# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name C.C.Cummins _publ_contact_author_email CCUMMINS@MIT.EDU loop_ _publ_author_name M.A.Rankin C.C.Cummins data_09047_mr _database_code_depnum_ccdc_archive 'CCDC 852392' #TrackingRef '- 09047_mr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ar(tBuCH2)N)3TaPPh _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H65 N3 P Ta' _chemical_formula_weight 859.92 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5963(16) _cell_length_b 12.3639(19) _cell_length_c 17.124(3) _cell_angle_alpha 82.977(3) _cell_angle_beta 87.201(3) _cell_angle_gamma 74.186(3) _cell_volume 2142.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1149 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.57 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 2.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4113 _exptl_absorpt_correction_T_max 0.7785 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 11540 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 29.13 _reflns_number_total 11540 _reflns_number_gt 11283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 3.0 (Bruker-AXS, 2008)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2008)' _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^ > 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^)+(0.0000P)^2^+5.5896P] 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 11540 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 Ta1 Ta 0.669556(16) 0.180369(15) 0.284201(10) 0.01307(3) Uani 1 1 d . . . P1 P 0.85347(10) 0.03069(9) 0.30779(6) 0.01776(19) Uani 1 1 d . . . N1 N 0.6185(3) 0.2223(3) 0.39205(19) 0.0169(6) Uani 1 1 d . . . N2 N 0.5293(3) 0.1507(3) 0.22374(18) 0.0153(6) Uani 1 1 d . . . N3 N 0.7463(3) 0.2957(3) 0.22158(19) 0.0153(6) Uani 1 1 d . . . C11 C 0.4827(4) 0.2779(4) 0.4074(2) 0.0175(8) Uani 1 1 d . . . C12 C 0.4172(4) 0.3732(3) 0.3589(2) 0.0179(7) Uani 1 1 d . . . H12 H 0.4651 0.4074 0.3196 0.022 Uiso 1 1 calc R . . C13 C 0.2812(4) 0.4196(4) 0.3669(2) 0.0205(8) Uani 1 1 d . . . C14 C 0.2137(4) 0.3704(4) 0.4263(2) 0.0247(9) Uani 1 1 d . . . H14 H 0.1218 0.4014 0.4323 0.030 Uiso 1 1 calc R . . C15 C 0.2772(4) 0.2771(4) 0.4772(2) 0.0251(9) Uani 1 1 d . . . C16 C 0.4111(4) 0.2304(4) 0.4666(2) 0.0198(8) Uani 1 1 d . . . H16 H 0.4549 0.1653 0.5001 0.024 Uiso 1 1 calc R . . C17 C 0.7020(4) 0.1860(4) 0.4638(2) 0.0198(8) Uani 1 1 d . . . H17A H 0.7710 0.1161 0.4552 0.024 Uiso 1 1 calc R . . H17B H 0.6466 0.1671 0.5089 0.024 Uiso 1 1 calc R . . C18 C 0.7682(4) 0.2740(4) 0.4861(2) 0.0224(8) Uani 1 1 d . . . C21 C 0.5437(4) 0.1402(3) 0.1415(2) 0.0151(7) Uani 1 1 d . . . C22 C 0.6607(4) 0.0723(3) 0.1131(2) 0.0174(7) Uani 1 1 d . . . H22 H 0.7269 0.0321 0.1494 0.021 Uiso 1 1 calc R . . C23 C 0.6832(4) 0.0619(3) 0.0337(2) 0.0207(8) Uani 1 1 d . . . C24 C 0.5846(4) 0.1201(3) -0.0191(2) 0.0195(8) Uani 1 1 d . . . H24 H 0.5986 0.1138 -0.0737 0.023 Uiso 1 1 calc R . . C25 C 0.4656(4) 0.1876(4) 0.0075(3) 0.0195(8) Uani 1 1 d . . . C26 C 0.4462(4) 0.1981(4) 0.0873(2) 0.0185(8) Uani 1 1 d . . . H26 H 0.3660 0.2450 0.1054 0.022 Uiso 1 1 calc R . . C27 C 0.3970(3) 0.1591(3) 0.2601(2) 0.0153(7) Uani 1 1 d . . . H27A H 0.3304 0.2035 0.2215 0.018 Uiso 1 1 calc R . . H27B H 0.3883 0.2020 0.3061 0.018 Uiso 1 1 calc R . . C28 C 0.3651(3) 0.0457(3) 0.2872(3) 0.0152(6) Uani 1 1 d . . . C31 C 0.6524(4) 0.4049(3) 0.2103(2) 0.0161(7) Uani 1 1 d . . . C32 C 0.5529(4) 0.4242(4) 0.1560(2) 0.0206(8) Uani 1 1 d . . . H32 H 0.5500 0.3661 0.1252 0.025 Uiso 1 1 calc R . . C33 C 0.4567(4) 0.5283(3) 0.1460(3) 0.0222(8) Uani 1 1 d . . . C34 C 0.4619(4) 0.6112(4) 0.1928(3) 0.0255(9) Uani 1 1 d . . . H34 H 0.3968 0.6816 0.1871 0.031 Uiso 1 1 calc R . . C35 C 0.5603(4) 0.5936(4) 0.2477(2) 0.0221(8) Uani 1 1 d . . . C36 C 0.6557(4) 0.4920(3) 0.2548(2) 0.0174(7) Uani 1 1 d . . . H36 H 0.7251 0.4808 0.2905 0.021 Uiso 1 1 calc R . . C37 C 0.8837(4) 0.2991(3) 0.2071(2) 0.0175(7) Uani 1 1 d . . . H37A H 0.9412 0.2264 0.2308 0.021 Uiso 1 1 calc R . . H37B H 0.8986 0.3595 0.2355 0.021 Uiso 1 1 calc R . . C38 C 0.9289(4) 0.3193(4) 0.1205(2) 0.0194(8) Uani 1 1 d . . . C41 C 0.9061(4) -0.0887(3) 0.2499(2) 0.0187(8) Uani 1 1 d . . . C42 C 0.8343(4) -0.1671(4) 0.2464(2) 0.0209(8) Uani 1 1 d . . . H42 H 0.7523 -0.1575 0.2736 0.025 Uiso 1 1 calc R . . C43 C 0.8808(5) -0.2593(4) 0.2038(3) 0.0266(9) Uani 1 1 d . . . H43 H 0.8306 -0.3120 0.2023 0.032 Uiso 1 1 calc R . . C44 C 0.9994(5) -0.2746(4) 0.1635(3) 0.0279(9) Uani 1 1 d . . . H44 H 1.0311 -0.3379 0.1348 0.033 Uiso 1 1 calc R . . C45 C 1.0717(4) -0.1973(4) 0.1653(3) 0.0292(9) Uani 1 1 d . . . H45 H 1.1519 -0.2062 0.1363 0.035 Uiso 1 1 calc R . . C46 C 1.0275(4) -0.1059(4) 0.2097(3) 0.0263(9) Uani 1 1 d . . . H46 H 1.0799 -0.0552 0.2127 0.032 Uiso 1 1 calc R . . C131 C 0.2113(4) 0.5193(4) 0.3110(3) 0.0292(9) Uani 1 1 d . . . H13A H 0.2183 0.4974 0.2575 0.044 Uiso 1 1 calc R . . H13B H 0.2515 0.5817 0.3124 0.044 Uiso 1 1 calc R . . H13C H 0.1186 0.5437 0.3267 0.044 Uiso 1 1 calc R . . C151 C 0.2020(5) 0.2241(5) 0.5403(3) 0.0383(13) Uani 1 1 d . . . H15A H 0.1345 0.1990 0.5161 0.057 Uiso 1 1 calc R . . H15B H 0.1604 0.2797 0.5763 0.057 Uiso 1 1 calc R . . H15C H 0.2622 0.1589 0.5696 0.057 Uiso 1 1 calc R . . C181 C 0.6694(5) 0.3879(4) 0.4929(3) 0.0309(10) Uani 1 1 d . . . H18A H 0.6000 0.3779 0.5308 0.046 Uiso 1 1 calc R . . H18B H 0.6307 0.4189 0.4414 0.046 Uiso 1 1 calc R . . H18C H 0.7137 0.4401 0.5108 0.046 Uiso 1 1 calc R . . C182 C 0.8743(4) 0.2876(4) 0.4245(3) 0.0291(10) Uani 1 1 d . . . H18D H 0.9137 0.3462 0.4373 0.044 Uiso 1 1 calc R . . H18E H 0.8348 0.3096 0.3724 0.044 Uiso 1 1 calc R . . H18F H 0.9423 0.2157 0.4243 0.044 Uiso 1 1 calc R . . C183 C 0.8334(5) 0.2263(5) 0.5657(3) 0.0293(10) Uani 1 1 d . . . H18G H 0.8822 0.2772 0.5807 0.044 Uiso 1 1 calc R . . H18H H 0.8938 0.1515 0.5613 0.044 Uiso 1 1 calc R . . H18I H 0.7659 0.2197 0.6058 0.044 Uiso 1 1 calc R . . C231 C 0.8111(4) -0.0118(4) 0.0051(3) 0.0274(9) Uani 1 1 d . . . H23A H 0.8656 0.0360 -0.0194 0.041 Uiso 1 1 calc R . . H23B H 0.7933 -0.0577 -0.0337 0.041 Uiso 1 1 calc R . . H23C H 0.8574 -0.0616 0.0497 0.041 Uiso 1 1 calc R . . C251 C 0.3599(4) 0.2477(4) -0.0503(3) 0.0282(9) Uani 1 1 d . . . H25A H 0.2739 0.2582 -0.0239 0.042 Uiso 1 1 calc R . . H25B H 0.3642 0.2024 -0.0940 0.042 Uiso 1 1 calc R . . H25C H 0.3726 0.3217 -0.0706 0.042 Uiso 1 1 calc R . . C281 C 0.3678(4) -0.0223(4) 0.2182(2) 0.0226(8) Uani 1 1 d . . . H28A H 0.4563 -0.0413 0.1949 0.034 Uiso 1 1 calc R . . H28B H 0.3054 0.0228 0.1784 0.034 Uiso 1 1 calc R . . H28C H 0.3433 -0.0920 0.2369 0.034 Uiso 1 1 calc R . . C282 C 0.4612(4) -0.0217(4) 0.3503(2) 0.0217(8) Uani 1 1 d . . . H28D H 0.4415 -0.0942 0.3669 0.033 Uiso 1 1 calc R . . H28E H 0.4528 0.0212 0.3956 0.033 Uiso 1 1 calc R . . H28F H 0.5509 -0.0356 0.3289 0.033 Uiso 1 1 calc R . . C283 C 0.2258(4) 0.0765(4) 0.3238(3) 0.0257(9) Uani 1 1 d . . . H28G H 0.2003 0.0071 0.3420 0.039 Uiso 1 1 calc R . . H28H H 0.1639 0.1227 0.2842 0.039 Uiso 1 1 calc R . . H28I H 0.2248 0.1193 0.3685 0.039 Uiso 1 1 calc R . . C331 C 0.3522(5) 0.5489(4) 0.0853(3) 0.0324(10) Uani 1 1 d . . . H33A H 0.2687 0.5459 0.1116 0.049 Uiso 1 1 calc R . . H33B H 0.3774 0.4905 0.0493 0.049 Uiso 1 1 calc R . . H33C H 0.3425 0.6235 0.0556 0.049 Uiso 1 1 calc R . . C351 C 0.5621(5) 0.6840(4) 0.2994(3) 0.0316(11) Uani 1 1 d . . . H35A H 0.4785 0.7044 0.3285 0.047 Uiso 1 1 calc R . . H35B H 0.5748 0.7510 0.2666 0.047 Uiso 1 1 calc R . . H35C H 0.6341 0.6552 0.3367 0.047 Uiso 1 1 calc R . . C381 C 0.8946(5) 0.2353(4) 0.0725(3) 0.0271(10) Uani 1 1 d . . . H38A H 0.9316 0.2427 0.0192 0.041 Uiso 1 1 calc R . . H38B H 0.7990 0.2510 0.0698 0.041 Uiso 1 1 calc R . . H38C H 0.9311 0.1581 0.0977 0.041 Uiso 1 1 calc R . . C382 C 0.8687(4) 0.4407(4) 0.0835(3) 0.0273(9) Uani 1 1 d . . . H38D H 0.8887 0.4939 0.1158 0.041 Uiso 1 1 calc R . . H38E H 0.7734 0.4545 0.0806 0.041 Uiso 1 1 calc R . . H38F H 0.9055 0.4513 0.0304 0.041 Uiso 1 1 calc R . . C383 C 1.0779(4) 0.2992(4) 0.1217(3) 0.0299(10) Uani 1 1 d . . . H38G H 1.1189 0.2198 0.1406 0.045 Uiso 1 1 calc R . . H38H H 1.0996 0.3480 0.1570 0.045 Uiso 1 1 calc R . . H38I H 1.1105 0.3168 0.0685 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.01092(5) 0.01451(6) 0.01365(5) -0.00171(7) -0.00059(6) -0.00311(4) P1 0.0146(4) 0.0168(5) 0.0210(5) -0.0019(4) -0.0029(3) -0.0023(4) N1 0.0172(15) 0.0211(16) 0.0134(15) -0.0017(12) -0.0020(12) -0.0069(13) N2 0.0143(14) 0.0202(16) 0.0125(14) -0.0013(12) 0.0001(11) -0.0065(12) N3 0.0117(14) 0.0153(15) 0.0169(15) -0.0019(12) -0.0002(11) -0.0001(12) C11 0.0181(18) 0.023(2) 0.0133(17) -0.0063(15) 0.0001(14) -0.0075(16) C12 0.0178(18) 0.0187(19) 0.0193(18) -0.0050(15) 0.0037(14) -0.0077(15) C13 0.0200(19) 0.024(2) 0.0183(19) -0.0059(16) -0.0006(15) -0.0064(16) C14 0.0160(18) 0.036(2) 0.023(2) -0.0066(18) 0.0015(15) -0.0071(17) C15 0.0204(19) 0.039(3) 0.0191(19) -0.0032(17) 0.0012(15) -0.0137(18) C16 0.0173(18) 0.028(2) 0.0143(17) 0.0000(15) -0.0030(14) -0.0075(16) C17 0.0157(17) 0.024(2) 0.0192(18) -0.0012(15) -0.0025(14) -0.0051(15) C18 0.0179(18) 0.034(2) 0.0189(19) -0.0040(16) -0.0029(15) -0.0119(17) C21 0.0165(16) 0.0162(17) 0.0147(16) -0.0023(13) -0.0005(13) -0.0079(14) C22 0.0202(18) 0.0192(19) 0.0127(16) -0.0032(14) -0.0026(14) -0.0041(15) C23 0.0184(19) 0.0181(18) 0.025(2) -0.0051(16) 0.0011(15) -0.0026(16) C24 0.0210(19) 0.0215(19) 0.0174(18) -0.0065(15) 0.0007(14) -0.0065(16) C25 0.0170(18) 0.021(2) 0.021(2) -0.0008(16) -0.0033(15) -0.0061(16) C26 0.0167(18) 0.0185(19) 0.0198(19) -0.0020(15) 0.0003(15) -0.0042(15) C27 0.0117(15) 0.0161(17) 0.0180(17) -0.0035(13) -0.0024(12) -0.0027(13) C28 0.0147(14) 0.0164(15) 0.0160(15) -0.0029(16) 0.0000(15) -0.0065(12) C31 0.0130(16) 0.0199(18) 0.0148(16) -0.0013(14) 0.0035(13) -0.0046(14) C32 0.0151(17) 0.0213(19) 0.025(2) -0.0025(16) 0.0028(15) -0.0054(15) C33 0.0175(18) 0.0200(19) 0.026(2) 0.0027(16) -0.0025(16) -0.0016(15) C34 0.021(2) 0.0149(19) 0.034(2) 0.0011(17) 0.0039(17) 0.0023(16) C35 0.027(2) 0.0192(19) 0.023(2) -0.0037(16) 0.0044(16) -0.0109(17) C36 0.0192(17) 0.0222(19) 0.0129(15) -0.0040(14) -0.0006(13) -0.0079(15) C37 0.0115(16) 0.0223(19) 0.0185(18) -0.0009(14) 0.0002(13) -0.0049(14) C38 0.0135(17) 0.025(2) 0.0185(18) 0.0010(15) 0.0031(14) -0.0042(15) C41 0.0140(17) 0.0178(19) 0.0215(19) -0.0013(15) -0.0014(14) 0.0005(14) C42 0.0168(18) 0.0208(19) 0.0233(19) -0.0007(15) 0.0019(15) -0.0034(15) C43 0.032(2) 0.022(2) 0.025(2) -0.0043(17) -0.0028(18) -0.0054(19) C44 0.031(2) 0.023(2) 0.024(2) -0.0083(17) -0.0007(17) 0.0035(18) C45 0.024(2) 0.030(2) 0.029(2) -0.0056(18) 0.0066(17) 0.0009(18) C46 0.0194(19) 0.027(2) 0.031(2) -0.0044(18) 0.0013(17) -0.0045(17) C131 0.023(2) 0.029(2) 0.032(2) -0.0013(18) 0.0021(17) -0.0025(18) C151 0.021(2) 0.068(4) 0.025(2) 0.010(2) -0.0001(18) -0.016(2) C181 0.034(2) 0.029(2) 0.034(2) -0.0117(19) -0.0042(19) -0.011(2) C182 0.023(2) 0.045(3) 0.024(2) -0.0008(19) -0.0025(17) -0.019(2) C183 0.025(2) 0.046(3) 0.021(2) -0.0011(19) -0.0022(17) -0.017(2) C231 0.026(2) 0.028(2) 0.022(2) -0.0058(18) 0.0056(17) 0.0033(18) C251 0.021(2) 0.041(3) 0.020(2) 0.0035(18) -0.0033(15) -0.0067(18) C281 0.028(2) 0.0203(19) 0.023(2) -0.0050(16) 0.0012(16) -0.0097(17) C282 0.026(2) 0.021(2) 0.0186(19) 0.0016(15) -0.0011(15) -0.0086(17) C283 0.021(2) 0.026(2) 0.031(2) -0.0023(18) 0.0032(17) -0.0084(17) C331 0.023(2) 0.035(3) 0.032(2) -0.003(2) -0.0073(18) 0.0057(19) C351 0.034(2) 0.023(2) 0.040(3) -0.0117(19) 0.0029(19) -0.0069(18) C381 0.025(2) 0.032(2) 0.025(2) -0.0080(18) 0.0061(17) -0.0073(19) C382 0.022(2) 0.029(2) 0.029(2) 0.0074(18) 0.0007(17) -0.0076(17) C383 0.0153(18) 0.043(3) 0.027(2) 0.003(2) 0.0046(16) -0.0056(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.989(3) . ? Ta1 N2 1.989(3) . ? Ta1 N3 2.005(3) . ? Ta1 P1 2.3052(11) . ? P1 C41 1.824(4) . ? N1 C11 1.443(5) . ? N1 C17 1.500(5) . ? N2 C21 1.426(5) . ? N2 C27 1.488(5) . ? N3 C31 1.440(5) . ? N3 C37 1.476(5) . ? C11 C12 1.390(6) . ? C11 C16 1.403(5) . ? C12 C13 1.405(5) . ? C13 C14 1.390(6) . ? C13 C131 1.506(6) . ? C14 C15 1.389(6) . ? C15 C16 1.390(6) . ? C15 C151 1.503(6) . ? C17 C18 1.539(6) . ? C18 C181 1.522(6) . ? C18 C182 1.533(6) . ? C18 C183 1.534(6) . ? C21 C22 1.397(5) . ? C21 C26 1.404(5) . ? C22 C23 1.386(5) . ? C23 C24 1.396(6) . ? C23 C231 1.509(6) . ? C24 C25 1.399(6) . ? C25 C26 1.389(6) . ? C25 C251 1.504(6) . ? C27 C28 1.542(5) . ? C28 C282 1.524(6) . ? C28 C281 1.527(6) . ? C28 C283 1.542(5) . ? C31 C32 1.392(5) . ? C31 C36 1.402(5) . ? C32 C33 1.404(6) . ? C33 C34 1.389(6) . ? C33 C331 1.505(6) . ? C34 C35 1.394(6) . ? C35 C36 1.377(6) . ? C35 C351 1.513(6) . ? C37 C38 1.548(5) . ? C38 C381 1.527(6) . ? C38 C383 1.530(5) . ? C38 C382 1.531(6) . ? C41 C42 1.395(6) . ? C41 C46 1.404(6) . ? C42 C43 1.392(6) . ? C43 C44 1.381(6) . ? C44 C45 1.383(7) . ? C45 C46 1.401(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ta1 N2 115.60(13) . . ? N1 Ta1 N3 110.88(13) . . ? N2 Ta1 N3 110.21(13) . . ? N1 Ta1 P1 101.91(10) . . ? N2 Ta1 P1 115.75(10) . . ? N3 Ta1 P1 101.39(9) . . ? C41 P1 Ta1 125.15(13) . . ? C11 N1 C17 114.6(3) . . ? C11 N1 Ta1 118.1(2) . . ? C17 N1 Ta1 126.5(3) . . ? C21 N2 C27 117.4(3) . . ? C21 N2 Ta1 121.7(2) . . ? C27 N2 Ta1 120.1(2) . . ? C31 N3 C37 114.0(3) . . ? C31 N3 Ta1 111.7(2) . . ? C37 N3 Ta1 131.2(2) . . ? C12 C11 C16 118.8(4) . . ? C12 C11 N1 120.4(3) . . ? C16 C11 N1 120.5(4) . . ? C11 C12 C13 121.0(4) . . ? C14 C13 C12 118.6(4) . . ? C14 C13 C131 121.4(4) . . ? C12 C13 C131 120.0(4) . . ? C15 C14 C13 121.7(4) . . ? C14 C15 C16 118.8(4) . . ? C14 C15 C151 120.8(4) . . ? C16 C15 C151 120.3(4) . . ? C15 C16 C11 121.2(4) . . ? N1 C17 C18 115.1(3) . . ? C181 C18 C182 110.0(4) . . ? C181 C18 C183 110.1(4) . . ? C182 C18 C183 109.0(3) . . ? C181 C18 C17 111.7(3) . . ? C182 C18 C17 109.5(3) . . ? C183 C18 C17 106.5(4) . . ? C22 C21 C26 118.4(3) . . ? C22 C21 N2 119.0(3) . . ? C26 C21 N2 122.6(3) . . ? C23 C22 C21 122.0(4) . . ? C22 C23 C24 118.5(4) . . ? C22 C23 C231 120.6(4) . . ? C24 C23 C231 120.9(4) . . ? C23 C24 C25 120.9(4) . . ? C26 C25 C24 119.5(4) . . ? C26 C25 C251 120.6(4) . . ? C24 C25 C251 119.9(4) . . ? C25 C26 C21 120.7(4) . . ? N2 C27 C28 115.8(3) . . ? C282 C28 C281 111.0(3) . . ? C282 C28 C27 109.6(3) . . ? C281 C28 C27 111.5(3) . . ? C282 C28 C283 108.9(4) . . ? C281 C28 C283 109.7(3) . . ? C27 C28 C283 106.0(3) . . ? C32 C31 C36 118.6(4) . . ? C32 C31 N3 119.8(3) . . ? C36 C31 N3 121.6(3) . . ? C31 C32 C33 121.1(4) . . ? C34 C33 C32 118.3(4) . . ? C34 C33 C331 121.4(4) . . ? C32 C33 C331 120.3(4) . . ? C33 C34 C35 121.7(4) . . ? C36 C35 C34 118.9(4) . . ? C36 C35 C351 120.3(4) . . ? C34 C35 C351 120.8(4) . . ? C35 C36 C31 121.4(4) . . ? N3 C37 C38 117.5(3) . . ? C381 C38 C383 109.9(4) . . ? C381 C38 C382 110.2(4) . . ? C383 C38 C382 108.2(3) . . ? C381 C38 C37 109.6(3) . . ? C383 C38 C37 106.4(3) . . ? C382 C38 C37 112.3(3) . . ? C42 C41 C46 118.1(4) . . ? C42 C41 P1 123.0(3) . . ? C46 C41 P1 118.8(3) . . ? C43 C42 C41 121.0(4) . . ? C44 C43 C42 120.4(4) . . ? C43 C44 C45 119.6(4) . . ? C44 C45 C46 120.4(4) . . ? C45 C46 C41 120.4(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.387 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.120 # Attachment '- 09140hb_e.cif' data_09140hb_e _database_code_depnum_ccdc_archive 'CCDC 852393' #TrackingRef '- 09140hb_e.