ? C25 C26 1.526(3) . ? C25 C27 1.541(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.400(3) . ? C29 C34 1.404(3) . ? C29 N2 1.427(3) . ? C30 C31 1.391(3) . ? C30 C35 1.506(3) . ? C31 C32 1.385(4) . ? C31 H31 0.9500 . ? C32 C33 1.374(4) . ? C32 H32 0.9500 . ? C33 C34 1.394(3) . ? C33 H33 0.9500 . ? C34 C36 1.499(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N1 Ta1 2.1195(16) . ? N2 HN2 0.80(2) . ? O1 Ta1 1.7500(13) . ? Cl1 Ta1 2.4057(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C14 C18 107.61(17) . . ? C15 C14 C19 126.6(2) . . ? C18 C14 C19 125.4(2) . . ? C15 C14 Ta1 73.30(11) . . ? C18 C14 Ta1 75.32(12) . . ? C19 C14 Ta1 122.76(14) . . ? C14 C15 C16 108.23(17) . . ? C14 C15 C20 127.3(2) . . ? C16 C15 C20 124.4(2) . . ? C14 C15 Ta1 73.09(11) . . ? C16 C15 Ta1 72.78(11) . . ? C20 C15 Ta1 121.08(14) . . ? C15 C16 C17 107.76(17) . . ? C15 C16 C21 123.65(18) . . ? C17 C16 C21 127.22(19) . . ? C15 C16 Ta1 73.45(11) . . ? C17 C16 Ta1 75.42(11) . . ? C21 C16 Ta1 127.37(14) . . ? C18 C17 C16 107.85(17) . . ? C18 C17 C22 125.78(18) . . ? C16 C17 C22 126.15(19) . . ? C18 C17 Ta1 73.80(11) . . ? C16 C17 Ta1 70.79(10) . . ? C22 C17 Ta1 125.22(14) . . ? C17 C18 C14 108.43(17) . . ? C17 C18 C23 126.1(2) . . ? C14 C18 C23 125.3(2) . . ? C17 C18 Ta1 73.64(11) . . ? C14 C18 Ta1 70.98(11) . . ? C23 C18 Ta1 124.93(15) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C1 C2 131.47(18) . . ? N1 C1 Ta1 71.06(11) . . ? C2 C1 Ta1 155.03(14) . . ? C1 C2 C5 110.06(17) . . ? C1 C2 C4 113.21(17) . . ? C5 C2 C4 108.99(17) . . ? C1 C2 C3 104.56(16) . . ? C5 C2 C3 110.34(18) . . ? C4 C2 C3 109.61(18) . . ? 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 . . ? 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 . . ? C11 C6 C7 122.68(19) . . ? C11 C6 N1 118.30(17) . . ? C7 C6 N1 118.87(18) . . ? C10 C11 C6 117.45(19) . . ? C10 C11 C13 121.7(2) . . ? C6 C11 C13 120.86(18) . . ? C9 C10 C11 121.3(2) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C7 C6 117.2(2) . . ? C8 C7 C12 121.66(19) . . ? C6 C7 C12 121.17(19) . . ? 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 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C24 N2 122.19(19) . . ? O2 C24 C25 122.66(18) . . ? N2 C24 C25 115.15(17) . . ? C28 C25 C26 110.0(2) . . ? C28 C25 C24 108.53(17) . . ? C26 C25 C24 109.58(18) . . ? C28 C25 C27 109.1(2) . . ? C26 C25 C27 109.89(19) . . ? C24 C25 C27 109.71(18) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 121.5(2) . . ? C30 C29 N2 119.79(19) . . ? C34 C29 N2 118.53(19) . . ? C31 C30 C29 118.3(2) . . ? C31 C30 C35 119.9(2) . . ? C29 C30 C35 121.8(2) . . ? C32 C31 C30 120.8(2) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 121.2(2) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C33 C34 C29 117.9(2) . . ? C33 C34 C36 120.3(2) . . ? C29 C34 C36 121.7(2) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 C6 136.50(17) . . ? C1 N1 Ta1 74.42(11) . . ? C6 N1 Ta1 148.22(13) . . ? C24 N2 C29 124.05(17) . . ? C24 N2 HN2 123.0(18) . . ? C29 N2 HN2 112.8(18) . . ? O1 Ta1 N1 106.39(6) . . ? O1 Ta1 C1 98.59(7) . . ? N1 Ta1 C1 34.52(6) . . ? O1 Ta1 Cl1 101.36(5) . . ? N1 Ta1 Cl1 83.17(5) . . ? C1 Ta1 Cl1 117.68(5) . . ? O1 Ta1 C16 102.77(6) . . ? N1 Ta1 C16 121.82(6) . . ? C1 Ta1 C16 92.51(7) . . ? Cl1 Ta1 C16 137.54(5) . . ? O1 Ta1 C14 102.76(7) . . ? N1 Ta1 C14 150.11(7) . . ? C1 Ta1 C14 145.09(7) . . ? Cl1 Ta1 C14 84.78(5) . . ? C16 Ta1 C14 56.09(7) . . ? O1 Ta1 C15 85.01(6) . . ? N1 Ta1 C15 155.58(7) . . ? C1 Ta1 C15 123.80(7) . . ? Cl1 Ta1 C15 116.33(5) . . ? C16 Ta1 C15 33.77(7) . . ? C14 Ta1 C15 33.61(7) . . ? O1 Ta1 C17 136.31(6) . . ? N1 Ta1 C17 104.79(6) . . ? C1 Ta1 C17 90.20(7) . . ? Cl1 Ta1 C17 112.10(5) . . ? C16 Ta1 C17 33.79(6) . . ? C14 Ta1 C17 55.47(6) . . ? C15 Ta1 C17 55.58(6) . . ? O1 Ta1 C18 136.20(6) . . ? N1 Ta1 C18 117.40(6) . . ? C1 Ta1 C18 117.88(7) . . ? Cl1 Ta1 C18 83.29(5) . . ? C16 Ta1 C18 55.32(6) . . ? C14 Ta1 C18 33.70(7) . . ? C15 Ta1 C18 55.36(7) . . ? C17 Ta1 C18 32.56(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.878 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.091 #END data_ls206_7b_ls307r_v2 #TrackingRef '- 7b_ls307r_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841454' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (eta5-pentamethylcyclopendienyl)(eta3-N-2,6-dimethylphenyl(tert-butyl)amidate) (mu-eta1,eta1-dinitrogen)tantalum ; _chemical_name_common ; (eta5-pentamethylcyclopendienyl)(eta3-N-2,6- dimethylphenyl(tert-butyl)amidate) (mu-eta1,eta1-dinitrogen)tantalum ; _chemical_melting_point ? _chemical_formula_moiety '2(C46 H66 Cl2 N4 O2 Ta2), 3(C7 H8)' _chemical_formula_sum 'C113 H156 Cl4 N8 O4 Ta4' _chemical_formula_weight 2556.06 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.798(2) _cell_length_b 18.392(4) _cell_length_c 28.086(6) _cell_angle_alpha 93.870(10) _cell_angle_beta 93.340(10) _cell_angle_gamma 90.310(10) _cell_volume 5555(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7547 _cell_measurement_theta_min 2.5345 _cell_measurement_theta_max 27.8985 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 4.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.665 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 105750 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.05 _reflns_number_total 26492 _reflns_number_gt 19547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; No additional symmetry was found after running ADDSYM in PLATON. 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^)+(0.0162P)^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 26492 _refine_ls_number_parameters 1241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Ta2 Ta 0.300677(13) 0.182617(9) 0.600801(6) 0.01411(4) Uani 1 1 d . . . Ta4 Ta 0.312846(13) 0.183869(9) 1.037931(6) 0.01569(4) Uani 1 1 d . . . Ta3 Ta 0.161481(13) 0.301040(9) 0.895426(6) 0.01355(4) Uani 1 1 d . . . Ta1 Ta 0.175201(13) 0.310875(9) 0.459785(6) 0.01515(4) Uani 1 1 d . . . Cl1 Cl -0.00118(8) 0.23610(5) 0.42970(4) 0.0216(2) Uani 1 1 d . . . Cl4 Cl 0.48375(8) 0.26647(6) 1.06217(4) 0.0225(2) Uani 1 1 d . . . Cl2 Cl 0.20051(8) 0.26087(5) 0.65897(4) 0.0204(2) Uani 1 1 d . . . Cl3 Cl 0.26372(8) 0.22478(5) 0.83678(4) 0.0199(2) Uani 1 1 d . . . C33 C 0.1365(4) 0.2948(2) 0.30845(15) 0.0270(10) Uani 1 1 d . . . H33A H 0.0915 0.3191 0.3333 0.040 Uiso 1 1 calc R . . H33B H 0.0902 0.2970 0.2784 0.040 Uiso 1 1 calc R . . H33C H 0.2156 0.3184 0.3069 0.040 Uiso 1 1 calc R . . C95 C 0.4067(4) -0.0043(3) 0.77996(17) 0.0321(12) Uani 1 1 d . . . H95 H 0.3229 -0.0168 0.7784 0.039 Uiso 1 1 calc R . . N2 N 0.2427(3) 0.22428(17) 0.54756(11) 0.0167(7) Uani 1 1 d . . . N6 N 0.2519(3) 0.23258(17) 0.98844(11) 0.0167(7) Uani 1 1 d . . . C58 C 0.3790(4) 0.0901(2) 0.97932(15) 0.0218(10) Uani 1 1 d . . . N1 N 0.2234(3) 0.25583(17) 0.50810(11) 0.0153(7) Uani 1 1 d . . . N5 N 0.2246(3) 0.26067(17) 0.94832(11) 0.0147(7) Uani 1 1 d . . . C47 C -0.0183(3) 0.2248(2) 0.86802(15) 0.0199(9) Uani 1 1 d . . . O2 O 0.2899(2) 0.07183(14) 0.57157(10) 0.0173(6) Uani 1 1 d . . . N8 N 0.2341(3) 0.24074(18) 1.10100(12) 0.0186(8) Uani 1 1 d . . . C12 C 0.4821(3) 0.2572(2) 0.62843(15) 0.0211(10) Uani 1 1 d . . . O4 O 0.1343(2) 0.15264(15) 1.06081(10) 0.0220(7) Uani 1 1 d . . . O3 O 0.1679(2) 0.41084(14) 0.92642(9) 0.0179(6) Uani 1 1 d . . . C2 C 0.1168(4) 0.4040(2) 0.52030(15) 0.0250(10) Uani 1 1 d . . . C34 C 0.1913(3) 0.0537(2) 0.59199(13) 0.0162(9) Uani 1 1 d . . . O1 O 0.3592(2) 0.33798(15) 0.44005(10) 0.0223(7) Uani 1 1 d . . . N3 N 0.2564(3) 0.25588(18) 0.39633(11) 0.0159(7) Uani 1 1 d . . . C28 C 0.1874(3) 0.0712(2) 0.33994(15) 0.0214(9) Uani 1 1 d . . . H28 H 0.1989 0.0227 0.3464 0.026 Uiso 1 1 calc R . . C57 C 0.2916(4) 0.0587(2) 1.00774(15) 0.0211(9) Uani 1 1 d . . . C44 C 0.0371(3) 0.1018(2) 0.69066(14) 0.0178(9) Uani 1 1 d . . . C29 C 0.1234(3) 0.0877(2) 0.29788(15) 0.0217(10) Uani 1 1 d . . . H29 H 0.0905 0.0505 0.2767 0.026 Uiso 1 1 calc R . . C46 C -0.0650(3) 0.1619(2) 0.56736(14) 0.0258(10) Uani 1 1 d . . . H46A H -0.1454 0.1781 0.5565 0.039 Uiso 1 1 calc R . . H46B H -0.0409 0.1210 0.5470 0.039 Uiso 1 1 calc R . . H46C H -0.0056 0.2007 0.5664 0.039 Uiso 1 1 calc R . . C74 C 0.5339(4) 0.3807(2) 0.78538(15) 0.0244(10) Uani 1 1 d . . . H74 H 0.5352 0.3917 0.7536 0.029 Uiso 1 1 calc R . . C77 C 0.5321(3) 0.3470(2) 0.88033(15) 0.0186(9) Uani 1 1 d . . . C72 C 0.4243(3) 0.3725(2) 0.85638(14) 0.0152(9) Uani 1 1 d . . . C26 C 0.2194(3) 0.1985(2) 0.36138(14) 0.0174(9) Uani 1 1 d . . . C43 C -0.0739(3) 0.1079(2) 0.71303(15) 0.0212(9) Uani 1 1 d . . . H43 H -0.0760 0.0972 0.7449 0.025 Uiso 1 1 calc R . . N4 N 0.1496(3) 0.10874(18) 0.61820(11) 0.0152(7) Uani 1 1 d . . . C51 C -0.0177(3) 0.2826(2) 0.83555(14) 0.0197(9) Uani 1 1 d . . . N7 N 0.3115(2) 0.37732(17) 0.88005(11) 0.0147(7) Uani 1 1 d . . . C39 C 0.0371(3) 0.1138(2) 0.64268(14) 0.0159(9) Uani 1 1 d . . . C19 C 0.5021(3) 0.0575(2) 0.65226(16) 0.0263(10) Uani 1 1 d . . . H19A H 0.5871 0.0428 0.6557 0.039 Uiso 1 1 calc R . . H19B H 0.4572 0.0238 0.6299 0.039 Uiso 1 1 calc R . . H19C H 0.4658 0.0578 0.6827 0.039 Uiso 1 1 calc R . . C63 C 0.3652(4) 0.1003(2) 0.92715(15) 0.0321(11) Uani 1 1 d . . . H63A H 0.3845 0.1499 0.9216 0.048 Uiso 1 1 calc R . . H63B H 0.2814 0.0891 0.9156 0.048 Uiso 1 1 calc R . . H63C H 0.4209 0.0684 0.9106 0.048 Uiso 1 1 calc R . . C80 C 0.1316(3) 0.2020(2) 1.09637(15) 0.0197(9) Uani 1 1 d . . . C87 C 0.2994(4) 0.4292(3) 1.15007(18) 0.0329(12) Uani 1 1 d . . . H87 H 0.2871 0.4767 1.1415 0.039 Uiso 1 1 calc R . . C93 C 0.5705(4) 0.0815(2) 0.80513(15) 0.0268(11) Uani 1 1 d . . . C60 C 0.4669(4) 0.0866(2) 1.05580(15) 0.0228(10) Uani 1 1 d . . . C3 C 0.2053(4) 0.4353(2) 0.49166(16) 0.0256(10) Uani 1 1 d . . . C53 C -0.0608(4) 0.2158(3) 0.95716(16) 0.0351(12) Uani 1 1 d . . . H53A H -0.0272 0.2441 0.9850 0.053 Uiso 1 1 calc R . . H53B H -0.0188 0.1700 0.9543 0.053 Uiso 1 1 calc R . . H53C H -0.1477 0.2073 0.9601 0.053 Uiso 1 1 calc R . . C98 C 0.6535(4) 0.0327(3) 0.78458(16) 0.0294(11) Uani 1 1 d . . . H98 H 0.7374 0.0447 0.7858 0.035 Uiso 1 1 calc R . . C32 C 0.3013(4) 0.1078(2) 0.41900(15) 0.0261(10) Uani 1 1 d . . . H32A H 0.2975 0.0562 0.4220 0.039 Uiso 1 1 calc R . . H32B H 0.2624 0.1326 0.4453 0.039 Uiso 1 1 calc R . . H32C H 0.3865 0.1232 0.4193 0.039 Uiso 1 1 calc R . . C91 C 0.1849(4) 0.3845(3) 1.07254(17) 0.0378(13) Uani 1 1 d . . . H91A H 0.2264 0.3595 1.0470 0.057 Uiso 1 1 calc R . . H91B H 0.1842 0.4358 1.0681 0.057 Uiso 1 1 calc R . . H91C H 0.1012 0.3667 1.0725 0.057 Uiso 1 1 calc R . . C41 C -0.1789(3) 0.1456(2) 0.64186(16) 0.0228(10) Uani 1 1 d . . . H41 H -0.2510 0.1606 0.6258 0.027 Uiso 1 1 calc R . . C35 C 0.1456(3) -0.0248(2) 0.58439(14) 0.0201(9) Uani 1 1 d . . . C92 C 0.3578(4) 0.2111(2) 1.19042(16) 0.0294(11) Uani 1 1 d . . . H92A H 0.2800 0.1880 1.1952 0.044 Uiso 1 1 calc R . . H92B H 0.4096 0.2120 1.2194 0.044 Uiso 1 1 calc R . . H92C H 0.3982 0.1843 1.1653 0.044 Uiso 1 1 calc R . . C90 C 0.3352(3) 0.2882(2) 1.17671(14) 0.0216(9) Uani 1 1 d . . . C55 C -0.0416(3) 0.4237(2) 0.84410(16) 0.0273(11) Uani 1 1 d . . . H55A H 0.0019 0.4241 0.8153 0.041 Uiso 1 1 calc R . . H55B H -0.0041 0.4585 0.8677 0.041 Uiso 1 1 calc R . . H55C H -0.1268 0.4363 0.8375 0.041 Uiso 1 1 calc R . . C40 C -0.0695(3) 0.1396(2) 0.61796(15) 0.0193(9) Uani 1 1 d . . . C50 C -0.0353(3) 0.3490(2) 0.86259(15) 0.0193(9) Uani 1 1 d . . . C48 C -0.0432(3) 0.2564(2) 0.91381(15) 0.0212(10) Uani 1 1 d . . . C11 C 0.5068(3) 0.2255(2) 0.58326(15) 0.0231(10) Uani 1 1 d . . . C61 C 0.3472(4) 0.0562(2) 1.05542(15) 0.0246(10) Uani 1 1 d . . . C49 C -0.0502(3) 0.3329(2) 0.91101(15) 0.0220(10) Uani 1 1 d . . . C18 C 0.4682(4) 0.2101(2) 0.71361(14) 0.0260(10) Uani 1 1 d . . . H18A H 0.4480 0.1646 0.7262 0.039 Uiso 1 1 calc R . . H18B H 0.4040 0.2446 0.7201 0.039 Uiso 1 1 calc R . . H18C H 0.5456 0.2283 0.7284 0.039 Uiso 1 1 calc R . . C85 C 0.2703(3) 0.3008(2) 1.13364(15) 0.0201(9) Uani 1 1 d . . . C9 C 0.2041(4) 0.4747(2) 0.40410(17) 0.0364(12) Uani 1 1 d . . . H9A H 0.1699 0.4526 0.3742 0.055 Uiso 1 1 calc R . . H9B H 0.2922 0.4677 0.4063 0.055 Uiso 1 1 calc R . . H9C H 0.1868 0.5260 0.4059 0.055 Uiso 1 1 calc R . . C67 C 0.2711(3) 0.4299(2) 0.90840(14) 0.0176(9) Uani 1 1 d . . . C31 C 0.1557(3) 0.2163(2) 0.31909(15) 0.0206(9) Uani 1 1 d . . . C109 C 0.1844(4) 0.7622(3) 0.70725(17) 0.0336(12) Uani 1 1 d . . . H109 H 0.1406 0.7699 0.6786 0.040 Uiso 1 1 calc R . . C14 C 0.4959(3) 0.1334(2) 0.63411(15) 0.0215(10) Uani 1 1 d . . . C42 C -0.1817(3) 0.1295(2) 0.68896(16) 0.0230(10) Uani 1 1 d . . . H42 H -0.2554 0.1331 0.7045 0.028 Uiso 1 1 calc R . . C6 C -0.1104(4) 0.3580(3) 0.50720(17) 0.0357(12) Uani 1 1 d . . . H6A H -0.0930 0.3293 0.5341 0.054 Uiso 1 1 calc R . . H6B H -0.1509 0.3280 0.4815 0.054 Uiso 1 1 calc R . . H6C H -0.1634 0.3976 0.5163 0.054 Uiso 1 1 calc R . . C83 C 0.0013(4) 0.1313(3) 1.14528(17) 0.0395(13) Uani 1 1 d . . . H83A H 0.0011 0.0935 1.1200 0.059 Uiso 1 1 calc R . . H83B H -0.0753 0.1296 1.1609 0.059 Uiso 1 1 calc R . . H83C H 0.0694 0.1243 1.1680 0.059 Uiso 1 1 calc R . . C45 C 0.1548(3) 0.0847(2) 0.71986(15) 0.0263(10) Uani 1 1 d . . . H45A H 0.2151 0.0647 0.6990 0.039 Uiso 1 1 calc R . . H45B H 0.1364 0.0500 0.7425 0.039 Uiso 1 1 calc R . . H45C H 0.1873 0.1286 0.7365 0.039 Uiso 1 1 calc R . . C66 C 0.2893(4) 0.0222(3) 1.09573(17) 0.0378(12) Uani 1 1 d . . . H66A H 0.3109 -0.0284 1.0954 0.057 Uiso 1 1 calc R . . H66B H 0.2007 0.0265 1.0921 0.057 Uiso 1 1 calc R . . H66C H 0.3190 0.0466 1.1255 0.057 Uiso 1 1 calc R . . C79 C 0.5275(3) 0.3262(2) 0.93083(15) 0.0260(11) Uani 1 1 d . . . H79A H 0.4675 0.2878 0.9322 0.039 Uiso 1 1 calc R . . H79B H 0.5043 0.3677 0.9508 0.039 Uiso 1 1 calc R . . H79C H 0.6077 0.3097 0.9418 0.039 Uiso 1 1 calc R . . C86 C 0.2523(4) 0.3714(2) 1.11962(16) 0.0266(10) Uani 1 1 d . . . C15 C 0.5114(3) 0.1490(2) 0.58558(14) 0.0206(10) Uani 1 1 d . . . C62 C 0.1669(4) 0.0275(2) 0.98994(17) 0.0318(11) Uani 1 1 d . . . H62A H 0.1376 0.0512 0.9621 0.048 Uiso 1 1 calc R . . H62B H 0.1091 0.0350 1.0145 0.048 Uiso 1 1 calc R . . H62C H 0.1745 -0.0238 0.9819 0.048 Uiso 1 1 calc R . . C76 C 0.6400(3) 0.3414(2) 0.85589(16) 0.0240(10) Uani 1 1 d . . . H76 H 0.7125 0.3258 0.8714 0.029 Uiso 1 1 calc R . . C23 C 0.5004(4) 0.3648(3) 0.35889(18) 0.0420(13) Uani 1 1 d . . . H23A H 0.4322 0.3769 0.3375 0.063 Uiso 1 1 calc R . . H23B H 0.5760 0.3653 0.3425 0.063 Uiso 1 1 calc R . . H23C H 0.5064 0.3998 0.3859 0.063 Uiso 1 1 calc R . . C112 C 0.3143(4) 0.7385(3) 0.79257(16) 0.0313(12) Uani 1 1 d . . . H112 H 0.3584 0.7309 0.8212 0.038 Uiso 1 1 calc R . . C16 C 0.5281(4) 0.2651(3) 0.53946(16) 0.0361(13) Uani 1 1 d . . . H16A H 0.4826 0.3098 0.5405 0.054 Uiso 1 1 calc R . . H16B H 0.5005 0.2351 0.5115 0.054 Uiso 1 1 calc R . . H16C H 0.6150 0.2757 0.5383 0.054 Uiso 1 1 calc R . . C13 C 0.4790(3) 0.1988(2) 0.66076(14) 0.0206(10) Uani 1 1 d . . . C105 C -0.1866(4) 0.4555(3) 0.71248(17) 0.0340(12) Uani 1 1 d . . . H105 H -0.2710 0.4460 0.7136 0.041 Uiso 1 1 calc R . . C68 C 0.3183(3) 0.5060(2) 0.92380(15) 0.0226(10) Uani 1 1 d . . . C64 C 0.6054(4) 0.1401(2) 0.99335(17) 0.0319(11) Uani 1 1 d . . . H64A H 0.6465 0.1694 1.0192 0.048 Uiso 1 1 calc R . . H64B H 0.5874 0.1696 0.9669 0.048 Uiso 1 1 calc R . . H64C H 0.6582 0.1007 0.9836 0.048 Uiso 1 1 calc R . . C73 C 0.4233(3) 0.3870(2) 0.80839(15) 0.0206(9) Uani 1 1 d . . . C7 C 0.1316(5) 0.3920(3) 0.57271(16) 0.0382(12) Uani 1 1 d . . . H7A H 0.0840 0.4275 0.5903 0.057 Uiso 1 1 calc R . . H7B H 0.2176 0.3970 0.5833 0.057 Uiso 1 1 calc R . . H7C H 0.1027 0.3440 0.5780 0.057 Uiso 1 1 calc R . . C97 C 0.6136(4) -0.0330(3) 0.76246(17) 0.0326(12) Uani 1 1 d . . . H97 H 0.6706 -0.0649 0.7491 0.039 Uiso 1 1 calc R . . C75 C 0.6414(4) 0.3586(2) 0.80878(16) 0.0278(11) Uani 1 1 d . . . H75 H 0.7147 0.3553 0.7929 0.033 Uiso 1 1 calc R . . C52 C -0.0089(4) 0.1453(2) 0.85418(16) 0.0276(11) Uani 1 1 d . . . H52A H 0.0169 0.1199 0.8818 0.041 Uiso 1 1 calc R . . H52B H 0.0508 0.1380 0.8303 0.041 Uiso 1 1 calc R . . H52C H -0.0883 0.1269 0.8415 0.041 Uiso 1 1 calc R . . C17 C 0.4744(4) 0.3364(2) 0.64286(16) 0.0303(11) Uani 1 1 d . . . H17A H 0.5548 0.3544 0.6548 0.045 Uiso 1 1 calc R . . H17B H 0.4166 0.3437 0.6674 0.045 Uiso 1 1 calc R . . H17C H 0.4469 0.3623 0.6157 0.045 Uiso 1 1 calc R . . C37 C 0.1616(4) -0.0615(2) 0.63197(16) 0.0295(11) Uani 1 1 d . . . H37A H 0.2466 -0.0572 0.6440 0.044 Uiso 1 1 calc R . . H37B H 0.1389 -0.1121 0.6269 0.044 Uiso 1 1 calc R . . H37C H 0.1093 -0.0381 0.6548 0.044 Uiso 1 1 calc R . . C56 C -0.0071(4) 0.2725(2) 0.78281(14) 0.0264(11) Uani 1 1 d . . . H56A H -0.0836 0.2529 0.7680 0.040 Uiso 1 1 calc R . . H56B H 0.0590 0.2394 0.7760 0.040 Uiso 1 1 calc R . . H56C H 0.0101 0.3187 0.7704 0.040 Uiso 1 1 calc R . . C25 C 0.4752(4) 0.2322(3) 0.33361(16) 0.0326(11) Uani 1 1 d . . . H25A H 0.4645 0.1844 0.3446 0.049 Uiso 1 1 calc R . . H25B H 0.5516 0.2343 0.3179 0.049 Uiso 1 1 calc R . . H25C H 0.4072 0.2424 0.3116 0.049 Uiso 1 1 calc R . . C107 C 0.2798(4) 0.6803(3) 0.76153(17) 0.0304(11) Uani 1 1 d . . . C4 C 0.1472(4) 0.4404(2) 0.44443(15) 0.0231(10) Uani 1 1 d . . . C78 C 0.3044(4) 0.4068(2) 0.78145(15) 0.0278(11) Uani 1 1 d . . . H78A H 0.2457 0.3674 0.7813 0.042 Uiso 1 1 calc R . . H78B H 0.3213 0.4157 0.7492 0.042 Uiso 1 1 calc R . . H78C H 0.2706 0.4499 0.7967 0.042 Uiso 1 1 calc R . . C110 C 0.2192(4) 0.8205(3) 0.73871(18) 0.0347(12) Uani 1 1 d . . . H110 H 0.1993 0.8677 0.7313 0.042 Uiso 1 1 calc R . . C5 C 0.0262(4) 0.4118(2) 0.44471(15) 0.0217(10) Uani 1 1 d . . . C100 C -0.1117(4) 0.4030(2) 0.69159(16) 0.0293(11) Uani 1 1 d . . . C111 C 0.2837(4) 0.8084(3) 0.78134(17) 0.0310(11) Uani 1 1 d . . . H111 H 0.3066 0.8477 0.8027 0.037 Uiso 1 1 calc R . . C27 C 0.2349(3) 0.1258(2) 0.37269(14) 0.0192(9) Uani 1 1 d . . . C65 C 0.5634(4) 0.0945(2) 1.09703(16) 0.0339(12) Uani 1 1 d . . . H65A H 0.5297 0.0770 1.1251 0.051 Uiso 1 1 calc R . . H65B H 0.5865 0.1449 1.1030 0.051 Uiso 1 1 calc R . . H65C H 0.6351 0.0666 1.0892 0.051 Uiso 1 1 calc R . . C94 C 0.4455(4) 0.0619(3) 0.80244(16) 0.0289(11) Uani 1 1 d . . . H94 H 0.3878 0.0934 0.8158 0.035 Uiso 1 1 calc R . . C8 C 0.3310(4) 0.4647(2) 0.50907(17) 0.0352(12) Uani 1 1 d . . . H8A H 0.3244 0.5153 0.5194 0.053 Uiso 1 1 calc R . . H8B H 0.3865 0.4595 0.4836 0.053 Uiso 1 1 calc R . . H8C H 0.3624 0.4380 0.5354 0.053 Uiso 1 1 calc R . . C102 C 0.0620(4) 0.4864(3) 0.70928(16) 0.0305(11) Uani 1 1 d . . . H102 H 0.1462 0.4966 0.7081 0.037 Uiso 1 1 calc R . . C104 C -0.1390(4) 0.5221(3) 0.73175(17) 0.0328(12) Uani 1 1 d . . . H104 H -0.1909 0.5563 0.7459 0.039 Uiso 1 1 calc R . . C21 C 0.3605(3) 0.2915(2) 0.40314(14) 0.0195(9) Uani 1 1 d . . . C81 C 0.0150(4) 0.2058(3) 1.12431(16) 0.0263(10) Uani 1 1 d . . . C1 C 0.0093(4) 0.3877(2) 0.49104(15) 0.0239(10) Uani 1 1 d . . . C99 C 0.6134(4) 0.1534(3) 0.82952(18) 0.0415(13) Uani 1 1 d . . . H99A H 0.6398 0.1466 0.8621 0.062 Uiso 1 1 calc R . . H99B H 0.5463 0.1874 0.8287 0.062 Uiso 1 1 calc R . . H99C H 0.6814 0.1720 0.8133 0.062 Uiso 1 1 calc R . . C101 C 0.0136(4) 0.4196(3) 0.69029(16) 0.0289(11) Uani 1 1 d . . . H101 H 0.0662 0.3854 0.6765 0.035 Uiso 1 1 calc R . . C10 C -0.0724(4) 0.4083(2) 0.40459(16) 0.0337(12) Uani 1 1 d . . . H10A H -0.1384 0.4407 0.4127 0.050 Uiso 1 1 calc R . . H10B H -0.1042 0.3593 0.3995 0.050 Uiso 1 1 calc R . . H10C H -0.0374 0.4225 0.3759 0.050 Uiso 1 1 calc R . . C59 C 0.4860(3) 0.1098(2) 1.00955(15) 0.0221(10) Uani 1 1 d . . . C30 C 0.1085(3) 0.1601(2) 0.28749(14) 0.0214(10) Uani 1 1 d . . . H30 H 0.0664 0.1711 0.2591 0.026 Uiso 1 1 calc R . . C88 C 0.3636(4) 0.4174(3) 1.19245(18) 0.0362(12) Uani 1 1 d . . . H88 H 0.3957 0.4567 1.2120 0.043 Uiso 1 1 calc R . . C89 C 0.3805(4) 0.3474(3) 1.20594(17) 0.0318(11) Uani 1 1 d . . . H89 H 0.4227 0.3397 1.2349 0.038 Uiso 1 1 calc R . . C82 C -0.0961(4) 0.2176(3) 1.08873(16) 0.0413(14) Uani 1 1 d . . . H82A H -0.0877 0.2641 1.0756 0.062 Uiso 1 1 calc R . . H82B H -0.1717 0.2163 1.1050 0.062 Uiso 1 1 calc R . . H82C H -0.0981 0.1798 1.0634 0.062 Uiso 1 1 calc R . . C84 C 0.0179(4) 0.2656(3) 1.16452(16) 0.0326(11) Uani 1 1 d . . . H84A H 0.0866 0.2580 1.1869 0.049 Uiso 1 1 calc R . . H84B H -0.0581 0.2645 1.1806 0.049 Uiso 1 1 calc R . . H84C H 0.0272 0.3122 1.1515 0.049 Uiso 1 1 calc R . . C108 C 0.2150(4) 0.6922(3) 0.71854(17) 0.0308(11) Uani 1 1 d . . . H108 H 0.1920 0.6529 0.6972 0.037 Uiso 1 1 calc R . . C38 C 0.0079(3) -0.0286(2) 0.56730(15) 0.0247(10) Uani 1 1 d . . . H38A H -0.0407 -0.0048 0.5912 0.037 Uiso 1 1 calc R . . H38B H -0.0179 -0.0787 0.5620 0.037 Uiso 1 1 calc R . . H38C H -0.0038 -0.0047 0.5380 0.037 Uiso 1 1 calc R . . C22 C 0.4789(4) 0.2884(3) 0.37610(16) 0.0265(10) Uani 1 1 d . . . C96 C 0.4894(4) -0.0518(3) 0.75998(16) 0.0323(12) Uani 1 1 d . . . H96 H 0.4622 -0.0961 0.7449 0.039 Uiso 1 1 calc R . . C54 C -0.0828(4) 0.3864(3) 0.95063(17) 0.0362(12) Uani 1 1 d . . . H54A H -0.1713 0.3915 0.9503 0.054 Uiso 1 1 calc R . . H54B H -0.0452 0.4327 0.9464 0.054 Uiso 1 1 calc R . . H54C H -0.0529 0.3693 0.9807 0.054 Uiso 1 1 calc R . . C20 C 0.5416(4) 0.0943(3) 0.54592(16) 0.0338(12) Uani 1 1 d . . . H20A H 0.5066 0.1096 0.5161 0.051 Uiso 1 1 calc R . . H20B H 0.5076 0.0476 0.5518 0.051 Uiso 1 1 calc R . . H20C H 0.6300 0.0907 0.5446 0.051 Uiso 1 1 calc R . . C36 C 0.2221(4) -0.0660(2) 0.54753(16) 0.0294(11) Uani 1 1 d . . . H36A H 0.2136 -0.0431 0.5178 0.044 Uiso 1 1 calc R . . H36B H 0.1929 -0.1155 0.5428 0.044 Uiso 1 1 calc R . . H36C H 0.3077 -0.0654 0.5588 0.044 Uiso 1 1 calc R . . C70 C 0.4436(3) 0.5239(2) 0.90419(17) 0.0294(11) Uani 1 1 d . . . H70A H 0.5053 0.4911 0.9159 0.044 Uiso 1 1 calc R . . H70B H 0.4673 0.5731 0.9145 0.044 Uiso 1 1 calc R . . H70C H 0.4367 0.5188 0.8699 0.044 Uiso 1 1 calc R . . C103 C -0.0149(4) 0.5370(3) 0.72972(17) 0.0318(11) Uani 1 1 d . . . H103 H 0.0172 0.5818 0.7423 0.038 Uiso 1 1 calc R . . C71 C 0.3294(4) 0.5125(3) 0.97818(16) 0.0369(12) Uani 1 1 d . . . H71A H 0.2498 0.5038 0.9903 0.055 Uiso 1 1 calc R . . H71B H 0.3582 0.5606 0.9891 0.055 Uiso 1 1 calc R . . H71C H 0.3873 0.4772 0.9894 0.055 Uiso 1 1 calc R . . C69 C 0.2205(4) 0.5599(2) 0.90608(19) 0.0386(13) Uani 1 1 d . . . H69A H 0.2062 0.5521 0.8721 0.058 Uiso 1 1 calc R . . H69B H 0.2498 0.6089 0.9139 0.058 Uiso 1 1 calc R . . H69C H 0.1445 0.5524 0.9212 0.058 Uiso 1 1 calc R . . C24 C 0.5881(4) 0.2716(3) 0.41124(16) 0.0407(13) Uani 1 1 d . . . H24A H 0.5912 0.3070 0.4380 0.061 Uiso 1 1 calc R . . H24B H 0.6643 0.2733 0.3953 0.061 Uiso 1 1 calc R . . H24C H 0.5768 0.2238 0.4223 0.061 Uiso 1 1 calc R . . C106 C -0.1618(5) 0.3314(3) 0.66992(19) 0.0526(16) Uani 1 1 d . . . H10D H -0.2255 0.3144 0.6890 0.079 Uiso 1 1 calc R . . H10E H -0.0960 0.2965 0.6688 0.079 Uiso 1 1 calc R . . H10F H -0.1959 0.3374 0.6381 0.079 Uiso 1 1 calc R . . C113 C 0.3092(4) 0.6030(3) 0.7743(2) 0.0513(16) Uani 1 1 d . . . H11A H 0.3660 0.6045 0.8019 0.077 Uiso 1 1 calc R . . H11B H 0.3462 0.5772 0.7479 0.077 Uiso 1 1 calc R . . H11C H 0.2341 0.5785 0.7810 0.077 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 Ta2 0.01340(7) 0.01568(10) 0.01340(9) 0.00257(7) 0.00015(6) 0.00214(6) Ta4 0.01730(7) 0.01649(10) 0.01343(9) 0.00237(7) 0.00037(6) 0.00258(6) Ta3 0.01252(7) 0.01472(9) 0.01327(9) 0.00079(7) -0.00048(6) 0.00197(6) Ta1 0.01912(7) 0.01381(9) 0.01260(9) 0.00193(7) 0.00029(6) 0.00147(6) Cl1 0.0186(4) 0.0196(6) 0.0261(6) -0.0015(5) 0.0008(4) 0.0000(4) Cl4 0.0213(4) 0.0209(6) 0.0250(6) -0.0027(5) 0.0027(4) 0.0004(4) Cl2 0.0219(4) 0.0187(6) 0.0203(6) -0.0020(4) 0.0024(4) 0.0037(4) Cl3 0.0211(4) 0.0183(6) 0.0200(6) -0.0020(4) 0.0021(4) 0.0038(4) C33 0.035(2) 0.030(3) 0.016(2) 0.004(2) -0.0031(18) 0.002(2) C95 0.026(2) 0.032(3) 0.039(3) 0.012(2) 0.000(2) 0.004(2) N2 0.0170(14) 0.0169(19) 0.0162(19) 0.0028(15) -0.0004(13) 0.0029(13) N6 0.0184(15) 0.0153(19) 0.0166(19) 0.0015(15) 0.0029(13) 0.0022(13) C58 0.029(2) 0.017(2) 0.020(2) 0.0016(19) -0.0023(17) 0.0075(18) N1 0.0183(14) 0.0161(19) 0.0121(18) 0.0025(14) 0.0036(13) 0.0037(13) N5 0.0158(14) 0.0152(18) 0.0131(18) 0.0027(14) 0.0000(12) 0.0015(13) C47 0.0157(17) 0.022(2) 0.021(2) -0.0032(19) -0.0024(16) -0.0050(16) O2 0.0175(12) 0.0146(16) 0.0202(16) 0.0009(12) 0.0055(11) 0.0009(11) N8 0.0217(15) 0.017(2) 0.017(2) 0.0016(15) 0.0014(14) 0.0021(14) C12 0.0184(18) 0.025(3) 0.021(2) 0.006(2) 0.0014(16) -0.0010(17) O4 0.0217(13) 0.0257(18) 0.0188(17) 0.0010(14) 0.0027(12) -0.0033(12) O3 0.0177(12) 0.0166(16) 0.0190(16) -0.0017(12) 0.0004(11) -0.0001(11) C2 0.047(2) 0.015(2) 0.013(2) -0.0006(18) 0.0012(19) 0.010(2) C34 0.0203(18) 0.023(2) 0.005(2) 0.0024(17) -0.0022(15) 0.0009(17) O1 0.0228(13) 0.0234(17) 0.0208(17) 0.0003(14) 0.0028(12) -0.0053(12) N3 0.0192(15) 0.021(2) 0.0084(18) 0.0048(15) 0.0023(13) -0.0008(14) C28 0.0218(18) 0.016(2) 0.027(3) -0.0023(19) 0.0094(17) 0.0017(17) C57 0.027(2) 0.014(2) 0.022(2) 0.0001(19) 0.0019(17) 0.0047(17) C44 0.0176(17) 0.017(2) 0.019(2) -0.0029(18) 0.0011(15) -0.0002(16) C29 0.0185(18) 0.026(3) 0.021(2) -0.006(2) 0.0108(16) -0.0023(17) C46 0.025(2) 0.030(3) 0.022(2) 0.005(2) -0.0058(18) 0.0036(19) C74 0.031(2) 0.023(3) 0.019(2) -0.001(2) 0.0076(18) -0.0065(19) C77 0.0154(17) 0.014(2) 0.026(2) -0.0007(18) -0.0002(16) -0.0020(16) C72 0.0142(16) 0.009(2) 0.023(2) 0.0015(17) 0.0032(15) -0.0022(15) C26 