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (HTa(N(CH2tBu)Ar)3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H124 N6 Ta2' _chemical_formula_weight 1507.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 12.9616(9) _cell_length_b 12.9616(9) _cell_length_c 38.840(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5651.0(7) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9689 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 31.30 _exptl_crystal_description hexagonal _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2340 _exptl_absorpt_coefficient_mu 2.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3507 _exptl_absorpt_correction_T_max 0.7571 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 36616 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 30.03 _reflns_number_total 3690 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 3.0 (Bruker-AXS, 2008)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2008)' _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^ > 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. The asymmetric unit contains one-sixth of the full molecule with a positional disorder of this moiety over two positions. The disorder was refined within SHELXL with the help of rigid bond restraints as well as similarity restraints on the anisotropic displacement parameters for neighboring atoms and on 1,2- and 1,3-distances throughout the disordered components. The hydride positions were located at probable locations and refined using distance and similarity restraints. ; _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^+24.0347P] 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 3690 _refine_ls_number_parameters 255 _refine_ls_number_restraints 384 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0529 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.0000 0.0000 0.035987(3) 0.01415(4) Uani 1 3 d SDU . . N1 N -0.1419(2) 0.0124(2) 0.05154(6) 0.0268(5) Uani 0.812(3) 1 d PDU A 1 C11 C -0.1971(3) -0.0452(3) 0.08350(8) 0.0296(6) Uani 0.812(3) 1 d PDU A 1 C12 C -0.1522(3) 0.0093(3) 0.11476(9) 0.0376(7) Uani 0.812(3) 1 d PDU A 1 H12 H -0.0813 0.0848 0.1155 0.045 Uiso 0.812(3) 1 calc PR A 1 C13 C -0.2105(4) -0.0460(4) 0.14539(10) 0.0544(9) Uani 0.812(3) 1 d PDU A 1 C14 C -0.3155(4) -0.1572(4) 0.14333(11) 0.0596(10) Uani 0.812(3) 1 d PDU A 1 H14 H -0.3561 -0.1953 0.1640 0.072 Uiso 0.812(3) 1 calc PR A 1 C15 C -0.3620(4) -0.2133(3) 0.11192(12) 0.0535(10) Uani 0.812(3) 1 d PDU A 1 C16 C -0.3006(3) -0.1564(3) 0.08238(10) 0.0419(8) Uani 0.812(3) 1 d PDU A 1 H16 H -0.3296 -0.1940 0.0607 0.050 Uiso 0.812(3) 1 calc PR A 1 C131 C -0.1621(7) 0.0193(7) 0.17950(13) 0.093(2) Uani 0.812(3) 1 d PDU A 1 H13A H -0.0915 0.0971 0.1751 0.139 Uiso 0.812(3) 1 calc PR A 1 H13B H -0.1404 -0.0279 0.1944 0.139 Uiso 0.812(3) 1 calc PR A 1 H13C H -0.2233 0.0305 0.1908 0.139 Uiso 0.812(3) 1 calc PR A 1 C151 C -0.4768(6) -0.3300(5) 0.11002(19) 0.090(2) Uani 0.812(3) 1 d PDU A 1 H15A H -0.5198 -0.3323 0.0890 0.136 Uiso 0.812(3) 1 calc PR A 1 H15B H -0.5260 -0.3382 0.1302 0.136 Uiso 0.812(3) 1 calc PR A 1 H15C H -0.4597 -0.3956 0.1097 0.136 Uiso 0.812(3) 1 calc PR A 1 C17 C -0.2217(3) 0.0387(3) 0.02934(8) 0.0338(6) Uani 0.812(3) 1 d PDU A 1 H17A H -0.2956 -0.0376 0.0247 0.041 Uiso 0.812(3) 1 calc PR A 1 H17B H -0.1812 0.0696 0.0070 0.041 Uiso 0.812(3) 1 calc PR A 1 C18 C -0.2571(5) 0.1269(6) 0.04357(12) 0.0334(9) Uani 0.812(3) 1 d PDU A 1 C181 C -0.3495(4) 0.0774(5) 0.07219(11) 0.0561(11) Uani 0.812(3) 1 d PDU A 1 H18A H -0.4195 0.0039 0.0643 0.084 Uiso 0.812(3) 1 calc PR A 1 H18B H -0.3731 0.1361 0.0782 0.084 Uiso 0.812(3) 1 calc PR A 1 H18C H -0.3155 0.0604 0.0925 0.084 Uiso 0.812(3) 1 calc PR A 1 C182 C -0.1479(4) 0.2393(3) 0.05705(10) 0.0486(9) Uani 0.812(3) 1 d PDU A 1 H18D H -0.1719 0.2956 0.0653 0.073 Uiso 0.812(3) 1 calc PR A 1 H18E H -0.0895 0.2761 0.0385 0.073 Uiso 0.812(3) 1 calc PR A 1 H18F H -0.1121 0.2181 0.0760 0.073 Uiso 0.812(3) 1 calc PR A 1 C183 C -0.3089(5) 0.1625(5) 0.01280(15) 0.0516(14) Uani 0.812(3) 1 d PDU A 1 H18G H -0.3722 0.0906 0.0018 0.077 Uiso 0.812(3) 1 calc PR A 1 H18H H -0.2456 0.2079 -0.0040 0.077 Uiso 0.812(3) 1 calc PR A 1 H18I H -0.3417 0.2117 0.0211 0.077 Uiso 0.812(3) 1 calc PR A 1 N2 N -0.0837(9) 0.0868(10) 0.0527(2) 0.0280(18) Uani 0.188(3) 1 d PDU A 2 C21 C -0.0416(9) 0.1527(9) 0.0845(3) 0.0253(18) Uani 0.188(3) 1 d PDU A 2 C22 C 0.0437(9) 0.2725(10) 0.0847(3) 0.032(2) Uani 0.188(3) 1 d PDU A 2 H22 H 0.0754 0.3129 0.0636 0.038 Uiso 0.188(3) 1 calc PR A 2 C23 C 0.0839(10) 0.3349(10) 0.1161(3) 0.036(3) Uani 0.188(3) 1 d PDU A 2 C24 C 0.0350(11) 0.2747(10) 0.1461(3) 0.035(2) Uani 0.188(3) 1 d PDU A 2 H24 H 0.0604 0.3167 0.1673 0.042 Uiso 0.188(3) 1 calc PR A 2 C25 C -0.0508(11) 0.1538(11) 0.1467(3) 0.034(2) Uani 0.188(3) 1 d PDU A 2 C26 C -0.0872(11) 0.0931(11) 0.1155(3) 0.031(2) Uani 0.188(3) 1 d PDU A 2 H26 H -0.1436 0.0103 0.1153 0.037 Uiso 0.188(3) 1 calc PR A 2 C231 C 0.171(2) 0.4684(15) 0.1132(8) 0.090(2) Uani 0.188(3) 1 d PDU A 2 H23A H 0.1870 0.5045 0.1362 0.136 Uiso 0.188(3) 1 calc PR A 2 H23B H 0.1369 0.5051 0.0985 0.136 Uiso 0.188(3) 1 calc PR A 2 H23C H 0.2460 0.4813 0.1030 0.136 Uiso 0.188(3) 1 calc PR A 2 C251 C -0.1085(15) 0.0852(16) 0.1798(3) 0.040(3) Uani 0.188(3) 1 d PDU A 2 H25A H -0.0463 0.0956 0.1961 0.060 Uiso 0.188(3) 1 calc PR A 2 H25B H -0.1591 0.0004 0.1744 0.060 Uiso 0.188(3) 1 calc PR A 2 H25C H -0.1571 0.1157 0.1900 0.060 Uiso 0.188(3) 1 calc PR A 2 C27 C -0.1482(11) 0.1337(11) 0.0313(3) 0.032(2) Uani 0.188(3) 1 d PDU A 2 H27A H -0.1605 0.0982 0.0080 0.038 Uiso 0.188(3) 1 calc PR A 2 H27B H -0.0953 0.2208 0.0287 0.038 Uiso 0.188(3) 1 calc PR A 2 C28 C -0.2685(18) 0.112(2) 0.0445(5) 0.035(3) Uani 0.188(3) 1 d PDU A 2 C281 C -0.2611(14) 0.1940(15) 0.0731(4) 0.048(3) Uani 0.188(3) 1 d PDU A 2 H28A H -0.2148 0.1886 0.0922 0.072 Uiso 0.188(3) 1 calc PR A 2 H28B H -0.3416 0.1707 0.0811 0.072 Uiso 0.188(3) 1 calc PR A 2 H28C H -0.2221 0.2760 0.0645 0.072 Uiso 0.188(3) 1 calc PR A 2 C282 C -0.3498(12) -0.0190(12) 0.0545(4) 0.044(3) Uani 0.188(3) 1 d PDU A 2 H28D H -0.3133 -0.0397 0.0734 0.066 Uiso 0.188(3) 1 calc PR A 2 H28E H -0.3608 -0.0699 0.0346 0.066 Uiso 0.188(3) 1 calc PR A 2 H28F H -0.4272 -0.0309 0.0619 0.066 Uiso 0.188(3) 1 calc PR A 2 C283 C -0.334(3) 0.130(3) 0.0138(6) 0.0516(14) Uani 0.188(3) 1 d PDU A 2 H28G H -0.3998 0.1387 0.0223 0.077 Uiso 0.188(3) 1 calc PR A 2 H28H H -0.3644 0.0604 -0.0015 0.077 Uiso 0.188(3) 1 calc PR A 2 H28I H -0.2777 0.2015 0.0011 0.077 Uiso 0.188(3) 1 calc PR A 2 H1 H 0.0815 0.0955 0.0029 0.062 Uiso 0.33 1 d PRD A -1 H1A H -0.0696 -0.0748 0.0013 0.062 Uiso 0.33 1 d PRD A -1 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 0.01502(5) 0.01502(5) 0.01242(6) 0.000 0.000 0.00751(2) N1 0.0251(11) 0.0260(12) 0.0327(12) 0.0082(9) 0.0097(9) 0.0154(10) C11 0.0282(13) 0.0299(13) 0.0375(14) 0.0091(11) 0.0144(11) 0.0196(11) C12 0.0376(16) 0.0450(18) 0.0348(14) 0.0112(12) 0.0038(12) 0.0241(14) C13 0.074(3) 0.067(2) 0.0335(16) 0.0161(15) 0.0124(16) 0.044(2) C14 0.083(3) 0.058(2) 0.0459(18) 0.0260(15) 0.0409(18) 0.0415(18) C15 0.062(2) 0.0344(17) 0.062(2) 0.0163(15) 0.0402(19) 0.0223(16) C16 0.0476(18) 0.0261(14) 0.0478(18) 0.0048(12) 0.0270(15) 0.0154(13) C131 0.122(6) 0.114(5) 0.030(2) 0.016(2) 0.001(3) 0.050(4) C151 0.087(4) 0.043(2) 0.101(4) 0.011(2) 0.062(3) 0.003(2) C17 0.0301(14) 0.0390(15) 0.0388(15) -0.0056(12) -0.0037(12) 0.0221(13) C18 0.0372(19) 0.048(2) 0.0305(17) 0.0002(15) 0.0022(14) 0.0328(18) C181 0.059(2) 0.085(3) 0.056(2) 0.014(2) 0.0205(18) 0.059(2) C182 0.071(2) 0.0466(18) 0.0437(19) -0.0092(15) -0.0111(17) 0.0410(18) C183 0.059(3) 0.074(4) 0.0490(17) 0.001(2) -0.0046(18) 0.053(3) N2 0.022(4) 0.037(5) 0.030(4) -0.005(3) 0.000(3) 0.018(4) C21 0.027(5) 0.027(4) 0.033(3) -0.003(3) 0.003(3) 0.022(3) C22 0.031(5) 0.035(4) 0.035(4) 0.003(3) 0.008(4) 0.021(4) C23 0.013(5) 0.036(4) 0.048(5) -0.015(3) 0.018(4) 0.004(4) C24 0.029(5) 0.040(4) 0.036(5) -0.012(3) -0.001(4) 0.018(4) C25 0.031(5) 0.039(5) 0.033(4) -0.001(4) -0.002(4) 0.017(4) C26 0.029(5) 0.034(5) 0.029(3) 0.000(3) 0.003(4) 0.016(4) C231 0.087(4) 0.043(2) 0.101(4) 0.011(2) 0.062(3) 0.003(2) C251 0.043(8) 0.070(8) 0.023(4) -0.001(5) 0.009(5) 0.040(7) C27 0.035(4) 0.025(5) 0.044(5) -0.001(4) 0.000(4) 0.022(4) C28 0.037(5) 0.038(5) 0.044(6) -0.004(5) -0.005(5) 0.029(5) C281 0.043(7) 0.059(7) 0.064(6) -0.022(7) -0.011(6) 0.041(6) C282 0.032(6) 0.044(5) 0.057(9) 0.002(5) 0.003(6) 0.020(5) C283 0.059(3) 0.074(4) 0.0490(17) 0.001(2) -0.0046(18) 0.053(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 2.017(2) . ? Ta1 N1 2.017(2) 3 ? Ta1 N1 2.017(2) 2 ? Ta1 N2 2.020(9) 3 ? Ta1 N2 2.020(9) 2 ? Ta1 N2 2.020(9) . ? Ta1 Ta1 2.7954(3) 10 ? Ta1 H1 1.7290 . ? Ta1 H1A 1.6417 . ? N1 C11 1.441(4) . ? N1 C17 1.510(4) . ? C11 C12 1.379(5) . ? C11 C16 1.394(4) . ? C12 C13 1.399(5) . ? C12 H12 0.9500 . ? C13 C14 1.406(7) . ? C13 C131 1.527(7) . ? C14 C15 1.393(7) . ? C14 H14 0.9500 . ? C15 C16 1.381(5) . ? C15 C151 1.503(6) . ? C16 H16 0.9500 . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C17 C18 1.533(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C181 1.521(6) . ? C18 C182 1.529(8) . ? C18 C183 1.550(5) . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C183 H18G 0.9800 . ? C183 H18H 0.9800 . ? C183 H18I 0.9800 . ? N2 C21 1.446(12) . ? N2 C27 1.507(12) . ? C21 C22 1.384(13) . ? C21 C26 1.390(13) . ? C22 C23 1.410(13) . ? C22 H22 0.9500 . ? C23 C24 1.370(14) . ? C23 C231 1.526(16) . ? C24 C25 1.396(14) . ? C24 H24 0.9500 . ? C25 C26 1.395(13) . ? C25 C251 1.527(14) . ? C26 H26 0.9500 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C27 C28 1.527(16) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C281 1.509(17) . ? C28 C282 1.53(2) . ? C28 C283 1.545(16) . ? C281 H28A 0.9800 . ? C281 H28B 0.9800 . ? C281 H28C 0.9800 . ? C282 H28D 0.9800 . ? C282 H28E 0.9800 . ? C282 H28F 0.9800 . ? C283 H28G 0.9800 . ? C283 H28H 0.9800 . ? C283 H28I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ta1 N1 111.43(7) . 3 ? N1 Ta1 N1 111.43(7) . 2 ? N1 Ta1 N1 111.43(7) 3 2 ? N1 Ta1 N2 131.1(3) . 3 ? N1 Ta1 N2 25.2(3) 3 3 ? N1 Ta1 N2 87.7(3) 2 3 ? N1 Ta1 N2 87.7(3) . 2 ? N1 Ta1 N2 131.1(3) 3 2 ? N1 Ta1 N2 25.2(3) 2 2 ? N2 Ta1 N2 110.2(3) 3 2 ? N1 Ta1 N2 25.2(3) . . ? N1 Ta1 N2 87.7(3) 3 . ? N1 Ta1 N2 131.1(3) 2 . ? N2 Ta1 N2 110.2(3) 3 . ? N2 Ta1 N2 110.2(3) 2 . ? N1 Ta1 Ta1 107.43(7) . 10 ? N1 Ta1 Ta1 107.43(7) 3 10 ? N1 Ta1 Ta1 107.43(7) 2 10 ? N2 Ta1 Ta1 108.7(3) 3 10 ? N2 Ta1 Ta1 108.7(3) 2 10 ? N2 Ta1 Ta1 108.7(3) . 10 ? N2 Ta1 H1 75.0 3 . ? N2 Ta1 H1 145.9 2 . ? N2 Ta1 H1 98.4 . . ? Ta1 Ta1 H1 42.0 10 . ? N2 Ta1 H1A 135.4 3 . ? N2 Ta1 H1A 77.1 2 . ? N2 Ta1 H1A 107.6 . . ? Ta1 Ta1 H1A 34.8 10 . ? C11 N1 C17 113.0(2) . . ? C11 N1 Ta1 116.94(18) . . ? C17 N1 Ta1 126.96(19) . . ? C12 C11 C16 119.9(3) . . ? C12 C11 N1 121.3(3) . . ? C16 C11 N1 118.7(3) . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 118.3(4) . . ? C12 C13 C131 119.1(5) . . ? C14 C13 C131 122.4(4) . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C16 C15 C14 117.7(4) . . ? C16 C15 C151 120.9(5) . . ? C14 C15 C151 121.4(4) . . ? C15 C16 C11 121.7(4) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? N1 C17 C18 117.2(3) . . ? N1 C17 H17A 108.0 . . ? C18 C17 H17A 108.0 . . ? N1 C17 H17B 108.0 . . ? C18 C17 H17B 108.0 . . ? H17A C17 H17B 107.2 . . ? C181 C18 C182 108.1(4) . . ? C181 C18 C17 114.5(4) . . ? C182 C18 C17 110.7(3) . . ? C181 C18 C183 108.8(4) . . ? C182 C18 C183 108.3(4) . . ? C17 C18 C183 106.3(4) . . ? C21 N2 C27 110.7(9) . . ? C21 N2 Ta1 117.1(6) . . ? C27 N2 Ta1 127.5(7) . . ? C22 C21 C26 119.8(10) . . ? C22 C21 N2 121.5(10) . . ? C26 C21 N2 118.7(10) . . ? C21 C22 C23 120.5(10) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 118.4(10) . . ? C24 C23 C231 125.3(14) . . ? C22 C23 C231 116.0(14) . . ? C23 C24 C25 122.4(11) . . ? C23 C24 H24 118.8 . . ? C25 C24 H24 118.8 . . ? C26 C25 C24 118.3(10) . . ? C26 C25 C251 118.3(11) . . ? C24 C25 C251 123.4(11) . . ? C21 C26 C25 120.6(11) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? N2 C27 C28 117.4(12) . . ? N2 C27 H27A 108.0 . . ? C28 C27 H27A 108.0 . . ? N2 C27 H27B 108.0 . . ? C28 C27 H27B 108.0 . . ? H27A C27 H27B 107.2 . . ? C281 C28 C27 114.7(16) . . ? C281 C28 C282 111.2(15) . . ? C27 C28 C282 111.5(13) . . ? C281 C28 C283 107.9(17) . . ? C27 C28 C283 107.2(17) . . ? C282 C28 C283 103.7(17) . . ? C28 C281 H28A 109.5 . . ? C28 C281 H28B 109.5 . . ? H28A C281 H28B 109.5 . . ? C28 C281 H28C 109.5 . . ? H28A C281 H28C 109.5 . . ? H28B C281 H28C 109.5 . . ? C28 C282 H28D 109.5 . . ? C28 C282 H28E 109.5 . . ? H28D C282 H28E 109.5 . . ? C28 C282 H28F 109.5 . . ? H28D C282 H28F 109.5 . . ? H28E C282 H28F 109.5 . . ? C28 C283 H28G 109.5 . . ? C28 C283 H28H 109.5 . . ? H28G C283 H28H 109.5 . . ? C28 C283 H28I 109.5 . . ? H28G C283 H28I 109.5 . . ? H28H C283 H28I 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.277 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.090 # Attachment '- 09187p_e.cif' data_09187p_e _database_code_depnum_ccdc_archive 'CCDC 852394' #TrackingRef '- 09187p_e.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ar(CH2tBu)N)3TaCl2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H61 Cl3.25 N3 Ta' _chemical_formula_weight 874.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.3937(19) _cell_length_b 13.1868(11) _cell_length_c 29.573(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.0310(10) _cell_angle_gamma 90.00 _cell_volume 8304.0(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 31.02 _exptl_crystal_description shard _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3578 _exptl_absorpt_coefficient_mu 2.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3633 _exptl_absorpt_correction_T_max 0.5096 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 103293 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 29.57 _reflns_number_total 11619 _reflns_number_gt 10572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2009)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. After location and refinement of atoms for (Ar[CMe3CH2]N)3TaCl2, attempts to refine the remaining peaks of residual electron density as CH2Cl2 and CHCl3 solvate molecules were unsuccessful. The data were corrected for disordered electron density through use of the SQUEEZE procedure, as implemented in PLATON. A total solvent-accessible void volume of 588 3 with a total electron count of 192 (consistent with two molecules of CHCl3 and two molecules of CH2Cl2 per asymmetric unit) was found in the unit cell. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 18 1 ' ' 2 0.000 0.076 0.250 147 48 ' ' 3 0.500 0.000 0.500 18 1 ' ' 4 0.000 -0.076 0.750 147 48 ' ' 5 0.500 0.424 0.750 147 48 ' ' 6 0.500 0.576 0.250 147 48 ' ' 7 0.000 0.500 0.000 18 1 ' ' 8 1.000 0.500 0.500 18 1 ' ' _platon_squeeze_details ; The unit cell contains 2 molecules of chloroform and 2 molecules of methylene chloride which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/ PLATON. ; _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^)+(0.0318P)^2^+66.5885P] 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 11619 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 0.362754(6) 0.221840(9) 0.119662(4) 0.01478(4) Uani 1 1 d . . . Cl1 Cl 0.39517(4) 0.23591(7) 0.20630(3) 0.02552(16) Uani 1 1 d . . . N1 N 0.44282(14) 0.1527(2) 0.12729(12) 0.0266(6) Uani 1 1 d . . . Cl2 Cl 0.33193(4) 0.20079(6) 0.03384(3) 0.02181(15) Uani 1 1 d . . . N2 N 0.28826(14) 0.1431(2) 0.11896(10) 0.0217(6) Uani 1 1 d . . . N3 N 0.35553(14) 0.3685(2) 0.11414(12) 0.0274(7) Uani 1 1 d . . . C11 C 0.49592(17) 0.2037(3) 0.11953(13) 0.0246(7) Uani 1 1 d . . . C12 C 0.54518(17) 0.2395(3) 0.15807(13) 0.0256(7) Uani 1 1 d . . . H12 H 0.5436 0.2308 0.1896 0.031 Uiso 1 1 calc R . . C13 C 0.59699(17) 0.2882(3) 0.15024(14) 0.0265(7) Uani 1 1 d . . . C14 C 0.59874(17) 0.2979(3) 0.10349(13) 0.0246(7) Uani 1 1 d . . . H14 H 0.6347 0.3271 0.0981 0.030 Uiso 1 1 calc R . . C15 C 0.54919(18) 0.2661(3) 0.06482(13) 0.0274(7) Uani 1 1 d . . . C16 C 0.49772(18) 0.2181(3) 0.07317(14) 0.0286(7) Uani 1 1 d . . . H16 H 0.4638 0.1951 0.0471 0.034 Uiso 1 1 calc R . . C17 C 0.4595(2) 0.0635(4) 0.15994(17) 0.0385(9) Uani 1 1 d . . . H17A H 0.4219 0.0428 0.1684 0.046 Uiso 1 1 calc R . . H17B H 0.4920 0.0847 0.1896 0.046 Uiso 1 1 calc R . . C18 C 0.48453(18) -0.0303(3) 0.13905(15) 0.0287(8) Uani 1 1 d . . . C21 C 0.29065(16) 0.0357(3) 0.12783(13) 0.0220(6) Uani 1 1 d . . . C22 C 0.27114(17) -0.0317(3) 0.08984(12) 0.0237(7) Uani 1 1 d . . . H22 H 0.2563 -0.0065 0.0582 0.028 Uiso 1 1 calc R . . C23 C 0.27320(18) -0.1359(3) 0.09784(13) 0.0264(7) Uani 1 1 d . . . C24 C 0.29397(16) -0.1709(3) 0.14495(13) 0.0236(7) Uani 1 1 d . . . H24 H 0.2934 -0.2417 0.1507 0.028 Uiso 1 1 calc R . . C25 C 0.31528(17) -0.1059(3) 0.18340(13) 0.0246(7) Uani 1 1 d . . . C26 C 0.31275(16) -0.0007(3) 0.17465(13) 0.0240(7) Uani 1 1 d . . . H26 H 0.3260 0.0456 0.2005 0.029 Uiso 1 1 calc R . . C27 C 0.22668(15) 0.1841(3) 0.09052(12) 0.0194(6) Uani 1 1 d . . . H27A H 0.2111 0.1430 0.0612 0.023 Uiso 1 1 calc R . . H27B H 0.2331 0.2540 0.0808 0.023 Uiso 1 1 calc R . . C28 C 0.17526(17) 0.1866(3) 0.11509(13) 0.0250(7) Uani 1 1 d . . . C31 C 0.30253(17) 0.4276(3) 0.11764(13) 0.0244(7) Uani 1 1 d . . . C32 C 0.25163(18) 0.4463(3) 0.07748(14) 0.0279(7) Uani 1 1 d . . . H32 H 0.2506 0.4184 0.0476 0.033 Uiso 1 1 calc R . . C33 C 0.20138(18) 0.5069(3) 0.08129(15) 0.0284(8) Uani 1 1 d . . . C34 C 0.20492(18) 0.5480(3) 0.12572(15) 0.0284(8) Uani 1 1 d . . . H34 H 0.1724 0.5919 0.1282 0.034 Uiso 1 1 calc R . . C35 C 0.2542(2) 0.5266(3) 0.16607(15) 0.0307(8) Uani 1 1 d . . . C36 C 0.30373(18) 0.4669(3) 0.16174(14) 0.0275(7) Uani 1 1 d . . . H36 H 0.3385 0.4529 0.1890 0.033 Uiso 1 1 calc R . . C37 C 0.41457(16) 0.4263(3) 0.12410(14) 0.0262(7) Uani 1 1 d . . . H37A H 0.4494 0.3773 0.1283 0.031 Uiso 1 1 calc R . . H37B H 0.4217 0.4621 0.1547 0.031 Uiso 1 1 calc R . . C38 C 0.41838(19) 0.5049(3) 0.08632(15) 0.0317(8) Uani 1 1 d . . . C131 C 0.65098(19) 0.3266(4) 0.19115(15) 0.0352(9) Uani 1 1 d . . . H13A H 0.6452 0.3990 0.1959 0.053 Uiso 1 1 calc R . . H13B H 0.6905 0.3163 0.1840 0.053 Uiso 1 1 calc R . . H13C H 0.6523 0.2894 0.2201 0.053 Uiso 1 1 calc R . . C151 C 0.5506(2) 0.2796(4) 0.01466(15) 0.0407(10) Uani 1 1 d . . . H15A H 0.5279 0.3417 0.0012 0.061 Uiso 1 1 calc R . . H15B H 0.5305 0.2212 -0.0046 0.061 Uiso 1 1 calc R . . H15C H 0.5942 0.2848 0.0147 0.061 Uiso 1 1 calc R . . C181 C 0.4417(3) -0.0538(5) 0.0890(2) 0.0648(16) Uani 1 1 d . . . H18A H 0.4550 -0.1173 0.0779 0.097 Uiso 1 1 calc R . . H18B H 0.4441 0.0015 0.0675 0.097 Uiso 1 1 calc R . . H18C H 0.3983 -0.0607 0.0895 0.097 Uiso 1 1 calc R . . C182 C 0.4837(3) -0.1186(4) 0.1715(3) 0.0659(17) Uani 1 1 d . . . H18D H 0.4403 -0.1334 0.1701 0.099 Uiso 1 1 calc R . . H18E H 0.5083 -0.1014 0.2042 0.099 Uiso 1 1 calc R . . H18F H 0.5020 -0.1784 0.1611 0.099 Uiso 1 1 calc R . . C183 C 0.5520(2) -0.0159(3) 0.13806(18) 0.0391(10) Uani 1 1 d . . . H18G H 0.5717 -0.0823 0.1384 0.059 Uiso 1 1 calc R . . H18H H 0.5759 0.0231 0.1660 0.059 Uiso 1 1 calc R . . H18I H 0.5515 0.0208 0.1091 0.059 Uiso 1 1 calc R . . C231 C 0.2521(2) -0.2073(3) 0.05659(15) 0.0364(9) Uani 1 1 d . . . H23A H 0.2200 -0.1743 0.0304 0.055 Uiso 1 1 calc R . . H23B H 0.2344 -0.2685 0.0663 0.055 Uiso 1 1 calc R . . H23C H 0.2880 -0.2259 0.0461 0.055 Uiso 1 1 calc R . . C251 C 0.3363(2) -0.1449(3) 0.23371(14) 0.0339(9) Uani 1 1 d . . . H25A H 0.2997 -0.1522 0.2450 0.051 Uiso 1 1 calc R . . H25B H 0.3660 -0.0970 0.2541 0.051 Uiso 1 1 calc R . . H25C H 0.3567 -0.2110 0.2347 0.051 Uiso 1 1 calc R . . C281 C 0.15307(19) 0.0817(3) 0.12380(18) 0.0370(10) Uani 1 1 d . . . H28A H 0.1863 0.0477 0.1488 0.055 Uiso 1 1 calc R . . H28B H 0.1432 0.0419 0.0944 0.055 Uiso 1 1 calc R . . H28C H 0.1154 0.0879 0.1338 0.055 Uiso 1 1 calc R . . C282 C 0.11864(19) 0.2432(3) 0.08023(16) 0.0341(9) Uani 1 1 d . . . H28D H 0.1040 0.2056 0.0502 0.051 Uiso 1 1 calc R . . H28E H 0.1317 0.3114 0.0742 0.051 Uiso 1 1 calc R . . H28F H 0.0845 0.2482 0.0943 0.051 Uiso 1 1 calc R . . C283 C 0.1978(2) 0.2470(4) 0.16105(16) 0.0382(10) Uani 1 1 d . . . H28G H 0.1636 0.2529 0.1751 0.057 Uiso 1 1 calc R . . H28H H 0.2107 0.3149 0.1543 0.057 Uiso 1 1 calc R . . H28I H 0.2335 0.2123 0.1834 0.057 Uiso 1 1 calc R . . C331 C 0.1473(2) 0.5316(3) 0.03766(17) 0.0388(10) Uani 1 1 d . . . H33A H 0.1617 0.5773 0.0171 0.058 Uiso 1 1 calc R . . H33B H 0.1138 0.5645 0.0472 0.058 Uiso 1 1 calc R . . H33C H 0.1312 0.4689 0.0204 0.058 Uiso 1 1 calc R . . C351 C 0.2560(2) 0.5675(3) 0.21449(16) 0.0387(10) Uani 1 1 d . . . H35A H 0.2910 0.6152 0.2258 0.058 Uiso 1 1 calc R . . H35B H 0.2616 0.5112 0.2371 0.058 Uiso 1 1 calc R . . H35C H 0.2164 0.6025 0.2119 0.058 Uiso 1 1 calc R . . C381 C 0.3826(2) 0.6024(3) 0.08943(19) 0.0408(10) Uani 1 1 d . . . H38A H 0.3373 0.5900 0.0766 0.061 Uiso 1 1 calc R . . H38B H 0.3946 0.6561 0.0710 0.061 Uiso 1 1 calc R . . H38C H 0.3930 0.6236 0.1227 0.061 Uiso 1 1 calc R . . C382 C 0.3946(2) 0.4594(4) 0.03573(15) 0.0396(10) Uani 1 1 d . . . H38D H 0.4165 0.3955 0.0349 0.059 Uiso 1 1 calc R . . H38E H 0.4028 0.5072 0.0130 0.059 Uiso 1 1 calc R . . H38F H 0.3493 0.4467 0.0273 0.059 Uiso 1 1 calc R . . C383 C 0.48767(19) 0.5323(3) 0.09753(16) 0.0365(9) Uani 1 1 d . . . H38G H 0.5036 0.5583 0.1301 0.055 Uiso 1 1 calc R . . H38H H 0.4924 0.5844 0.0752 0.055 Uiso 1 1 calc R . . H38I H 0.5115 0.4718 0.0944 0.055 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 0.01404(6) 0.01517(6) 0.01526(6) 0.00173(4) 0.00472(4) 0.00057(4) Cl1 0.0303(4) 0.0287(4) 0.0152(3) -0.0003(3) 0.0036(3) 0.0010(3) N1 0.0210(14) 0.0279(15) 0.0304(16) 0.0064(12) 0.0071(12) 0.0010(12) Cl2 0.0222(4) 0.0273(4) 0.0151(3) 0.0001(3) 0.0046(3) 0.0006(3) N2 0.0212(13) 0.0212(13) 0.0222(14) 0.0003(11) 0.0062(11) -0.0002(11) N3 0.0230(15) 0.0184(13) 0.0404(18) -0.0002(12) 0.0093(13) -0.0023(11) C11 0.0224(16) 0.0241(16) 0.0282(18) 0.0038(13) 0.0092(14) 0.0033(13) C12 0.0244(17) 0.0273(17) 0.0256(17) 0.0023(14) 0.0086(14) 0.0006(13) C13 0.0205(16) 0.0309(18) 0.0280(18) 0.0009(14) 0.0074(14) 0.0015(14) C14 0.0215(16) 0.0245(16) 0.0312(18) 0.0082(14) 0.0131(14) 0.0020(13) C15 0.0279(18) 0.0321(19) 0.0246(17) 0.0063(14) 0.0118(14) 0.0034(14) C16 0.0263(18) 0.0323(19) 0.0256(17) 0.0045(15) 0.0057(14) 0.0018(15) C17 0.035(2) 0.043(2) 0.038(2) 0.0065(19) 0.0128(18) 0.0047(18) C18 0.0241(17) 0.0275(18) 0.035(2) 0.0029(15) 0.0100(15) 0.0072(14) C21 0.0194(15) 0.0222(15) 0.0255(17) 0.0018(13) 0.0084(13) -0.0013(12) C22 0.0254(16) 0.0267(17) 0.0192(15) -0.0009(13) 0.0073(13) 0.0004(13) C23 0.0292(18) 0.0242(17) 0.0261(17) -0.0039(13) 0.0089(14) 0.0001(14) C24 0.0218(16) 0.0177(15) 0.0317(18) 0.0034(13) 0.0089(14) 0.0000(12) C25 0.0232(16) 0.0268(17) 0.0235(17) 0.0048(13) 0.0068(13) -0.0029(13) C26 0.0233(16) 0.0262(17) 0.0225(16) -0.0003(13) 0.0069(13) -0.0022(13) C27 0.0194(15) 0.0200(14) 0.0194(15) 0.0001(12) 0.0069(12) -0.0003(12) C28 0.0212(16) 0.0283(17) 0.0269(17) -0.0040(14) 0.0097(13) -0.0055(13) C31 0.0251(17) 0.0178(15) 0.0302(18) 0.0000(13) 0.0086(14) -0.0022(12) C32 0.0300(18) 0.0233(17) 0.0279(18) -0.0006(14) 0.0056(15) -0.0010(14) C33 0.0262(17) 0.0197(16) 0.036(2) 0.0028(14) 0.0048(15) 0.0015(13) C34 0.0270(18) 0.0170(15) 0.044(2) -0.0013(14) 0.0143(16) 0.0002(13) C35 0.037(2) 0.0236(17) 0.034(2) -0.0048(15) 0.0147(17) 0.0006(15) C36 0.0312(19) 0.0231(16) 0.0272(18) -0.0025(14) 0.0078(15) -0.0049(14) C37 0.0197(16) 0.0225(16) 0.0337(19) 0.0046(14) 0.0045(14) -0.0027(13) C38 0.0309(19) 0.0216(17) 0.040(2) 0.0085(15) 0.0075(16) -0.0043(14) C131 0.0282(19) 0.043(2) 0.032(2) 0.0013(17) 0.0054(16) -0.0121(17) C151 0.042(2) 0.057(3) 0.0264(19) 0.0108(19) 0.0149(18) -0.001(2) C181 0.057(3) 0.069(4) 0.067(4) -0.023(3) 0.016(3) 0.000(3) C182 0.049(3) 0.047(3) 0.104(5) 0.022(3) 0.026(3) 0.014(2) C183 0.031(2) 0.035(2) 0.059(3) 0.012(2) 0.024(2) 0.0107(17) C231 0.046(2) 0.0288(19) 0.033(2) -0.0086(16) 0.0099(18) -0.0004(17) C251 0.037(2) 0.031(2) 0.0283(19) 0.0102(15) 0.0026(16) -0.0013(16) C281 0.0250(18) 0.0296(19) 0.060(3) 0.0100(19) 0.0188(19) 0.0001(15) C282 0.0263(19) 0.035(2) 0.041(2) 0.0021(17) 0.0113(17) 0.0050(16) C283 0.035(2) 0.050(2) 0.035(2) -0.0128(19) 0.0183(18) -0.0070(19) C331 0.028(2) 0.037(2) 0.044(2) 0.0057(19) 0.0016(17) 0.0079(17) C351 0.048(3) 0.034(2) 0.041(2) -0.0114(18) 0.025(2) 0.0005(18) C381 0.036(2) 0.0240(18) 0.063(3) 0.0117(19) 0.016(2) 0.0001(16) C382 0.047(3) 0.038(2) 0.031(2) 0.0070(17) 0.0091(19) -0.0090(19) C383 0.030(2) 0.039(2) 0.039(2) 0.0040(18) 0.0093(17) -0.0120(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N3 1.943(3) . ? Ta1 N2 1.960(3) . ? Ta1 N1 1.961(3) . ? Ta1 Cl2 2.4311(8) . ? Ta1 Cl1 2.4444(8) . ? N1 C11 1.445(5) . ? N1 C17 1.494(5) . ? N2 C21 1.438(4) . ? N2 C27 1.478(4) . ? N3 C31 1.450(5) . ? N3 C37 1.475(4) . ? C11 C16 1.397(5) . ? C11 C12 1.400(5) . ? C12 C13 1.407(5) . ? C13 C14 1.401(5) . ? C13 C131 1.509(5) . ? C14 C15 1.389(5) . ? C15 C16 1.402(5) . ? C15 C151 1.504(5) . ? C17 C18 1.562(6) . ? C18 C182 1.512(7) . ? C18 C181 1.525(7) . ? C18 C183 1.531(5) . ? C21 C22 1.393(5) . ? C21 C26 1.403(5) . ? C22 C23 1.392(5) . ? C23 C24 1.403(5) . ? C23 C231 1.497(5) . ? C24 C25 1.386(5) . ? C25 C26 1.409(5) . ? C25 C251 1.505(5) . ? C27 C28 1.540(5) . ? C28 C281 1.519(5) . ? C28 C283 1.521(5) . ? C28 C282 1.555(5) . ? C31 C32 1.390(5) . ? C31 C36 1.396(5) . ? C32 C33 1.413(5) . ? C33 C34 1.401(6) . ? C33 C331 1.507(5) . ? C34 C35 1.381(6) . ? C35 C36 1.397(5) . ? C35 C351 1.519(6) . ? C37 C38 1.546(5) . ? C38 C383 1.526(5) . ? C38 C381 1.533(6) . ? C38 C382 1.546(6) . ? 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 N3 Ta1 N2 118.56(12) . . ? N3 Ta1 N1 121.43(13) . . ? N2 Ta1 N1 120.00(13) . . ? N3 Ta1 Cl2 92.09(10) . . ? N2 Ta1 Cl2 87.86(9) . . ? N1 Ta1 Cl2 91.21(10) . . ? N3 Ta1 Cl1 90.15(10) . . ? N2 Ta1 Cl1 91.55(9) . . ? N1 Ta1 Cl1 87.16(10) . . ? Cl2 Ta1 Cl1 177.70(3) . . ? C11 N1 C17 114.5(3) . . ? C11 N1 Ta1 122.2(2) . . ? C17 N1 Ta1 118.5(3) . . ? C21 N2 C27 116.1(3) . . ? C21 N2 Ta1 122.4(2) . . ? C27 N2 Ta1 117.0(2) . . ? C31 N3 C37 114.3(3) . . ? C31 N3 Ta1 125.3(2) . . ? C37 N3 Ta1 116.8(2) . . ? C16 C11 C12 119.9(3) . . ? C16 C11 N1 119.6(3) . . ? C12 C11 N1 120.5(3) . . ? C11 C12 C13 120.1(3) . . ? C14 C13 C12 118.7(3) . . ? C14 C13 C131 120.0(3) . . ? C12 C13 C131 121.2(3) . . ? C15 C14 C13 121.7(3) . . ? C14 C15 C16 118.8(3) . . ? C14 C15 C151 121.4(4) . . ? C16 C15 C151 119.7(4) . . ? C11 C16 C15 120.6(4) . . ? N1 C17 C18 114.6(4) . . ? C182 C18 C181 109.3(5) . . ? C182 C18 C183 108.2(4) . . ? C181 C18 C183 109.6(4) . . ? C182 C18 C17 106.5(4) . . ? C181 C18 C17 110.5(4) . . ? C183 C18 C17 112.7(4) . . ? C22 C21 C26 120.3(3) . . ? C22 C21 N2 119.8(3) . . ? C26 C21 N2 119.9(3) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 118.5(3) . . ? C22 C23 C231 119.8(3) . . ? C24 C23 C231 121.7(3) . . ? C25 C24 C23 122.4(3) . . ? C24 C25 C26 118.3(3) . . ? C24 C25 C251 121.5(3) . . ? C26 C25 C251 120.1(3) . . ? C21 C26 C25 120.0(3) . . ? N2 C27 C28 116.2(3) . . ? C281 C28 C283 111.2(4) . . ? C281 C28 C27 113.1(3) . . ? C283 C28 C27 110.1(3) . . ? C281 C28 C282 107.9(3) . . ? C283 C28 C282 108.5(3) . . ? C27 C28 C282 105.8(3) . . ? C32 C31 C36 120.4(4) . . ? C32 C31 N3 120.5(3) . . ? C36 C31 N3 119.1(3) . . ? C31 C32 C33 119.7(4) . . ? C34 C33 C32 118.6(3) . . ? C34 C33 C331 121.1(4) . . ? C32 C33 C331 120.2(4) . . ? C35 C34 C33 122.0(3) . . ? C34 C35 C36 118.7(4) . . ? C34 C35 C351 121.5(4) . . ? C36 C35 C351 119.8(4) . . ? C31 C36 C35 120.6(4) . . ? N3 C37 C38 116.7(3) . . ? C383 C38 C381 107.7(3) . . ? C383 C38 C382 108.9(4) . . ? C381 C38 C382 110.7(4) . . ? C383 C38 C37 106.4(3) . . ? C381 C38 C37 111.9(4) . . ? C382 C38 C37 111.1(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.234 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.128 # Attachment '- 09212_mr_e.cif' data_09212_mr_e _database_code_depnum_ccdc_archive 'CCDC 852395' #TrackingRef '- 09212_mr_e.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ar(tBuCH2)N)2(tBuC(H)NAr)TaCl _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H59 Cl N3 Ta' _chemical_formula_weight 786.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 11.9313(16) _cell_length_b 35.046(5) _cell_length_c 9.5018(12) _cell_angle_alpha 90.00 _cell_angle_beta 106.182(2) _cell_angle_gamma 90.00 _cell_volume 3815.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9819 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.54 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 2.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6635 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 85345 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 29.57 _reflns_number_total 10700 _reflns_number_gt 8801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _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^ > 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^)+(0.0186P)^2^+8.8427P] 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 10700 _refine_ls_number_parameters 415 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Ta1 Ta 0.800244(11) -0.111422(3) 0.937178(14) 0.01370(4) Uani 1 1 d . . . Cl1 Cl 0.82960(7) -0.05763(2) 1.09721(9) 0.02073(16) Uani 1 1 d . . . N1 N 0.6955(2) -0.15630(7) 0.9050(3) 0.0158(5) Uani 1 1 d . . . N2 N 0.9418(2) -0.14325(7) 1.0077(3) 0.0154(5) Uani 1 1 d . . . N3 N 0.7770(2) -0.09210(8) 0.7380(3) 0.0162(5) Uani 1 1 d . . . C11 C 0.6492(3) -0.18118(9) 0.7871(4) 0.0164(6) Uani 1 1 d . . . C12 C 0.7218(3) -0.19272(9) 0.7002(4) 0.0174(6) Uani 1 1 d . . . H12 H 0.8013 -0.1850 0.7264 0.021 Uiso 1 1 calc R . . C13 C 0.6779(3) -0.21535(9) 0.5765(4) 0.0222(7) Uani 1 1 d . . . C14 C 0.5619(3) -0.22705(9) 0.5419(4) 0.0247(8) Uani 1 1 d . . . H14 H 0.5314 -0.2422 0.4570 0.030 Uiso 1 1 calc R . . C15 C 0.4899(3) -0.21724(10) 0.6277(4) 0.0225(7) Uani 1 1 d . . . C16 C 0.5342(3) -0.19384(9) 0.7509(4) 0.0193(7) Uani 1 1 d . . . H16 H 0.4852 -0.1866 0.8099 0.023 Uiso 1 1 calc R . . C17 C 0.6346(3) -0.12859(9) 0.9691(4) 0.0169(6) Uani 1 1 d D . . H17 H 0.566(2) -0.1173(10) 0.901(3) 0.020 Uiso 1 1 d D . . C18 C 0.6096(3) -0.13551(10) 1.1167(4) 0.0194(7) Uani 1 1 d . . . C21 C 1.0437(3) -0.12636(10) 0.9786(4) 0.0183(7) Uani 1 1 d . . . C22 C 1.0946(3) -0.09388(10) 1.0544(4) 0.0215(7) Uani 1 1 d . . . H22 H 1.0626 -0.0829 1.1261 0.026 Uiso 1 1 calc R . . C23 C 1.1930(3) -0.07729(10) 1.0252(5) 0.0279(8) Uani 1 1 d . . . C24 C 1.2384(3) -0.09366(11) 0.9224(5) 0.0286(8) Uani 1 1 d . . . H24 H 1.3050 -0.0824 0.9030 0.034 Uiso 1 1 calc R . . C25 C 1.1899(3) -0.12642(12) 0.8449(4) 0.0270(8) Uani 1 1 d . . . C26 C 1.0922(3) -0.14239(10) 0.8743(4) 0.0217(7) Uani 1 1 d . . . H26 H 1.0578 -0.1646 0.8226 0.026 Uiso 1 1 calc R . . C27 C 0.9554(3) -0.18328(9) 1.0572(4) 0.0190(7) Uani 1 1 d . . . H27A H 0.9728 -0.1987 0.9784 0.023 Uiso 1 1 calc R . . H27B H 0.8791 -0.1921 1.0671 0.023 Uiso 1 1 calc R . . C28 C 1.0492(3) -0.19271(10) 1.2023(4) 0.0238(7) Uani 1 1 d . . . C31 C 0.6553(3) -0.08205(9) 0.6807(4) 0.0174(6) Uani 1 1 d . . . C32 C 0.6122(3) -0.05100(9) 0.7417(4) 0.0190(7) Uani 1 1 d . . . H32 H 0.6646 -0.0354 0.8121 0.023 Uiso 1 1 calc R . . C33 C 0.4928(3) -0.04249(11) 0.7006(4) 0.0254(8) Uani 1 1 d . . . C34 C 0.4181(3) -0.06513(11) 0.5958(4) 0.0242(7) Uani 1 1 d . . . H34 H 0.3371 -0.0594 0.5660 0.029 Uiso 1 1 calc R . . C35 C 0.4595(3) -0.09633(10) 0.5329(4) 0.0202(7) Uani 1 1 d . . . C36 C 0.5785(3) -0.10475(9) 0.5767(4) 0.0184(7) Uani 1 1 d . . . H36 H 0.6073 -0.1260 0.5355 0.022 Uiso 1 1 calc R . . C37 C 0.8497(3) -0.09448(10) 0.6353(4) 0.0198(7) Uani 1 1 d . . . H37A H 0.8033 -0.1071 0.5444 0.024 Uiso 1 1 calc R . . H37B H 0.9174 -0.1111 0.6794 0.024 Uiso 1 1 calc R . . C38 C 0.8958(3) -0.05637(10) 0.5933(4) 0.0212(7) Uani 1 1 d . . . C131 C 0.7540(4) -0.22757(11) 0.4822(4) 0.0297(9) Uani 1 1 d . . . H13A H 0.8230 -0.2111 0.5017 0.045 Uiso 1 1 calc R . . H13B H 0.7100 -0.2255 0.3787 0.045 Uiso 1 1 calc R . . H13C H 0.7786 -0.2541 0.5047 0.045 Uiso 1 1 calc R . . C151 C 0.3659(4) -0.23168(12) 0.5925(5) 0.0351(10) Uani 1 1 d . . . H15A H 0.3501 -0.2410 0.6823 0.053 Uiso 1 1 calc R . . H15B H 0.3552 -0.2525 0.5212 0.053 Uiso 1 1 calc R . . H15C H 0.3119 -0.2109 0.5512 0.053 Uiso 1 1 calc R . . C181 C 0.5157(3) -0.16658(11) 1.1056(4) 0.0250(8) Uani 1 1 d . . . H18A H 0.4442 -0.1593 1.0309 0.038 Uiso 1 1 calc R . . H18B H 0.4992 -0.1693 1.2005 0.038 Uiso 1 1 calc R . . H18C H 0.5442 -0.1909 1.0784 0.038 Uiso 1 1 calc R . . C182 C 0.7212(3) -0.14782(11) 1.2328(4) 0.0255(8) Uani 1 1 d . . . H18D H 0.7493 -0.1719 1.2031 0.038 Uiso 1 1 calc R . . H18E H 0.7042 -0.1512 1.3272 0.038 Uiso 1 1 calc R . . H18F H 0.7812 -0.1281 1.2424 0.038 Uiso 1 1 calc R . . C183 C 0.5655(3) -0.09688(9) 1.1621(4) 0.0230(7) Uani 1 1 d . . . H18G H 0.6252 -0.0772 1.1690 0.034 Uiso 1 1 calc R . . H18H H 0.5498 -0.0998 1.2575 0.034 Uiso 1 1 calc R . . H18I H 0.4936 -0.0893 1.0885 0.034 Uiso 1 1 calc R . . C231 C 1.2462(4) -0.04157(11) 1.1063(6) 0.0404(11) Uani 1 1 d . . . H23A H 1.3308 -0.0418 1.1209 0.061 Uiso 1 1 calc R . . H23B H 1.2297 -0.0407 1.2017 0.061 Uiso 1 1 calc R . . H23C H 1.2124 -0.0191 1.0487 0.061 Uiso 1 1 calc R . . C251 C 1.2405(4) -0.14353(14) 0.7312(5) 0.0390(10) Uani 1 1 d . . . H25A H 1.3207 -0.1345 0.7468 0.059 Uiso 1 1 calc R . . H25B H 1.1934 -0.1359 0.6334 0.059 Uiso 1 1 calc R . . H25C H 1.2404 -0.1714 0.7392 0.059 Uiso 1 1 calc R . . C281 C 1.0247(4) -0.23369(12) 1.2420(5) 0.0394(11) Uani 1 1 d . . . H28A H 1.0814 -0.2410 1.3343 0.059 Uiso 1 1 calc R . . H28B H 1.0314 -0.2511 1.1639 0.059 Uiso 1 1 calc R . . H28C H 0.9456 -0.2352 1.2533 0.059 Uiso 1 1 calc R . . C282 C 1.1735(3) -0.19122(11) 1.1854(5) 0.0296(9) Uani 1 1 d . . . H28D H 1.2286 -0.2012 1.2744 0.044 Uiso 1 1 calc R . . H28E H 1.1936 -0.1648 1.1697 0.044 Uiso 1 1 calc R . . H28F H 1.1774 -0.2068 1.1012 0.044 Uiso 1 1 calc R . . C283 C 1.0398(4) -0.16587(12) 1.3254(4) 0.0299(8) Uani 1 1 d . . . H28G H 0.9624 -0.1685 1.3412 0.045 Uiso 1 1 calc R . . H28H H 1.0511 -0.1395 1.2981 0.045 Uiso 1 1 calc R . . H28I H 1.0998 -0.1725 1.4157 0.045 Uiso 1 1 calc R . . C331 C 0.4474(4) -0.00904(12) 0.7692(5) 0.0391(11) Uani 1 1 d . . . H33A H 0.4873 -0.0082 0.8743 0.059 Uiso 1 1 calc R . . H33B H 0.3633 -0.0120 0.7549 0.059 Uiso 1 1 calc R . . H33C H 0.4622 0.0147 0.7229 0.059 Uiso 1 1 calc R . . C351 C 0.3753(3) -0.12152(10) 0.4215(4) 0.0249(8) Uani 1 1 d . . . H35A H 0.2967 -0.1189 0.4335 0.037 Uiso 1 1 calc R . . H35B H 0.4004 -0.1482 0.4370 0.037 Uiso 1 1 calc R . . H35C H 0.3745 -0.1137 0.3222 0.037 Uiso 1 1 calc R . . C381 C 0.7971(3) -0.03233(11) 0.4955(4) 0.0279(8) Uani 1 1 d . . . H38A H 0.7452 -0.0236 0.5526 0.042 Uiso 1 1 calc R . . H38B H 0.7527 -0.0478 0.4129 0.042 Uiso 1 1 calc R . . H38C H 0.8304 -0.0102 0.4584 0.042 Uiso 1 1 calc R . . C382 C 0.9586(4) -0.03398(11) 0.7315(4) 0.0300(9) Uani 1 1 d . . . H38D H 1.0220 -0.0495 0.7923 0.045 Uiso 1 1 calc R . . H38E H 0.9031 -0.0277 0.7871 0.045 Uiso 1 1 calc R . . H38F H 0.9908 -0.0104 0.7034 0.045 Uiso 1 1 calc R . . C383 C 0.9836(4) -0.06672(12) 0.5071(5) 0.0325(9) Uani 1 1 d . . . H38G H 1.0129 -0.0433 0.4734 0.049 Uiso 1 1 calc R . . H38H H 0.9447 -0.0825 0.4223 0.049 Uiso 1 1 calc R . . H38I H 1.0489 -0.0810 0.5707 0.049 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 0.01479(6) 0.01293(6) 0.01258(6) -0.00120(5) 0.00248(4) -0.00043(5) Cl1 0.0240(4) 0.0175(3) 0.0189(4) -0.0051(3) 0.0032(3) -0.0007(3) N1 0.0172(14) 0.0141(12) 0.0163(13) -0.0013(10) 0.0051(11) 0.0006(10) N2 0.0189(14) 0.0114(12) 0.0157(13) -0.0007(10) 0.0047(11) -0.0011(10) N3 0.0157(14) 0.0165(13) 0.0157(13) -0.0012(10) 0.0031(11) -0.0002(10) C11 0.0210(17) 0.0138(14) 0.0138(15) 0.0016(12) 0.0038(13) -0.0001(12) C12 0.0227(17) 0.0142(14) 0.0158(16) -0.0015(12) 0.0062(13) -0.0022(12) C13 0.036(2) 0.0124(14) 0.0177(17) 0.0016(12) 0.0066(15) 0.0037(13) C14 0.036(2) 0.0138(15) 0.0199(17) -0.0033(13) 0.0001(15) -0.0019(14) C15 0.0259(19) 0.0168(15) 0.0210(17) 0.0001(13) 0.0000(14) -0.0044(13) C16 0.0226(18) 0.0166(15) 0.0177(16) 0.0008(12) 0.0041(14) -0.0006(13) C17 0.0181(17) 0.0158(14) 0.0158(15) -0.0022(12) 0.0033(13) 0.0006(12) C18 0.0198(17) 0.0224(16) 0.0179(16) -0.0003(13) 0.0085(14) -0.0021(13) C21 0.0152(16) 0.0212(15) 0.0165(16) 0.0030(13) 0.0010(13) 0.0028(12) C22 0.0186(17) 0.0193(16) 0.0235(18) -0.0010(13) 0.0005(14) 0.0010(13) C23 0.0189(18) 0.0196(16) 0.039(2) 0.0036(15) -0.0017(17) -0.0010(13) C24 0.0156(18) 0.0300(19) 0.039(2) 0.0110(17) 0.0047(16) 0.0004(14) C25 0.0200(19) 0.037(2) 0.0239(19) 0.0013(16) 0.0052(15) 0.0053(15) C26 0.0177(17) 0.0225(17) 0.0221(18) -0.0009(14) 0.0007(14) 0.0011(13) C27 0.0220(18) 0.0117(14) 0.0210(17) 0.0007(12) 0.0022(14) 0.0011(12) C28 0.0238(19) 0.0198(16) 0.0248(18) 0.0023(14) 0.0020(15) 0.0017(13) C31 0.0206(17) 0.0143(14) 0.0167(16) 0.0020(12) 0.0042(13) -0.0014(12) C32 0.0212(17) 0.0155(15) 0.0175(16) 0.0001(12) 0.0008(13) 0.0000(12) C33 0.0249(19) 0.0250(17) 0.0245(19) -0.0014(15) 0.0039(15) 0.0045(14) C34 0.0165(17) 0.0289(19) 0.0245(18) 0.0002(15) 0.0011(14) 0.0014(14) C35 0.0218(18) 0.0220(16) 0.0161(16) -0.0012(13) 0.0043(14) -0.0042(13) C36 0.0221(17) 0.0180(16) 0.0156(15) 0.0002(12) 0.0060(13) -0.0023(12) C37 0.0230(18) 0.0208(16) 0.0150(16) -0.0011(13) 0.0042(13) -0.0012(13) C38 0.0194(17) 0.0232(16) 0.0193(17) 0.0029(13) 0.0026(14) -0.0033(13) C131 0.045(2) 0.0228(18) 0.0216(19) -0.0051(15) 0.0094(17) 0.0076(16) C151 0.033(2) 0.036(2) 0.031(2) -0.0069(18) 0.0000(18) -0.0132(18) C181 0.032(2) 0.0244(17) 0.0225(18) -0.0015(15) 0.0132(16) -0.0055(15) C182 0.029(2) 0.0308(19) 0.0169(17) -0.0002(14) 0.0059(15) 0.0002(15) C183 0.031(2) 0.0103(14) 0.0292(19) 0.0006(13) 0.0108(16) 0.0067(13) C231 0.029(2) 0.0187(18) 0.069(3) -0.0049(19) 0.006(2) -0.0058(16) C251 0.026(2) 0.059(3) 0.036(2) -0.002(2) 0.0154(19) 0.005(2) C281 0.044(3) 0.028(2) 0.039(2) 0.0135(18) -0.002(2) -0.0010(18) C282 0.0220(19) 0.0281(19) 0.033(2) 0.0021(16) -0.0028(16) 0.0068(15) C283 0.030(2) 0.036(2) 0.0201(18) 0.0015(16) 0.0011(16) 0.0053(17) C331 0.028(2) 0.037(2) 0.046(3) -0.017(2) 0.0002(19) 0.0106(18) C351 0.0228(19) 0.0266(18) 0.0239(18) -0.0043(14) 0.0039(15) -0.0078(14) C381 0.028(2) 0.0295(19) 0.0244(19) 0.0082(15) 0.0050(16) -0.0022(15) C382 0.035(2) 0.0257(19) 0.027(2) 0.0011(15) 0.0040(17) -0.0101(16) C383 0.032(2) 0.039(2) 0.030(2) 0.0084(17) 0.0140(18) -0.0006(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N3 1.956(3) . ? Ta1 N2 1.978(3) . ? Ta1 N1 1.979(3) . ? Ta1 C17 2.166(3) . ? Ta1 Cl1 2.3856(8) . ? N1 C11 1.405(4) . ? N1 C17 1.445(4) . ? N2 C21 1.447(4) . ? N2 C27 1.474(4) . ? N3 C31 1.446(4) . ? N3 C37 1.477(4) . ? C11 C16 1.391(5) . ? C11 C12 1.412(5) . ? C12 C13 1.394(5) . ? C13 C14 1.392(5) . ? C13 C131 1.505(5) . ? C14 C15 1.381(5) . ? C15 C16 1.406(5) . ? C15 C151 1.511(5) . ? C17 H17 0.975(18) . ? C17 C18 1.532(5) . ? C18 C182 1.535(5) . ? C18 C181 1.545(5) . ? C18 C183 1.557(5) . ? C21 C22 1.392(5) . ? C21 C26 1.398(5) . ? C22 C23 1.406(5) . ? C23 C24 1.368(6) . ? C23 C231 1.514(5) . ? C24 C25 1.400(6) . ? C25 C26 1.389(5) . ? C25 C251 1.502(6) . ? C27 C28 1.550(5) . ? C28 C283 1.529(5) . ? C28 C281 1.534(5) . ? C28 C282 1.536(5) . ? C31 C36 1.394(5) . ? C31 C32 1.397(5) . ? C32 C33 1.400(5) . ? C33 C34 1.387(5) . ? C33 C331 1.513(5) . ? C34 C35 1.401(5) . ? C35 C36 1.395(5) . ? C35 C351 1.523(5) . ? C37 C38 1.539(5) . ? C38 C381 1.533(5) . ? C38 C382 1.534(5) . ? C38 C383 1.542(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 N3 Ta1 N2 113.58(11) . . ? N3 Ta1 N1 102.27(11) . . ? N2 Ta1 N1 92.70(11) . . ? N3 Ta1 C17 110.04(12) . . ? N2 Ta1 C17 121.46(12) . . ? N1 Ta1 C17 40.48(11) . . ? N3 Ta1 Cl1 107.42(8) . . ? N2 Ta1 Cl1 105.66(8) . . ? N1 Ta1 Cl1 134.48(8) . . ? C17 Ta1 Cl1 96.19(9) . . ? C11 N1 C17 128.4(3) . . ? C11 N1 Ta1 135.0(2) . . ? C17 N1 Ta1 76.75(17) . . ? C21 N2 C27 115.2(3) . . ? C21 N2 Ta1 112.9(2) . . ? C27 N2 Ta1 130.7(2) . . ? C31 N3 C37 118.6(3) . . ? C31 N3 Ta1 107.8(2) . . ? C37 N3 Ta1 132.0(2) . . ? C16 C11 N1 122.4(3) . . ? C16 C11 C12 119.2(3) . . ? N1 C11 C12 118.4(3) . . ? C13 C12 C11 120.6(3) . . ? C14 C13 C12 118.8(3) . . ? C14 C13 C131 120.1(3) . . ? C12 C13 C131 121.1(3) . . ? C15 C14 C13 121.9(3) . . ? C14 C15 C16 119.0(3) . . ? C14 C15 C151 121.2(3) . . ? C16 C15 C151 119.8(3) . . ? C11 C16 C15 120.5(3) . . ? H17 C17 N1 115(2) . . ? H17 C17 C18 109(2) . . ? N1 C17 C18 121.9(3) . . ? H17 C17 Ta1 115(2) . . ? N1 C17 Ta1 62.77(16) . . ? C18 C17 Ta1 126.1(2) . . ? C17 C18 C182 110.6(3) . . ? C17 C18 C181 111.8(3) . . ? C182 C18 C181 108.5(3) . . ? C17 C18 C183 106.5(3) . . ? C182 C18 C183 109.7(3) . . ? C181 C18 C183 109.7(3) . . ? C22 C21 C26 119.2(3) . . ? C22 C21 N2 120.3(3) . . ? C26 C21 N2 120.5(3) . . ? C21 C22 C23 120.3(3) . . ? C24 C23 C22 119.1(3) . . ? C24 C23 C231 121.1(4) . . ? C22 C23 C231 119.8(4) . . ? C23 C24 C25 122.1(4) . . ? C26 C25 C24 118.2(4) . . ? C26 C25 C251 120.8(4) . . ? C24 C25 C251 121.0(4) . . ? C25 C26 C21 121.1(3) . . ? N2 C27 C28 118.3(3) . . ? C283 C28 C281 109.1(3) . . ? C283 C28 C282 109.7(3) . . ? C281 C28 C282 108.3(3) . . ? C283 C28 C27 111.1(3) . . ? C281 C28 C27 106.2(3) . . ? C282 C28 C27 112.3(3) . . ? C36 C31 C32 119.6(3) . . ? C36 C31 N3 121.4(3) . . ? C32 C31 N3 118.8(3) . . ? C31 C32 C33 120.9(3) . . ? C34 C33 C32 118.6(3) . . ? C34 C33 C331 121.1(3) . . ? C32 C33 C331 120.2(3) . . ? C33 C34 C35 121.3(3) . . ? C36 C35 C34 119.3(3) . . ? C36 C35 C351 120.3(3) . . ? C34 C35 C351 120.4(3) . . ? C31 C36 C35 120.3(3) . . ? N3 C37 C38 116.1(3) . . ? C381 C38 C382 110.3(3) . . ? C381 C38 C37 111.4(3) . . ? C382 C38 C37 110.3(3) . . ? C381 C38 C383 109.1(3) . . ? C382 C38 C383 109.5(3) . . ? C37 C38 C383 106.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.513 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.122 # Attachment '- 09415_mrb_e.cif' data_09415_mrb_e _database_code_depnum_ccdc_archive 'CCDC 852396' #TrackingRef '- 09415_mrb_e.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ar(tBuCH2)N)2(tBuC(H)NAr)TaP(H)Ph _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.75 H73 N3 P Ta' _chemical_formula_weight 913.02 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' P P 0.1023 0.0942 '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 12.8823(8) _cell_length_b 17.7431(12) _cell_length_c 21.9477(15) _cell_angle_alpha 84.4240(10) _cell_angle_beta 74.1600(10) _cell_angle_gamma 87.8070(10) _cell_volume 4802.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9061 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.12 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1898 _exptl_absorpt_coefficient_mu 2.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6502 _exptl_absorpt_correction_T_max 0.7986 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 87774 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.22 _reflns_number_total 23487 _reflns_number_gt 17533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _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^ > 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. The disordered pentane solvates were refined within SHELXL with the help of rigid bond restraints as well as similarity restraints on the anisotropic displacement parameters for neighboring atoms and on 1,2- and 1,3-distances throughout the disordered components. The hydrogen atoms attached to C17 and C47 were located in the Fourier difference map and refined using appropriate distance restraints. ; _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^)+(0.0310P)^2^+7.5070P] 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 23487 _refine_ls_number_parameters 1055 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.015 _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 0.506673(12) 0.306701(9) 0.307824(7) 0.01844(5) Uani 1 1 d . . . Ta2 Ta -0.007795(12) 0.167489(9) 0.781709(7) 0.01889(5) Uani 1 1 d . . . P2 P 0.10241(9) 0.17523(7) 0.66480(5) 0.0259(2) Uani 1 1 d . . . P1 P 0.61544(10) 0.27072(9) 0.19847(6) 0.0442(4) Uani 1 1 d . . . N1 N 0.3500(3) 0.32504(18) 0.32847(15) 0.0204(7) Uani 1 1 d . . . N2 N 0.5460(3) 0.40816(18) 0.32283(15) 0.0206(7) Uani 1 1 d . . . N4 N -0.1660(3) 0.17828(19) 0.80551(15) 0.0210(7) Uani 1 1 d . . . N3 N 0.5237(3) 0.22210(18) 0.36934(16) 0.0230(7) Uani 1 1 d . . . N6 N 0.0211(3) 0.07379(19) 0.83039(15) 0.0225(7) Uani 1 1 d . . . N5 N 0.0200(3) 0.26378(19) 0.81206(15) 0.0222(7) Uani 1 1 d . . . C71 C 0.7591(3) 0.2871(3) 0.1845(2) 0.0279(9) Uani 1 1 d . . . C17 C 0.3656(3) 0.2891(2) 0.27115(18) 0.0215(8) Uani 1 1 d D . . H17 H 0.348(3) 0.2336(12) 0.2783(19) 0.026 Uiso 1 1 d D . . C81 C 0.2459(3) 0.1537(2) 0.65695(18) 0.0232(9) Uani 1 1 d . . . C52 C 0.2062(3) 0.2320(2) 0.81142(19) 0.0240(9) Uani 1 1 d . . . H52 H 0.2223 0.2283 0.7669 0.029 Uiso 1 1 calc R . . C47 C -0.1482(3) 0.1528(2) 0.74408(18) 0.0223(8) Uani 1 1 d D . . H47 H -0.165(3) 0.0987(12) 0.7436(19) 0.027 Uiso 1 1 d D . . C12 C 0.1754(3) 0.2738(2) 0.39342(19) 0.0236(9) Uani 1 1 d . . . H12 H 0.1646 0.2512 0.3582 0.028 Uiso 1 1 calc R . . C48 C -0.1920(3) 0.1997(2) 0.69348(18) 0.0238(9) Uani 1 1 d . . . C16 C 0.2830(3) 0.3485(2) 0.43857(19) 0.0265(9) Uani 1 1 d . . . H16 H 0.3462 0.3769 0.4336 0.032 Uiso 1 1 