0.0168(17) 0.020(2) 0.016(2) -0.0003(18) 0.0045(15) 0.0003(16) C43 0.026(2) 0.022(2) 0.015(2) -0.0039(19) 0.0053(16) -0.0035(18) N4 0.0129(14) 0.0192(19) 0.0139(18) 0.0027(15) 0.0025(12) 0.0028(13) C51 0.0131(16) 0.024(2) 0.021(2) -0.0002(19) -0.0055(16) 0.0008(16) N7 0.0122(13) 0.0181(19) 0.0140(18) 0.0022(15) 0.0019(12) 0.0001(13) C39 0.0156(16) 0.016(2) 0.016(2) -0.0003(17) 0.0018(15) -0.0011(15) C19 0.0208(19) 0.030(3) 0.029(3) 0.005(2) -0.0014(18) 0.0034(18) C63 0.046(3) 0.029(3) 0.021(3) 0.002(2) -0.002(2) 0.010(2) C80 0.0200(18) 0.021(2) 0.019(2) 0.0067(19) 0.0016(16) 0.0019(17) C87 0.032(2) 0.019(3) 0.051(3) 0.003(2) 0.028(2) 0.003(2) C93 0.036(2) 0.028(3) 0.018(2) 0.012(2) -0.0014(19) 0.002(2) C60 0.028(2) 0.017(2) 0.023(3) 0.0031(19) -0.0054(18) 0.0064(18) C3 0.035(2) 0.014(2) 0.026(3) -0.003(2) -0.0057(19) 0.0019(19) C53 0.030(2) 0.046(3) 0.031(3) 0.007(2) 0.006(2) -0.005(2) C98 0.027(2) 0.033(3) 0.030(3) 0.014(2) 0.0044(19) 0.001(2) C32 0.030(2) 0.026(3) 0.024(3) 0.008(2) 0.0050(18) 0.0042(19) C91 0.053(3) 0.030(3) 0.035(3) 0.019(2) 0.019(2) 0.017(2) C41 0.0160(17) 0.015(2) 0.037(3) -0.003(2) -0.0033(17) -0.0021(16) C35 0.0246(19) 0.017(2) 0.019(2) -0.0007(19) 0.0018(17) 0.0004(17) C92 0.031(2) 0.029(3) 0.028(3) 0.003(2) -0.0017(19) 0.001(2) C90 0.0217(19) 0.027(3) 0.016(2) -0.0078(19) 0.0087(16) 0.0004(18) C55 0.0206(19) 0.024(3) 0.036(3) 0.004(2) -0.0046(18) 0.0070(18) C40 0.0148(17) 0.016(2) 0.026(2) -0.0047(19) 0.0002(16) 0.0016(16) C50 0.0125(16) 0.017(2) 0.028(3) 0.0035(19) -0.0053(16) 0.0023(16) C48 0.0110(16) 0.033(3) 0.020(2) 0.001(2) 0.0026(15) -0.0038(17) C11 0.0148(17) 0.031(3) 0.025(3) 0.010(2) 0.0008(16) -0.0030(17) C61 0.034(2) 0.019(2) 0.022(3) 0.008(2) 0.0018(18) 0.0040(19) C49 0.0135(17) 0.023(3) 0.028(3) -0.004(2) 0.0003(16) 0.0000(17) C18 0.029(2) 0.030(3) 0.018(2) 0.001(2) -0.0060(17) 0.0014(19) C85 0.0202(18) 0.022(2) 0.019(2) 0.0001(19) 0.0101(16) 0.0009(17) C9 0.057(3) 0.025(3) 0.029(3) 0.010(2) 0.009(2) 0.002(2) C67 0.0148(17) 0.016(2) 0.021(2) -0.0015(18) -0.0035(16) 0.0041(16) C31 0.0154(17) 0.024(3) 0.023(2) 0.0006(19) 0.0026(16) 0.0027(17) C109 0.022(2) 0.046(3) 0.034(3) 0.013(3) -0.0031(19) -0.003(2) C14 0.0126(17) 0.024(3) 0.027(3) 0.002(2) -0.0045(16) 0.0049(16) C42 0.0158(18) 0.021(2) 0.032(3) -0.005(2) 0.0108(17) -0.0017(17) C6 0.038(2) 0.034(3) 0.037(3) 0.008(2) 0.015(2) 0.012(2) C83 0.044(3) 0.047(4) 0.030(3) 0.001(3) 0.018(2) -0.007(2) C45 0.0222(19) 0.036(3) 0.021(2) 0.004(2) -0.0026(17) -0.0001(19) C66 0.057(3) 0.032(3) 0.026(3) 0.007(2) 0.012(2) 0.001(2) C79 0.0180(18) 0.031(3) 0.029(3) 0.010(2) -0.0068(17) -0.0011(18) C86 0.029(2) 0.022(3) 0.031(3) 0.003(2) 0.0172(19) 0.0078(19) C15 0.0131(16) 0.032(3) 0.016(2) -0.0031(19) 0.0005(15) 0.0019(17) C62 0.029(2) 0.028(3) 0.037(3) -0.007(2) -0.001(2) 0.000(2) C76 0.0140(17) 0.023(3) 0.034(3) -0.003(2) -0.0016(17) -0.0007(16) C23 0.045(3) 0.042(3) 0.041(3) 0.006(3) 0.020(2) -0.017(2) C112 0.0205(19) 0.046(3) 0.029(3) 0.015(2) 0.0026(18) -0.004(2) C16 0.027(2) 0.053(4) 0.031(3) 0.020(3) 0.0016(19) -0.009(2) C13 0.0134(17) 0.030(3) 0.018(2) 0.005(2) -0.0041(15) -0.0016(17) C105 0.027(2) 0.033(3) 0.044(3) 0.014(3) 0.010(2) 0.004(2) C68 0.0228(19) 0.017(2) 0.027(3) -0.0046(19) 0.0022(17) -0.0031(17) C64 0.025(2) 0.027(3) 0.044(3) -0.002(2) 0.009(2) 0.0073(19) C73 0.0190(18) 0.016(2) 0.027(3) 0.0035(19) 0.0000(17) -0.0041(16) C7 0.063(3) 0.031(3) 0.020(3) 0.000(2) 0.000(2) 0.014(3) C97 0.035(2) 0.036(3) 0.030(3) 0.012(2) 0.014(2) 0.014(2) C75 0.023(2) 0.025(3) 0.036(3) -0.012(2) 0.0125(19) -0.0052(18) C52 0.026(2) 0.022(3) 0.035(3) 0.005(2) -0.0058(19) -0.0041(18) C17 0.033(2) 0.025(3) 0.033(3) 0.004(2) -0.007(2) -0.004(2) C37 0.032(2) 0.023(3) 0.032(3) 0.003(2) -0.004(2) -0.0002(19) C56 0.031(2) 0.022(3) 0.024(3) -0.002(2) -0.0103(18) 0.0016(19) C25 0.025(2) 0.048(3) 0.025(3) -0.003(2) 0.0117(19) -0.002(2) C107 0.0181(19) 0.033(3) 0.042(3) 0.018(2) 0.0023(19) -0.0018(19) C4 0.041(2) 0.010(2) 0.019(2) 0.0024(19) 0.0003(19) 0.0048(19) C78 0.027(2) 0.032(3) 0.025(3) 0.009(2) 0.0000(18) 0.0044(19) C110 0.0185(19) 0.040(3) 0.048(3) 0.014(3) 0.005(2) 0.000(2) C5 0.031(2) 0.012(2) 0.022(2) 0.0009(18) -0.0005(18) 0.0096(18) C100 0.042(2) 0.022(3) 0.024(3) 0.011(2) -0.005(2) 0.003(2) C111 0.025(2) 0.035(3) 0.034(3) 0.002(2) 0.0079(19) -0.003(2) C27 0.0175(17) 0.024(3) 0.017(2) 0.0015(19) 0.0072(16) 0.0022(17) C65 0.036(2) 0.029(3) 0.034(3) -0.004(2) -0.016(2) 0.009(2) C94 0.026(2) 0.031(3) 0.031(3) 0.008(2) 0.0033(19) 0.016(2) C8 0.040(2) 0.025(3) 0.039(3) -0.006(2) -0.005(2) -0.002(2) C102 0.024(2) 0.035(3) 0.034(3) 0.013(2) 0.0010(19) 0.007(2) C104 0.041(3) 0.027(3) 0.032(3) 0.007(2) 0.016(2) 0.016(2) C21 0.027(2) 0.018(2) 0.013(2) 0.0015(18) -0.0028(16) 0.0011(17) C81 0.024(2) 0.033(3) 0.022(3) 0.005(2) 0.0050(18) -0.0032(19) C1 0.032(2) 0.018(2) 0.022(3) 0.003(2) 0.0069(18) 0.0082(18) C99 0.049(3) 0.034(3) 0.040(3) 0.004(3) -0.008(2) 0.001(2) C101 0.034(2) 0.031(3) 0.024(3) 0.006(2) 0.0067(19) 0.015(2) C10 0.041(2) 0.026(3) 0.033(3) 0.002(2) -0.012(2) 0.006(2) C59 0.0247(19) 0.018(2) 0.024(3) 0.0011(19) 0.0012(17) 0.0074(17) C30 0.0195(18) 0.029(3) 0.016(2) 0.0012(19) 0.0005(16) 0.0008(17) C88 0.030(2) 0.030(3) 0.048(3) -0.017(3) 0.023(2) -0.008(2) C89 0.026(2) 0.034(3) 0.034(3) -0.011(2) 0.010(2) -0.002(2) C82 0.022(2) 0.075(4) 0.027(3) 0.002(3) 0.0071(19) 0.002(2) C84 0.028(2) 0.042(3) 0.028(3) -0.004(2) 0.0141(19) -0.001(2) C108 0.024(2) 0.036(3) 0.033(3) 0.005(2) 0.0016(19) -0.006(2) C38 0.0237(19) 0.025(3) 0.025(3) 0.000(2) 0.0003(17) -0.0033(18) C22 0.023(2) 0.035(3) 0.022(3) 0.004(2) 0.0036(17) -0.0042(19) C96 0.039(2) 0.030(3) 0.029(3) 0.007(2) 0.004(2) 0.005(2) C54 0.022(2) 0.049(3) 0.036(3) -0.011(3) 0.009(2) 0.000(2) C20 0.022(2) 0.048(3) 0.031(3) -0.001(2) 0.0042(19) 0.006(2) C36 0.032(2) 0.022(3) 0.034(3) -0.006(2) 0.006(2) -0.0010(19) C70 0.026(2) 0.021(3) 0.041(3) -0.005(2) 0.0051(19) -0.0014(18) C103 0.040(2) 0.026(3) 0.031(3) 0.006(2) 0.001(2) 0.007(2) C71 0.032(2) 0.040(3) 0.036(3) -0.018(2) 0.002(2) -0.009(2) C69 0.032(2) 0.015(3) 0.068(4) -0.004(2) 0.003(2) 0.003(2) C24 0.020(2) 0.073(4) 0.029(3) 0.000(3) 0.0053(19) -0.002(2) C106 0.070(4) 0.039(3) 0.047(4) 0.009(3) -0.018(3) -0.004(3) C113 0.033(2) 0.047(4) 0.074(4) 0.026(3) -0.015(3) -0.006(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ta2 N2 1.807(3) . ? Ta2 O2 2.145(3) . ? Ta2 N4 2.215(3) . ? Ta2 Cl2 2.4115(11) . ? Ta2 C15 2.416(4) . ? Ta2 C12 2.444(4) . ? Ta2 C11 2.445(4) . ? Ta2 C14 2.459(3) . ? Ta2 C13 2.486(3) . ? Ta2 C34 2.633(4) . ? Ta4 N6 1.799(3) . ? Ta4 O4 2.154(3) . ? Ta4 N8 2.211(3) . ? Ta4 C57 2.403(4) . ? Ta4 Cl4 2.4209(10) . ? Ta4 C58 2.442(4) . ? Ta4 C61 2.457(4) . ? Ta4 C59 2.458(4) . ? Ta4 C60 2.505(4) . ? Ta4 C80 2.635(4) . ? Ta3 N5 1.805(3) . ? Ta3 O3 2.143(3) . ? Ta3 N7 2.218(3) . ? Ta3 Cl3 2.4115(11) . ? Ta3 C49 2.420(4) . ? Ta3 C47 2.445(4) . ? Ta3 C48 2.449(4) . ? Ta3 C50 2.458(3) . ? Ta3 C51 2.495(3) . ? Ta3 C67 2.636(4) . ? Ta1 N1 1.802(3) . ? Ta1 O1 2.159(3) . ? Ta1 N3 2.217(3) . ? Ta1 C3 2.414(4) . ? Ta1 Cl1 2.4207(10) . ? Ta1 C2 2.443(4) . ? Ta1 C1 2.453(4) . ? Ta1 C4 2.466(4) . ? Ta1 C5 2.505(4) . ? Ta1 C21 2.639(4) . ? C33 C31 1.508(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C95 C96 1.369(6) . ? C95 C94 1.385(6) . ? C95 H95 0.9300 . ? N2 N1 1.292(4) . ? N6 N5 1.290(4) . ? C58 C57 1.416(6) . ? C58 C59 1.424(5) . ? C58 C63 1.489(6) . ? C47 C48 1.416(6) . ? C47 C51 1.446(5) . ? C47 C52 1.493(6) . ? O2 C34 1.291(4) . ? N8 C80 1.309(5) . ? N8 C85 1.425(5) . ? C12 C11 1.401(6) . ? C12 C13 1.453(5) . ? C12 C17 1.490(6) . ? O4 C80 1.305(5) . ? O3 C67 1.307(4) . ? C2 C1 1.402(5) . ? C2 C3 1.427(6) . ? C2 C7 1.503(6) . ? C34 N4 1.308(5) . ? C34 C35 1.521(6) . ? O1 C21 1.299(5) . ? N3 C21 1.296(5) . ? N3 C26 1.431(5) . ? C28 C29 1.386(5) . ? C28 C27 1.389(6) . ? C28 H28 0.9300 . ? C57 C61 1.439(5) . ? C57 C62 1.506(5) . ? C44 C39 1.380(5) . ? C44 C43 1.386(5) . ? C44 C45 1.518(5) . ? C29 C30 1.391(6) . ? C29 H29 0.9300 . ? C46 C40 1.509(6) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C74 C75 1.378(5) . ? C74 C73 1.393(5) . ? C74 H74 0.9300 . ? C77 C76 1.388(5) . ? C77 C72 1.408(5) . ? C77 C79 1.497(5) . ? C72 C73 1.391(5) . ? C72 N7 1.422(5) . ? C26 C31 1.397(5) . ? C26 C27 1.403(5) . ? C43 C42 1.386(5) . ? C43 H43 0.9300 . ? N4 C39 1.430(5) . ? C51 C50 1.414(6) . ? C51 C56 1.491(6) . ? N7 C67 1.303(5) . ? C39 C40 1.411(5) . ? C19 C14 1.518(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C80 C81 1.522(6) . ? C87 C88 1.373(7) . ? C87 C86 1.393(6) . ? C87 H87 0.9300 . ? C93 C94 1.392(6) . ? C93 C98 1.394(6) . ? C93 C99 1.504(6) . ? C60 C61 1.405(6) . ? C60 C59 1.420(6) . ? C60 C65 1.511(5) . ? C3 C4 1.443(5) . ? C3 C8 1.500(5) . ? C53 C48 1.491(6) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C98 C97 1.375(6) . ? C98 H98 0.9300 . ? C32 C27 1.506(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C91 C86 1.506(6) . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C41 C42 1.377(6) . ? C41 C40 1.393(5) . ? C41 H41 0.9300 . ? C35 C36 1.526(6) . ? C35 C38 1.535(5) . ? C35 C37 1.539(5) . ? C92 C90 1.513(6) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C90 C89 1.387(6) . ? C90 C85 1.396(5) . ? C55 C50 1.503(5) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C50 C49 1.429(6) . ? C48 C49 1.416(6) . ? C11 C15 1.414(6) . ? C11 C16 1.500(6) . ? C61 C66 1.495(6) . ? C49 C54 1.494(6) . ? C18 C13 1.496(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C85 C86 1.394(6) . ? C9 C4 1.495(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C67 C68 1.514(5) . ? C31 C30 1.390(6) . ? C109 C110 1.378(7) . ? C109 C108 1.384(6) . ? C109 H109 0.9300 . ? C14 C13 1.393(6) . ? C14 C15 1.431(6) . ? C42 H42 0.9300 . ? C6 C1 1.506(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C83 C81 1.537(6) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C15 C20 1.501(6) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C76 C75 1.382(6) . ? C76 H76 0.9300 . ? C23 C22 1.536(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C112 C107 1.370(7) . ? C112 C111 1.382(6) . ? C112 H112 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C105 C100 1.385(6) . ? C105 C104 1.388(6) . ? C105 H105 0.9300 . ? C68 C71 1.521(6) . ? C68 C70 1.533(5) . ? C68 C69 1.537(5) . ? C64 C59 1.508(6) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C73 C78 1.510(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C97 C96 1.380(6) . ? C97 H97 0.9300 . ? C75 H75 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C25 C22 1.524(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C107 C108 1.391(6) . ? C107 C113 1.520(6) . ? C4 C5 1.406(6) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C110 C111 1.381(6) . ? C110 H110 0.9300 . ? C5 C1 1.424(6) . ? C5 C10 1.502(5) . ? C100 C101 1.388(6) . ? C100 C106 1.498(6) . ? C111 H111 0.9300 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C94 H94 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C102 C103 1.371(6) . ? C102 C101 1.393(6) . ? C102 H102 0.9300 . ? C104 C103 1.371(6) . ? C104 H104 0.9300 . ? C21 C22 1.524(6) . ? C81 C84 1.521(6) . ? C81 C82 1.542(5) . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? C101 H101 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C30 H30 0.9300 . ? C88 C89 1.377(6) . ? C88 H88 0.9300 . ? C89 H89 0.9300 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C108 H108 0.9300 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C22 C24 1.539(5) . ? C96 H96 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C103 H103 0.9300 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C106 H10D 0.9600 . ? C106 H10E 0.9600 . ? C106 H10F 0.9600 . ? C113 H11A 0.9600 . ? C113 H11B 0.9600 . ? C113 H11C 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 N2 Ta2 O2 96.97(12) . . ? N2 Ta2 N4 104.97(12) . . ? O2 Ta2 N4 58.87(11) . . ? N2 Ta2 Cl2 98.27(11) . . ? O2 Ta2 Cl2 138.85(7) . . ? N4 Ta2 Cl2 80.29(9) . . ? N2 Ta2 C15 105.00(14) . . ? O2 Ta2 C15 74.51(12) . . ? N4 Ta2 C15 126.65(13) . . ? Cl2 Ta2 C15 136.20(10) . . ? N2 Ta2 C12 103.66(13) . . ? O2 Ta2 C12 129.83(12) . . ? N4 Ta2 C12 148.41(12) . . ? Cl2 Ta2 C12 82.67(11) . . ? C15 Ta2 C12 56.19(14) . . ? N2 Ta2 C11 87.14(13) . . ? O2 Ta2 C11 104.99(13) . . ? N4 Ta2 C11 160.37(13) . . ? Cl2 Ta2 C11 113.73(11) . . ? C15 Ta2 C11 33.81(14) . . ? C12 Ta2 C11 33.31(14) . . ? N2 Ta2 C14 138.88(14) . . ? O2 Ta2 C14 78.62(12) . . ? N4 Ta2 C14 107.08(12) . . ? Cl2 Ta2 C14 111.89(11) . . ? C15 Ta2 C14 34.12(13) . . ? C12 Ta2 C14 55.93(13) . . ? C11 Ta2 C14 55.81(13) . . ? N2 Ta2 C13 137.84(14) . . ? O2 Ta2 C13 110.21(12) . . ? N4 Ta2 C13 116.51(12) . . ? Cl2 Ta2 C13 82.23(10) . . ? C15 Ta2 C13 55.71(13) . . ? C12 Ta2 C13 34.28(13) . . ? C11 Ta2 C13 55.57(13) . . ? C14 Ta2 C13 32.72(13) . . ? N2 Ta2 C34 102.72(12) . . ? O2 Ta2 C34 29.12(11) . . ? N4 Ta2 C34 29.74(11) . . ? Cl2 Ta2 C34 109.89(9) . . ? C15 Ta2 C34 100.56(13) . . ? C12 Ta2 C34 148.66(12) . . ? C11 Ta2 C34 133.22(14) . . ? C14 Ta2 C34 92.86(12) . . ? C13 Ta2 C34 116.83(12) . . ? N6 Ta4 O4 95.27(12) . . ? N6 Ta4 N8 104.08(13) . . ? O4 Ta4 N8 59.21(11) . . ? N6 Ta4 C57 102.76(14) . . ? O4 Ta4 C57 76.87(13) . . ? N8 Ta4 C57 129.86(14) . . ? N6 Ta4 Cl4 96.94(10) . . ? O4 Ta4 Cl4 140.14(8) . . ? N8 Ta4 Cl4 81.01(9) . . ? C57 Ta4 Cl4 135.92(10) . . ? N6 Ta4 C58 87.44(14) . . ? O4 Ta4 C58 108.39(13) . . ? N8 Ta4 C58 163.32(13) . . ? C57 Ta4 C58 33.97(14) . . ? Cl4 Ta4 C58 109.94(10) . . ? N6 Ta4 C61 137.18(14) . . ? O4 Ta4 C61 78.13(13) . . ? N8 Ta4 C61 108.04(14) . . ? C57 Ta4 C61 34.42(13) . . ? Cl4 Ta4 C61 115.27(10) . . ? C58 Ta4 C61 56.28(14) . . ? N6 Ta4 C59 107.31(14) . . ? O4 Ta4 C59 131.00(13) . . ? N8 Ta4 C59 145.08(12) . . ? C57 Ta4 C59 56.24(13) . . ? Cl4 Ta4 C59 80.40(10) . . ? C58 Ta4 C59 33.79(12) . . ? C61 Ta4 C59 55.63(14) . . ? N6 Ta4 C60 140.03(14) . . ? O4 Ta4 C60 109.25(12) . . ? N8 Ta4 C60 115.47(13) . . ? C57 Ta4 C60 55.71(13) . . ? Cl4 Ta4 C60 84.24(10) . . ? C58 Ta4 C60 55.47(13) . . ? C61 Ta4 C60 32.88(13) . . ? C59 Ta4 C60 33.24(13) . . ? N6 Ta4 C80 100.31(13) . . ? O4 Ta4 C80 29.51(11) . . ? N8 Ta4 C80 29.73(12) . . ? C57 Ta4 C80 104.01(14) . . ? Cl4 Ta4 C80 110.73(9) . . ? C58 Ta4 C80 137.21(14) . . ? C61 Ta4 C80 94.05(14) . . ? C59 Ta4 C80 148.80(13) . . ? C60 Ta4 C80 116.69(13) . . ? N5 Ta3 O3 95.42(12) . . ? N5 Ta3 N7 102.45(12) . . ? O3 Ta3 N7 59.01(11) . . ? N5 Ta3 Cl3 98.13(10) . . ? O3 Ta3 Cl3 139.72(8) . . ? N7 Ta3 Cl3 81.03(9) . . ? N5 Ta3 C49 106.09(14) . . ? O3 Ta3 C49 73.76(12) . . ? N7 Ta3 C49 126.35(13) . . ? Cl3 Ta3 C49 136.43(10) . . ? N5 Ta3 C47 104.81(13) . . ? O3 Ta3 C47 129.37(12) . . ? N7 Ta3 C47 150.02(12) . . ? Cl3 Ta3 C47 83.01(10) . . ? C49 Ta3 C47 56.24(14) . . ? N5 Ta3 C48 88.15(13) . . ? O3 Ta3 C48 103.76(12) . . ? N7 Ta3 C48 160.17(13) . . ? Cl3 Ta3 C48 114.40(11) . . ? C49 Ta3 C48 33.82(13) . . ? C47 Ta3 C48 33.63(13) . . ? N5 Ta3 C50 139.98(14) . . ? O3 Ta3 C50 78.63(11) . . ? N7 Ta3 C50 107.64(12) . . ? Cl3 Ta3 C50 111.97(10) . . ? C49 Ta3 C50 34.05(13) . . ? C47 Ta3 C50 56.11(13) . . ? C48 Ta3 C50 56.06(13) . . ? N5 Ta3 C51 138.78(14) . . ? O3 Ta3 C51 110.91(11) . . ? N7 Ta3 C51 118.12(12) . . ? Cl3 Ta3 C51 82.14(10) . . ? C49 Ta3 C51 55.82(14) . . ? C47 Ta3 C51 34.03(13) . . ? C48 Ta3 C51 55.79(13) . . ? C50 Ta3 C51 33.15(13) . . ? N5 Ta3 C67 99.07(13) . . ? O3 Ta3 C67 29.49(11) . . ? N7 Ta3 C67 29.57(12) . . ? Cl3 Ta3 C67 110.56(9) . . ? C49 Ta3 C67 100.84(13) . . ? C47 Ta3 C67 150.58(12) . . ? C48 Ta3 C67 132.86(14) . . ? C50 Ta3 C67 94.49(12) . . ? C51 Ta3 C67 119.59(12) . . ? N1 Ta1 O1 96.46(12) . . ? N1 Ta1 N3 104.12(13) . . ? O1 Ta1 N3 58.63(11) . . ? N1 Ta1 C3 105.18(14) . . ? O1 Ta1 C3 76.37(13) . . ? N3 Ta1 C3 128.20(14) . . ? N1 Ta1 Cl1 96.68(10) . . ? O1 Ta1 Cl1 139.42(8) . . ? N3 Ta1 Cl1 80.94(8) . . ? C3 Ta1 Cl1 135.51(10) . . ? N1 Ta1 C2 87.49(14) . . ? O1 Ta1 C2 107.30(13) . . ? N3 Ta1 C2 162.21(13) . . ? C3 Ta1 C2 34.18(15) . . ? Cl1 Ta1 C2 111.49(11) . . ? N1 Ta1 C1 104.94(14) . . ? O1 Ta1 C1 131.21(13) . . ? N3 Ta1 C1 147.38(12) . . ? C3 Ta1 C1 56.00(14) . . ? Cl1 Ta1 C1 81.28(10) . . ? C2 Ta1 C1 33.28(13) . . ? N1 Ta1 C4 139.39(14) . . ? O1 Ta1 C4 79.78(13) . . ? N3 Ta1 C4 107.79(13) . . ? C3 Ta1 C4 34.38(13) . . ? Cl1 Ta1 C4 112.45(10) . . ? C2 Ta1 C4 56.32(14) . . ? C1 Ta1 C4 55.54(14) . . ? N1 Ta1 C5 138.20(14) . . ? O1 Ta1 C5 111.38(12) . . ? N3 Ta1 C5 116.79(12) . . ? C3 Ta1 C5 55.67(13) . . ? Cl1 Ta1 C5 82.27(10) . . ? C2 Ta1 C5 55.36(13) . . ? C1 Ta1 C5 33.37(13) . . ? C4 Ta1 C5 32.84(13) . . ? N1 Ta1 C21 101.29(13) . . ? O1 Ta1 C21 29.30(11) . . ? N3 Ta1 C21 29.34(11) . . ? C3 Ta1 C21 102.89(14) . . ? Cl1 Ta1 C21 110.25(9) . . ? C2 Ta1 C21 135.89(14) . . ? C1 Ta1 C21 149.87(13) . . ? C4 Ta1 C21 94.65(14) . . ? C5 Ta1 C21 118.37(13) . . ? 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 . . ? C96 C95 C94 121.3(4) . . ? C96 C95 H95 119.4 . . ? C94 C95 H95 119.4 . . ? N1 N2 Ta2 169.0(3) . . ? N5 N6 Ta4 168.7(3) . . ? C57 C58 C59 107.6(4) . . ? C57 C58 C63 127.3(4) . . ? C59 C58 C63 125.0(4) . . ? C57 C58 Ta4 71.5(2) . . ? C59 C58 Ta4 73.7(2) . . ? C63 C58 Ta4 121.1(3) . . ? N2 N1 Ta1 168.5(3) . . ? N6 N5 Ta3 170.8(3) . . ? C48 C47 C51 107.8(4) . . ? C48 C47 C52 126.3(4) . . ? C51 C47 C52 125.5(4) . . ? C48 C47 Ta3 73.3(2) . . ? C51 C47 Ta3 74.9(2) . . ? C52 C47 Ta3 122.9(2) . . ? C34 O2 Ta2 96.9(2) . . ? C80 N8 C85 130.7(4) . . ? C80 N8 Ta4 93.4(3) . . ? C85 N8 Ta4 135.8(3) . . ? C11 C12 C13 107.3(4) . . ? C11 C12 C17 127.2(4) . . ? C13 C12 C17 125.2(4) . . ? C11 C12 Ta2 73.4(2) . . ? C13 C12 Ta2 74.5(2) . . ? C17 C12 Ta2 122.9(2) . . ? C80 O4 Ta4 96.1(2) . . ? C67 O3 Ta3 96.7(2) . . ? C1 C2 C3 107.7(4) . . ? C1 C2 C7 124.9(4) . . ? C3 C2 C7 127.4(4) . . ? C1 C2 Ta1 73.8(2) . . ? C3 C2 Ta1 71.8(2) . . ? C7 C2 Ta1 121.4(3) . . ? O2 C34 N4 111.1(3) . . ? O2 C34 C35 118.2(4) . . ? N4 C34 C35 130.6(4) . . ? O2 C34 Ta2 53.98(19) . . ? N4 C34 Ta2 57.2(2) . . ? C35 C34 Ta2 171.8(3) . . ? C21 O1 Ta1 96.3(2) . . ? C21 N3 C26 130.1(3) . . ? C21 N3 Ta1 93.7(3) . . ? C26 N3 Ta1 136.1(2) . . ? C29 C28 C27 121.3(4) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C58 C57 C61 108.1(3) . . ? C58 C57 C62 125.6(4) . . ? C61 C57 C62 126.1(4) . . ? C58 C57 Ta4 74.5(2) . . ? C61 C57 Ta4 74.8(2) . . ? C62 C57 Ta4 120.9(3) . . ? C39 C44 C43 118.6(3) . . ? C39 C44 C45 122.2(3) . . ? C43 C44 C45 119.2(4) . . ? C28 C29 C30 119.7(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C75 C74 C73 121.3(4) . . ? C75 C74 H74 119.3 . . ? C73 C74 H74 119.3 . . ? C76 C77 C72 118.4(4) . . ? C76 C77 C79 121.8(3) . . ? C72 C77 C79 119.7(3) . . ? C73 C72 C77 121.0(4) . . ? C73 C72 N7 118.9(3) . . ? C77 C72 N7 119.8(3) . . ? C31 C26 C27 121.5(4) . . ? C31 C26 N3 118.7(4) . . ? C27 C26 N3 119.3(3) . . ? C42 C43 C44 121.4(4) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C34 N4 C39 128.8(3) . . ? C34 N4 Ta2 93.1(2) . . ? C39 N4 Ta2 137.7(3) . . ? C50 C51 C47 107.5(4) . . ? C50 C51 C56 126.8(4) . . ? C47 C51 C56 125.6(4) . . ? C50 C51 Ta3 72.02(19) . . ? C47 C51 Ta3 71.10(19) . . ? C56 C51 Ta3 124.7(3) . . ? C67 N7 C72 129.5(3) . . ? C67 N7 Ta3 93.3(2) . . ? C72 N7 Ta3 136.3(3) . . ? C44 C39 C40 121.0(4) . . ? C44 C39 N4 120.5(3) . . ? C40 C39 N4 118.0(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O4 C80 N8 111.2(4) . . ? O4 C80 C81 117.4(3) . . ? N8 C80 C81 131.4(4) . . ? O4 C80 Ta4 54.39(19) . . ? N8 C80 Ta4 56.9(2) . . ? C81 C80 Ta4 171.3(3) . . ? C88 C87 C86 121.3(4) . . ? C88 C87 H87 119.3 . . ? C86 C87 H87 119.3 . . ? C94 C93 C98 117.9(4) . . ? C94 C93 C99 120.5(5) . . ? C98 C93 C99 121.6(4) . . ? C61 C60 C59 108.6(3) . . ? C61 C60 C65 127.9(4) . . ? C59 C60 C65 123.5(4) . . ? C61 C60 Ta4 71.7(2) . . ? C59 C60 Ta4 71.6(2) . . ? C65 C60 Ta4 122.9(3) . . ? C2 C3 C4 107.6(4) . . ? C2 C3 C8 125.8(4) . . ? C4 C3 C8 126.3(4) . . ? C2 C3 Ta1 74.0(2) . . ? C4 C3 Ta1 74.8(2) . . ? C8 C3 Ta1 121.8(3) . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C97 C98 C93 121.2(4) . . ? C97 C98 H98 119.4 . . ? C93 C98 H98 119.4 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C86 C91 H91A 109.5 . . ? C86 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C86 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C42 C41 C40 120.9(4) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C34 C35 C36 109.7(3) . . ? C34 C35 C38 111.2(3) . . ? C36 C35 C38 109.4(3) . . ? C34 C35 C37 109.1(3) . . ? C36 C35 C37 108.8(3) . . ? C38 C35 C37 108.6(3) . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C89 C90 C85 118.9(4) . . ? C89 C90 C92 120.9(4) . . ? C85 C90 C92 120.1(4) . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C41 C40 C39 118.3(4) . . ? C41 C40 C46 120.7(3) . . ? C39 C40 C46 121.0(3) . . ? C51 C50 C49 108.1(3) . . ? C51 C50 C55 126.7(4) . . ? C49 C50 C55 125.2(4) . . ? C51 C50 Ta3 74.83(19) . . ? C49 C50 Ta3 71.5(2) . . ? C55 C50 Ta3 121.0(2) . . ? C47 C48 C49 108.1(4) . . ? C47 C48 C53 125.7(4) . . ? C49 C48 C53 126.1(4) . . ? C47 C48 Ta3 73.0(2) . . ? C49 C48 Ta3 72.0(2) . . ? C53 C48 Ta3 121.5(2) . . ? C12 C11 C15 108.8(4) . . ? C12 C11 C16 126.4(4) . . ? C15 C11 C16 124.8(4) . . ? C12 C11 Ta2 73.3(2) . . ? C15 C11 Ta2 72.0(2) . . ? C16 C11 Ta2 121.9(2) . . ? C60 C61 C57 107.6(4) . . ? C60 C61 C66 127.1(4) . . ? C57 C61 C66 125.2(4) . . ? C60 C61 Ta4 75.4(2) . . ? C57 C61 Ta4 70.7(2) . . ? C66 C61 Ta4 122.6(3) . . ? C48 C49 C50 108.3(4) . . ? C48 C49 C54 125.5(4) . . ? C50 C49 C54 125.8(4) . . ? C48 C49 Ta3 74.2(2) . . ? C50 C49 Ta3 74.4(2) . . ? C54 C49 Ta3 122.9(2) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C86 C85 C90 121.0(4) . . ? C86 C85 N8 119.0(4) . . ? C90 C85 N8 119.6(4) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N7 C67 O3 110.9(3) . . ? N7 C67 C68 133.6(4) . . ? O3 C67 C68 115.6(4) . . ? N7 C67 Ta3 57.1(2) . . ? O3 C67 Ta3 53.86(19) . . ? C68 C67 Ta3 169.0(3) . . ? C30 C31 C26 118.6(4) . . ? C30 C31 C33 120.8(4) . . ? C26 C31 C33 120.6(4) . . ? C110 C109 C108 119.7(4) . . ? C110 C109 H109 120.1 . . ? C108 C109 H109 120.1 . . ? C13 C14 C15 108.5(4) . . ? C13 C14 C19 127.3(4) . . ? C15 C14 C19 124.2(4) . . ? C13 C14 Ta2 74.74(19) . . ? C15 C14 Ta2 71.3(2) . . ? C19 C14 Ta2 121.5(2) . . ? C41 C42 C43 119.5(4) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C87 C86 C85 118.2(4) . . ? C87 C86 C91 121.1(4) . . ? C85 C86 C91 120.7(4) . . ? C11 C15 C14 107.6(4) . . ? C11 C15 C20 126.5(4) . . ? C14 C15 C20 125.6(4) . . ? C11 C15 Ta2 74.2(2) . . ? C14 C15 Ta2 74.6(2) . . ? C20 C15 Ta2 122.2(2) . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C75 C76 C77 121.0(4) . . ? C75 C76 H76 119.5 . . ? C77 C76 H76 119.5 . . ? 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 . . ? C107 C112 C111 120.0(4) . . ? C107 C112 H112 120.0 . . ? C111 C112 H112 120.0 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C13 C12 107.7(4) . . ? C14 C13 C18 127.6(4) . . ? C12 C13 C18 124.5(4) . . ? C14 C13 Ta2 72.54(19) . . ? C12 C13 Ta2 71.2(2) . . ? C18 C13 Ta2 124.9(3) . . ? C100 C105 C104 121.7(4) . . ? C100 C105 H105 119.1 . . ? C104 C105 H105 119.1 . . ? C67 C68 C71 107.5(4) . . ? C67 C68 C70 113.5(4) . . ? C71 C68 C70 109.7(3) . . ? C67 C68 C69 107.5(3) . . ? C71 C68 C69 109.2(4) . . ? C70 C68 C69 109.3(4) . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C72 C73 C74 118.3(4) . . ? C72 C73 C78 120.9(4) . . ? C74 C73 C78 120.7(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C98 C97 C96 120.4(5) . . ? C98 C97 H97 119.8 . . ? C96 C97 H97 119.8 . . ? C74 C75 C76 119.7(4) . . ? C74 C75 H75 120.1 . . ? C76 C75 H75 120.1 . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C112 C107 C108 119.6(4) . . ? C112 C107 C113 120.5(4) . . ? C108 C107 C113 120.0(5) . . ? C5 C4 C3 107.5(4) . . ? C5 C4 C9 127.0(4) . . ? C3 C4 C9 125.3(4) . . ? C5 C4 Ta1 75.1(2) . . ? C3 C4 Ta1 70.8(2) . . ? C9 C4 Ta1 122.8(3) . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C109 C110 C111 119.7(5) . . ? C109 C110 H110 120.2 . . ? C111 C110 H110 120.2 . . ? C4 C5 C1 108.2(3) . . ? C4 C5 C10 127.6(4) . . ? C1 C5 C10 124.2(4) . . ? C4 C5 Ta1 72.1(2) . . ? C1 C5 Ta1 71.3(2) . . ? C10 C5 Ta1 123.6(3) . . ? C105 C100 C101 117.4(4) . . ? C105 C100 C106 122.5(5) . . ? C101 C100 C106 120.1(5) . . ? C110 C111 C112 120.6(5) . . ? C110 C111 H111 119.7 . . ? C112 C111 H111 119.7 . . ? C28 C27 C26 118.1(4) . . ? C28 C27 C32 121.2(4) . . ? C26 C27 C32 120.7(4) . . ? C60 C65 H65A 109.5 . . ? C60 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C60 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C95 C94 C93 120.2(4) . . ? C95 C94 H94 119.9 . . ? C93 C94 H94 119.9 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C103 C102 C101 119.7(4) . . ? C103 C102 H102 120.2 . . ? C101 C102 H102 120.2 . . ? C103 C104 C105 119.6(5) . . ? C103 C104 H104 120.2 . . ? C105 C104 H104 120.2 . . ? N3 C21 O1 111.3(4) . . ? N3 C21 C22 132.0(4) . . ? O1 C21 C22 116.7(3) . . ? N3 C21 Ta1 57.0(2) . . ? O1 C21 Ta1 54.39(19) . . ? C22 C21 Ta1 171.0(3) . . ? C84 C81 C80 114.2(4) . . ? C84 C81 C83 109.4(4) . . ? C80 C81 C83 106.4(4) . . ? C84 C81 C82 109.5(4) . . ? C80 C81 C82 107.8(3) . . ? C83 C81 C82 109.3(4) . . ? C2 C1 C5 108.8(4) . . ? C2 C1 C6 125.7(4) . . ? C5 C1 C6 125.0(4) . . ? C2 C1 Ta1 72.9(2) . . ? C5 C1 Ta1 75.3(2) . . ? C6 C1 Ta1 123.7(3) . . ? C93 C99 H99A 109.5 . . ? C93 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C93 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C100 C101 C102 121.3(5) . . ? C100 C101 H101 119.4 . . ? C102 C101 H101 119.4 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C60 C59 C58 108.1(4) . . ? C60 C59 C64 125.9(4) . . ? C58 C59 C64 125.5(4) . . ? C60 C59 Ta4 75.2(2) . . ? C58 C59 Ta4 72.5(2) . . ? C64 C59 Ta4 124.8(3) . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C87 C88 C89 119.9(5) . . ? C87 C88 H88 120.0 . . ? C89 C88 H88 120.0 . . ? C88 C89 C90 120.7(5) . . ? C88 C89 H89 119.7 . . ? C90 C89 H89 119.7 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C109 C108 C107 120.4(5) . . ? C109 C108 H108 119.8 . . ? C107 C108 H108 119.8 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C21 C22 C25 114.1(3) . . ? C21 C22 C23 107.2(4) . . ? C25 C22 C23 109.7(4) . . ? C21 C22 C24 108.5(3) . . ? C25 C22 C24 109.1(4) . . ? C23 C22 C24 108.0(4) . . ? C95 C96 C97 119.1(5) . . ? C95 C96 H96 120.5 . . ? C97 C96 H96 120.5 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C102 C103 C104 120.4(5) . . ? C102 C103 H103 119.8 . . ? C104 C103 H103 119.8 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 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 . . ? C100 C106 H10D 109.5 . . ? C100 C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C100 C106 H10F 109.5 . . ? H10D C106 H10F 109.5 . . ? H10E C106 H10F 109.5 . . ? C107 C113 H11A 109.5 . . ? C107 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C107 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 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 O2 Ta2 N2 N1 -96.3(15) . . . . ? N4 Ta2 N2 N1 -155.9(15) . . . . ? Cl2 Ta2 N2 N1 122.0(15) . . . . ? C15 Ta2 N2 N1 -20.6(16) . . . . ? C12 Ta2 N2 N1 37.6(16) . . . . ? C11 Ta2 N2 N1 8.4(15) . . . . ? C14 Ta2 N2 N1 -15.7(16) . . . . ? C13 Ta2 N2 N1 34.5(16) . . . . ? C34 Ta2 N2 N1 -125.3(15) . . . . ? O4 Ta4 N6 N5 -134.3(14) . . . . ? N8 Ta4 N6 N5 166.2(14) . . . . ? C57 Ta4 N6 N5 -56.6(14) . . . . ? Cl4 Ta4 N6 N5 83.8(14) . . . . ? C58 Ta4 N6 N5 -26.0(14) . . . . ? C61 Ta4 N6 N5 -56.1(15) . . . . ? C59 Ta4 N6 N5 1.7(14) . . . . ? C60 Ta4 N6 N5 -5.5(15) . . . . ? C80 Ta4 N6 N5 -163.6(14) . . . . ? N6 Ta4 C58 C57 -117.5(2) . . . . ? O4 Ta4 C58 C57 -22.8(2) . . . . ? N8 Ta4 C58 C57 16.9(5) . . . . ? Cl4 Ta4 C58 C57 146.03(19) . . . . ? C61 Ta4 C58 C57 38.3(2) . . . . ? C59 Ta4 C58 C57 115.4(3) . . . . ? C60 Ta4 C58 C57 78.3(2) . . . . ? C80 Ta4 C58 C57 -15.1(3) . . . . ? N6 Ta4 C58 C59 127.0(3) . . . . ? O4 Ta4 C58 C59 -138.3(2) . . . . ? N8 Ta4 C58 C59 -98.6(4) . . . . ? C57 Ta4 C58 C59 -115.4(3) . . . . ? Cl4 Ta4 C58 C59 30.6(3) . . . . ? C61 Ta4 C58 C59 -77.1(3) . . . . ? C60 Ta4 C58 C59 -37.1(2) . . . . ? C80 Ta4 C58 C59 -130.5(2) . . . . ? N6 Ta4 C58 C63 5.5(3) . . . . ? O4 Ta4 C58 C63 100.2(3) . . . . ? N8 Ta4 C58 C63 139.9(4) . . . . ? C57 Ta4 C58 C63 123.1(4) . . . . ? Cl4 Ta4 C58 C63 -90.9(3) . . . . ? C61 Ta4 C58 C63 161.4(4) . . . . ? C59 Ta4 C58 C63 -121.5(5) . . . . ? C60 Ta4 C58 C63 -158.6(4) . . . . ? C80 Ta4 C58 C63 108.0(3) . . . . ? Ta2 N2 N1 Ta1 -131.2(13) . . . . ? O1 Ta1 N1 N2 130.3(14) . . . . ? N3 Ta1 N1 N2 -170.4(13) . . . . ? C3 Ta1 N1 N2 52.8(14) . . . . ? Cl1 Ta1 N1 N2 -88.1(14) . . . . ? C2 Ta1 N1 N2 23.2(14) . . . . ? C1 Ta1 N1 N2 -5.4(14) . . . . ? C4 Ta1 N1 N2 48.5(14) . . . . ? C5 Ta1 N1 N2 -2.3(15) . . . . ? C21 Ta1 N1 N2 159.6(13) . . . . ? Ta4 N6 N5 Ta3 150.5(11) . . . . ? O3 Ta3 N5 N6 80.9(18) . . . . ? N7 Ta3 N5 N6 140.3(18) . . . . ? Cl3 Ta3 N5 N6 -137.2(18) . . . . ? C49 Ta3 N5 N6 6.2(18) . . . . ? C47 Ta3 N5 N6 -52.3(18) . . . . ? C48 Ta3 N5 N6 -22.8(18) . . . . ? C50 Ta3 N5 N6 2.1(19) . . . . ? C51 Ta3 N5 N6 -49.8(19) . . . . ? C67 Ta3 N5 N6 110.4(18) . . . . ? N5 Ta3 C47 C48 62.8(3) . . . . ? O3 Ta3 C47 C48 -47.3(3) . . . . ? N7 Ta3 C47 C48 -142.5(3) . . . . ? Cl3 Ta3 C47 C48 159.4(2) . . . . ? C49 Ta3 C47 C48 -36.9(2) . . . . ? C50 Ta3 C47 C48 -78.2(3) . . . . ? C51 Ta3 C47 C48 -114.4(3) . . . . ? C67 Ta3 C47 C48 -80.5(4) . . . . ? N5 Ta3 C47 C51 177.1(2) . . . . ? O3 Ta3 C47 C51 67.0(3) . . . . ? N7 Ta3 C47 C51 -28.1(4) . . . . ? Cl3 Ta3 C47 C51 -86.3(2) . . . . ? C49 Ta3 C47 C51 77.4(3) . . . . ? C48 Ta3 C47 C51 114.4(3) . . . . ? C50 Ta3 C47 C51 36.2(2) . . . . ? C67 Ta3 C47 C51 33.9(4) . . . . ? N5 Ta3 C47 C52 -60.1(4) . . . . ? O3 Ta3 C47 C52 -170.1(3) . . . . ? N7 Ta3 C47 C52 94.7(4) . . . . ? Cl3 Ta3 C47 C52 36.5(3) . . . . ? C49 Ta3 C47 C52 -159.7(4) . . . . ? C48 Ta3 C47 C52 -122.8(4) . . . . ? C50 Ta3 C47 C52 159.0(4) . . . . ? C51 Ta3 C47 C52 122.8(5) . . . . ? C67 Ta3 C47 C52 156.7(3) . . . . ? N2 Ta2 O2 C34 -103.7(2) . . . . ? N4 Ta2 O2 C34 -0.37(19) . . . . ? Cl2 Ta2 O2 C34 7.4(3) . . . . ? C15 Ta2 O2 C34 152.6(2) . . . . ? C12 Ta2 O2 C34 142.0(2) . . . . ? C11 Ta2 O2 C34 167.4(2) . . . . ? C14 Ta2 O2 C34 117.8(2) . . . . ? C13 Ta2 O2 C34 109.1(2) . . . . ? N6 Ta4 N8 C80 86.1(2) . . . . ? O4 Ta4 N8 C80 -1.6(2) . . . . ? C57 Ta4 N8 C80 -34.3(3) . . . . ? Cl4 Ta4 N8 C80 -178.9(2) . . . . ? C58 Ta4 N8 C80 -46.5(5) . . . . ? C61 Ta4 N8 C80 -65.1(2) . . . . ? C59 Ta4 N8 C80 -120.3(3) . . . . ? C60 Ta4 N8 C80 -99.7(2) . . . . ? N6 Ta4 N8 C85 -89.3(4) . . . . ? O4 Ta4 N8 C85 -177.0(4) . . . . ? C57 Ta4 N8 C85 150.3(3) . . . . ? Cl4 Ta4 N8 C85 5.7(3) . . . . ? C58 Ta4 N8 C85 138.1(4) . . . . ? C61 Ta4 N8 C85 119.4(4) . . . . ? C59 Ta4 N8 C85 64.2(4) . . . . ? C60 Ta4 N8 C85 84.8(4) . . . . ? C80 Ta4 N8 C85 -175.4(5) . . . . ? N2 Ta2 C12 C11 -62.4(3) . . . . ? O2 Ta2 C12 C11 49.0(3) . . . . ? N4 Ta2 C12 C11 143.1(3) . . . . ? Cl2 Ta2 C12 C11 -159.2(2) . . . . ? C15 Ta2 C12 C11 36.7(2) . . . . ? C14 Ta2 C12 C11 78.1(3) . . . . ? C13 Ta2 C12 C11 113.9(4) . . . . ? C34 Ta2 C12 C11 84.2(3) . . . . ? N2 Ta2 C12 C13 -176.3(2) . . . . ? O2 Ta2 C12 C13 -64.9(3) . . . . ? N4 Ta2 C12 C13 29.2(4) . . . . ? Cl2 Ta2 C12 C13 86.9(2) . . . . ? C15 Ta2 C12 C13 -77.2(3) . . . . ? C11 Ta2 C12 C13 -113.9(4) . . . . ? C14 Ta2 C12 C13 -35.8(2) . . . . ? C34 Ta2 C12 C13 -29.7(4) . . . . ? N2 Ta2 C12 C17 61.5(4) . . . . ? O2 Ta2 C12 C17 172.9(3) . . . . ? N4 Ta2 C12 C17 -93.0(4) . . . . ? Cl2 Ta2 C12 C17 -35.3(3) . . . . ? C15 Ta2 C12 C17 160.6(4) . . . . ? C11 Ta2 C12 C17 123.9(4) . . . . ? C14 Ta2 C12 C17 -158.0(4) . . . . ? C13 Ta2 C12 C17 -122.2(5) . . . . ? C34 Ta2 C12 C17 -151.9(3) . . . . ? N6 Ta4 O4 C80 -101.6(2) . . . . ? N8 Ta4 O4 C80 1.6(2) . . . . ? C57 Ta4 O4 C80 156.5(2) . . . . ? Cl4 Ta4 O4 C80 5.8(3) . . . . ? C58 Ta4 O4 C80 169.3(2) . . . . ? C61 Ta4 O4 C80 121.2(2) . . . . ? C59 Ta4 O4 C80 139.9(2) . . . . ? C60 Ta4 O4 C80 110.4(2) . . . . ? N5 Ta3 O3 C67 98.9(2) . . . . ? N7 Ta3 O3 C67 -2.4(2) . . . . ? Cl3 Ta3 O3 C67 -10.5(3) . . . . ? C49 Ta3 O3 C67 -155.9(2) . . . . ? C47 Ta3 O3 C67 -146.9(2) . . . . ? C48 Ta3 O3 C67 -171.7(2) . . . . ? C50 Ta3 O3 C67 -121.2(2) . . . . ? C51 Ta3 O3 C67 -113.5(2) . . . . ? N1 Ta1 C2 C1 -122.5(3) . . . . ? O1 Ta1 C2 C1 141.5(2) . . . . ? N3 Ta1 C2 C1 106.0(4) . . . . ? C3 Ta1 C2 C1 115.4(3) . . . . ? Cl1 Ta1 C2 C1 -26.3(3) . . . . ? C4 Ta1 C2 C1 77.1(3) . . . . ? C5 Ta1 C2 C1 37.1(2) . . . . ? C21 Ta1 C2 C1 133.9(2) . . . . ? N1 Ta1 C2 C3 122.1(2) . . . . ? O1 Ta1 C2 C3 26.1(2) . . . . ? N3 Ta1 C2 C3 -9.4(5) . . . . ? Cl1 Ta1 C2 C3 -141.7(2) . . . . ? C1 Ta1 C2 C3 -115.4(3) . . . . ? C4 Ta1 C2 C3 -38.4(2) . . . . ? C5 Ta1 C2 C3 -78.3(2) . . . . ? C21 Ta1 C2 C3 18.4(3) . . . . ? N1 Ta1 C2 C7 -1.1(4) . . . . ? O1 Ta1 C2 C7 -97.1(4) . . . . ? N3 Ta1 C2 C7 -132.6(4) . . . . ? C3 Ta1 C2 C7 -123.2(5) . . . . ? Cl1 Ta1 C2 C7 95.1(4) . . . . ? C1 Ta1 C2 C7 121.4(5) . . . . ? C4 Ta1 C2 C7 -161.6(4) . . . . ? C5 Ta1 C2 C7 158.5(4) . . . . ? C21 Ta1 C2 C7 -104.8(4) . . . . ? Ta2 O2 C34 N4 0.6(3) . . . . ? Ta2 O2 C34 C35 -177.0(3) . . . . ? N2 Ta2 C34 O2 81.4(2) . . . . ? N4 Ta2 C34 O2 179.4(3) . . . . ? Cl2 Ta2 C34 O2 -174.81(18) . . . . ? C15 Ta2 C34 O2 -26.8(2) . . . . ? C12 Ta2 C34 O2 -65.3(3) . . . . ? C11 Ta2 C34 O2 -16.8(3) . . . . ? C14 Ta2 C34 O2 -60.3(2) . . . . ? C13 Ta2 C34 O2 -83.6(2) . . . . ? N2 Ta2 C34 N4 -98.0(2) . . . . ? O2 Ta2 C34 N4 -179.4(3) . . . . ? Cl2 Ta2 C34 N4 5.8(2) . . . . ? C15 Ta2 C34 N4 153.9(2) . . . . ? C12 Ta2 C34 N4 115.3(3) . . . . ? C11 Ta2 C34 N4 163.9(2) . . . . ? C14 Ta2 C34 N4 120.3(2) . . . . ? C13 Ta2 C34 N4 97.1(2) . . . . ? N2 Ta2 C34 C35 100.2(18) . . . . ? O2 Ta2 C34 C35 18.8(17) . . . . ? N4 Ta2 C34 C35 -161.9(19) . . . . ? Cl2 Ta2 C34 C35 -156.0(18) . . . . ? C15 Ta2 C34 C35 -8.0(18) . . . . ? C12 Ta2 C34 C35 -46.6(19) . . . . ? C11 Ta2 C34 C35 2.0(19) . . . . ? C14 Ta2 C34 C35 -41.5(18) . . . . ? C13 Ta2 C34 C35 -64.8(18) . . . . ? N1 Ta1 O1 C21 101.6(2) . . . . ? N3 Ta1 O1 C21 -1.0(2) . . . . ? C3 Ta1 O1 C21 -154.3(2) . . . . ? Cl1 Ta1 O1 C21 -6.6(3) . . . . ? C2 Ta1 O1 C21 -169.0(2) . . . . ? C1 Ta1 O1 C21 -142.1(2) . . . . ? C4 Ta1 O1 C21 -119.3(2) . . . . ? C5 Ta1 O1 C21 -110.2(2) . . . . ? N1 Ta1 N3 C21 -88.0(2) . . . . ? O1 Ta1 N3 C21 1.0(2) . . . . ? C3 Ta1 N3 C21 34.8(3) . . . . ? Cl1 Ta1 N3 C21 177.4(2) . . . . ? C2 Ta1 N3 C21 41.6(5) . . . . ? C1 Ta1 N3 C21 119.7(3) . . . . ? C4 Ta1 N3 C21 66.6(2) . . . . ? C5 Ta1 N3 C21 100.9(2) . . . . ? N1 Ta1 N3 C26 87.5(3) . . . . ? O1 Ta1 N3 C26 176.5(4) . . . . ? C3 Ta1 N3 C26 -149.7(3) . . . . ? Cl1 Ta1 N3 C26 -7.1(3) . . . . ? C2 Ta1 N3 C26 -142.9(4) . . . . ? C1 Ta1 N3 C26 -64.8(4) . . . . ? C4 Ta1 N3 C26 -117.9(3) . . . . ? C5 Ta1 N3 C26 -83.6(4) . . . . ? C21 Ta1 N3 C26 175.5(5) . . . . ? C59 C58 C57 C61 -2.5(5) . . . . ? C63 C58 C57 C61 176.6(4) . . . . ? Ta4 C58 C57 C61 -67.9(3) . . . . ? C59 C58 C57 C62 -177.4(4) . . . . ? C63 C58 C57 C62 1.6(7) . . . . ? Ta4 C58 C57 C62 117.1(4) . . . . ? C59 C58 C57 Ta4 65.4(3) . . . . ? C63 C58 C57 Ta4 -115.5(4) . . . . ? N6 Ta4 C57 C58 65.3(2) . . . . ? O4 Ta4 C57 C58 157.8(2) . . . . ? N8 Ta4 C57 C58 -173.77(19) . . . . ? Cl4 Ta4 C57 C58 -49.0(3) . . . . ? C61 Ta4 C57 C58 -114.1(3) . . . . ? C59 Ta4 C57 C58 -37.2(2) . . . . ? C60 Ta4 C57 C58 -77.5(2) . . . . ? C80 Ta4 C57 C58 169.5(2) . . . . ? N6 Ta4 C57 C61 179.4(2) . . . . ? O4 Ta4 C57 C61 -88.1(2) . . . . ? N8 Ta4 C57 C61 -59.7(3) . . . . ? Cl4 Ta4 C57 C61 65.1(3) . . . . ? C58 Ta4 C57 C61 114.1(3) . . . . ? C59 Ta4 C57 C61 76.9(2) . . . . ? C60 Ta4 C57 C61 36.6(2) . . . . ? C80 Ta4 C57 C61 -76.4(2) . . . . ? N6 Ta4 C57 C62 -57.3(4) . . . . ? O4 Ta4 C57 C62 35.2(3) . . . . ? N8 Ta4 C57 C62 63.6(4) . . . . ? Cl4 Ta4 C57 C62 -171.6(3) . . . . ? C58 Ta4 C57 C62 -122.6(4) . . . . ? C61 Ta4 C57 C62 123.3(5) . . . . ? C59 Ta4 C57 C62 -159.7(4) . . . . ? C60 Ta4 C57 C62 159.9(4) . . . . ? C80 Ta4 C57 C62 46.9(3) . . . . ? C27 C28 C29 C30 1.5(6) . . . . ? C76 C77 C72 C73 4.4(6) . . . . ? C79 C77 C72 C73 -175.1(4) . . . . ? C76 C77 C72 N7 178.6(4) . . . . ? C79 C77 C72 N7 -0.9(6) . . . . ? C21 N3 C26 C31 -94.3(5) . . . . ? Ta1 N3 C26 C31 91.6(4) . . . . ? C21 N3 C26 C27 93.1(5) . . . . ? Ta1 N3 C26 C27 -81.0(4) . . . . ? C39 C44 C43 C42 -3.6(6) . . . . ? C45 C44 C43 C42 174.4(4) . . . . ? O2 C34 N4 C39 173.3(3) . . . . ? C35 C34 N4 C39 -9.5(6) . . . . ? Ta2 C34 N4 C39 173.8(4) . . . . ? O2 C34 N4 Ta2 -0.6(3) . . . . ? C35 C34 N4 Ta2 176.7(3) . . . . ? N2 Ta2 N4 C34 89.5(2) . . . . ? O2 Ta2 N4 C34 0.36(19) . . . . ? Cl2 Ta2 N4 C34 -174.4(2) . . . . ? C15 Ta2 N4 C34 -32.7(3) . . . . ? C12 Ta2 N4 C34 -116.1(3) . . . . ? C11 Ta2 N4 C34 -37.1(5) . . . . ? C14 Ta2 N4 C34 -64.4(2) . . . . ? C13 Ta2 N4 C34 -98.2(2) . . . . ? N2 Ta2 N4 C39 -83.3(4) . . . . ? O2 Ta2 N4 C39 -172.5(4) . . . . ? Cl2 Ta2 N4 C39 12.7(3) . . . . ? C15 Ta2 N4 C39 154.5(3) . . . . ? C12 Ta2 N4 C39 71.0(4) . . . . ? C11 Ta2 N4 C39 150.1(4) . . . . ? C14 Ta2 N4 C39 122.8(3) . . . . ? C13 Ta2 N4 C39 88.9(4) . . . . ? C34 Ta2 N4 C39 -172.8(5) . . . . ? C48 C47 C51 C50 3.2(4) . . . . ? C52 C47 C51 C50 176.8(3) . . . . ? Ta3 C47 C51 C50 -63.3(2) . . . . ? C48 C47 C51 C56 -173.8(3) . . . . ? C52 C47 C51 C56 -0.2(6) . . . . ? Ta3 C47 C51 C56 119.7(4) . . . . ? C48 C47 C51 Ta3 66.5(2) . . . . ? C52 C47 C51 Ta3 -119.9(4) . . . . ? N5 Ta3 C51 C50 112.2(3) . . . . ? O3 Ta3 C51 C50 -13.9(3) . . . . ? N7 Ta3 C51 C50 -79.1(3) . . . . ? Cl3 Ta3 C51 C50 -154.4(2) . . . . ? C49 Ta3 C51 C50 37.6(2) . . . . ? C47 Ta3 C51 C50 116.4(4) . . . . ? C48 Ta3 C51 C50 78.8(3) . . . . ? C67 Ta3 C51 C50 -45.2(3) . . . . ? N5 Ta3 C51 C47 -4.2(3) . . . . ? O3 Ta3 C51 C47 -130.4(2) . . . . ? N7 Ta3 C51 C47 164.5(2) . . . . ? Cl3 Ta3 C51 C47 89.1(2) . . . . ? C49 Ta3 C51 C47 -78.8(3) . . . . ? C48 Ta3 C51 C47 -37.6(2) . . . . ? C50 Ta3 C51 C47 -116.4(4) . . . . ? C67 Ta3 C51 C47 -161.6(2) . . . . ? N5 Ta3 C51 C56 -125.0(3) . . . . ? O3 Ta3 C51 C56 108.9(3) . . . . ? N7 