calc R . . C41 C -0.2499(3) 0.1625(2) 0.86128(18) 0.0224(8) Uani 1 1 d . . . C181 C 0.2027(3) 0.3334(3) 0.2355(2) 0.0305(10) Uani 1 1 d . . . H18A H 0.1737 0.2822 0.2473 0.046 Uiso 1 1 calc R . . H18B H 0.1777 0.3569 0.1997 0.046 Uiso 1 1 calc R . . H18C H 0.1776 0.3638 0.2719 0.046 Uiso 1 1 calc R . . C21 C 0.6277(3) 0.4040(2) 0.35659(19) 0.0218(8) Uani 1 1 d . . . C13 C 0.0980(3) 0.2649(3) 0.4523(2) 0.0285(10) Uani 1 1 d . . . C45 C -0.4208(3) 0.1059(2) 0.9197(2) 0.0293(10) Uani 1 1 d . . . C24 C 0.7829(3) 0.3860(2) 0.4229(2) 0.0278(9) Uani 1 1 d . . . H24 H 0.8362 0.3804 0.4457 0.033 Uiso 1 1 calc R . . C18 C 0.3266(3) 0.3293(2) 0.21627(19) 0.0243(9) Uani 1 1 d . . . C11 C 0.2678(3) 0.3155(2) 0.38607(18) 0.0218(8) Uani 1 1 d . . . C42 C -0.2417(3) 0.1906(2) 0.91799(19) 0.0274(9) Uani 1 1 d . . . H42 H -0.1797 0.2181 0.9175 0.033 Uiso 1 1 calc R . . C231 C 0.9236(3) 0.3451(3) 0.3265(2) 0.0312(10) Uani 1 1 d . . . H23A H 0.9734 0.3571 0.3508 0.047 Uiso 1 1 calc R . . H23B H 0.9462 0.3713 0.2837 0.047 Uiso 1 1 calc R . . H23C H 0.9244 0.2903 0.3235 0.047 Uiso 1 1 calc R . . C51 C 0.1021(3) 0.2525(2) 0.84480(19) 0.0232(9) Uani 1 1 d . . . C26 C 0.6016(3) 0.4184(2) 0.42064(19) 0.0250(9) Uani 1 1 d . . . H26 H 0.5306 0.4345 0.4412 0.030 Uiso 1 1 calc R . . C62 C -0.1376(3) -0.0094(2) 0.86579(19) 0.0229(8) Uani 1 1 d . . . H62 H -0.1572 0.0114 0.9057 0.028 Uiso 1 1 calc R . . C482 C -0.3161(3) 0.1993(3) 0.7137(2) 0.0312(10) Uani 1 1 d . . . H48A H -0.3427 0.2224 0.7539 0.047 Uiso 1 1 calc R . . H48B H -0.3412 0.1469 0.7192 0.047 Uiso 1 1 calc R . . H48C H -0.3434 0.2281 0.6808 0.047 Uiso 1 1 calc R . . C23 C 0.8108(3) 0.3708(2) 0.35966(19) 0.0232(9) Uani 1 1 d . . . C46 C -0.3398(3) 0.1198(2) 0.86328(19) 0.0253(9) Uani 1 1 d . . . H46 H -0.3457 0.1000 0.8257 0.030 Uiso 1 1 calc R . . C27 C 0.4841(3) 0.4800(2) 0.3223(2) 0.0238(9) Uani 1 1 d . . . H27A H 0.4576 0.4936 0.3666 0.029 Uiso 1 1 calc R . . H27B H 0.4200 0.4708 0.3075 0.029 Uiso 1 1 calc R . . C67 C 0.0621(4) 0.0620(2) 0.88752(19) 0.0274(9) Uani 1 1 d . . . H67A H -0.0006 0.0535 0.9252 0.033 Uiso 1 1 calc R . . H67B H 0.0965 0.1094 0.8918 0.033 Uiso 1 1 calc R . . C61 C -0.0432(3) 0.0141(2) 0.81971(19) 0.0227(8) Uani 1 1 d . . . C22 C 0.7315(3) 0.3798(2) 0.32643(19) 0.0212(8) Uani 1 1 d . . . H22 H 0.7488 0.3694 0.2831 0.025 Uiso 1 1 calc R . . C483 C -0.1557(4) 0.2823(3) 0.6834(2) 0.0341(11) Uani 1 1 d . . . H48D H -0.1806 0.3056 0.7236 0.051 Uiso 1 1 calc R . . H48E H -0.1864 0.3100 0.6514 0.051 Uiso 1 1 calc R . . H48F H -0.0767 0.2840 0.6687 0.051 Uiso 1 1 calc R . . C53 C 0.2876(3) 0.2165(2) 0.8424(2) 0.0282(9) Uani 1 1 d . . . C85 C 0.4298(4) 0.2004(3) 0.6346(2) 0.0373(11) Uani 1 1 d . . . H85 H 0.4777 0.2418 0.6261 0.045 Uiso 1 1 calc R . . C25 C 0.6788(3) 0.4094(2) 0.4542(2) 0.0270(9) Uani 1 1 d . . . C37 C 0.5673(3) 0.2216(2) 0.42562(19) 0.0252(9) Uani 1 1 d . . . H37A H 0.5056 0.2207 0.4642 0.030 Uiso 1 1 calc R . . H37B H 0.6055 0.2698 0.4224 0.030 Uiso 1 1 calc R . . C15 C 0.2076(4) 0.3403(3) 0.4976(2) 0.0302(10) Uani 1 1 d . . . C56 C 0.0798(4) 0.2582(3) 0.9104(2) 0.0310(10) Uani 1 1 d . . . H56 H 0.0092 0.2724 0.9335 0.037 Uiso 1 1 calc R . . C68 C 0.1440(4) -0.0041(3) 0.8896(2) 0.0314(10) Uani 1 1 d . . . C531 C 0.4002(3) 0.1937(3) 0.8051(2) 0.0362(11) Uani 1 1 d . . . H53A H 0.4015 0.1398 0.7984 0.054 Uiso 1 1 calc R . . H53B H 0.4520 0.2028 0.8290 0.054 Uiso 1 1 calc R . . H53C H 0.4198 0.2238 0.7638 0.054 Uiso 1 1 calc R . . C86 C 0.3191(4) 0.2135(3) 0.6430(2) 0.0323(10) Uani 1 1 d . . . H86 H 0.2930 0.2641 0.6391 0.039 Uiso 1 1 calc R . . C183 C 0.3678(4) 0.4106(2) 0.1983(2) 0.0342(11) Uani 1 1 d . . . H18D H 0.4468 0.4100 0.1862 0.051 Uiso 1 1 calc R . . H18E H 0.3405 0.4405 0.2348 0.051 Uiso 1 1 calc R . . H18F H 0.3422 0.4332 0.1624 0.051 Uiso 1 1 calc R . . C54 C 0.2627(4) 0.2233(3) 0.9072(2) 0.0369(11) Uani 1 1 d . . . H54 H 0.3175 0.2141 0.9286 0.044 Uiso 1 1 calc R . . C182 C 0.3628(4) 0.2833(3) 0.1584(2) 0.0316(10) Uani 1 1 d . . . H18G H 0.4418 0.2795 0.1453 0.047 Uiso 1 1 calc R . . H18H H 0.3374 0.3085 0.1233 0.047 Uiso 1 1 calc R . . H18I H 0.3324 0.2324 0.1695 0.047 Uiso 1 1 calc R . . C31 C 0.4528(3) 0.1614(2) 0.3700(2) 0.0279(10) Uani 1 1 d . . . C63 C -0.2026(3) -0.0631(2) 0.8531(2) 0.0266(9) Uani 1 1 d . . . C57 C -0.0461(3) 0.3340(2) 0.8213(2) 0.0266(9) Uani 1 1 d . . . H57A H -0.0724 0.3389 0.8676 0.032 Uiso 1 1 calc R . . H57B H -0.1102 0.3280 0.8056 0.032 Uiso 1 1 calc R . . C282 C 0.6228(4) 0.5823(2) 0.3120(2) 0.0349(11) Uani 1 1 d . . . H28A H 0.6590 0.6257 0.2844 0.052 Uiso 1 1 calc R . . H28B H 0.6768 0.5437 0.3177 0.052 Uiso 1 1 calc R . . H28C H 0.5834 0.5988 0.3534 0.052 Uiso 1 1 calc R . . C66 C -0.0148(3) -0.0159(2) 0.76120(19) 0.0238(9) Uani 1 1 d . . . H66 H 0.0503 -0.0005 0.7306 0.029 Uiso 1 1 calc R . . C82 C 0.2889(4) 0.0807(2) 0.66049(19) 0.0284(9) Uani 1 1 d . . . H82 H 0.2419 0.0387 0.6693 0.034 Uiso 1 1 calc R . . C38 C 0.6451(3) 0.1556(2) 0.4352(2) 0.0263(9) Uani 1 1 d . . . C481 C -0.1526(4) 0.1633(3) 0.63097(19) 0.0339(11) Uani 1 1 d . . . H48G H -0.1795 0.1927 0.5982 0.051 Uiso 1 1 calc R . . H48H H -0.1794 0.1114 0.6367 0.051 Uiso 1 1 calc R . . H48I H -0.0735 0.1623 0.6178 0.051 Uiso 1 1 calc R . . C43 C -0.3225(4) 0.1786(3) 0.9741(2) 0.0321(10) Uani 1 1 d . . . C36 C 0.4714(4) 0.1220(2) 0.3162(2) 0.0328(11) Uani 1 1 d . . . H36 H 0.5330 0.1332 0.2815 0.039 Uiso 1 1 calc R . . C583 C 0.0940(4) 0.4332(3) 0.8207(2) 0.0381(11) Uani 1 1 d . . . H58A H 0.1514 0.3947 0.8171 0.057 Uiso 1 1 calc R . . H58B H 0.0595 0.4389 0.8657 0.057 Uiso 1 1 calc R . . H58C H 0.1249 0.4817 0.7996 0.057 Uiso 1 1 calc R . . C65 C -0.0807(3) -0.0685(2) 0.7467(2) 0.0278(9) Uani 1 1 d . . . C451 C -0.5183(3) 0.0604(3) 0.9210(2) 0.0365(11) Uani 1 1 d . . . H45A H -0.5092 0.0416 0.8793 0.055 Uiso 1 1 calc R . . H45B H -0.5831 0.0926 0.9312 0.055 Uiso 1 1 calc R . . H45C H -0.5257 0.0174 0.9535 0.055 Uiso 1 1 calc R . . C14 C 0.1152(4) 0.2982(3) 0.5038(2) 0.0328(11) Uani 1 1 d . . . H14 H 0.0629 0.2922 0.5439 0.039 Uiso 1 1 calc R . . C28 C 0.5436(4) 0.5487(2) 0.2812(2) 0.0311(10) Uani 1 1 d . . . C64 C -0.1738(3) -0.0917(2) 0.7932(2) 0.0280(9) Uani 1 1 d . . . H64 H -0.2189 -0.1278 0.7842 0.034 Uiso 1 1 calc R . . C32 C 0.3627(4) 0.1444(2) 0.4216(2) 0.0340(11) Uani 1 1 d . . . H32 H 0.3494 0.1717 0.4581 0.041 Uiso 1 1 calc R . . C131 C -0.0035(4) 0.2205(3) 0.4599(2) 0.0375(11) Uani 1 1 d . . . H13A H -0.0040 0.1753 0.4894 0.056 Uiso 1 1 calc R . . H13B H -0.0053 0.2053 0.4185 0.056 Uiso 1 1 calc R . . H13C H -0.0669 0.2522 0.4767 0.056 Uiso 1 1 calc R . . C44 C -0.4112(4) 0.1360(3) 0.9744(2) 0.0357(11) Uani 1 1 d . . . H44 H -0.4668 0.1272 1.0129 0.043 Uiso 1 1 calc R . . C84 C 0.4690(4) 0.1274(3) 0.6388(2) 0.0355(11) Uani 1 1 d . . . H84 H 0.5440 0.1181 0.6330 0.043 Uiso 1 1 calc R . . C58 C 0.0094(4) 0.4087(2) 0.7889(2) 0.0315(10) Uani 1 1 d . . . C631 C -0.3041(4) -0.0894(3) 0.9026(2) 0.0345(11) Uani 1 1 d . . . H63A H -0.3648 -0.0863 0.8835 0.052 Uiso 1 1 calc R . . H63B H -0.3192 -0.0571 0.9379 0.052 Uiso 1 1 calc R . . H63C H -0.2942 -0.1420 0.9187 0.052 Uiso 1 1 calc R . . C55 C 0.1590(4) 0.2435(3) 0.9419(2) 0.0362(11) Uani 1 1 d . . . C283 C 0.6035(4) 0.5289(3) 0.2147(2) 0.0375(11) Uani 1 1 d . . . H28D H 0.6408 0.5738 0.1901 0.056 Uiso 1 1 calc R . . H28E H 0.5518 0.5118 0.1936 0.056 Uiso 1 1 calc R . . H28F H 0.6563 0.4884 0.2175 0.056 Uiso 1 1 calc R . . C683 C 0.0880(4) -0.0811(3) 0.9062(2) 0.0389(12) Uani 1 1 d . . . H68A H 0.0548 -0.0910 0.8727 0.058 Uiso 1 1 calc R . . H68B H 0.0322 -0.0805 0.9468 0.058 Uiso 1 1 calc R . . H68C H 0.1413 -0.1210 0.9099 0.058 Uiso 1 1 calc R . . C682 C 0.2308(4) -0.0036(3) 0.8265(2) 0.0421(12) Uani 1 1 d . . . H68D H 0.1975 -0.0123 0.7926 0.063 Uiso 1 1 calc R . . H68E H 0.2840 -0.0439 0.8294 0.063 Uiso 1 1 calc R . . H68F H 0.2667 0.0455 0.8168 0.063 Uiso 1 1 calc R . . C582 C 0.0654(4) 0.4009(3) 0.7187(2) 0.0367(11) Uani 1 1 d . . . H58D H 0.1232 0.3627 0.7152 0.055 Uiso 1 1 calc R . . H58E H 0.0960 0.4497 0.6983 0.055 Uiso 1 1 calc R . . H58F H 0.0127 0.3853 0.6976 0.055 Uiso 1 1 calc R . . C83 C 0.3983(4) 0.0678(3) 0.6515(2) 0.0330(10) Uani 1 1 d . . . H83 H 0.4251 0.0174 0.6541 0.040 Uiso 1 1 calc R . . C383 C 0.7288(4) 0.1439(3) 0.3727(2) 0.0352(11) Uani 1 1 d . . . H38A H 0.7667 0.1914 0.3557 0.053 Uiso 1 1 calc R . . H38B H 0.6929 0.1279 0.3422 0.053 Uiso 1 1 calc R . . H38C H 0.7808 0.1047 0.3801 0.053 Uiso 1 1 calc R . . C382 C 0.5852(4) 0.0818(2) 0.4632(2) 0.0322(10) Uani 1 1 d . . . H38D H 0.5312 0.0905 0.5031 0.048 Uiso 1 1 calc R . . H38E H 0.6369 0.0428 0.4715 0.048 Uiso 1 1 calc R . . H38F H 0.5494 0.0649 0.4329 0.048 Uiso 1 1 calc R . . C381 C 0.7018(4) 0.1797(3) 0.4835(2) 0.0380(11) Uani 1 1 d . . . H38G H 0.6479 0.1875 0.5236 0.057 Uiso 1 1 calc R . . H38H H 0.7406 0.2270 0.4666 0.057 Uiso 1 1 calc R . . H38I H 0.7531 0.1400 0.4909 0.057 Uiso 1 1 calc R . . C651 C -0.0502(4) -0.1003(3) 0.6826(2) 0.0369(11) Uani 1 1 d . . . H65A H -0.0168 -0.0607 0.6496 0.055 Uiso 1 1 calc R . . H65B H -0.1151 -0.1183 0.6738 0.055 Uiso 1 1 calc R . . H65C H 0.0009 -0.1425 0.6830 0.055 Uiso 1 1 calc R . . C681 C 0.1947(4) 0.0095(3) 0.9431(2) 0.0416(12) Uani 1 1 d . . . H68G H 0.2309 0.0585 0.9336 0.062 Uiso 1 1 calc R . . H68H H 0.2475 -0.0308 0.9466 0.062 Uiso 1 1 calc R . . H68I H 0.1382 0.0094 0.9834 0.062 Uiso 1 1 calc R . . C581 C -0.0806(4) 0.4686(3) 0.7950(3) 0.0453(13) Uani 1 1 d . . . H58G H -0.1343 0.4530 0.7747 0.068 Uiso 1 1 calc R . . H58H H -0.0501 0.5172 0.7742 0.068 Uiso 1 1 calc R . . H58I H -0.1152 0.4738 0.8401 0.068 Uiso 1 1 calc R . . C35 C 0.4001(5) 0.0659(3) 0.3127(3) 0.0505(16) Uani 1 1 d . . . C72 C 0.8232(4) 0.2302(3) 0.2041(2) 0.0437(13) Uani 1 1 d . . . H72 H 0.7913 0.1847 0.2268 0.052 Uiso 1 1 calc R . . C151 C 0.2236(4) 0.3774(3) 0.5536(2) 0.0414(12) Uani 1 1 d . . . H15A H 0.1943 0.4292 0.5531 0.062 Uiso 1 1 calc R . . H15B H 0.3008 0.3788 0.5506 0.062 Uiso 1 1 calc R . . H15C H 0.1861 0.3484 0.5932 0.062 Uiso 1 1 calc R . . C33 C 0.2922(4) 0.0872(3) 0.4194(3) 0.0468(14) Uani 1 1 d . . . C431 C -0.3157(5) 0.2125(3) 1.0331(2) 0.0492(14) Uani 1 1 d . . . H43A H -0.2405 0.2248 1.0293 0.074 Uiso 1 1 calc R . . H43B H -0.3420 0.1760 1.0703 0.074 Uiso 1 1 calc R . . H43C H -0.3601 0.2588 1.0384 0.074 Uiso 1 1 calc R . . C251 C 0.6501(4) 0.4218(3) 0.5241(2) 0.0411(12) Uani 1 1 d . . . H25A H 0.6776 0.4708 0.5293 0.062 Uiso 1 1 calc R . . H25B H 0.6825 0.3813 0.5468 0.062 Uiso 1 1 calc R . . H25C H 0.5714 0.4213 0.5414 0.062 Uiso 1 1 calc R . . C76 C 0.8107(4) 0.3517(3) 0.1509(2) 0.0487(14) Uani 1 1 d . . . H76 H 0.7688 0.3915 0.1370 0.058 Uiso 1 1 calc R . . C281 C 0.4550(4) 0.6087(3) 0.2774(3) 0.0452(13) Uani 1 1 d . . . H28G H 0.4881 0.6543 0.2519 0.068 Uiso 1 1 calc R . . H28H H 0.4169 0.6213 0.3204 0.068 Uiso 1 1 calc R . . H28I H 0.4037 0.5884 0.2576 0.068 Uiso 1 1 calc R . . C34 C 0.3129(4) 0.0496(3) 0.3644(4) 0.0566(18) Uani 1 1 d . . . H34 H 0.2649 0.0111 0.3624 0.068 Uiso 1 1 calc R . . C551 C 0.1323(5) 0.2467(4) 1.0134(2) 0.0589(17) Uani 1 1 d . . . H55A H 0.1248 0.1951 1.0345 0.088 Uiso 1 1 calc R . . H55B H 0.0643 0.2748 1.0280 0.088 Uiso 1 1 calc R . . H55C H 0.1903 0.2723 1.0240 0.088 Uiso 1 1 calc R . . C73 C 0.9364(5) 0.2402(5) 0.1902(3) 0.066(2) Uani 1 1 d . . . H73 H 0.9804 0.2017 0.2041 0.079 Uiso 1 1 calc R . . C351 C 0.4199(6) 0.0238(3) 0.2534(3) 0.076(2) Uani 1 1 d . . . H35A H 0.3538 -0.0020 0.2537 0.114 Uiso 1 1 calc R . . H35B H 0.4780 -0.0136 0.2528 0.114 Uiso 1 1 calc R . . H35C H 0.4406 0.0599 0.2156 0.114 Uiso 1 1 calc R . . C74 C 0.9817(5) 0.3051(6) 0.1570(3) 0.081(3) Uani 1 1 d . . . H74 H 1.0574 0.3117 0.1478 0.098 Uiso 1 1 calc R . . C75 C 0.9209(6) 0.3598(5) 0.1371(3) 0.077(2) Uani 1 1 d . . . H75 H 0.9538 0.4043 0.1133 0.092 Uiso 1 1 calc R . . C331 C 0.1974(4) 0.0676(3) 0.4751(3) 0.071(2) Uani 1 1 d . . . H33A H 0.1319 0.0674 0.4606 0.106 Uiso 1 1 calc R . . H33B H 0.1893 0.1052 0.5060 0.106 Uiso 1 1 calc R . . H33C H 0.2089 0.0174 0.4952 0.106 Uiso 1 1 calc R . . C1T C 0.629(2) 0.3700(11) 0.8888(12) 0.117(10) Uani 0.383(14) 1 d PDU A 1 H1T1 H 0.6920 0.3425 0.8962 0.176 Uiso 0.383(14) 1 calc PR A 1 H1T2 H 0.6506 0.4194 0.8657 0.176 Uiso 0.383(14) 1 calc PR A 1 H1T3 H 0.5953 0.3408 0.8636 0.176 Uiso 0.383(14) 1 calc PR A 1 C2T C 0.553(4) 0.381(3) 0.9479(16) 0.24(2) Uani 0.383(14) 1 d PDU A 1 H2T1 H 0.5946 0.4050 0.9723 0.294 Uiso 0.383(14) 1 calc PR A 1 H2T2 H 0.5377 0.3289 0.9692 0.294 Uiso 0.383(14) 1 calc PR A 1 C3T C 0.438(3) 0.424(2) 0.9635(19) 0.179(15) Uani 0.383(14) 1 d PDU A 1 H3T1 H 0.4098 0.3992 0.9326 0.214 Uiso 0.383(14) 1 calc PR A 1 H3T2 H 0.4648 0.4727 0.9402 0.214 Uiso 0.383(14) 1 calc PR A 1 C4T C 0.321(3) 0.457(2) 1.0028(17) 0.178(14) Uani 0.383(14) 1 d PDU A 1 H4T1 H 0.2658 0.4235 0.9961 0.213 Uiso 0.383(14) 1 calc PR A 1 H4T2 H 0.3187 0.4477 1.0484 0.213 Uiso 0.383(14) 1 calc PR A 1 C5T C 0.284(4) 0.533(2) 0.993(2) 0.30(3) Uani 0.383(14) 1 d PDU A 1 H5T1 H 0.2106 0.5393 1.0210 0.443 Uiso 0.383(14) 1 calc PR A 1 H5T2 H 0.2830 0.5446 0.9488 0.443 Uiso 0.383(14) 1 calc PR A 1 H5T3 H 0.3321 0.5684 1.0036 0.443 Uiso 0.383(14) 1 calc PR A 1 C1TB C 0.5244(12) 0.3470(8) 0.9117(6) 0.089(5) Uani 0.617(14) 1 d PDU A 2 H1T4 H 0.5848 0.3191 0.9228 0.133 Uiso 0.617(14) 1 calc PR A 2 H1T5 H 0.5516 0.3921 0.8831 0.133 Uiso 0.617(14) 1 calc PR A 2 H1T6 H 0.4881 0.3145 0.8905 0.133 Uiso 0.617(14) 1 calc PR A 2 C2TB C 0.4509(19) 0.3691(16) 0.9672(10) 0.172(9) Uani 0.617(14) 1 d PDU A 2 H2T3 H 0.4930 0.3976 0.9887 0.206 Uiso 0.617(14) 1 calc PR A 2 H2T4 H 0.4282 0.3218 0.9949 0.206 Uiso 0.617(14) 1 calc PR A 2 C3TB C 0.3417(13) 0.4179(12) 0.9694(8) 0.139(7) Uani 0.617(14) 1 d PDU A 2 H3T3 H 0.3684 0.4579 0.9344 0.167 Uiso 0.617(14) 1 calc PR A 2 H3T4 H 0.3012 0.3834 0.9518 0.167 Uiso 0.617(14) 1 calc PR A 2 C4TB C 0.244(2) 0.4623(16) 1.0154(10) 0.190(10) Uani 0.617(14) 1 d PDU A 2 H4T3 H 0.2108 0.4235 1.0501 0.228 Uiso 0.617(14) 1 calc PR A 2 H4T4 H 0.2805 0.4976 1.0350 0.228 Uiso 0.617(14) 1 calc PR A 2 C5TB C 0.154(3) 0.5054(17) 1.0030(9) 0.277(19) Uani 0.617(14) 1 d PDU A 2 H5T4 H 0.1122 0.5267 1.0419 0.415 Uiso 0.617(14) 1 calc PR A 2 H5T5 H 0.1081 0.4723 0.9886 0.415 Uiso 0.617(14) 1 calc PR A 2 H5T6 H 0.1807 0.5466 0.9698 0.415 Uiso 0.617(14) 1 calc PR A 2 C1SA C 0.1539(9) 0.5064(6) 0.3698(5) 0.042(2) Uani 0.50 1 d PU B -1 H1S1 H 0.1630 0.4824 0.3303 0.063 Uiso 0.50 1 calc PR B -1 H1S2 H 0.2159 0.4937 0.3867 0.063 Uiso 0.50 1 calc PR B -1 H1S3 H 0.1489 0.5615 0.3612 0.063 Uiso 0.50 1 calc PR B -1 C2SA C 0.0525(19) 0.4784(16) 0.4176(9) 0.033(3) Uani 0.50 1 d PU B -1 H2S1 H 0.0556 0.4224 0.4235 0.040 Uiso 0.50 1 calc PR B -1 H2S2 H -0.0101 0.4929 0.4008 0.040 Uiso 0.50 1 calc PR B -1 C3SA C 0.0354(18) 0.5105(14) 0.4831(8) 0.033(4) Uani 0.50 1 d PU B -1 H3S1 H 0.1019 0.5015 0.4972 0.040 Uiso 0.50 1 calc PR B -1 H3S2 H 0.0237 0.5660 0.4779 0.040 Uiso 0.50 1 calc PR B -1 C4SA C -0.061(2) 0.4756(17) 0.5357(9) 0.045(5) Uani 0.50 1 d PU B -1 H4S1 H -0.1273 0.4839 0.5213 0.054 Uiso 0.50 1 calc PR B -1 H4S2 H -0.0488 0.4202 0.5414 0.054 Uiso 0.50 1 calc PR B -1 C5SA C -0.079(2) 0.5077(17) 0.5995(11) 0.054(6) Uani 0.50 1 d PU B -1 