Ta3 C51 C56 43.7(4) . . . . ? Cl3 Ta3 C51 C56 -31.6(3) . . . . ? C49 Ta3 C51 C56 160.5(4) . . . . ? C47 Ta3 C51 C56 -120.8(4) . . . . ? C48 Ta3 C51 C56 -158.4(4) . . . . ? C50 Ta3 C51 C56 122.8(5) . . . . ? C67 Ta3 C51 C56 77.6(4) . . . . ? C73 C72 N7 C67 -100.0(5) . . . . ? C77 C72 N7 C67 85.7(5) . . . . ? C73 C72 N7 Ta3 93.7(4) . . . . ? C77 C72 N7 Ta3 -80.6(5) . . . . ? N5 Ta3 N7 C67 -86.5(2) . . . . ? O3 Ta3 N7 C67 2.41(19) . . . . ? Cl3 Ta3 N7 C67 177.1(2) . . . . ? C49 Ta3 N7 C67 34.5(3) . . . . ? C47 Ta3 N7 C67 118.5(3) . . . . ? C48 Ta3 N7 C67 34.5(5) . . . . ? C50 Ta3 N7 C67 66.8(2) . . . . ? C51 Ta3 N7 C67 101.1(2) . . . . ? N5 Ta3 N7 C72 83.0(4) . . . . ? O3 Ta3 N7 C72 171.9(4) . . . . ? Cl3 Ta3 N7 C72 -13.4(3) . . . . ? C49 Ta3 N7 C72 -156.0(3) . . . . ? C47 Ta3 N7 C72 -72.0(4) . . . . ? C48 Ta3 N7 C72 -156.0(4) . . . . ? C50 Ta3 N7 C72 -123.7(3) . . . . ? C51 Ta3 N7 C72 -89.4(4) . . . . ? C67 Ta3 N7 C72 169.5(5) . . . . ? C43 C44 C39 C40 7.1(6) . . . . ? C45 C44 C39 C40 -170.9(4) . . . . ? C43 C44 C39 N4 179.4(4) . . . . ? C45 C44 C39 N4 1.5(6) . . . . ? C34 N4 C39 C44 97.0(5) . . . . ? Ta2 N4 C39 C44 -92.2(4) . . . . ? C34 N4 C39 C40 -90.4(5) . . . . ? Ta2 N4 C39 C40 80.4(5) . . . . ? Ta4 O4 C80 N8 -2.5(3) . . . . ? Ta4 O4 C80 C81 176.9(3) . . . . ? C85 N8 C80 O4 178.2(4) . . . . ? Ta4 N8 C80 O4 2.4(3) . . . . ? C85 N8 C80 C81 -1.1(7) . . . . ? Ta4 N8 C80 C81 -176.9(4) . . . . ? C85 N8 C80 Ta4 175.8(4) . . . . ? N6 Ta4 C80 O4 82.4(2) . . . . ? N8 Ta4 C80 O4 -177.2(4) . . . . ? C57 Ta4 C80 O4 -23.6(2) . . . . ? Cl4 Ta4 C80 O4 -176.03(19) . . . . ? C58 Ta4 C80 O4 -15.0(3) . . . . ? C61 Ta4 C80 O4 -57.1(2) . . . . ? C59 Ta4 C80 O4 -69.7(3) . . . . ? C60 Ta4 C80 O4 -82.0(2) . . . . ? N6 Ta4 C80 N8 -100.4(2) . . . . ? O4 Ta4 C80 N8 177.2(4) . . . . ? C57 Ta4 C80 N8 153.6(2) . . . . ? Cl4 Ta4 C80 N8 1.2(2) . . . . ? C58 Ta4 C80 N8 162.2(2) . . . . ? C61 Ta4 C80 N8 120.1(2) . . . . ? C59 Ta4 C80 N8 107.5(3) . . . . ? C60 Ta4 C80 N8 95.2(2) . . . . ? N6 Ta4 C80 C81 64(2) . . . . ? O4 Ta4 C80 C81 -18.6(18) . . . . ? N8 Ta4 C80 C81 164(2) . . . . ? C57 Ta4 C80 C81 -42(2) . . . . ? Cl4 Ta4 C80 C81 165.3(19) . . . . ? C58 Ta4 C80 C81 -34(2) . . . . ? C61 Ta4 C80 C81 -75.7(19) . . . . ? C59 Ta4 C80 C81 -88.4(19) . . . . ? C60 Ta4 C80 C81 -100.7(19) . . . . ? N6 Ta4 C60 C61 -104.9(3) . . . . ? O4 Ta4 C60 C61 19.7(3) . . . . ? N8 Ta4 C60 C61 84.0(3) . . . . ? C57 Ta4 C60 C61 -38.3(3) . . . . ? Cl4 Ta4 C60 C61 161.1(3) . . . . ? C58 Ta4 C60 C61 -79.8(3) . . . . ? C59 Ta4 C60 C61 -117.6(4) . . . . ? C80 Ta4 C60 C61 50.8(3) . . . . ? N6 Ta4 C60 C59 12.7(3) . . . . ? O4 Ta4 C60 C59 137.3(2) . . . . ? N8 Ta4 C60 C59 -158.4(2) . . . . ? C57 Ta4 C60 C59 79.3(3) . . . . ? Cl4 Ta4 C60 C59 -81.3(2) . . . . ? C58 Ta4 C60 C59 37.8(2) . . . . ? C61 Ta4 C60 C59 117.6(4) . . . . ? C80 Ta4 C60 C59 168.4(2) . . . . ? N6 Ta4 C60 C65 131.2(4) . . . . ? O4 Ta4 C60 C65 -104.1(4) . . . . ? N8 Ta4 C60 C65 -39.9(4) . . . . ? C57 Ta4 C60 C65 -162.2(4) . . . . ? Cl4 Ta4 C60 C65 37.3(4) . . . . ? C58 Ta4 C60 C65 156.3(4) . . . . ? C61 Ta4 C60 C65 -123.8(5) . . . . ? C59 Ta4 C60 C65 118.6(5) . . . . ? C80 Ta4 C60 C65 -73.0(4) . . . . ? C1 C2 C3 C4 2.3(5) . . . . ? C7 C2 C3 C4 -176.1(4) . . . . ? Ta1 C2 C3 C4 67.8(3) . . . . ? C1 C2 C3 C8 176.4(4) . . . . ? C7 C2 C3 C8 -2.0(7) . . . . ? Ta1 C2 C3 C8 -118.0(4) . . . . ? C1 C2 C3 Ta1 -65.6(3) . . . . ? C7 C2 C3 Ta1 116.1(4) . . . . ? N1 Ta1 C3 C2 -61.3(2) . . . . ? O1 Ta1 C3 C2 -154.4(2) . . . . ? N3 Ta1 C3 C2 176.3(2) . . . . ? Cl1 Ta1 C3 C2 55.3(3) . . . . ? C1 Ta1 C3 C2 36.7(2) . . . . ? C4 Ta1 C3 C2 113.8(3) . . . . ? C5 Ta1 C3 C2 77.3(2) . . . . ? C21 Ta1 C3 C2 -167.0(2) . . . . ? N1 Ta1 C3 C4 -175.1(2) . . . . ? O1 Ta1 C3 C4 91.8(3) . . . . ? N3 Ta1 C3 C4 62.5(3) . . . . ? Cl1 Ta1 C3 C4 -58.5(3) . . . . ? C2 Ta1 C3 C4 -113.8(3) . . . . ? C1 Ta1 C3 C4 -77.1(3) . . . . ? C5 Ta1 C3 C4 -36.5(2) . . . . ? C21 Ta1 C3 C4 79.2(3) . . . . ? N1 Ta1 C3 C8 61.3(4) . . . . ? O1 Ta1 C3 C8 -31.8(3) . . . . ? N3 Ta1 C3 C8 -61.0(4) . . . . ? Cl1 Ta1 C3 C8 178.0(3) . . . . ? C2 Ta1 C3 C8 122.6(5) . . . . ? C1 Ta1 C3 C8 159.3(4) . . . . ? C4 Ta1 C3 C8 -123.6(5) . . . . ? C5 Ta1 C3 C8 -160.1(4) . . . . ? C21 Ta1 C3 C8 -44.4(4) . . . . ? C94 C93 C98 C97 -0.2(6) . . . . ? C99 C93 C98 C97 179.8(4) . . . . ? O2 C34 C35 C36 -6.7(5) . . . . ? N4 C34 C35 C36 176.2(3) . . . . ? Ta2 C34 C35 C36 -23.9(19) . . . . ? O2 C34 C35 C38 -127.9(4) . . . . ? N4 C34 C35 C38 55.1(5) . . . . ? Ta2 C34 C35 C38 -145.1(17) . . . . ? O2 C34 C35 C37 112.4(4) . . . . ? N4 C34 C35 C37 -64.7(5) . . . . ? Ta2 C34 C35 C37 95.2(18) . . . . ? C42 C41 C40 C39 2.6(6) . . . . ? C42 C41 C40 C46 -176.0(4) . . . . ? C44 C39 C40 C41 -6.6(6) . . . . ? N4 C39 C40 C41 -179.1(3) . . . . ? C44 C39 C40 C46 172.1(4) . . . . ? N4 C39 C40 C46 -0.5(6) . . . . ? C47 C51 C50 C49 -1.6(4) . . . . ? C56 C51 C50 C49 175.4(3) . . . . ? Ta3 C51 C50 C49 -64.2(2) . . . . ? C47 C51 C50 C55 -179.8(3) . . . . ? C56 C51 C50 C55 -2.8(6) . . . . ? Ta3 C51 C50 C55 117.6(3) . . . . ? C47 C51 C50 Ta3 62.7(2) . . . . ? C56 C51 C50 Ta3 -120.4(4) . . . . ? N5 Ta3 C50 C51 -108.4(3) . . . . ? O3 Ta3 C50 C51 166.7(3) . . . . ? N7 Ta3 C50 C51 114.7(2) . . . . ? Cl3 Ta3 C50 C51 27.4(3) . . . . ? C49 Ta3 C50 C51 -115.5(3) . . . . ? C47 Ta3 C50 C51 -37.1(2) . . . . ? C48 Ta3 C50 C51 -77.9(3) . . . . ? C67 Ta3 C50 C51 141.7(2) . . . . ? N5 Ta3 C50 C49 7.1(3) . . . . ? O3 Ta3 C50 C49 -77.8(2) . . . . ? N7 Ta3 C50 C49 -129.8(2) . . . . ? Cl3 Ta3 C50 C49 143.0(2) . . . . ? C47 Ta3 C50 C49 78.4(3) . . . . ? C48 Ta3 C50 C49 37.6(2) . . . . ? C51 Ta3 C50 C49 115.5(3) . . . . ? C67 Ta3 C50 C49 -102.7(2) . . . . ? N5 Ta3 C50 C55 127.6(3) . . . . ? O3 Ta3 C50 C55 42.7(3) . . . . ? N7 Ta3 C50 C55 -9.3(4) . . . . ? Cl3 Ta3 C50 C55 -96.5(3) . . . . ? C49 Ta3 C50 C55 120.5(4) . . . . ? C47 Ta3 C50 C55 -161.1(4) . . . . ? C48 Ta3 C50 C55 158.1(4) . . . . ? C51 Ta3 C50 C55 -124.0(5) . . . . ? C67 Ta3 C50 C55 17.8(3) . . . . ? C51 C47 C48 C49 -3.6(4) . . . . ? C52 C47 C48 C49 -177.2(3) . . . . ? Ta3 C47 C48 C49 63.9(2) . . . . ? C51 C47 C48 C53 175.6(3) . . . . ? C52 C47 C48 C53 2.0(6) . . . . ? Ta3 C47 C48 C53 -117.0(4) . . . . ? C51 C47 C48 Ta3 -67.5(2) . . . . ? C52 C47 C48 Ta3 118.9(3) . . . . ? N5 Ta3 C48 C47 -120.7(3) . . . . ? O3 Ta3 C48 C47 144.2(2) . . . . ? N7 Ta3 C48 C47 116.2(4) . . . . ? Cl3 Ta3 C48 C47 -22.6(3) . . . . ? C49 Ta3 C48 C47 116.2(3) . . . . ? C50 Ta3 C48 C47 78.4(2) . . . . ? C51 Ta3 C48 C47 38.1(2) . . . . ? C67 Ta3 C48 C47 138.6(2) . . . . ? N5 Ta3 C48 C49 123.1(2) . . . . ? O3 Ta3 C48 C49 28.0(2) . . . . ? N7 Ta3 C48 C49 0.0(5) . . . . ? Cl3 Ta3 C48 C49 -138.8(2) . . . . ? C47 Ta3 C48 C49 -116.2(3) . . . . ? C50 Ta3 C48 C49 -37.8(2) . . . . ? C51 Ta3 C48 C49 -78.1(3) . . . . ? C67 Ta3 C48 C49 22.4(3) . . . . ? N5 Ta3 C48 C53 1.3(4) . . . . ? O3 Ta3 C48 C53 -93.9(4) . . . . ? N7 Ta3 C48 C53 -121.8(4) . . . . ? Cl3 Ta3 C48 C53 99.4(3) . . . . ? C49 Ta3 C48 C53 -121.8(5) . . . . ? C47 Ta3 C48 C53 122.0(5) . . . . ? C50 Ta3 C48 C53 -159.7(4) . . . . ? C51 Ta3 C48 C53 160.0(4) . . . . ? C67 Ta3 C48 C53 -99.4(4) . . . . ? C13 C12 C11 C15 3.6(4) . . . . ? C17 C12 C11 C15 177.2(3) . . . . ? Ta2 C12 C11 C15 -63.7(3) . . . . ? C13 C12 C11 C16 -175.0(3) . . . . ? C17 C12 C11 C16 -1.4(6) . . . . ? Ta2 C12 C11 C16 117.7(4) . . . . ? C13 C12 C11 Ta2 67.3(2) . . . . ? C17 C12 C11 Ta2 -119.1(4) . . . . ? N2 Ta2 C11 C12 120.4(3) . . . . ? O2 Ta2 C11 C12 -143.1(2) . . . . ? N4 Ta2 C11 C12 -110.5(4) . . . . ? Cl2 Ta2 C11 C12 22.7(3) . . . . ? C15 Ta2 C11 C12 -116.9(3) . . . . ? C14 Ta2 C11 C12 -78.5(3) . . . . ? C13 Ta2 C11 C12 -38.6(2) . . . . ? C34 Ta2 C11 C12 -134.8(2) . . . . ? N2 Ta2 C11 C15 -122.7(2) . . . . ? O2 Ta2 C11 C15 -26.3(2) . . . . ? N4 Ta2 C11 C15 6.3(5) . . . . ? Cl2 Ta2 C11 C15 139.5(2) . . . . ? C12 Ta2 C11 C15 116.9(3) . . . . ? C14 Ta2 C11 C15 38.3(2) . . . . ? C13 Ta2 C11 C15 78.2(2) . . . . ? C34 Ta2 C11 C15 -17.9(3) . . . . ? N2 Ta2 C11 C16 -2.4(4) . . . . ? O2 Ta2 C11 C16 94.0(4) . . . . ? N4 Ta2 C11 C16 126.6(4) . . . . ? Cl2 Ta2 C11 C16 -100.2(4) . . . . ? C15 Ta2 C11 C16 120.3(5) . . . . ? C12 Ta2 C11 C16 -122.9(5) . . . . ? C14 Ta2 C11 C16 158.6(4) . . . . ? C13 Ta2 C11 C16 -161.5(4) . . . . ? C34 Ta2 C11 C16 102.4(4) . . . . ? C59 C60 C61 C57 1.4(5) . . . . ? C65 C60 C61 C57 -178.2(4) . . . . ? Ta4 C60 C61 C57 63.9(3) . . . . ? C59 C60 C61 C66 177.5(4) . . . . ? C65 C60 C61 C66 -2.2(7) . . . . ? Ta4 C60 C61 C66 -120.0(5) . . . . ? C59 C60 C61 Ta4 -62.5(3) . . . . ? C65 C60 C61 Ta4 117.9(4) . . . . ? C58 C57 C61 C60 0.7(5) . . . . ? C62 C57 C61 C60 175.6(4) . . . . ? Ta4 C57 C61 C60 -67.0(3) . . . . ? C58 C57 C61 C66 -175.5(4) . . . . ? C62 C57 C61 C66 -0.5(7) . . . . ? Ta4 C57 C61 C66 116.8(4) . . . . ? C58 C57 C61 Ta4 67.7(3) . . . . ? C62 C57 C61 Ta4 -117.4(4) . . . . ? N6 Ta4 C61 C60 114.1(3) . . . . ? O4 Ta4 C61 C60 -161.0(3) . . . . ? N8 Ta4 C61 C60 -109.2(3) . . . . ? C57 Ta4 C61 C60 114.9(4) . . . . ? Cl4 Ta4 C61 C60 -20.8(3) . . . . ? C58 Ta4 C61 C60 77.1(3) . . . . ? C59 Ta4 C61 C60 36.1(2) . . . . ? C80 Ta4 C61 C60 -136.0(3) . . . . ? N6 Ta4 C61 C57 -0.9(3) . . . . ? O4 Ta4 C61 C57 84.0(2) . . . . ? N8 Ta4 C61 C57 135.8(2) . . . . ? Cl4 Ta4 C61 C57 -135.8(2) . . . . ? C58 Ta4 C61 C57 -37.8(2) . . . . ? C59 Ta4 C61 C57 -78.9(3) . . . . ? C60 Ta4 C61 C57 -114.9(4) . . . . ? C80 Ta4 C61 C57 109.0(2) . . . . ? N6 Ta4 C61 C66 -121.0(3) . . . . ? O4 Ta4 C61 C66 -36.1(3) . . . . ? N8 Ta4 C61 C66 15.7(4) . . . . ? C57 Ta4 C61 C66 -120.1(4) . . . . ? Cl4 Ta4 C61 C66 104.1(3) . . . . ? C58 Ta4 C61 C66 -157.9(4) . . . . ? C59 Ta4 C61 C66 161.0(4) . . . . ? C60 Ta4 C61 C66 125.0(5) . . . . ? C80 Ta4 C61 C66 -11.1(3) . . . . ? C47 C48 C49 C50 2.6(4) . . . . ? C53 C48 C49 C50 -176.5(3) . . . . ? Ta3 C48 C49 C50 67.2(2) . . . . ? C47 C48 C49 C54 175.9(3) . . . . ? C53 C48 C49 C54 -3.2(6) . . . . ? Ta3 C48 C49 C54 -119.5(3) . . . . ? C47 C48 C49 Ta3 -64.6(2) . . . . ? C53 C48 C49 Ta3 116.3(4) . . . . ? C51 C50 C49 C48 -0.6(4) . . . . ? C55 C50 C49 C48 177.6(3) . . . . ? Ta3 C50 C49 C48 -67.1(2) . . . . ? C51 C50 C49 C54 -173.9(3) . . . . ? C55 C50 C49 C54 4.3(6) . . . . ? Ta3 C50 C49 C54 119.7(4) . . . . ? C51 C50 C49 Ta3 66.4(2) . . . . ? C55 C50 C49 Ta3 -115.3(3) . . . . ? N5 Ta3 C49 C48 -60.6(3) . . . . ? O3 Ta3 C49 C48 -151.6(3) . . . . ? N7 Ta3 C49 C48 -180.0(2) . . . . ? Cl3 Ta3 C49 C48 60.5(3) . . . . ? C47 Ta3 C49 C48 36.7(2) . . . . ? C50 Ta3 C49 C48 114.7(3) . . . . ? C51 Ta3 C49 C48 78.0(2) . . . . ? C67 Ta3 C49 C48 -163.4(2) . . . . ? N5 Ta3 C49 C50 -175.3(2) . . . . ? O3 Ta3 C49 C50 93.7(2) . . . . ? N7 Ta3 C49 C50 65.4(3) . . . . ? Cl3 Ta3 C49 C50 -54.1(3) . . . . ? C47 Ta3 C49 C50 -77.9(2) . . . . ? C48 Ta3 C49 C50 -114.7(3) . . . . ? C51 Ta3 C49 C50 -36.6(2) . . . . ? C67 Ta3 C49 C50 81.9(2) . . . . ? N5 Ta3 C49 C54 61.8(4) . . . . ? O3 Ta3 C49 C54 -29.2(3) . . . . ? N7 Ta3 C49 C54 -57.6(4) . . . . ? Cl3 Ta3 C49 C54 -177.1(3) . . . . ? C47 Ta3 C49 C54 159.1(4) . . . . ? C48 Ta3 C49 C54 122.4(5) . . . . ? C50 Ta3 C49 C54 -122.9(5) . . . . ? C51 Ta3 C49 C54 -159.6(4) . . . . ? C67 Ta3 C49 C54 -41.0(4) . . . . ? C89 C90 C85 C86 0.8(6) . . . . ? C92 C90 C85 C86 -177.8(4) . . . . ? C89 C90 C85 N8 173.7(4) . . . . ? C92 C90 C85 N8 -4.9(6) . . . . ? C80 N8 C85 C86 -95.2(5) . . . . ? Ta4 N8 C85 C86 78.8(5) . . . . ? C80 N8 C85 C90 91.8(5) . . . . ? Ta4 N8 C85 C90 -94.2(4) . . . . ? C72 N7 C67 O3 -174.2(3) . . . . ? Ta3 N7 C67 O3 -3.6(3) . . . . ? C72 N7 C67 C68 6.2(7) . . . . ? Ta3 N7 C67 C68 176.8(4) . . . . ? C72 N7 C67 Ta3 -170.6(4) . . . . ? Ta3 O3 C67 N7 3.8(3) . . . . ? Ta3 O3 C67 C68 -176.5(3) . . . . ? N5 Ta3 C67 N7 99.3(2) . . . . ? O3 Ta3 C67 N7 -175.8(3) . . . . ? Cl3 Ta3 C67 N7 -3.0(2) . . . . ? C49 Ta3 C67 N7 -152.3(2) . . . . ? C47 Ta3 C67 N7 -116.6(3) . . . . ? C48 Ta3 C67 N7 -164.8(2) . . . . ? C50 Ta3 C67 N7 -118.5(2) . . . . ? C51 Ta3 C67 N7 -95.6(2) . . . . ? N5 Ta3 C67 O3 -84.9(2) . . . . ? N7 Ta3 C67 O3 175.8(3) . . . . ? Cl3 Ta3 C67 O3 172.77(18) . . . . ? C49 Ta3 C67 O3 23.5(2) . . . . ? C47 Ta3 C67 O3 59.2(4) . . . . ? C48 Ta3 C67 O3 11.0(3) . . . . ? C50 Ta3 C67 O3 57.3(2) . . . . ? C51 Ta3 C67 O3 80.2(2) . . . . ? N5 Ta3 C67 C68 -68.3(13) . . . . ? O3 Ta3 C67 C68 16.6(12) . . . . ? N7 Ta3 C67 C68 -167.6(15) . . . . ? Cl3 Ta3 C67 C68 -170.6(13) . . . . ? C49 Ta3 C67 C68 40.1(14) . . . . ? C47 Ta3 C67 C68 75.8(14) . . . . ? C48 Ta3 C67 C68 27.6(14) . . . . ? C50 Ta3 C67 C68 73.9(13) . . . . ? C51 Ta3 C67 C68 96.8(13) . . . . ? C27 C26 C31 C30 -0.9(6) . . . . ? N3 C26 C31 C30 -173.3(4) . . . . ? C27 C26 C31 C33 177.9(4) . . . . ? N3 C26 C31 C33 5.5(6) . . . . ? N2 