H5S1 H -0.1397 0.4821 0.6305 0.080 Uiso 0.50 1 calc PR B -1 H5S2 H -0.0948 0.5620 0.5949 0.080 Uiso 0.50 1 calc PR B -1 H5S3 H -0.0137 0.4996 0.6142 0.080 Uiso 0.50 1 calc PR B -1 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 0.01405(8) 0.02114(9) 0.02124(8) -0.00658(6) -0.00532(7) 0.00178(6) Ta2 0.01552(9) 0.02245(9) 0.01877(8) -0.00142(6) -0.00481(6) -0.00086(6) P2 0.0203(6) 0.0346(6) 0.0216(5) -0.0014(4) -0.0043(4) 0.0022(5) P1 0.0230(6) 0.0804(11) 0.0317(6) -0.0280(7) -0.0037(5) 0.0003(7) N1 0.0174(17) 0.0217(17) 0.0241(17) -0.0063(13) -0.0072(14) -0.0003(13) N2 0.0138(16) 0.0234(18) 0.0257(17) -0.0055(14) -0.0065(14) 0.0006(13) N4 0.0159(17) 0.0269(18) 0.0207(16) -0.0032(14) -0.0049(14) -0.0032(14) N3 0.0244(19) 0.0179(17) 0.0274(18) -0.0070(14) -0.0069(15) 0.0012(14) N6 0.0221(18) 0.0262(18) 0.0200(16) 0.0001(14) -0.0070(14) -0.0052(14) N5 0.0160(17) 0.0255(18) 0.0252(17) -0.0047(14) -0.0052(14) 0.0000(14) C71 0.023(2) 0.035(2) 0.025(2) -0.0131(18) -0.0021(18) 0.0030(19) C17 0.021(2) 0.021(2) 0.023(2) -0.0008(16) -0.0068(17) 0.0003(16) C81 0.023(2) 0.029(2) 0.0182(19) -0.0034(16) -0.0056(17) 0.0025(17) C52 0.027(2) 0.020(2) 0.026(2) -0.0039(16) -0.0079(18) -0.0036(17) C47 0.018(2) 0.027(2) 0.0219(19) -0.0023(17) -0.0058(16) -0.0009(17) C12 0.019(2) 0.027(2) 0.024(2) -0.0050(17) -0.0048(17) 0.0053(17) C48 0.019(2) 0.032(2) 0.023(2) -0.0034(17) -0.0085(17) -0.0019(17) C16 0.021(2) 0.029(2) 0.030(2) -0.0003(18) -0.0080(18) 0.0046(17) C41 0.018(2) 0.025(2) 0.0224(19) 0.0005(16) -0.0041(16) 0.0023(16) C181 0.020(2) 0.045(3) 0.030(2) 0.000(2) -0.0124(19) 0.0008(19) C21 0.020(2) 0.0162(19) 0.031(2) -0.0052(16) -0.0101(17) -0.0018(15) C13 0.021(2) 0.035(2) 0.027(2) -0.0007(18) -0.0025(18) 0.0061(18) C45 0.022(2) 0.031(2) 0.034(2) 0.0027(19) -0.0068(19) -0.0028(18) C24 0.023(2) 0.028(2) 0.037(2) -0.0115(19) -0.0142(19) 0.0030(18) C18 0.022(2) 0.026(2) 0.026(2) -0.0025(17) -0.0087(18) -0.0003(17) C11 0.018(2) 0.026(2) 0.0200(19) -0.0022(16) -0.0042(16) 0.0061(16) C42 0.022(2) 0.034(2) 0.025(2) -0.0065(18) -0.0040(18) -0.0009(18) C231 0.020(2) 0.039(3) 0.036(2) -0.012(2) -0.0074(19) 0.0074(19) C51 0.022(2) 0.022(2) 0.028(2) -0.0047(17) -0.0079(17) -0.0032(16) C26 0.018(2) 0.027(2) 0.030(2) -0.0109(17) -0.0040(17) 0.0027(17) C62 0.022(2) 0.023(2) 0.025(2) -0.0004(16) -0.0083(17) -0.0014(17) C482 0.018(2) 0.042(3) 0.035(2) -0.001(2) -0.0125(19) 0.0010(19) C23 0.018(2) 0.022(2) 0.030(2) -0.0091(17) -0.0058(17) 0.0030(16) C46 0.021(2) 0.032(2) 0.022(2) -0.0017(17) -0.0055(17) 0.0011(18) C27 0.017(2) 0.025(2) 0.030(2) -0.0087(17) -0.0057(17) 0.0034(16) C67 0.031(2) 0.031(2) 0.023(2) 0.0021(17) -0.0132(19) -0.0103(19) C61 0.020(2) 0.025(2) 0.026(2) -0.0014(16) -0.0102(17) 0.0001(16) C22 0.019(2) 0.020(2) 0.025(2) -0.0060(16) -0.0061(17) -0.0002(16) C483 0.031(3) 0.035(3) 0.038(3) 0.007(2) -0.016(2) -0.001(2) C53 0.021(2) 0.027(2) 0.038(2) -0.0055(19) -0.0093(19) -0.0013(17) C85 0.023(2) 0.045(3) 0.041(3) -0.001(2) -0.003(2) -0.006(2) C25 0.027(2) 0.027(2) 0.030(2) -0.0136(18) -0.0092(19) 0.0021(18) C37 0.026(2) 0.026(2) 0.024(2) -0.0027(17) -0.0073(18) -0.0026(17) C15 0.033(3) 0.033(2) 0.025(2) -0.0046(18) -0.0103(19) 0.012(2) C56 0.024(2) 0.038(3) 0.033(2) -0.011(2) -0.0088(19) 0.0013(19) C68 0.030(2) 0.034(3) 0.033(2) 0.0064(19) -0.015(2) -0.005(2) C531 0.022(2) 0.039(3) 0.046(3) 0.004(2) -0.010(2) 0.001(2) C86 0.025(2) 0.029(2) 0.039(3) -0.002(2) -0.002(2) 0.0006(19) C183 0.038(3) 0.031(2) 0.039(3) 0.000(2) -0.020(2) -0.002(2) C54 0.030(3) 0.046(3) 0.041(3) -0.009(2) -0.018(2) 0.002(2) C182 0.030(2) 0.039(3) 0.029(2) -0.0044(19) -0.013(2) -0.005(2) C31 0.025(2) 0.018(2) 0.046(3) -0.0017(18) -0.019(2) 0.0046(17) C63 0.021(2) 0.024(2) 0.034(2) -0.0007(18) -0.0072(18) 0.0003(17) C57 0.018(2) 0.029(2) 0.033(2) -0.0081(18) -0.0066(18) 0.0020(17) C282 0.036(3) 0.023(2) 0.049(3) -0.010(2) -0.012(2) -0.0038(19) C66 0.019(2) 0.027(2) 0.025(2) 0.0021(17) -0.0074(17) 0.0025(17) C82 0.028(2) 0.030(2) 0.027(2) -0.0051(18) -0.0061(19) 0.0010(19) C38 0.022(2) 0.028(2) 0.030(2) 0.0018(18) -0.0093(18) -0.0012(17) C481 0.030(3) 0.049(3) 0.024(2) -0.002(2) -0.0090(19) -0.002(2) C43 0.034(3) 0.038(3) 0.022(2) -0.0057(19) -0.0037(19) 0.000(2) C36 0.042(3) 0.017(2) 0.049(3) -0.0071(19) -0.028(2) 0.0078(19) C583 0.041(3) 0.035(3) 0.040(3) -0.007(2) -0.011(2) -0.007(2) C65 0.023(2) 0.032(2) 0.029(2) -0.0061(18) -0.0098(19) 0.0011(18) C451 0.019(2) 0.046(3) 0.040(3) 0.006(2) -0.002(2) -0.006(2) C14 0.024(2) 0.043(3) 0.024(2) 0.0010(19) 0.0029(18) 0.008(2) C28 0.030(2) 0.025(2) 0.038(3) -0.0038(19) -0.008(2) -0.0020(19) C64 0.022(2) 0.027(2) 0.038(2) -0.0056(19) -0.0112(19) -0.0025(18) C32 0.024(2) 0.024(2) 0.057(3) -0.002(2) -0.019(2) 0.0023(18) C131 0.024(2) 0.049(3) 0.034(2) 0.008(2) -0.002(2) -0.003(2) C44 0.030(3) 0.046(3) 0.023(2) 0.002(2) 0.0030(19) 0.000(2) C84 0.022(2) 0.056(3) 0.029(2) -0.013(2) -0.0074(19) 0.009(2) C58 0.024(2) 0.027(2) 0.045(3) -0.003(2) -0.012(2) 0.0017(18) C631 0.028(2) 0.034(3) 0.040(3) -0.003(2) -0.005(2) -0.005(2) C55 0.042(3) 0.042(3) 0.029(2) -0.012(2) -0.014(2) 0.004(2) C283 0.034(3) 0.037(3) 0.041(3) 0.002(2) -0.010(2) -0.010(2) C683 0.040(3) 0.028(2) 0.055(3) 0.009(2) -0.027(2) -0.007(2) C682 0.033(3) 0.046(3) 0.049(3) 0.001(2) -0.016(2) 0.003(2) C582 0.038(3) 0.030(3) 0.039(3) 0.002(2) -0.006(2) -0.008(2) C83 0.034(3) 0.033(3) 0.034(2) -0.010(2) -0.013(2) 0.011(2) C383 0.024(2) 0.036(3) 0.042(3) 0.001(2) -0.005(2) 0.005(2) C382 0.033(3) 0.032(2) 0.034(2) 0.0019(19) -0.015(2) -0.003(2) C381 0.037(3) 0.042(3) 0.042(3) 0.003(2) -0.022(2) -0.007(2) C651 0.029(3) 0.048(3) 0.036(3) -0.016(2) -0.009(2) 0.003(2) C681 0.035(3) 0.054(3) 0.042(3) 0.007(2) -0.025(2) -0.009(2) C581 0.041(3) 0.031(3) 0.061(3) -0.003(2) -0.012(3) 0.007(2) C35 0.057(4) 0.019(2) 0.099(5) -0.013(3) -0.059(4) 0.009(2) C72 0.047(3) 0.054(3) 0.028(2) -0.014(2) -0.005(2) 0.018(3) C151 0.052(3) 0.047(3) 0.026(2) -0.011(2) -0.010(2) 0.011(2) C33 0.022(2) 0.027(3) 0.095(4) 0.008(3) -0.028(3) 0.000(2) C431 0.057(4) 0.066(4) 0.023(2) -0.017(2) -0.003(2) -0.003(3) C251 0.037(3) 0.058(3) 0.031(2) -0.019(2) -0.012(2) 0.007(2) C76 0.046(3) 0.038(3) 0.048(3) -0.018(2) 0.016(3) -0.004(2) C281 0.039(3) 0.029(3) 0.067(4) 0.006(2) -0.018(3) 0.005(2) C34 0.035(3) 0.026(3) 0.125(6) -0.003(3) -0.051(4) -0.001(2) C551 0.055(4) 0.095(5) 0.033(3) -0.024(3) -0.019(3) 0.016(3) C73 0.046(4) 0.120(6) 0.043(3) -0.047(4) -0.025(3) 0.050(4) C351 0.105(6) 0.036(3) 0.124(6) -0.025(4) -0.090(5) 0.012(3) C74 0.033(4) 0.163(9) 0.057(4) -0.070(5) -0.005(3) -0.005(5) C75 0.056(4) 0.088(5) 0.074(5) -0.048(4) 0.021(4) -0.040(4) C331 0.030(3) 0.039(3) 0.134(6) 0.025(4) -0.019(4) -0.006(2) C1T 0.13(2) 0.046(12) 0.20(2) 0.050(14) -0.098(17) -0.005(12) C2T 0.24(3) 0.18(3) 0.26(3) 0.04(3) -0.02(3) 0.07(3) C3T 0.19(3) 0.21(3) 0.16(3) 0.00(2) -0.09(2) 0.03(2) C4T 0.18(3) 0.25(3) 0.16(3) -0.04(3) -0.13(2) 0.04(3) C5T 0.21(4) 0.33(5) 0.23(4) 0.16(4) 0.06(3) 0.10(3) C1TB 0.095(11) 0.098(10) 0.079(8) 0.039(7) -0.047(7) -0.026(7) C2TB 0.166(17) 0.25(3) 0.115(14) -0.036(16) -0.058(11) -0.003(15) C3TB 0.108(12) 0.24(2) 0.081(10) -0.054(11) -0.019(9) -0.046(10) C4TB 0.20(2) 0.22(2) 0.117(16) -0.044(15) 0.041(14) -0.029(15) C5TB 0.31(4) 0.33(4) 0.088(14) 0.053(18) 0.077(19) 0.11(3) C1SA 0.040(6) 0.040(6) 0.046(6) 0.001(5) -0.013(5) 0.004(5) C2SA 0.029(9) 0.029(7) 0.047(9) -0.010(7) -0.019(6) 0.003(6) C3SA 0.028(10) 0.030(10) 0.052(10) -0.019(10) -0.023(7) 0.002(7) C4SA 0.039(12) 0.047(12) 0.053(10) -0.012(8) -0.016(7) 0.010(9) C5SA 0.042(14) 0.060(18) 0.064(12) -0.024(12) -0.018(9) 0.016(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N1 1.966(3) . ? Ta1 N3 1.966(3) . ? Ta1 N2 1.970(3) . ? Ta1 C17 2.222(4) . ? Ta1 P1 2.5543(12) . ? Ta2 N6 1.967(3) . ? Ta2 N4 1.967(3) . ? Ta2 N5 1.972(3) . ? Ta2 C47 2.217(4) . ? Ta2 P2 2.5645(11) . ? P2 C81 1.838(4) . ? P1 C71 1.822(5) . ? N1 C11 1.410(5) . ? N1 C17 1.427(5) . ? N2 C21 1.440(5) . ? N2 C27 1.478(5) . ? N4 C41 1.407(5) . ? N4 C47 1.420(5) . ? N3 C31 1.435(5) . ? N3 C37 1.489(5) . ? N6 C61 1.443(5) . ? N6 C67 1.482(5) . ? N5 C51 1.431(5) . ? N5 C57 1.480(5) . ? C71 C76 1.387(7) . ? C71 C72 1.390(6) . ? C17 H17 1.006(18) . ? C17 C18 1.532(5) . ? C81 C82 1.393(6) . ? C81 C86 1.402(6) . ? C52 C51 1.395(6) . ? C52 C53 1.402(6) . ? C47 H47 0.994(19) . ? C47 C48 1.539(5) . ? C12 C11 1.389(6) . ? C12 C13 1.399(6) . ? C48 C481 1.524(6) . ? C48 C483 1.533(6) . ? C48 C482 1.537(6) . ? C16 C15 1.390(6) . ? C16 C11 1.404(6) . ? C41 C46 1.396(6) . ? C41 C42 1.416(6) . ? C181 C18 1.537(6) . ? C21 C22 1.392(5) . ? C21 C26 1.400(5) . ? C13 C14 1.398(6) . ? C13 C131 1.514(6) . ? C45 C46 1.393(6) . ? C45 C44 1.397(6) . ? C45 C451 1.511(6) . ? C24 C23 1.387(6) . ? C24 C25 1.397(6) . ? C18 C182 1.532(6) . ? C18 C183 1.533(6) . ? C42 C43 1.382(6) . ? C231 C23 1.512(5) . ? C51 C56 1.402(6) . ? C26 C25 1.386(6) . ? C62 C63 1.389(6) . ? C62 C61 1.401(5) . ? C23 C22 1.404(5) . ? C27 C28 1.539(6) . ? C67 C68 1.552(6) . ? C61 C66 1.388(6) . ? C53 C54 1.387(6) . ? C53 C531 1.520(6) . ? C85 C84 1.376(7) . ? C85 C86 1.401(6) . ? C25 C251 1.512(6) . ? C37 C38 1.548(6) . ? C15 C14 1.397(6) . ? C15 C151 1.513(6) . ? C56 C55 1.385(6) . ? C68 C682 1.524(6) . ? C68 C681 1.533(6) . ? C68 C683 1.536(6) . ? C54 C55 1.398(7) . ? C31 C36 1.390(6) . ? C31 C32 1.401(6) . ? C63 C64 1.403(6) . ? C63 C631 1.511(6) . ? C57 C58 1.545(6) . ? C282 C28 1.534(6) . ? C66 C65 1.399(6) . ? C82 C83 1.381(6) . ? C38 C383 1.522(6) . ? C38 C382 1.533(6) . ? C38 C381 1.542(6) . ? C43 C44 1.392(6) . ? C43 C431 1.506(6) . ? C36 C35 1.401(7) . ? C583 C58 1.541(6) . ? C65 C64 1.392(6) . ? C65 C651 1.512(6) . ? C28 C283 1.522(6) . ? C28 C281 1.544(6) . ? C32 C33 1.400(6) . ? C84 C83 1.379(7) . ? C58 C581 1.530(6) . ? C58 C582 1.530(6) . ? C55 C551 1.519(6) . ? C35 C34 1.378(9) . ? C35 C351 1.518(8) . ? C72 C73 1.421(8) . ? C33 C34 1.394(8) . ? C33 C331 1.498(8) . ? C76 C75 1.378(8) . ? C73 C74 1.362(10) . ? C74 C75 1.338(11) . ? C1T C2T 1.42(2) . ? C2T C3T 1.61(2) . ? C3T C4T 1.63(2) . ? C4T C5T 1.44(2) . ? C1TB C2TB 1.403(19) . ? C2TB C3TB 1.615(18) . ? C3TB C4TB 1.615(17) . ? C4TB C5TB 1.44(2) . ? C1SA C2SA 1.501(18) . ? C2SA C3SA 1.56(2) . ? C3SA C4SA 1.546(16) . ? C4SA C5SA 1.52(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ta1 N3 104.07(13) . . ? N1 Ta1 N2 96.66(13) . . ? N3 Ta1 N2 117.12(13) . . ? N1 Ta1 C17 39.25(13) . . ? N3 Ta1 C17 110.86(14) . . ? N2 Ta1 C17 121.75(14) . . ? N1 Ta1 P1 122.06(10) . . ? N3 Ta1 P1 106.44(10) . . ? N2 Ta1 P1 110.86(10) . . ? C17 Ta1 P1 83.76(11) . . ? N6 Ta2 N4 104.86(13) . . ? N6 Ta2 N5 116.85(13) . . ? N4 Ta2 N5 96.00(13) . . ? N6 Ta2 C47 110.36(14) . . ? N4 Ta2 C47 39.10(13) . . ? N5 Ta2 C47 122.17(14) . . ? N6 Ta2 P2 112.71(10) . . ? N4 Ta2 P2 121.27(9) . . ? N5 Ta2 P2 104.68(10) . . ? C47 Ta2 P2 85.03(10) . . ? C81 P2 Ta2 111.59(12) . . ? C71 P1 Ta1 111.94(14) . . ? C11 N1 C17 130.1(3) . . ? C11 N1 Ta1 132.1(2) . . ? C17 N1 Ta1 80.1(2) . . ? C21 N2 C27 116.9(3) . . ? C21 N2 Ta1 111.5(2) . . ? C27 N2 Ta1 128.7(2) . . ? C41 N4 C47 130.5(3) . . ? C41 N4 Ta2 135.6(3) . . ? C47 N4 Ta2 80.0(2) . . ? C31 N3 C37 116.2(3) . . ? C31 N3 Ta1 110.8(2) . . ? C37 N3 Ta1 129.7(3) . . ? C61 N6 C67 116.8(3) . . ? C61 N6 Ta2 108.5(2) . . ? C67 N6 Ta2 130.8(3) . . ? C51 N5 C57 117.3(3) . . ? C51 N5 Ta2 109.7(2) . . ? C57 N5 Ta2 130.6(3) . . ? C76 C71 C72 117.3(5) . . ? C76 C71 P1 123.5(4) . . ? C72 C71 P1 119.0(4) . . ? H17 C17 N1 114(2) . . ? H17 C17 C18 112(2) . . ? N1 C17 C18 119.3(3) . . ? H17 C17 Ta1 108(2) . . ? N1 C17 Ta1 60.64(19) . . ? C18 C17 Ta1 132.6(3) . . ? C82 C81 C86 116.9(4) . . ? C82 C81 P2 124.2(3) . . ? C86 C81 P2 118.9(3) . . ? C51 C52 C53 121.2(4) . . ? H47 C47 N4 115(2) . . ? H47 C47 C48 108(2) . . ? N4 C47 C48 119.9(3) . . ? H47 C47 Ta2 113(2) . . ? N4 C47 Ta2 60.90(19) . . ? C48 C47 Ta2 132.5(3) . . ? C11 C12 C13 120.6(4) . . ? C481 C48 C483 109.4(4) . . ? C481 C48 C482 108.5(3) . . ? C483 C48 C482 108.1(4) . . ? C481 C48 C47 108.6(3) . . ? C483 C48 C47 112.4(3) . . ? C482 C48 C47 109.9(3) . . ? C15 C16 C11 121.4(4) . . ? C46 C41 N4 123.0(4) . . ? C46 C41 C42 118.8(4) . . ? N4 C41 C42 118.2(4) . . ? C22 C21 C26 119.9(4) . . ? C22 C21 N2 119.3(4) . . ? C26 C21 N2 120.6(4) . . ? C14 C13 C12 119.1(4) . . ? C14 C13 C131 120.5(4) . . ? C12 C13 C131 120.4(4) . . ? C46 C45 C44 118.8(4) . . ? C46 C45 C451 120.2(4) . . ? C44 C45 C451 120.9(4) . . ? C23 C24 C25 121.9(4) . . ? C182 C18 C17 109.2(3) . . ? C182 C18 C183 109.9(4) . . ? C17 C18 C183 112.7(3) . . ? C182 C18 C181 107.9(3) . . ? C17 C18 C181 109.5(3) . . ? C183 C18 C181 107.4(4) . . ? C12 C11 C16 119.2(4) . . ? C12 C11 N1 123.3(4) . . ? C16 C11 N1 117.5(4) . . ? C43 C42 C41 121.2(4) . . ? C52 C51 C56 118.8(4) . . ? C52 C51 N5 119.4(4) . . ? C56 C51 N5 121.7(4) . . ? C25 C26 C21 120.4(4) . . ? C63 C62 C61 119.9(4) . . ? C24 C23 C22 118.5(4) . . ? C24 C23 C231 121.4(4) . . ? C22 C23 C231 120.1(4) . . ? C45 C46 C41 120.8(4) . . ? N2 C27 C28 117.1(3) . . ? N6 C67 C68 117.2(4) . . ? C66 C61 C62 120.1(4) . . ? C66 C61 N6 119.1(4) . . ? C62 C61 N6 120.6(4) . . ? C21 C22 C23 120.4(4) . . ? C54 C53 C52 118.4(4) . . ? C54 C53 C531 121.4(4) . . ? C52 C53 C531 120.2(4) . . ? C84 C85 C86 120.0(5) . . ? C26 C25 C24 118.9(4) . . ? C26 C25 C251 120.7(4) . . ? C24 C25 C251 120.4(4) . . ? N3 C37 C38 116.7(3) . . ? C16 C15 C14 118.3(4) . . ? C16 C15 C151 121.0(4) . . ? C14 C15 C151 120.7(4) . . ? C55 C56 C51 121.0(4) . . ? C682 C68 C681 110.2(4) . . ? C682 C68 C683 110.3(4) . . ? C681 C68 C683 108.0(4) . . ? C682 C68 C67 110.5(3) . . ? C681 C68 C67 106.0(4) . . ? C683 C68 C67 111.7(4) . . ? C85 C86 C81 121.4(4) . . ? C53 C54 C55 121.6(4) . . ? C36 C31 C32 119.9(4) . . ? C36 C31 N3 118.4(4) . . ? C32 C31 N3 121.6(4) . . ? C62 C63 C64 119.1(4) . . ? C62 C63 C631 120.4(4) . . ? C64 C63 C631 120.4(4) . . ? N5 C57 C58 116.9(3) . . ? C61 C66 C65 120.9(4) . . ? C83 C82 C81 121.6(4) . . ? C383 C38 C382 110.5(4) . . ? C383 C38 C381 109.4(4) . . ? C382 C38 C381 108.0(3) . . ? C383 C38 C37 110.4(3) . . ? C382 C38 C37 112.3(3) . . ? C381 C38 C37 106.0(4) . . ? C42 C43 C44 118.6(4) . . ? C42 C43 C431 120.6(4) . . ? C44 C43 C431 120.8(4) . . ? C31 C36 C35 120.7(5) . . ? C64 C65 C66 118.2(4) . . ? C64 C65 C651 121.0(4) . . ? C66 C65 C651 120.8(4) . . ? C15 C14 C13 121.4(4) . . ? C283 C28 C282 109.4(4) . . ? C283 C28 C27 111.7(4) . . ? C282 C28 C27 112.0(4) . . ? C283 C28 C281 109.8(4) . . ? C282 C28 C281 108.2(4) . . ? C27 C28 C281 105.5(4) . . ? C65 C64 C63 121.6(4) . . ? C33 C32 C31 120.1(5) . . ? C43 C44 C45 121.8(4) . . ? C85 C84 C83 119.3(4) . . ? C581 C58 C582 110.0(4) . . ? C581 C58 C583 109.5(4) . . ? C582 C58 C583 108.3(4) . . ? C581 C58 C57 106.0(4) . . ? C582 C58 C57 110.6(4) . . ? C583 C58 C57 112.5(4) . . ? C56 C55 C54 119.0(4) . . ? C56 C55 C551 120.3(5) . . ? C54 C55 C551 120.6(4) . . ? C84 C83 C82 120.9(4) . . ? C34 C35 C36 118.3(5) . . ? C34 C35 C351 121.2(5) . . ? C36 C35 C351 120.5(6) . . ? C71 C72 C73 119.8(6) . . ? C34 C33 C32 118.3(5) . . ? C34 C33 C331 121.4(5) . . ? C32 C33 C331 120.3(6) . . ? C75 C76 C71 122.0(6) . . ? C35 C34 C33 122.7(5) . . ? C74 C73 C72 119.7(6) . . ? C75 C74 C73 120.9(6) . . ? C74 C75 C76 120.3(7) . . ? C1T C2T C3T 130(3) . . ? C2T C3T C4T 161(3) . . ? C5T C4T C3T 124(3) . . ? C1TB C2TB C3TB 125.1(18) . . ? C4TB C3TB C2TB 143.7(18) . . ? C5TB C4TB C3TB 132(2) . . ? C1SA C2SA C3SA 112.7(16) . . ? C4SA C3SA C2SA 114.0(10) . . ? C5SA C4SA C3SA 114.1(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.785 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.125 # Attachment '- 10106_e.cif' data_10106_e _database_code_depnum_ccdc_archive 'CCDC 852397' #TrackingRef '- 10106_e.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ar(tBuCH2)N)3TaPCy _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H71 N3 P Ta' _chemical_formula_weight 865.97 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9320(12) _cell_length_b 11.5291(12) _cell_length_c 18.468(2) _cell_angle_alpha 102.234(2) _cell_angle_beta 91.533(2) _cell_angle_gamma 103.933(2) _cell_volume 2200.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.38 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 2.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5335 _exptl_absorpt_correction_T_max 0.8019 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 51261 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 30.47 _reflns_number_total 13168 _reflns_number_gt 11355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _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^ > 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. The disordered tert-butyl portion of the neo-pentyl substituent attached to N1 was refined within SHELXL with the help of rigid bond restraints as well as similarity restraints on the anisotropic displacement parameters for neighboring atoms and on 1,2- and 1,3-distances throughout the disordered components. The hydrogen atom attached to C41 was located in the Fourier difference map and refined using an appropriate distance restraint. ; _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^)+(0.0244P)^2^+1.4693P] 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 13168 _refine_ls_number_parameters 503 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.118 _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 Ta1 Ta 0.904439(11) 0.737989(10) 0.752189(7) 0.01990(4) Uani 1 1 d . . . P1 P 1.09529(8) 0.71520(8) 0.79245(5) 0.02880(17) Uani 1 1 d D . . N1 N 0.9489(2) 0.8164(2) 0.66678(13) 0.0223(5) Uani 1 1 d . B . N2 N 0.8136(2) 0.82308(19) 0.82903(13) 0.0194(5) Uani 1 1 d . . . N3 N 0.7996(2) 0.5629(2) 0.71927(14) 0.0236(5) Uani 1 1 d . . . C11 C 0.8449(3) 0.8207(2) 0.61826(16) 0.0225(6) Uani 1 1 d . . . C12 C 0.7782(3) 0.9103(3) 0.63833(17) 0.0244(6) Uani 1 1 d . . . H12 H 0.8031 0.9701 0.6836 0.029 Uiso 1 1 calc R . . C13 C 0.6755(3) 0.9134(3) 0.59291(19) 0.0299(7) Uani 1 1 d . . . C14 C 0.6391(3) 0.8235(3) 0.52729(19) 0.0369(8) Uani 1 1 d . . . H14 H 0.5684 0.8239 0.4964 0.044 Uiso 1 1 calc R . . C15 C 0.7036(3) 0.7333(3) 0.50582(18) 0.0362(8) Uani 1 1 d . . . C16 C 0.8062(3) 0.7334(3) 0.55117(17) 0.0297(7) Uani 1 1 d . . . H16 H 0.8516 0.6728 0.5365 0.036 Uiso 1 1 calc R . . C17 C 1.0714(3) 0.8332(3) 0.63114(18) 0.0281(6) Uani 1 1 d . . . H17A H 1.1200 0.7806 0.6484 0.034 Uiso 1 1 calc R A 1 H17B H 1.0521 0.8023 0.5768 0.034 Uiso 1 1 calc R A 1 C18 C 1.1542(15) 0.9587(15) 0.6444(6) 0.034(3) Uani 0.504(8) 1 d PDU B 1 C181 C 1.0836(6) 1.0524(6) 0.6299(5) 0.038(2) Uani 0.504(8) 1 d PDU B 1 H18A H 1.1423 1.1340 0.6396 0.057 Uiso 0.504(8) 1 calc PR B 1 H18B H 1.0148 1.0537 0.6628 0.057 Uiso 0.504(8) 1 calc PR B 1 H18C H 1.0484 1.0295 0.5780 0.057 Uiso 0.504(8) 1 calc PR B 1 C182 C 1.2549(13) 0.9519(18) 0.5873(7) 0.045(3) Uani 0.504(8) 1 d PDU B 1 H18D H 1.3137 1.0329 0.5933 0.067 Uiso 0.504(8) 1 calc PR B 1 H18E H 1.2131 0.9258 0.5368 0.067 Uiso 0.504(8) 1 calc PR B 1 H18F H 1.3018 0.8927 0.5956 0.067 Uiso 0.504(8) 1 calc PR B 1 C183 C 1.2142(7) 0.9971(6) 0.7235(4) 0.043(2) Uani 0.504(8) 1 d PDU B 1 H18G H 1.2690 1.0805 0.7321 0.064 Uiso 0.504(8) 1 calc PR B 1 H18H H 1.2645 0.9405 0.7315 0.064 Uiso 0.504(8) 1 calc PR B 1 H18I H 1.1478 0.9954 0.7582 0.064 Uiso 0.504(8) 1 calc PR B 1 C58 C 1.1412(14) 0.9704(13) 0.6296(6) 0.027(2) Uani 0.496(8) 1 d PDU B 2 C581 C 1.0774(7) 1.0140(7) 0.5689(5) 0.040(2) Uani 0.496(8) 1 d PDU B 2 H58A H 1.0735 0.9566 0.5210 0.060 Uiso 0.496(8) 1 calc PR B 2 H58B H 1.1265 1.0958 0.5659 0.060 Uiso 0.496(8) 1 calc PR B 2 H58C H 0.9916 1.0175 0.5812 0.060 Uiso 0.496(8) 1 calc PR B 2 C582 C 1.2781(12) 0.9685(19) 0.6104(7) 0.036(3) Uani 0.496(8) 1 d PDU B 2 H58D H 1.2757 0.9118 0.5623 0.055 Uiso 0.496(8) 1 calc PR B 2 H58E H 1.3198 0.9415 0.6491 0.055 Uiso 0.496(8) 1 calc PR B 2 H58F H 1.3253 1.0511 0.6077 0.055 Uiso 0.496(8) 1 calc PR B 2 C583 C 1.1472(9) 1.0592(8) 0.7041(5) 0.058(3) Uani 0.496(8) 1 d PD B 2 H58G H 1.1886 1.0317 0.7426 0.088 Uiso 0.496(8) 1 calc PR B 2 H58H H 1.0613 1.0621 0.7167 0.088 Uiso 0.496(8) 1 calc PR B 2 H58I H 1.1955 1.1413 0.7010 0.088 Uiso 0.496(8) 1 calc PR B 2 C21 C 0.7923(3) 0.9407(2) 0.82873(15) 0.0210(5) Uani 1 1 d . . . C22 C 0.8968(3) 1.0385(2) 0.83155(16) 0.0252(6) Uani 1 1 d . . . H22 H 0.9794 1.0264 0.8359 0.030 Uiso 1 1 calc R . . C23 C 0.8820(3) 1.1545(3) 0.82804(17) 0.0317(7) Uani 1 1 d . . . C24 C 0.7611(4) 1.1704(3) 0.82269(18) 0.0381(8) Uani 1 1 d . . . H24 H 0.7501 1.2489 0.8206 0.046 Uiso 1 1 calc R . . C25 C 0.6548(3) 1.0739(3) 0.82022(18) 0.0335(7) Uani 1 1 d . . . C26 C 0.6709(3) 0.9579(3) 0.82255(17) 0.0269(6) Uani 1 1 d . . . H26 H 0.5992 0.8910 0.8199 0.032 Uiso 1 1 calc R . . C27 C 0.7389(3) 0.7528(2) 0.87892(15) 0.0197(5) Uani 1 1 d . . . H27A H 0.7475 0.6675 0.8654 0.024 Uiso 1 1 calc R . . H27B H 0.6487 0.7498 0.8687 0.024 Uiso 1 1 calc R . . C28 C 0.7733(3) 0.8012(2) 0.96355(16) 0.0219(6) Uani 1 1 d . . . C31 C 0.6660(3) 0.5491(2) 0.72270(16) 0.0219(6) Uani 1 1 d . . . C32 C 0.6062(3) 0.6224(2) 0.69055(16) 0.0235(6) Uani 1 1 d . . . H32 H 0.6523 0.6734 0.6611 0.028 Uiso 1 1 calc R . . C33 C 0.4797(3) 0.6224(2) 0.70081(16) 0.0236(6) Uani 1 1 d . . . C34 C 0.4117(3) 0.5441(2) 0.74191(16) 0.0248(6) Uani 1 1 d . . . H34 H 0.3257 0.5430 0.7489 0.030 Uiso 1 1 calc R . . C35 C 0.4677(3) 0.4671(2) 0.77308(17) 0.0254(6) Uani 1 1 d . . . C36 C 0.5944(3) 0.4710(2) 0.76373(16) 0.0243(6) Uani 1 1 d . . . H36 H 0.6333 0.4198 0.7855 0.029 Uiso 1 1 calc R . . C37 C 0.8437(3) 0.4483(3) 0.70601(18) 0.0284(7) Uani 1 1 d . . . H37A H 0.7783 0.3835 0.7206 0.034 Uiso 1 1 calc R . . H37B H 0.9213 0.4629 0.7391 0.034 Uiso 1 1 calc R . . C38 C 0.8723(3) 0.4001(3) 0.62560(18) 0.0325(7) Uani 1 1 d . . . C41 C 1.1609(3) 0.7249(2) 0.88790(17) 0.0220(6) Uani 1 1 d D . . H41 H 1.125(3) 0.782(3) 0.9219(18) 0.026 Uiso 1 1 d . . . C42 C 1.1213(3) 0.5990(2) 0.90766(17) 0.0253(6) Uani 1 1 d . . . H42A H 1.0279 0.5716 0.9040 0.030 Uiso 1 1 calc R . . H42B H 1.1525 0.5387 0.8712 0.030 Uiso 1 1 calc R . . C43 C 1.1730(3) 0.6019(3) 0.98594(18) 0.0323(7) Uani 1 1 d . . . H43A H 1.1342 0.6547 1.0229 0.039 Uiso 1 1 calc R . . H43B H 1.1498 0.5180 0.9950 0.039 Uiso 1 1 calc R . . C44 C 1.3167(3) 0.6508(3) 0.9960(2) 0.0354(8) Uani 1 1 d . . . H44A H 1.3469 0.6574 1.0481 0.042 Uiso 1 1 calc R . . H44B H 1.3564 0.5931 0.9632 0.042 Uiso 1 1 calc R . . C45 C 1.3555(3) 0.7764(3) 0.9772(2) 0.0342(7) Uani 1 1 d . . . H45A H 1.4489 0.8051 0.9819 0.041 Uiso 1 1 calc R . . H45B H 1.3224 0.8357 1.0132 0.041 Uiso 1 1 calc R . . C46 C 1.3059(3) 0.7732(3) 0.89843(19) 0.0282(7) Uani 1 1 d . . . H46A H 1.3447 0.7195 0.8620 0.034 Uiso 1 1 calc R . . H46B H 1.3303 0.8568 0.8890 0.034 Uiso 1 1 calc R . . C131 C 0.6058(3) 1.0119(3) 0.6139(2) 0.0446(9) Uani 1 1 d . . . H13A H 0.6030 1.0530 0.5728 0.067 Uiso 1 1 calc R . . H13B H 0.6497 1.0720 0.6583 0.067 Uiso 1 1 calc R . . H13C H 0.5195 0.9750 0.6243 0.067 Uiso 1 1 calc R . . C151 C 0.6623(5) 0.6367(4) 0.4344(2) 0.0588(12) Uani 1 1 d . . . H15A H 0.6045 0.6624 0.4032 0.088 Uiso 1 1 calc R . . H15B H 0.6191 0.5586 0.4459 0.088 Uiso 1 1 calc R . . H15C H 0.7367 0.6264 0.4077 0.088 Uiso 1 1 calc R . . C231 C 0.9973(4) 1.2603(3) 0.8320(2) 0.0435(9) Uani 1 1 d . . . H23A H 1.0314 1.2936 0.8838 0.065 Uiso 1 1 calc R . . H23B H 0.9732 1.3246 0.8120 0.065 Uiso 1 1 calc R . . H23C H 1.0617 1.2312 0.8026 0.065 Uiso 1 1 calc R . . C251 C 0.5226(4) 1.0928(4) 0.8154(2) 0.0499(10) Uani 1 1 d . . . H25A H 0.5021 1.1295 0.8650 0.075 Uiso 1 1 calc R . . H25B H 0.4618 1.0136 0.7962 0.075 Uiso 1 1 calc R . . H25C H 0.5186 1.1477 0.7820 0.075 Uiso 1 1 calc R . . C281 C 0.6942(3) 0.7050(3) 1.00141(19) 0.0303(7) Uani 1 1 d . . . H28G H 0.7157 0.6265 0.9843 0.045 Uiso 1 1 calc R . . H28H H 0.6041 0.6950 0.9886 0.045 Uiso 1 1 calc R . . H28I H 0.7125 0.7324 1.0554 0.045 Uiso 1 1 calc R . . C282 C 0.7428(3) 0.9254(3) 0.99403(18) 0.0294(7) Uani 1 1 d . . . H28D H 0.7559 0.9461 1.0484 0.044 Uiso 1 1 calc R . . H28E H 0.6545 0.9198 0.9790 0.044 Uiso 1 1 calc R . . H28F H 0.7986 0.9892 0.9741 0.044 Uiso 1 1 calc R . . C283 C 0.9128(3) 0.8141(3) 0.98152(17) 0.0271(6) Uani 1 1 d . . . H28A H 0.9338 0.8446 1.0352 0.041 Uiso 1 1 calc R . . H28B H 0.9631 0.8721 0.9552 0.041 Uiso 1 1 calc R . . H28C H 0.9317 0.7340 0.9658 0.041 Uiso 1 1 calc R . . C331 C 0.4171(3) 0.7035(3) 0.6662(2) 0.0337(7) Uani 1 1 d . . . H33A H 0.3318 0.6972 0.6827 0.051 Uiso 1 1 calc R . . H33B H 0.4120 0.6770 0.6119 0.051 Uiso 1 1 calc R . . H33C H 0.4671 0.7888 0.6816 0.051 Uiso 1 1 calc R . . C351 C 0.3933(3) 0.3840(3) 0.8184(2) 0.0356(8) Uani 1 1 d . . . H35A H 0.3654 0.3003 0.7879 0.053 Uiso 1 1 calc R . . H35B H 0.3194 0.4133 0.8348 0.053 Uiso 1 1 calc R . . H35C H 0.4469 0.3845 0.8619 0.053 Uiso 1 1 calc R . . C381 C 0.7575(4) 0.3773(3) 0.5718(2) 0.0490(10) Uani 1 1 d . . . H38G H 0.6867 0.3184 0.5859 0.073 Uiso 1 1 calc R . . H38H H 0.7773 0.3440 0.5214 0.073 Uiso 1 1 calc R . . H38I H 0.7342 0.4546 0.5732 0.073 Uiso 1 1 calc R . . C382 C 0.9853(4) 0.4913(3) 0.6038(2) 0.0394(8) Uani 1 1 d . . . H38D H 1.0066 0.4569 0.5540 0.059 Uiso 1 1 calc R . . H38E H 1.0583 0.5064 0.6396 0.059 Uiso 1 1 calc R . . H38F H 0.9629 0.5688 0.6041 0.059 Uiso 1 1 calc R . . C383 C 0.9118(4) 0.2806(3) 0.6243(2) 0.0409(9) Uani 1 1 d . . . H38A H 0.8436 0.2222 0.6409 0.061 Uiso 1 1 calc R . . H38B H 0.9885 0.2980 0.6576 0.061 Uiso 1 1 calc R . . H38C H 0.9285 0.2452 0.5736 0.061 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 0.02184(6) 0.01926(5) 0.02204(6) 0.00879(4) 0.00381(4) 0.00787(4) P1 0.0277(4) 0.0379(4) 0.0285(4) 0.0138(3) 0.0054(3) 0.0172(3) N1 0.0225(12) 0.0204(11) 0.0250(13) 0.0094(9) 0.0017(10) 0.0034(9) N2 0.0220(11) 0.0149(10) 0.0215(12) 0.0050(8) 0.0007(9) 0.0042(8) N3 0.0268(12) 0.0194(11) 0.0289(14) 0.0093(9) 0.0070(10) 0.0100(9) C11 0.0239(14) 0.0224(13) 0.0221(14) 0.0104(10) 0.0023(11) 0.0028(11) C12 0.0235(14) 0.0221(13) 0.0275(16) 0.0098(11) 0.0020(11) 0.0019(11) C13 0.0238(14) 0.0290(15) 0.0378(18) 0.0180(13) -0.0009(13) -0.0005(12) C14 0.0305(17) 0.0432(19) 0.0360(19) 0.0230(15) -0.0086(14) -0.0034(14) C15 0.0416(19) 0.0346(17) 0.0262(17) 0.0117(13) -0.0041(14) -0.0054(14) C16 0.0370(17) 0.0255(14) 0.0256(16) 0.0091(12) 0.0031(13) 0.0030(12) C17 0.0269(15) 0.0323(15) 0.0336(17) 0.0180(13) 0.0116(13) 0.0131(12) C18 0.022(4) 0.030(4) 0.054(6) 0.020(5) 0.002(4) 0.008(3) C181 0.026(3) 0.025(3) 0.067(6) 0.027(3) 0.000(3) 0.002(2) C182 0.030(6) 0.046(6) 0.068(8) 0.033(7) 0.007(5) 0.008(5) C183 0.028(3) 0.027(3) 0.065(5) 0.012(3) -0.017(3) -0.008(3) C58 0.024(5) 0.027(5) 0.027(4) 0.008(3) 0.006(3) 0.000(3) C581 0.033(4) 0.034(4) 0.064(6) 0.033(4) 0.009(4) 0.010(3) C582 0.021(4) 0.055(7) 0.042(6) 0.030(6) 0.008(4) 0.008(5) C583 0.058(6) 0.044(5) 0.054(6) -0.003(4) 0.016(4) -0.015(4) C21 0.0293(14) 0.0160(12) 0.0186(14) 0.0044(10) 0.0025(11) 0.0071(10) C22 0.0319(15) 0.0204(13) 0.0221(15) 0.0056(10) 0.0015(12) 0.0035(11) C23 0.052(2) 0.0175(13) 0.0235(16) 0.0065(11) 0.0016(14) 0.0039(13) C24 0.070(3) 0.0225(15) 0.0286(18) 0.0088(12) 0.0070(17) 0.0219(16) C25 0.048(2) 0.0341(17) 0.0288(17) 0.0125(13) 0.0085(15) 0.0243(15) C26 0.0320(16) 0.0255(14) 0.0262(16) 0.0077(11) 0.0039(12) 0.0114(12) C27 0.0193(12) 0.0142(11) 0.0268(15) 0.0080(10) 0.0043(11) 0.0034(9) C28 0.0230(13) 0.0205(13) 0.0277(15) 0.0114(11) 0.0080(11) 0.0100(10) C31 0.0266(14) 0.0156(12) 0.0236(15) 0.0036(10) 0.0034(11) 0.0061(10) C32 0.0275(14) 0.0193(12) 0.0222(14) 0.0059(10) 0.0017(11) 0.0019(11) C33 0.0267(14) 0.0192(13) 0.0245(15) 0.0037(10) 0.0009(12) 0.0063(11) C34 0.0260(14) 0.0218(13) 0.0249(15) 0.0034(11) 0.0049(12) 0.0039(11) C35 0.0317(15) 0.0160(12) 0.0258(15) 0.0022(10) 0.0075(12) 0.0025(11) C36 0.0319(15) 0.0153(12) 0.0275(15) 0.0067(10) 0.0068(12) 0.0073(11) C37 0.0386(17) 0.0214(13) 0.0331(17) 0.0135(12) 0.0114(14) 0.0152(12) C38 0.047(2) 0.0237(14) 0.0314(17) 0.0049(12) 0.0068(15) 0.0188(14) C41 0.0219(13) 0.0185(12) 0.0272(15) 0.0071(11) 0.0011(11) 0.0065(10) C42 0.0252(14) 0.0191(13) 0.0311(16) 0.0063(11) 0.0006(12) 0.0044(11) C43 0.0395(18) 0.0293(15) 0.0336(18) 0.0127(13) 0.0017(14) 0.0146(13) C44 0.0387(19) 0.0349(17) 0.0358(19) 0.0060(14) -0.0072(15) 0.0184(14) C45 0.0248(15) 0.0277(15) 0.045(2) -0.0005(14) -0.0062(14) 0.0062(12) C46 0.0212(14) 0.0173(13) 0.0453(19) 0.0045(12) 0.0053(13) 0.0053(10) C131 0.0280(17) 0.0385(19) 0.073(3) 0.0240(18) -0.0058(17) 0.0097(15) C151 0.073(3) 0.054(2) 0.035(2) 0.0005(18) -0.017(2) -0.002(2) C231 0.067(3) 0.0199(15) 0.037(2) 0.0097(13) 0.0006(18) -0.0038(15) C251 0.060(3) 0.058(2) 0.052(2) 0.0228(19) 0.013(2) 0.043(2) C281 0.0304(16) 0.0304(15) 0.0392(19) 0.0194(13) 0.0142(14) 0.0138(13) C282 0.0368(17) 0.0234(14) 0.0326(17) 0.0093(12) 0.0113(14) 0.0132(12) C283 0.0259(15) 0.0309(15) 0.0265(16) 0.0083(12) 0.0034(12) 0.0090(12) C331 0.0283(16) 0.0327(16) 0.045(2) 0.0192(14) 0.0029(14) 0.0087(13) C351 0.0407(19) 0.0269(15) 0.044(2) 0.0158(14) 0.0192(16) 0.0090(13) C381 0.071(3) 0.039(2) 0.039(2) -0.0017(16) -0.0044(19) 0.0267(19) C382 0.061(2) 0.0345(17) 0.0329(19) 0.0144(14) 0.0220(17) 0.0241(16) C383 0.063(2) 0.0278(16) 0.040(2) 0.0083(14) 0.0151(18) 0.0248(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N2 1.979(2) . ? Ta1 N1 1.994(2) . ? Ta1 N3 2.021(2) . ? Ta1 P1 2.2888(8) . ? P1 C41 1.856(3) . ? N1 C11 1.445(4) . ? N1 C17 1.498(4) . ? N2 C21 1.431(3) . ? N2 C27 1.486(3) . ? N3 C31 1.435(4) . ? N3 C37 1.488(3) . ? C11 C12 1.397(4) . ? C11 C16 1.402(4) . ? C12 C13 1.396(4) . ? C13 C14 1.395(5) . ? C13 C131 1.505(5) . ? C14 C15 1.388(5) . ? C15 C16 1.381(5) . ? C15 C151 1.513(5) . ? C17 C18 1.476(19) . ? C17 C58 1.588(16) . ? C18 C183 1.515(12) . ? C18 C181 1.532(12) . ? C18 C182 1.549(12) . ? C58 C583 1.522(12) . ? C58 C581 1.536(11) . ? C58 C582 1.551(12) . ? C21 C22 1.390(4) . ? C21 C26 1.394(4) . ? C22 C23 1.400(4) . ? C23 C24 1.381(5) . ? C23 C231 1.516(4) . ? C24 C25 1.394(5) . ? C25 C26 1.400(4) . ? C25 C251 1.515(5) . ? C27 C28 1.547(4) . ? C28 C283 1.517(4) . ? C28 C281 1.537(4) . ? C28 C282 1.542(4) . ? C31 C32 1.397(4) . ? C31 C36 1.407(4) . ? C32 C33 1.401(4) . ? C33 C34 1.393(4) . ? C33 C331 1.513(4) . ? C34 C35 1.397(4) . ? C35 C36 1.392(4) . ? C35 C351 1.510(4) . ? C37 C38 1.540(4) . ? C38 C381 1.515(5) . ? C38 C383 1.536(4) . ? C38 C382 1.541(5) . ? C41 H41 0.97(3) . ? C41 C42 1.535(4) . ? C41 C46 1.540(4) . ? C42 C43 1.529(4) . ? C43 C44 1.528(5) . ? C44 C45 