Ta2 C14 C13 107.6(3) . . . . ? O2 Ta2 C14 C13 -164.8(3) . . . . ? N4 Ta2 C14 C13 -112.7(2) . . . . ? Cl2 Ta2 C14 C13 -26.5(3) . . . . ? C15 Ta2 C14 C13 116.0(4) . . . . ? C12 Ta2 C14 C13 37.5(2) . . . . ? C11 Ta2 C14 C13 78.1(3) . . . . ? C34 Ta2 C14 C13 -139.3(2) . . . . ? N2 Ta2 C14 C15 -8.4(4) . . . . ? O2 Ta2 C14 C15 79.1(2) . . . . ? N4 Ta2 C14 C15 131.3(2) . . . . ? Cl2 Ta2 C14 C15 -142.5(2) . . . . ? C12 Ta2 C14 C15 -78.5(3) . . . . ? C11 Ta2 C14 C15 -38.0(2) . . . . ? C13 Ta2 C14 C15 -116.0(4) . . . . ? C34 Ta2 C14 C15 104.7(2) . . . . ? N2 Ta2 C14 C19 -127.7(3) . . . . ? O2 Ta2 C14 C19 -40.1(3) . . . . ? N4 Ta2 C14 C19 12.0(4) . . . . ? Cl2 Ta2 C14 C19 98.2(3) . . . . ? C15 Ta2 C14 C19 -119.3(5) . . . . ? C12 Ta2 C14 C19 162.2(4) . . . . ? C11 Ta2 C14 C19 -157.2(4) . . . . ? C13 Ta2 C14 C19 124.7(5) . . . . ? C34 Ta2 C14 C19 -14.6(3) . . . . ? C40 C41 C42 C43 0.7(6) . . . . ? C44 C43 C42 C41 -0.2(6) . . . . ? C88 C87 C86 C85 1.0(7) . . . . ? C88 C87 C86 C91 -178.3(4) . . . . ? C90 C85 C86 C87 -0.8(6) . . . . ? N8 C85 C86 C87 -173.7(4) . . . . ? C90 C85 C86 C91 178.5(4) . . . . ? N8 C85 C86 C91 5.6(6) . . . . ? C12 C11 C15 C14 -3.2(4) . . . . ? C16 C11 C15 C14 175.5(3) . . . . ? Ta2 C11 C15 C14 -67.7(2) . . . . ? C12 C11 C15 C20 -176.8(3) . . . . ? C16 C11 C15 C20 1.9(6) . . . . ? Ta2 C11 C15 C20 118.7(3) . . . . ? C12 C11 C15 Ta2 64.5(3) . . . . ? C16 C11 C15 Ta2 -116.8(4) . . . . ? C13 C14 C15 C11 1.4(4) . . . . ? C19 C14 C15 C11 -176.6(3) . . . . ? Ta2 C14 C15 C11 67.4(2) . . . . ? C13 C14 C15 C20 175.1(3) . . . . ? C19 C14 C15 C20 -2.9(6) . . . . ? Ta2 C14 C15 C20 -118.9(4) . . . . ? C13 C14 C15 Ta2 -66.0(2) . . . . ? C19 C14 C15 Ta2 115.9(3) . . . . ? N2 Ta2 C15 C11 60.5(3) . . . . ? O2 Ta2 C15 C11 153.7(2) . . . . ? N4 Ta2 C15 C11 -177.4(2) . . . . ? Cl2 Ta2 C15 C11 -59.2(3) . . . . ? C12 Ta2 C15 C11 -36.1(2) . . . . ? C14 Ta2 C15 C11 -113.8(3) . . . . ? C13 Ta2 C15 C11 -77.8(3) . . . . ? C34 Ta2 C15 C11 166.8(2) . . . . ? N2 Ta2 C15 C14 174.3(2) . . . . ? O2 Ta2 C15 C14 -92.5(2) . . . . ? N4 Ta2 C15 C14 -63.6(3) . . . . ? Cl2 Ta2 C15 C14 54.6(3) . . . . ? C12 Ta2 C15 C14 77.7(3) . . . . ? C11 Ta2 C15 C14 113.8(3) . . . . ? C13 Ta2 C15 C14 36.0(2) . . . . ? C34 Ta2 C15 C14 -79.4(2) . . . . ? N2 Ta2 C15 C20 -63.1(4) . . . . ? O2 Ta2 C15 C20 30.2(3) . . . . ? N4 Ta2 C15 C20 59.1(4) . . . . ? Cl2 Ta2 C15 C20 177.3(3) . . . . ? C12 Ta2 C15 C20 -159.7(4) . . . . ? C11 Ta2 C15 C20 -123.5(5) . . . . ? C14 Ta2 C15 C20 122.7(5) . . . . ? C13 Ta2 C15 C20 158.7(4) . . . . ? C34 Ta2 C15 C20 43.3(4) . . . . ? C72 C77 C76 C75 -1.6(6) . . . . ? C79 C77 C76 C75 177.9(4) . . . . ? C15 C14 C13 C12 0.8(4) . . . . ? C19 C14 C13 C12 178.8(3) . . . . ? Ta2 C14 C13 C12 -63.0(2) . . . . ? C15 C14 C13 C18 -175.3(3) . . . . ? C19 C14 C13 C18 2.7(6) . . . . ? Ta2 C14 C13 C18 120.9(4) . . . . ? C15 C14 C13 Ta2 63.8(2) . . . . ? C19 C14 C13 Ta2 -118.2(4) . . . . ? C11 C12 C13 C14 -2.8(4) . . . . ? C17 C12 C13 C14 -176.5(3) . . . . ? Ta2 C12 C13 C14 63.8(2) . . . . ? C11 C12 C13 C18 173.5(3) . . . . ? C17 C12 C13 C18 -0.3(6) . . . . ? Ta2 C12 C13 C18 -119.9(3) . . . . ? C11 C12 C13 Ta2 -66.6(2) . . . . ? C17 C12 C13 Ta2 119.7(4) . . . . ? N2 Ta2 C13 C14 -110.9(3) . . . . ? O2 Ta2 C13 C14 15.9(3) . . . . ? N4 Ta2 C13 C14 80.3(3) . . . . ? Cl2 Ta2 C13 C14 155.3(2) . . . . ? C15 Ta2 C13 C14 -37.6(2) . . . . ? C12 Ta2 C13 C14 -116.3(4) . . . . ? C11 Ta2 C13 C14 -78.8(3) . . . . ? C34 Ta2 C13 C14 46.9(3) . . . . ? N2 Ta2 C13 C12 5.4(4) . . . . ? O2 Ta2 C13 C12 132.2(2) . . . . ? N4 Ta2 C13 C12 -163.4(2) . . . . ? Cl2 Ta2 C13 C12 -88.4(2) . . . . ? C15 Ta2 C13 C12 78.7(3) . . . . ? C11 Ta2 C13 C12 37.5(2) . . . . ? C14 Ta2 C13 C12 116.3(4) . . . . ? C34 Ta2 C13 C12 163.2(2) . . . . ? N2 Ta2 C13 C18 124.9(3) . . . . ? O2 Ta2 C13 C18 -108.2(3) . . . . ? N4 Ta2 C13 C18 -43.8(4) . . . . ? Cl2 Ta2 C13 C18 31.2(3) . . . . ? C15 Ta2 C13 C18 -161.7(4) . . . . ? C12 Ta2 C13 C18 119.6(5) . . . . ? C11 Ta2 C13 C18 157.1(4) . . . . ? C14 Ta2 C13 C18 -124.1(5) . . . . ? C34 Ta2 C13 C18 -77.2(4) . . . . ? N7 C67 C68 C71 -125.5(4) . . . . ? O3 C67 C68 C71 54.9(4) . . . . ? Ta3 C67 C68 C71 40.1(15) . . . . ? N7 C67 C68 C70 -4.0(6) . . . . ? O3 C67 C68 C70 176.4(3) . . . . ? Ta3 C67 C68 C70 161.6(12) . . . . ? N7 C67 C68 C69 117.1(5) . . . . ? O3 C67 C68 C69 -62.5(5) . . . . ? Ta3 C67 C68 C69 -77.4(14) . . . . ? C77 C72 C73 C74 -4.5(6) . . . . ? N7 C72 C73 C74 -178.8(4) . . . . ? C77 C72 C73 C78 173.6(4) . . . . ? N7 C72 C73 C78 -0.7(6) . . . . ? C75 C74 C73 C72 1.9(6) . . . . ? C75 C74 C73 C78 -176.2(4) . . . . ? C93 C98 C97 C96 0.3(7) . . . . ? C73 C74 C75 C76 0.8(7) . . . . ? C77 C76 C75 C74 -0.9(6) . . . . ? C111 C112 C107 C108 0.7(7) . . . . ? C111 C112 C107 C113 -177.9(4) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C8 C3 C4 C5 -174.7(4) . . . . ? Ta1 C3 C4 C5 66.7(3) . . . . ? C2 C3 C4 C9 175.5(4) . . . . ? C8 C3 C4 C9 1.4(7) . . . . ? Ta1 C3 C4 C9 -117.2(4) . . . . ? C2 C3 C4 Ta1 -67.3(3) . . . . ? C8 C3 C4 Ta1 118.6(4) . . . . ? N1 Ta1 C4 C5 -107.8(3) . . . . ? O1 Ta1 C4 C5 164.2(3) . . . . ? N3 Ta1 C4 C5 112.1(2) . . . . ? C3 Ta1 C4 C5 -115.0(4) . . . . ? Cl1 Ta1 C4 C5 24.7(3) . . . . ? C2 Ta1 C4 C5 -76.9(3) . . . . ? C1 Ta1 C4 C5 -36.4(2) . . . . ? C21 Ta1 C4 C5 138.9(3) . . . . ? N1 Ta1 C4 C3 7.3(4) . . . . ? O1 Ta1 C4 C3 -80.8(3) . . . . ? N3 Ta1 C4 C3 -132.9(2) . . . . ? Cl1 Ta1 C4 C3 139.7(2) . . . . ? C2 Ta1 C4 C3 38.1(2) . . . . ? C1 Ta1 C4 C3 78.6(3) . . . . ? C5 Ta1 C4 C3 115.0(4) . . . . ? C21 Ta1 C4 C3 -106.1(3) . . . . ? N1 Ta1 C4 C9 127.5(3) . . . . ? O1 Ta1 C4 C9 39.5(3) . . . . ? N3 Ta1 C4 C9 -12.6(3) . . . . ? C3 Ta1 C4 C9 120.3(4) . . . . ? Cl1 Ta1 C4 C9 -100.0(3) . . . . ? C2 Ta1 C4 C9 158.4(4) . . . . ? C1 Ta1 C4 C9 -161.1(4) . . . . ? C5 Ta1 C4 C9 -124.7(4) . . . . ? C21 Ta1 C4 C9 14.2(3) . . . . ? C108 C109 C110 C111 -0.4(7) . . . . ? C3 C4 C5 C1 -1.3(5) . . . . ? C9 C4 C5 C1 -177.3(4) . . . . ? Ta1 C4 C5 C1 62.6(3) . . . . ? C3 C4 C5 C10 177.1(4) . . . . ? C9 C4 C5 C10 1.0(7) . . . . ? Ta1 C4 C5 C10 -119.1(4) . . . . ? C3 C4 C5 Ta1 -63.9(3) . . . . ? C9 C4 C5 Ta1 120.1(4) . . . . ? N1 Ta1 C5 C4 111.6(3) . . . . ? O1 Ta1 C5 C4 -16.7(3) . . . . ? N3 Ta1 C5 C4 -81.3(3) . . . . ? C3 Ta1 C5 C4 38.3(3) . . . . ? Cl1 Ta1 C5 C4 -157.0(3) . . . . ? C2 Ta1 C5 C4 80.1(3) . . . . ? C1 Ta1 C5 C4 117.1(4) . . . . ? C21 Ta1 C5 C4 -48.2(3) . . . . ? N1 Ta1 C5 C1 -5.5(3) . . . . ? O1 Ta1 C5 C1 -133.8(2) . . . . ? N3 Ta1 C5 C1 161.6(2) . . . . ? C3 Ta1 C5 C1 -78.8(3) . . . . ? Cl1 Ta1 C5 C1 85.9(2) . . . . ? C2 Ta1 C5 C1 -37.0(2) . . . . ? C4 Ta1 C5 C1 -117.1(4) . . . . ? C21 Ta1 C5 C1 -165.3(2) . . . . ? N1 Ta1 C5 C10 -124.8(4) . . . . ? O1 Ta1 C5 C10 107.0(4) . . . . ? N3 Ta1 C5 C10 42.3(4) . . . . ? C3 Ta1 C5 C10 162.0(4) . . . . ? Cl1 Ta1 C5 C10 -33.4(4) . . . . ? C2 Ta1 C5 C10 -156.3(4) . . . . ? C1 Ta1 C5 C10 -119.2(5) . . . . ? C4 Ta1 C5 C10 123.7(5) . . . . ? C21 Ta1 C5 C10 75.5(4) . . . . ? C104 C105 C100 C101 -0.4(7) . . . . ? C104 C105 C100 C106 -179.0(4) . . . . ? C109 C110 C111 C112 0.4(7) . . . . ? C107 C112 C111 C110 -0.6(7) . . . . ? C29 C28 C27 C26 -1.9(6) . . . . ? C29 C28 C27 C32 178.3(4) . . . . ? C31 C26 C27 C28 1.6(6) . . . . ? N3 C26 C27 C28 173.9(3) . . . . ? C31 C26 C27 C32 -178.6(4) . . . . ? N3 C26 C27 C32 -6.2(6) . . . . ? C96 C95 C94 C93 0.0(7) . . . . ? C98 C93 C94 C95 0.1(6) . . . . ? C99 C93 C94 C95 -179.9(4) . . . . ? C100 C105 C104 C103 0.8(7) . . . . ? C26 N3 C21 O1 -177.5(3) . . . . ? Ta1 N3 C21 O1 -1.6(3) . . . . ? C26 N3 C21 C22 2.9(7) . . . . ? Ta1 N3 C21 C22 178.8(4) . . . . ? C26 N3 C21 Ta1 -175.9(4) . . . . ? Ta1 O1 C21 N3 1.6(3) . . . . ? Ta1 O1 C21 C22 -178.7(3) . . . . ? N1 Ta1 C21 N3 98.8(2) . . . . ? O1 Ta1 C21 N3 -178.2(4) . . . . ? C3 Ta1 C21 N3 -152.6(2) . . . . ? Cl1 Ta1 C21 N3 -2.8(2) . . . . ? C2 Ta1 C21 N3 -163.1(2) . . . . ? C1 Ta1 C21 N3 -111.0(3) . . . . ? C4 Ta1 C21 N3 -118.8(2) . . . . ? C5 Ta1 C21 N3 -94.8(2) . . . . ? N1 Ta1 C21 O1 -83.0(2) . . . . ? N3 Ta1 C21 O1 178.2(4) . . . . ? C3 Ta1 C21 O1 25.6(2) . . . . ? Cl1 Ta1 C21 O1 175.43(19) . . . . ? C2 Ta1 C21 O1 15.1(3) . . . . ? C1 Ta1 C21 O1 67.1(3) . . . . ? C4 Ta1 C21 O1 59.4(2) . . . . ? C5 Ta1 C21 O1 83.3(2) . . . . ? N1 Ta1 C21 C22 -75.7(19) . . . . ? O1 Ta1 C21 C22 7.4(17) . . . . ? N3 Ta1 C21 C22 -174(2) . . . . ? C3 Ta1 C21 C22 33.0(19) . . . . ? Cl1 Ta1 C21 C22 -177.2(18) . . . . ? C2 Ta1 C21 C22 22.5(19) . . . . ? C1 Ta1 C21 C22 74.5(19) . . . . ? C4 Ta1 C21 C22 66.8(19) . . . . ? C5 Ta1 C21 C22 90.7(18) . . . . ? O4 C80 C81 C84 -178.8(3) . . . . ? N8 C80 C81 C84 0.4(6) . . . . ? Ta4 C80 C81 C84 -161.8(18) . . . . ? O4 C80 C81 C83 60.3(5) . . . . ? N8 C80 C81 C83 -120.4(5) . . . . ? Ta4 C80 C81 C83 77(2) . . . . ? O4 C80 C81 C82 -56.9(5) . . . . ? N8 C80 C81 C82 122.4(5) . . . . ? Ta4 C80 C81 C82 -40(2) . . . . ? C3 C2 C1 C5 -3.1(5) . . . . ? C7 C2 C1 C5 175.3(4) . . . . ? Ta1 C2 C1 C5 -67.3(3) . . . . ? C3 C2 C1 C6 -176.2(4) . . . . ? C7 C2 C1 C6 2.2(7) . . . . ? Ta1 C2 C1 C6 119.6(4) . . . . ? C3 C2 C1 Ta1 64.2(3) . . . . ? C7 C2 C1 Ta1 -117.3(4) . . . . ? C4 C5 C1 C2 2.7(5) . . . . ? C10 C5 C1 C2 -175.7(4) . . . . ? Ta1 C5 C1 C2 65.8(3) . . . . ? C4 C5 C1 C6 175.9(4) . . . . ? C10 C5 C1 C6 -2.5(7) . . . . ? Ta1 C5 C1 C6 -121.0(4) . . . . ? C4 C5 C1 Ta1 -63.1(3) . . . . ? C10 C5 C1 Ta1 118.5(4) . . . . ? N1 Ta1 C1 C2 60.7(3) . . . . ? O1 Ta1 C1 C2 -52.1(3) . . . . ? N3 Ta1 C1 C2 -147.0(3) . . . . ? C3 Ta1 C1 C2 -37.7(2) . . . . ? Cl1 Ta1 C1 C2 155.4(3) . . . . ? C4 Ta1 C1 C2 -79.6(3) . . . . ? C5 Ta1 C1 C2 -115.5(4) . . . . ? C21 Ta1 C1 C2 -89.0(3) . . . . ? N1 Ta1 C1 C5 176.2(2) . . . . ? O1 Ta1 C1 C5 63.3(3) . . . . ? N3 Ta1 C1 C5 -31.5(4) . . . . ? C3 Ta1 C1 C5 77.7(3) . . . . ? Cl1 Ta1 C1 C5 -89.2(2) . . . . ? C2 Ta1 C1 C5 115.5(4) . . . . ? C4 Ta1 C1 C5 35.8(2) . . . . ? C21 Ta1 C1 C5 26.5(4) . . . . ? N1 Ta1 C1 C6 -61.3(4) . . . . ? O1 Ta1 C1 C6 -174.1(3) . . . . ? N3 Ta1 C1 C6 91.0(4) . . . . ? C3 Ta1 C1 C6 -159.7(4) . . . . ? Cl1 Ta1 C1 C6 33.4(3) . . . . ? C2 Ta1 C1 C6 -122.0(5) . . . . ? C4 Ta1 C1 C6 158.4(4) . . . . ? C5 Ta1 C1 C6 122.5(5) . . . . ? C21 Ta1 C1 C6 149.1(3) . . . . ? C105 C100 C101 C102 0.0(6) . . . . ? C106 C100 C101 C102 178.6(4) . . . . ? C103 C102 C101 C100 0.0(7) . . . . ? C61 C60 C59 C58 -3.0(5) . . . . ? C65 C60 C59 C58 176.7(4) . . . . ? Ta4 C60 C59 C58 -65.5(3) . . . . ? C61 C60 C59 C64 -175.0(4) . . . . ? C65 C60 C59 C64 4.7(7) . . . . ? Ta4 C60 C59 C64 122.5(4) . . . . ? C61 C60 C59 Ta4 62.6(3) . . . . ? C65 C60 C59 Ta4 -117.8(4) . . . . ? C57 C58 C59 C60 3.4(5) . . . . ? C63 C58 C59 C60 -175.7(4) . . . . ? Ta4 C58 C59 C60 67.3(3) . . . . ? C57 C58 C59 C64 175.4(4) . . . . ? C63 C58 C59 C64 -3.7(7) . . . . ? Ta4 C58 C59 C64 -120.6(4) . . . . ? C57 C58 C59 Ta4 -64.0(3) . . . . ? C63 C58 C59 Ta4 116.9(4) . . . . ? N6 Ta4 C59 C60 -171.5(2) . . . . ? O4 Ta4 C59 C60 -58.0(3) . . . . ? N8 Ta4 C59 C60 35.4(4) . . . . ? C57 Ta4 C59 C60 -77.5(3) . . . . ? Cl4 Ta4 C59 C60 94.1(2) . . . . ? C58 Ta4 C59 C60 -114.9(4) . . . . ? C61 Ta4 C59 C60 -35.7(2) . . . . ? C80 Ta4 C59 C60 -20.3(4) . . . . ? N6 Ta4 C59 C58 -56.6(3) . . . . ? O4 Ta4 C59 C58 56.8(3) . . . . ? N8 Ta4 C59 C58 150.3(2) . . . . ? C57 Ta4 C59 C58 37.4(2) . . . . ? Cl4 Ta4 C59 C58 -151.0(2) . . . . ? C61 Ta4 C59 C58 79.2(3) . . . . ? C60 Ta4 C59 C58 114.9(4) . . . . ? C80 Ta4 C59 C58 94.6(3) . . . . ? N6 Ta4 C59 C64 64.8(4) . . . . ? O4 Ta4 C59 C64 178.2(3) . . . . ? N8 Ta4 C59 C64 -88.3(4) . . . . ? C57 Ta4 C59 C64 158.8(4) . . . . ? Cl4 Ta4 C59 C64 -29.6(3) . . . . ? C58 Ta4 C59 C64 121.4(5) . . . . ? C61 Ta4 C59 C64 -159.4(4) . . . . ? C60 Ta4 C59 C64 -123.7(5) . . . . ? C80 Ta4 C59 C64 -144.0(3) . . . . ? C26 C31 C30 C29 0.5(6) . . . . ? C33 C31 C30 C29 -178.3(4) . . . . ? C28 C29 C30 C31 -0.8(6) . . . . ? C86 C87 C88 C89 -1.2(7) . . . . ? C87 C88 C89 C90 1.2(7) . . . . ? C85 C90 C89 C88 -1.0(6) . . . . ? C92 C90 C89 C88 177.6(4) . . . . ? C110 C109 C108 C107 0.4(7) . . . . ? C112 C107 C108 C109 -0.6(7) . . . . ? C113 C107 C108 C109 178.0(4) . . . . ? N3 C21 C22 C25 -1.2(6) . . . . ? O1 C21 C22 C25 179.2(3) . . . . ? Ta1 C21 C22 C25 172.5(16) . . . . ? N3 C21 C22 C23 120.5(5) . . . . ? O1 C21 C22 C23 -59.1(5) . . . . ? Ta1 C21 C22 C23 -65.8(19) . . . . ? N3 C21 C22 C24 -123.1(5) . . . . ? O1 C21 C22 C24 57.3(5) . . . . ? Ta1 C21 C22 C24 51(2) . . . . ? C94 C95 C96 C97 0.1(7) . . . . ? C98 C97 C96 C95 -0.2(7) . . . . ? C101 C102 C103 C104 0.3(7) . . . . ? C105 C104 C103 C102 -0.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.164 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.151 #END data_ls195 #TrackingRef '- CpTaMe4_ls195_v2.cif' _database_code_depnum_ccdc_archive 'CCDC 841455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetramethyl(eta5-pentamethylcyclopentadienyl)tantalum ; _chemical_name_common Tetramethyl(eta5-pentamethylcyclopentadienyl)tantalum _chemical_melting_point ? _chemical_formula_moiety 'C14 H27 Ta' _chemical_formula_sum 'C14 H27 Ta' _chemical_formula_weight 376.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' _cell_length_a 13.8058(7) _cell_length_b 15.1978(7) _cell_length_c 14.0101(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2939.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 7898 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 30.013 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 7.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.145 _exptl_absorpt_correction_T_max 0.225 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8384 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.90 _reflns_number_total 1828 _reflns_number_gt 1680 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0142P)^2^+19.6073P] 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 1828 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0472 _refine_ls_wR_factor_gt 0.0455 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C1 C 0.3345(4) 0.3882(4) 0.1672(4) 0.0185(11) Uani 0.50 1 d P A -1 C2 C 0.3328(4) 0.3369(4) 0.2511(4) 0.0206(11) Uani 0.50 1 d P A -1 C3 C 0.3409(4) 0.3935(4) 0.3308(4) 0.0191(11) Uani 0.50 1 d P A -1 C4 C 0.3484(4) 0.4814(4) 0.2962(4) 0.0172(10) Uani 0.50 1 d P A -1 C5 C 0.3445(4) 0.4782(4) 0.1942(4) 0.0163(10) Uani 0.50 1 d P A -1 C6 C 0.3194(6) 0.3555(5) 0.0669(5) 0.0340(16) Uani 0.50 1 d P A -1 H6A H 0.3453 0.2957 0.0611 0.06(3) Uiso 0.50 1 calc PR A -1 H6B H 0.3532 0.3945 0.0221 0.05(3) Uiso 0.50 1 calc PR A -1 H6C H 0.2500 0.3552 0.0522 0.07(5) Uiso 0.50 1 calc PR A -1 C7 C 0.3195(5) 0.2385(4) 0.2553(6) 0.0356(16) Uani 0.50 1 d P A -1 H7A H 0.3439 0.2163 0.3164 0.06(3) Uiso 0.50 1 calc PR A -1 H7B H 0.3555 0.2109 0.2029 0.05(2) Uiso 0.50 1 calc PR A -1 H7C H 0.2505 0.2243 0.2493 0.050(18) Uiso 0.50 2 calc SR A -1 C8 C 0.3371(5) 0.3672(5) 0.4339(5) 0.0332(15) Uani 0.50 1 d P A -1 H8A H 0.2694 0.3607 0.4537 0.04(3) Uiso 0.50 1 calc PR A -1 H8B H 0.3684 0.4127 0.4729 0.07(3) Uiso 0.50 1 calc PR A -1 H8C H 0.3711 0.3112 0.4425 0.05(3) Uiso 0.50 1 calc PR A -1 C9 C 0.3501(5) 0.5633(4) 0.3551(4) 0.0258(13) Uani 0.50 1 d P A -1 H9A H 0.2836 0.5837 0.3657 0.03(2) Uiso 0.50 1 calc PR A -1 H9B H 0.3868 0.6090 0.3215 0.03(2) Uiso 0.50 1 calc PR A -1 H9C H 0.3809 0.5509 0.4166 0.04(2) Uiso 0.50 1 calc PR A -1 C10 C 0.3389(5) 0.5562(4) 0.1295(4) 0.0252(12) Uani 0.50 1 d P A -1 H10A H 0.3616 0.5397 0.0657 0.04(2) Uiso 0.50 1 calc PR A -1 H10B H 0.3798 0.6035 0.1548 0.025(18) Uiso 0.50 1 calc PR A -1 H10C H 0.2717 0.5766 0.1256 0.029(19) Uiso 0.50 1 calc PR A -1 C14 C 0.5632(5) 0.5018(6) 0.1497(6) 0.0383(17) Uani 0.50 1 d P A -1 H14A H 0.5464 0.5605 0.1735 0.09(4) Uiso 0.50 1 calc PR A -1 H14B H 0.5383 0.4948 0.0847 0.07(3) Uiso 0.50 1 calc PR A -1 H14C H 0.6338 0.4950 0.1495 0.04(2) Uiso 0.50 1 calc PR A -1 C13 C 0.5658(5) 0.4815(6) 0.3504(5) 0.0399(17) Uani 0.50 1 d P A -1 H13A H 0.5505 0.5437 0.3400 0.05(3) Uiso 0.50 1 calc PR A -1 H13B H 0.6361 0.4732 0.3488 0.05(3) Uiso 0.50 1 calc PR A -1 H13C H 0.5408 0.4630 0.4128 0.017(16) Uiso 0.50 1 calc PR A -1 C11 C 0.5431(6) 0.3165(6) 0.1271(7) 0.049(2) Uani 0.50 1 d P A -1 H11A H 0.6134 0.3075 0.1296 0.10(4) Uiso 0.50 1 calc PR A -1 H11B H 0.5255 0.3425 0.0655 0.06(3) Uiso 0.50 1 calc PR A -1 H11C H 0.5101 0.2598 0.1346 0.10(3) Uiso 0.50 1 calc PR A -1 C12 C 0.5485(6) 0.2960(6) 0.3288(7) 0.049(2) Uani 0.50 1 d P A -1 H12A H 0.6181 0.2867 0.3190 0.15(6) Uiso 0.50 1 calc PR A -1 H12B H 0.5132 0.2424 0.3114 0.16(5) Uiso 0.50 1 calc PR A -1 H12C H 0.5364 0.3099 0.3961 0.05(3) Uiso 0.50 1 calc PR A -1 Ta1 Ta 0.5000 0.403826(11) 0.240661(12) 0.02282(7) Uani 1 2 d S . . 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 C1 0.014(3) 0.018(3) 0.023(3) -0.004(2) -0.001(2) 0.001(2) C2 0.009(3) 0.022(3) 0.031(3) 0.000(2) 0.000(2) -0.001(2) C3 0.015(3) 0.020(3) 0.022(3) 0.005(2) 0.001(2) 0.000(2) C4 0.014(2) 0.020(3) 0.018(3) 0.001(2) -0.0012(19) 0.002(2) C5 0.010(2) 0.020(3) 0.018(3) 0.001(2) -0.0018(19) 0.001(2) C6 0.033(4) 0.040(4) 0.029(3) -0.015(3) -0.004(3) 0.001(3) C7 0.027(3) 0.018(3) 0.062(5) 0.003(3) 0.002(3) -0.003(3) C8 0.030(4) 0.042(4) 0.027(3) 0.013(3) 0.006(3) 0.002(3) C9 0.026(3) 0.022(3) 0.029(3) -0.009(2) -0.005(2) 0.005(2) C10 0.025(3) 0.023(3) 0.027(3) 0.008(2) 0.001(2) 0.001(2) C14 0.017(3) 0.053(5) 0.044(4) 0.011(3) 0.006(3) -0.008(3) C13 0.020(3) 0.058(5) 0.041(4) -0.008(4) -0.007(3) -0.003(3) C11 0.030(4) 0.047(5) 0.070(6) -0.029(4) 0.006(4) 0.006(4) C12 0.028(4) 0.044(5) 0.075(6) 0.023(4) -0.005(4) 0.008(4) Ta1 0.02114(10) 0.02026(10) 0.02706(10) 0.00049(7) 0.000 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.411(8) . ? C1 C5 1.426(7) . ? C1 C6 1.504(8) . ? C1 Ta1 2.518(5) . ? C2 C3 1.415(8) . ? C2 C7 1.508(8) . ? C2 Ta1 2.527(6) . ? C3 C4 1.424(8) . ? C3 C8 1.500(8) . ? C3 Ta1 2.538(6) . ? C4 C5 1.431(7) . ? C4 C9 1.493(8) . ? C4 Ta1 2.526(5) . ? C5 C10 1.494(8) . ? C5 Ta1 2.512(5) . ? 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 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C14 Ta1 2.146(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 Ta1 2.141(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C11 Ta1 2.156(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Ta1 2.159(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Ta1 C13 2.141(7) 11_655 ? Ta1 C14 2.146(7) 11_655 ? Ta1 C11 2.156(7) 11_655 ? Ta1 C12 2.159(8) 11_655 ? Ta1 C5 2.512(5) 11_655 ? Ta1 C1 2.518(6) 11_655 ? 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 C2 C1 C5 108.1(5) . . ? C2 C1 C6 126.4(5) . . ? C5 C1 C6 125.3(5) . . ? C2 C1 Ta1 74.1(3) . . ? C5 C1 Ta1 73.3(3) . . ? C6 C1 Ta1 122.6(4) . . ? C1 C2 C3 108.7(5) . . ? C1 C2 C7 125.7(6) . . ? C3 C2 C7 125.6(6) . . ? C1 C2 Ta1 73.4(3) . . ? C3 C2 Ta1 74.2(3) . . ? C7 C2 Ta1 120.9(4) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 C8 126.5(6) . . ? C4 C3 C8 125.5(6) . . ? C2 C3 Ta1 73.3(3) . . ? C4 C3 Ta1 73.2(3) . . ? C8 C3 Ta1 121.7(4) . . ? C3 C4 C5 107.8(5) . . ? C3 C4 C9 126.5(5) . . ? C5 C4 C9 125.5(5) . . ? C3 C4 Ta1 74.2(3) . . ? C5 C4 Ta1 73.0(3) . . ? C9 C4 Ta1 123.1(4) . . ? C1 C5 C4 107.6(5) . . ? C1 C5 C10 126.5(5) . . ? C4 C5 C10 125.5(5) . . ? C1 C5 Ta1 73.7(3) . . ? C4 C5 Ta1 74.0(3) . . ? C10 C5 Ta1 123.9(4) . . ? Ta1 C14 H14A 109.5 . . ? Ta1 C14 H14B 109.5 . . ? Ta1 C14 H14C 109.5 . . ? Ta1 C13 H13A 109.5 . . ? Ta1 C13 H13B 109.5 . . ? Ta1 C13 H13C 109.5 . . ? Ta1 C11 H11A 109.5 . . ? Ta1 C11 H11B 109.5 . . ? Ta1 C11 H11C 109.5 . . ? Ta1 C12 H12A 109.5 . . ? Ta1 C12 H12B 109.5 . . ? Ta1 C12 H12C 109.5 . . ? C13 Ta1 C13 50.2(4) . 11_655 ? C13 Ta1 C14 82.6(3) . . ? C13 Ta1 C14 102.5(3) 11_655 . ? C13 Ta1 C14 102.5(3) . 11_655 ? C13 Ta1 C14 82.6(3) 11_655 11_655 ? C14 Ta1 C14 48.0(4) . 11_655 ? C13 Ta1 C11 170.7(3) . 11_655 ? C13 Ta1 C11 138.8(3) 11_655 11_655 ? C14 Ta1 C11 95.8(4) . 11_655 ? C14 Ta1 C11 82.9(4) 11_655 11_655 ? C13 Ta1 C11 138.8(3) . . ? C13 Ta1 C11 170.7(3) 11_655 . ? C14 Ta1 C11 82.9(4) . . ? C14 Ta1 C11 95.8(4) 11_655 . ? C11 Ta1 C11 32.1(4) 11_655 . ? C13 Ta1 C12 98.0(4) . 11_655 ? C13 Ta1 C12 82.9(4) 11_655 11_655 ? C14 Ta1 C12 173.2(3) . 11_655 ? C14 Ta1 C12 137.8(3) 11_655 11_655 ? C11 Ta1 C12 82.5(4) 11_655 11_655 ? C11 Ta1 C12 92.3(4) . 11_655 ? C13 Ta1 C12 82.9(4) . . ? C13 Ta1 C12 98.0(4) 11_655 . ? C14 Ta1 C12 137.8(3) . . ? C14 Ta1 C12 173.2(3) 11_655 . ? C11 Ta1 C12 92.3(4) 11_655 . ? C11 Ta1 C12 82.5(4) . . ? C12 Ta1 C12 36.2(4) 11_655 . ? C13 Ta1 C5 107.5(2) . . ? C13 Ta1 C5 64.9(2) 11_655 . ? C14 Ta1 C5 83.2(2) . . ? C14 Ta1 C5 35.5(2) 11_655 . ? C11 Ta1 C5 81.4(3) 11_655 . ? C11 Ta1 C5 108.8(3) . . ? C12 Ta1 C5 103.0(3) 11_655 . ? C12 Ta1 C5 139.0(3) . . ? C13 Ta1 C5 64.9(2) . 11_655 ? C13 Ta1 C5 107.5(2) 11_655 11_655 ? C14 Ta1 C5 35.5(2) . 11_655 ? C14 Ta1 C5 83.2(2) 11_655 11_655 ? C11 Ta1 C5 108.8(3) 11_655 11_655 ? C11 Ta1 C5 81.4(3) . 11_655 ? C12 Ta1 C5 139.0(3) 11_655 11_655 ? C12 Ta1 C5 103.0(3) . 11_655 ? C5 Ta1 C5 117.4(3) . 11_655 ? C13 Ta1 C1 137.0(2) . . ? C13 Ta1 C1 87.8(2) 11_655 . ? C14 Ta1 C1 101.1(2) . . ? C14 Ta1 C1 56.9(2) 11_655 . ? C11 Ta1 C1 52.4(3) 11_655 . ? C11 Ta1 C1 83.7(3) . . ? C12 Ta1 C1 83.1(3) 11_655 . ? C12 Ta1 C1 116.4(3) . . ? C5 Ta1 C1 32.95(17) . . ? C5 Ta1 C1 135.42(18) 11_655 . ? C13 Ta1 C1 87.8(2) . 11_655 ? C13 Ta1 C1 137.0(2) 11_655 11_655 ? C14 Ta1 C1 56.9(2) . 11_655 ? C14 Ta1 C1 101.1(2) 11_655 11_655 ? C11 Ta1 C1 83.7(3) 11_655 11_655 ? C11 Ta1 C1 52.4(3) . 11_655 ? C12 Ta1 C1 116.4(3) 11_655 11_655 ? C12 Ta1 C1 83.1(3) . 11_655 ? C5 Ta1 C1 135.42(18) . 11_655 ? C5 Ta1 C1 32.95(17) 11_655 11_655 ? C1 Ta1 C1 130.4(3) . 11_655 ? 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 C5 C1 C2 C3 0.5(6) . . . . ? C6 C1 C2 C3 -174.5(6) . . . . ? Ta1 C1 C2 C3 66.4(4) . . . . ? C5 C1 C2 C7 177.6(6) . . . . ? C6 C1 C2 C7 2.6(10) . . . . ? Ta1 C1 C2 C7 -116.4(6) . . . . ? C5 C1 C2 Ta1 -66.0(4) . . . . ? C6 C1 C2 Ta1 119.1(6) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C7 C2 C3 C4 -177.5(6) . . . . ? Ta1 C2 C3 C4 65.5(4) . . . . ? C1 C2 C3 C8 176.7(6) . . . . ? C7 C2 C3 C8 -0.5(10) . . . . ? Ta1 C2 C3 C8 -117.4(6) . . . . ? C1 C2 C3 Ta1 -65.9(4) . . . . ? C7 C2 C3 Ta1 117.0(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C8 C3 C4 C5 -176.9(5) . . . . ? Ta1 C3 C4 C5 65.8(4) . . . . ? C2 C3 C4 C9 174.6(5) . . . . ? C8 C3 C4 C9 -2.4(9) . . . . ? Ta1 C3 C4 C9 -119.8(6) . . . . ? C2 C3 C4 Ta1 -65.6(4) . . . . ? C8 C3 C4 Ta1 117.3(6) . . . . ? C2 C1 C5 C4 -0.3(6) . . . . ? C6 C1 C5 C4 174.7(6) . . . . ? Ta1 C1 C5 C4 -66.9(4) . . . . ? C2 C1 C5 C10 -173.0(5) . . . . ? C6 C1 C5 C10 2.0(9) . . . . ? Ta1 C1 C5 C10 120.5(6) . . . . ? C2 C1 C5 Ta1 66.5(4) . . . . ? C6 C1 C5 Ta1 -118.5(6) . . . . ? C3 C4 C5 C1 0.1(6) . . . . ? C9 C4 C5 C1 -174.4(5) . . . . ? Ta1 C4 C5 C1 66.7(4) . . . . ? C3 C4 C5 C10 172.9(5) . . . . ? C9 C4 C5 C10 -1.7(9) . . . . ? Ta1 C4 C5 C10 -120.6(5) . . . . ? C3 C4 C5 Ta1 -66.6(4) . . . . ? C9 C4 C5 Ta1 118.9(5) . . . . ? C1 C5 Ta1 C13 -157.3(4) . . . . ? C4 C5 Ta1 C13 -43.1(4) . . . . ? C10 C5 Ta1 C13 79.2(5) . . . . ? C1 C5 Ta1 C13 -130.1(4) . . . 11_655 ? C4 C5 Ta1 C13 -15.8(4) . . . 11_655 ? C10 C5 Ta1 C13 106.5(5) . . . 11_655 ? C1 C5 Ta1 C14 122.7(4) . . . . ? C4 C5 Ta1 C14 -123.1(4) . . . . ? C10 C5 Ta1 C14 -0.8(5) . . . . ? C1 C5 Ta1 C14 115.6(6) . . . 11_655 ? C4 C5 Ta1 C14 -130.2(6) . . . 11_655 ? C10 C5 Ta1 C14 -7.8(5) . . . 11_655 ? C1 C5 Ta1 C11 25.7(4) . . . 11_655 ? C4 C5 Ta1 C11 139.9(4) . . . 11_655 ? C10 C5 Ta1 C11 -97.8(5) . . . 11_655 ? C1 C5 Ta1 C11 42.5(4) . . . . ? C4 C5 Ta1 C11 156.8(4) . . . . ? C10 C5 Ta1 C11 -80.9(5) . . . . ? C1 C5 Ta1 C12 -54.5(4) . . . 11_655 ? C4 C5 Ta1 C12 59.8(4) . . . 11_655 ? C10 C5 Ta1 C12 -177.9(5) . . . 11_655 ? C1 C5 Ta1 C12 -57.9(6) . . . . ? C4 C5 Ta1 C12 56.4(6) . . . . ? C10 C5 Ta1 C12 178.7(6) . . . . ? C1 C5 Ta1 C5 132.4(3) . . . 11_655 ? C4 C5 Ta1 C5 -113.3(3) . . . 11_655 ? C10 C5 Ta1 C5 9.0(6) . . . 11_655 ? C4 C5 Ta1 C1 114.2(5) . . . . ? C10 C5 Ta1 C1 -123.4(6) . . . . ? C1 C5 Ta1 C1 97.5(4) . . . 11_655 ? C4 C5 Ta1 C1 -148.2(3) . . . 11_655 ? C10 C5 Ta1 C1 -25.9(6) . . . 11_655 ? C2 C1 Ta1 C13 -82.4(5) . . . . ? C5 C1 Ta1 C13 32.6(5) . . . . ? C6 C1 Ta1 C13 154.2(5) . . . . ? C2 C1 Ta1 C13 -71.1(4) . . . 11_655 ? C5 C1 Ta1 C13 43.9(4) . . . 11_655 ? C6 C1 Ta1 C13 165.5(5) . . . 11_655 ? C2 C1 Ta1 C14 -173.4(4) . . . . ? C5 C1 Ta1 C14 -58.4(4) . . . . ? C6 C1 Ta1 C14 63.2(6) . . . . ? C2 C1 Ta1 C14 -153.7(4) . . . 11_655 ? C5 C1 Ta1 C14 -38.7(4) . . . 11_655 ? C6 C1 Ta1 C14 82.9(6) . . . 11_655 ? C2 C1 Ta1 C11 97.8(5) . . . 11_655 ? C5 C1 Ta1 C11 -147.3(5) . . . 11_655 ? C6 C1 Ta1 C11 -25.6(6) . . . 11_655 ? C2 C1 Ta1 C11 105.1(4) . . . . ? C5 C1 Ta1 C11 -139.9(4) . . . . ? C6 C1 Ta1 C11 -18.3(6) . . . . ? C2 C1 Ta1 C12 12.0(4) . . . 11_655 ? C5 C1 Ta1 C12 127.0(4) . . . 11_655 ? C6 C1 Ta1 C12 -111.4(6) . . . 11_655 ? C2 C1 Ta1 C12 26.7(5) . . . . ? C5 C1 Ta1 C12 141.7(4) . . . . ? C6 C1 Ta1 C12 -96.7(6) . . . . ? C2 C1 Ta1 C5 -115.0(5) . . . . ? C6 C1 Ta1 C5 121.6(6) . . . . ? C2 C1 Ta1 C5 176.0(3) . . . 11_655 ? C5 C1 Ta1 C5 -69.0(4) . . . 11_655 ? C6 C1 Ta1 C5 52.6(6) . . . 11_655 ? C2 C1 Ta1 C1 131.0(3) . . . 11_655 ? C5 C1 Ta1 C1 -114.0(3) . . . 11_655 ? C6 C1 Ta1 C1 7.6(7) . . . 11_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.876 _refine_diff_density_min -2.005 _refine_diff_density_rms 0.115