1.524(5) . ? C45 C46 1.528(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 N2 Ta1 N1 116.11(9) . . ? N2 Ta1 N3 106.80(9) . . ? N1 Ta1 N3 112.40(10) . . ? N2 Ta1 P1 115.71(7) . . ? N1 Ta1 P1 102.31(7) . . ? N3 Ta1 P1 102.87(7) . . ? C41 P1 Ta1 130.07(10) . . ? C11 N1 C17 112.6(2) . . ? C11 N1 Ta1 116.82(17) . . ? C17 N1 Ta1 127.22(19) . . ? C21 N2 C27 116.6(2) . . ? C21 N2 Ta1 122.82(18) . . ? C27 N2 Ta1 119.10(16) . . ? C31 N3 C37 116.6(2) . . ? C31 N3 Ta1 114.18(17) . . ? C37 N3 Ta1 128.2(2) . . ? C12 C11 C16 118.4(3) . . ? C12 C11 N1 120.5(3) . . ? C16 C11 N1 121.0(3) . . ? C13 C12 C11 121.1(3) . . ? C14 C13 C12 118.5(3) . . ? C14 C13 C131 120.7(3) . . ? C12 C13 C131 120.9(3) . . ? C15 C14 C13 121.8(3) . . ? C16 C15 C14 118.6(3) . . ? C16 C15 C151 120.6(4) . . ? C14 C15 C151 120.8(3) . . ? C15 C16 C11 121.6(3) . . ? C18 C17 N1 117.5(6) . . ? C18 C17 C58 13.2(6) . . ? N1 C17 C58 115.9(5) . . ? C17 C18 C183 109.8(9) . . ? C17 C18 C181 112.6(10) . . ? C183 C18 C181 109.7(10) . . ? C17 C18 C182 105.3(11) . . ? C183 C18 C182 111.5(11) . . ? C181 C18 C182 107.9(11) . . ? C583 C58 C581 109.6(9) . . ? C583 C58 C582 108.6(11) . . ? C581 C58 C582 108.9(10) . . ? C583 C58 C17 112.7(9) . . ? C581 C58 C17 110.9(9) . . ? C582 C58 C17 106.0(10) . . ? C22 C21 C26 119.8(3) . . ? C22 C21 N2 118.2(3) . . ? C26 C21 N2 122.0(2) . . ? C21 C22 C23 120.9(3) . . ? C24 C23 C22 118.6(3) . . ? C24 C23 C231 121.3(3) . . ? C22 C23 C231 120.1(3) . . ? C23 C24 C25 121.6(3) . . ? C24 C25 C26 119.2(3) . . ? C24 C25 C251 121.1(3) . . ? C26 C25 C251 119.7(3) . . ? C21 C26 C25 119.9(3) . . ? N2 C27 C28 117.1(2) . . ? C283 C28 C281 109.5(2) . . ? C283 C28 C282 109.0(2) . . ? C281 C28 C282 108.6(2) . . ? C283 C28 C27 110.0(2) . . ? C281 C28 C27 106.6(2) . . ? C282 C28 C27 113.1(2) . . ? C32 C31 C36 118.2(3) . . ? C32 C31 N3 119.9(2) . . ? C36 C31 N3 121.6(3) . . ? C31 C32 C33 121.4(3) . . ? C34 C33 C32 118.8(3) . . ? C34 C33 C331 120.6(3) . . ? C32 C33 C331 120.6(3) . . ? C33 C34 C35 121.2(3) . . ? C36 C35 C34 119.0(3) . . ? C36 C35 C351 120.4(3) . . ? C34 C35 C351 120.6(3) . . ? C35 C36 C31 121.3(3) . . ? N3 C37 C38 115.6(2) . . ? C381 C38 C383 110.8(3) . . ? C381 C38 C37 111.1(3) . . ? C383 C38 C37 106.7(3) . . ? C381 C38 C382 110.4(3) . . ? C383 C38 C382 107.5(3) . . ? C37 C38 C382 110.2(3) . . ? H41 C41 C42 108.3(19) . . ? H41 C41 C46 108.0(19) . . ? C42 C41 C46 109.9(2) . . ? H41 C41 P1 107.5(19) . . ? C42 C41 P1 110.11(19) . . ? C46 C41 P1 112.9(2) . . ? C43 C42 C41 112.3(2) . . ? C44 C43 C42 111.3(3) . . ? C45 C44 C43 110.3(3) . . ? C44 C45 C46 111.9(3) . . ? C45 C46 C41 110.9(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.449 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.112 # Attachment '- 10245_mr.cif' data_10245_mr _database_code_depnum_ccdc_archive 'CCDC 852398' #TrackingRef '- 10245_mr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ar(tBuCH2)N)2(tBuC(H)NAr)TaPPh2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H69 N3 P Ta' _chemical_formula_weight 936.01 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9124(7) _cell_length_b 11.6952(7) _cell_length_c 19.3712(12) _cell_angle_alpha 90.0170(10) _cell_angle_beta 101.3980(10) _cell_angle_gamma 103.3620(10) _cell_volume 2355.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 31.02 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6855 _exptl_absorpt_correction_T_max 0.8218 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _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 Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 51078 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13630 _reflns_number_gt 12042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.6741P] 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 13630 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.009 _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 0.582177(8) 1.677665(8) 0.218653(5) 0.01273(3) Uani 1 1 d . . . P1 P 0.53013(6) 1.55711(5) 0.10358(3) 0.01577(11) Uani 1 1 d . . . N1 N 0.68502(19) 1.84174(17) 0.23417(10) 0.0178(4) Uani 1 1 d . . . N2 N 0.40034(18) 1.68196(17) 0.21726(10) 0.0162(4) Uani 1 1 d . . . N3 N 0.67918(18) 1.59313(17) 0.28887(10) 0.0167(4) Uani 1 1 d . . . C11 C 0.7490(2) 1.91278(19) 0.29475(11) 0.0157(4) Uani 1 1 d . . . C12 C 0.8821(2) 1.9573(2) 0.31009(12) 0.0194(5) Uani 1 1 d . . . H12 H 0.9322 1.9428 0.2776 0.023 Uiso 1 1 calc R . . C13 C 0.9422(2) 2.0231(2) 0.37299(13) 0.0240(5) Uani 1 1 d . . . C14 C 0.8679(3) 2.0463(2) 0.41938(13) 0.0263(5) Uani 1 1 d . . . H14 H 0.9086 2.0916 0.4619 0.032 Uiso 1 1 calc R . . C15 C 0.7349(3) 2.0045(2) 0.40484(13) 0.0240(5) Uani 1 1 d . . . C16 C 0.6764(2) 1.9379(2) 0.34279(12) 0.0194(5) Uani 1 1 d . . . H16 H 0.5856 1.9088 0.3326 0.023 Uiso 1 1 calc R . . C17 C 0.7331(2) 1.8017(2) 0.17813(12) 0.0185(5) Uani 1 1 d D . . H17 H 0.8209(18) 1.784(2) 0.1939(13) 0.022 Uiso 1 1 d D . . C18 C 0.7315(2) 1.8723(2) 0.11064(12) 0.0177(4) Uani 1 1 d . . . C21 C 0.3375(2) 1.6219(2) 0.26981(12) 0.0169(4) Uani 1 1 d . . . C22 C 0.3845(2) 1.6612(2) 0.34037(12) 0.0196(5) Uani 1 1 d . . . H22 H 0.4555 1.7272 0.3521 0.024 Uiso 1 1 calc R . . C23 C 0.3284(3) 1.6046(2) 0.39375(13) 0.0245(5) Uani 1 1 d . . . C24 C 0.2235(2) 1.5090(2) 0.37497(13) 0.0250(5) Uani 1 1 d . . . H24 H 0.1841 1.4704 0.4109 0.030 Uiso 1 1 calc R . . C25 C 0.1745(2) 1.4683(2) 0.30525(13) 0.0210(5) Uani 1 1 d . . . C26 C 0.2332(2) 1.5250(2) 0.25277(12) 0.0185(5) Uani 1 1 d . . . H26 H 0.2019 1.4972 0.2050 0.022 Uiso 1 1 calc R . . C27 C 0.3183(2) 1.7237(2) 0.15760(12) 0.0188(5) Uani 1 1 d . . . H27A H 0.2499 1.6552 0.1355 0.023 Uiso 1 1 calc R . . H27B H 0.3715 1.7515 0.1223 0.023 Uiso 1 1 calc R . . C28 C 0.2525(2) 1.8228(2) 0.17245(13) 0.0219(5) Uani 1 1 d . . . C31 C 0.6317(2) 1.4684(2) 0.29433(11) 0.0156(4) Uani 1 1 d . . . C32 C 0.5293(2) 1.4247(2) 0.32693(12) 0.0190(5) Uani 1 1 d . . . H32 H 0.4879 1.4774 0.3453 0.023 Uiso 1 1 calc R . . C33 C 0.4865(2) 1.3034(2) 0.33288(13) 0.0215(5) Uani 1 1 d . . . C34 C 0.5492(2) 1.2280(2) 0.30680(13) 0.0215(5) Uani 1 1 d . . . H34 H 0.5216 1.1458 0.3118 0.026 Uiso 1 1 calc R . . C35 C 0.6517(2) 1.2696(2) 0.27332(12) 0.0193(5) Uani 1 1 d . . . C36 C 0.6914(2) 1.3901(2) 0.26699(12) 0.0166(4) Uani 1 1 d . . . H36 H 0.7603 1.4199 0.2437 0.020 Uiso 1 1 calc R . . C37 C 0.8182(2) 1.6384(2) 0.31983(12) 0.0175(4) Uani 1 1 d . . . H37A H 0.8440 1.7213 0.3073 0.021 Uiso 1 1 calc R . . H37B H 0.8673 1.5932 0.2973 0.021 Uiso 1 1 calc R . . C38 C 0.8592(2) 1.6331(2) 0.40070(13) 0.0221(5) Uani 1 1 d . . . C41 C 0.6483(2) 1.4702(2) 0.09913(11) 0.0161(4) Uani 1 1 d . . . C42 C 0.6084(2) 1.3545(2) 0.06947(12) 0.0191(5) Uani 1 1 d . . . H42 H 0.5191 1.3200 0.0546 0.023 Uiso 1 1 calc R . . C43 C 0.6966(2) 1.2901(2) 0.06158(13) 0.0219(5) Uani 1 1 d . . . H43 H 0.6673 1.2113 0.0426 0.026 Uiso 1 1 calc R . . C44 C 0.8278(2) 1.3396(2) 0.08115(14) 0.0247(5) Uani 1 1 d . . . H44 H 0.8882 1.2954 0.0752 0.030 Uiso 1 1 calc R . . C45 C 0.8695(2) 1.4541(2) 0.10955(13) 0.0227(5) Uani 1 1 d . . . H45 H 0.9590 1.4887 0.1228 0.027 Uiso 1 1 calc R . . C46 C 0.7809(2) 1.5191(2) 0.11889(12) 0.0187(5) Uani 1 1 d . . . H46 H 0.8108 1.5972 0.1389 0.022 Uiso 1 1 calc R . . C51 C 0.3840(2) 1.4440(2) 0.10873(11) 0.0156(4) Uani 1 1 d . . . C52 C 0.3803(2) 1.3470(2) 0.15197(12) 0.0181(4) Uani 1 1 d . . . H52 H 0.4574 1.3375 0.1817 0.022 Uiso 1 1 calc R . . C53 C 0.1536(2) 1.3724(2) 0.06591(12) 0.0200(5) Uani 1 1 d . . . H53 H 0.0760 1.3814 0.0365 0.024 Uiso 1 1 calc R . . C54 C 0.1519(2) 1.2775(2) 0.10863(13) 0.0216(5) Uani 1 1 d . . . H54 H 0.0736 1.2212 0.1085 0.026 Uiso 1 1 calc R . . C55 C 0.2660(2) 1.2651(2) 0.15188(13) 0.0218(5) Uani 1 1 d . . . H55 H 0.2654 1.2002 0.1814 0.026 Uiso 1 1 calc R . . C56 C 0.2682(2) 1.4549(2) 0.06565(11) 0.0163(4) Uani 1 1 d . . . H56 H 0.2679 1.5195 0.0359 0.020 Uiso 1 1 calc R . . C131 C 1.0867(3) 2.0681(3) 0.38909(16) 0.0354(7) Uani 1 1 d . . . H13A H 1.1161 2.0926 0.4392 0.053 Uiso 1 1 calc R . . H13B H 1.1108 2.1355 0.3604 0.053 Uiso 1 1 calc R . . H13C H 1.1269 2.0055 0.3781 0.053 Uiso 1 1 calc R . . C151 C 0.6547(3) 2.0306(3) 0.45573(15) 0.0375(7) Uani 1 1 d . . . H15A H 0.5886 2.0687 0.4310 0.056 Uiso 1 1 calc R . . H15B H 0.7102 2.0831 0.4947 0.056 Uiso 1 1 calc R . . H15C H 0.6135 1.9569 0.4744 0.056 Uiso 1 1 calc R . . C181 C 0.8314(2) 1.9908(2) 0.12706(13) 0.0236(5) Uani 1 1 d . . . H18A H 0.8307 2.0355 0.0843 0.035 Uiso 1 1 calc R . . H18B H 0.9171 1.9765 0.1436 0.035 Uiso 1 1 calc R . . H18C H 0.8098 2.0358 0.1637 0.035 Uiso 1 1 calc R . . C182 C 0.7692(3) 1.8023(2) 0.05465(13) 0.0251(5) Uani 1 1 d . . . H18D H 0.7055 1.7273 0.0429 0.038 Uiso 1 1 calc R . . H18E H 0.8540 1.7872 0.0730 0.038 Uiso 1 1 calc R . . H18F H 0.7721 1.8476 0.0122 0.038 Uiso 1 1 calc R . . C183 C 0.5998(2) 1.8960(2) 0.08176(14) 0.0266(5) Uani 1 1 d . . . H18G H 0.6036 1.9426 0.0399 0.040 Uiso 1 1 calc R . . H18H H 0.5748 1.9396 0.1178 0.040 Uiso 1 1 calc R . . H18I H 0.5362 1.8211 0.0691 0.040 Uiso 1 1 calc R . . C231 C 0.3814(3) 1.6468(3) 0.46964(14) 0.0379(7) Uani 1 1 d . . . H23A H 0.4594 1.7097 0.4727 0.057 Uiso 1 1 calc R . . H23B H 0.4022 1.5812 0.4974 0.057 Uiso 1 1 calc R . . H23C H 0.3170 1.6768 0.4882 0.057 Uiso 1 1 calc R . . C251 C 0.0614(2) 1.3648(2) 0.28623(14) 0.0277(6) Uani 1 1 d . . . H25A H -0.0136 1.3916 0.2616 0.042 Uiso 1 1 calc R . . H25B H 0.0423 1.3269 0.3292 0.042 Uiso 1 1 calc R . . H25C H 0.0817 1.3083 0.2555 0.042 Uiso 1 1 calc R . . C281 C 0.1357(3) 1.7766(3) 0.20644(16) 0.0313(6) Uani 1 1 d . . . H28A H 0.0911 1.8396 0.2098 0.047 Uiso 1 1 calc R . . H28B H 0.1648 1.7508 0.2537 0.047 Uiso 1 1 calc R . . H28C H 0.0768 1.7101 0.1774 0.047 Uiso 1 1 calc R . . C282 C 0.2060(3) 1.8702(3) 0.10079(15) 0.0374(7) Uani 1 1 d . . . H28D H 0.1475 1.8059 0.0698 0.056 Uiso 1 1 calc R . . H28E H 0.2801 1.9035 0.0796 0.056 Uiso 1 1 calc R . . H28F H 0.1608 1.9314 0.1072 0.056 Uiso 1 1 calc R . . C283 C 0.3476(3) 1.9213(2) 0.22033(16) 0.0303(6) Uani 1 1 d . . . H28G H 0.3068 1.9865 0.2250 0.045 Uiso 1 1 calc R . . H28H H 0.4237 1.9491 0.1998 0.045 Uiso 1 1 calc R . . H28I H 0.3732 1.8915 0.2669 0.045 Uiso 1 1 calc R . . C331 C 0.3722(3) 1.2555(3) 0.36601(15) 0.0313(6) Uani 1 1 d . . . H33A H 0.2929 1.2450 0.3301 0.047 Uiso 1 1 calc R . . H33B H 0.3706 1.3109 0.4036 0.047 Uiso 1 1 calc R . . H33C H 0.3788 1.1795 0.3858 0.047 Uiso 1 1 calc R . . C351 C 0.7176(3) 1.1870(2) 0.24353(14) 0.0261(5) Uani 1 1 d . . . H35A H 0.7833 1.1676 0.2810 0.039 Uiso 1 1 calc R . . H35B H 0.7584 1.2249 0.2060 0.039 Uiso 1 1 calc R . . H35C H 0.6541 1.1148 0.2242 0.039 Uiso 1 1 calc R . . C381 C 0.9985(3) 1.7082(2) 0.41985(15) 0.0317(6) Uani 1 1 d . . . H38A H 0.9994 1.7903 0.4092 0.048 Uiso 1 1 calc R . . H38B H 1.0518 1.6786 0.3922 0.048 Uiso 1 1 calc R . . H38C H 1.0327 1.7034 0.4702 0.048 Uiso 1 1 calc R . . C382 C 0.8600(2) 1.5072(2) 0.42371(13) 0.0235(5) Uani 1 1 d . . . H38D H 0.8922 1.5088 0.4747 0.035 Uiso 1 1 calc R . . H38E H 0.9160 1.4751 0.3992 0.035 Uiso 1 1 calc R . . H38F H 0.7724 1.4576 0.4118 0.035 Uiso 1 1 calc R . . C383 C 0.7723(3) 1.6841(3) 0.43808(14) 0.0324(6) Uani 1 1 d . . . H38G H 0.6837 1.6372 0.4242 0.049 Uiso 1 1 calc R . . H38H H 0.7759 1.7655 0.4250 0.049 Uiso 1 1 calc R . . H38I H 0.8013 1.6823 0.4892 0.049 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 0.01018(4) 0.01112(4) 0.01652(4) -0.00103(3) 0.00202(3) 0.00235(3) P1 0.0122(3) 0.0147(3) 0.0192(3) -0.0015(2) 0.0016(2) 0.0020(2) N1 0.0168(10) 0.0174(10) 0.0182(9) -0.0018(8) 0.0041(7) 0.0018(8) N2 0.0139(9) 0.0161(9) 0.0196(9) -0.0022(8) 0.0046(7) 0.0044(8) N3 0.0137(9) 0.0134(9) 0.0216(9) -0.0017(8) 0.0010(7) 0.0029(7) C11 0.0173(11) 0.0096(10) 0.0182(10) 0.0003(8) 0.0008(8) 0.0014(8) C12 0.0189(11) 0.0144(11) 0.0251(11) 0.0002(9) 0.0055(9) 0.0031(9) C13 0.0236(13) 0.0149(11) 0.0277(12) 0.0011(10) -0.0029(10) -0.0004(10) C14 0.0363(15) 0.0178(12) 0.0204(11) -0.0064(10) -0.0030(10) 0.0047(11) C15 0.0337(14) 0.0168(12) 0.0227(11) -0.0013(10) 0.0053(10) 0.0084(11) C16 0.0183(11) 0.0163(11) 0.0232(11) 0.0002(9) 0.0034(9) 0.0043(9) C17 0.0171(11) 0.0173(11) 0.0206(10) -0.0023(9) 0.0034(8) 0.0031(9) C18 0.0185(11) 0.0154(11) 0.0194(10) -0.0006(9) 0.0062(8) 0.0028(9) C21 0.0142(11) 0.0167(11) 0.0217(10) 0.0010(9) 0.0052(8) 0.0061(9) C22 0.0169(11) 0.0188(12) 0.0229(11) -0.0017(9) 0.0023(9) 0.0051(9) C23 0.0254(13) 0.0290(14) 0.0211(11) 0.0009(10) 0.0067(9) 0.0092(11) C24 0.0253(13) 0.0282(14) 0.0241(12) 0.0064(10) 0.0101(10) 0.0069(11) C25 0.0167(11) 0.0196(12) 0.0281(12) 0.0031(10) 0.0065(9) 0.0053(9) C26 0.0140(11) 0.0204(12) 0.0224(11) -0.0006(9) 0.0039(8) 0.0064(9) C27 0.0170(11) 0.0202(12) 0.0199(10) -0.0010(9) 0.0040(8) 0.0054(9) C28 0.0195(12) 0.0215(12) 0.0255(11) 0.0006(10) 0.0020(9) 0.0089(10) C31 0.0133(10) 0.0142(10) 0.0179(10) -0.0006(8) -0.0007(8) 0.0034(8) C32 0.0164(11) 0.0209(12) 0.0203(10) 0.0022(9) 0.0027(8) 0.0063(9) C33 0.0158(11) 0.0232(12) 0.0253(11) 0.0059(10) 0.0036(9) 0.0045(10) C34 0.0203(12) 0.0153(11) 0.0265(12) 0.0053(10) 0.0001(9) 0.0033(9) C35 0.0181(11) 0.0160(11) 0.0224(11) 0.0021(9) 0.0004(9) 0.0045(9) C36 0.0128(10) 0.0155(11) 0.0213(10) 0.0008(9) 0.0024(8) 0.0037(9) C37 0.0137(11) 0.0153(11) 0.0219(11) -0.0003(9) 0.0006(8) 0.0028(9) C38 0.0228(12) 0.0190(12) 0.0222(11) -0.0016(10) -0.0036(9) 0.0073(10) C41 0.0151(11) 0.0182(11) 0.0159(9) 0.0009(9) 0.0029(8) 0.0060(9) C42 0.0157(11) 0.0208(12) 0.0209(10) 0.0006(9) 0.0044(8) 0.0038(9) C43 0.0216(12) 0.0187(12) 0.0277(12) 0.0003(10) 0.0080(9) 0.0068(10) C44 0.0221(13) 0.0249(13) 0.0316(13) 0.0041(11) 0.0094(10) 0.0114(11) C45 0.0136(11) 0.0287(13) 0.0252(11) 0.0031(10) 0.0042(9) 0.0035(10) C46 0.0159(11) 0.0203(12) 0.0196(10) -0.0004(9) 0.0031(8) 0.0040(9) C51 0.0135(10) 0.0149(11) 0.0191(10) -0.0030(9) 0.0039(8) 0.0038(9) C52 0.0160(11) 0.0165(11) 0.0214(10) -0.0031(9) 0.0025(8) 0.0042(9) C53 0.0136(11) 0.0234(12) 0.0223(11) -0.0058(10) 0.0020(8) 0.0043(9) C54 0.0135(11) 0.0207(12) 0.0291(12) -0.0040(10) 0.0068(9) -0.0012(9) C55 0.0212(12) 0.0180(12) 0.0267(12) 0.0022(10) 0.0068(9) 0.0042(10) C56 0.0152(11) 0.0168(11) 0.0174(10) -0.0031(9) 0.0039(8) 0.0041(9) C131 0.0220(14) 0.0291(15) 0.0443(16) 0.0029(13) -0.0057(12) -0.0049(12) C151 0.0463(18) 0.0396(18) 0.0299(14) -0.0091(13) 0.0086(13) 0.0163(15) C181 0.0244(13) 0.0180(12) 0.0268(12) 0.0011(10) 0.0083(10) -0.0007(10) C182 0.0285(14) 0.0219(13) 0.0259(12) 0.0000(10) 0.0098(10) 0.0044(11) C183 0.0229(13) 0.0286(14) 0.0295(13) 0.0067(11) 0.0056(10) 0.0081(11) C231 0.0475(19) 0.0395(17) 0.0215(12) -0.0025(12) 0.0066(12) 0.0001(14) C251 0.0199(13) 0.0268(14) 0.0346(14) 0.0047(11) 0.0079(10) 0.0000(11) C281 0.0236(14) 0.0292(15) 0.0461(16) -0.0011(13) 0.0107(12) 0.0130(12) C282 0.0453(18) 0.0366(17) 0.0349(15) 0.0051(13) 0.0014(13) 0.0244(15) C283 0.0253(14) 0.0217(13) 0.0440(16) -0.0061(12) 0.0034(12) 0.0088(11) C331 0.0223(13) 0.0339(15) 0.0386(15) 0.0115(13) 0.0102(11) 0.0052(12) C351 0.0291(14) 0.0169(12) 0.0347(13) 0.0007(11) 0.0090(11) 0.0084(11) C381 0.0302(15) 0.0202(13) 0.0357(14) -0.0041(11) -0.0124(11) 0.0038(11) C382 0.0252(13) 0.0220(12) 0.0223(11) 0.0023(10) -0.0009(9) 0.0085(10) C383 0.0449(17) 0.0337(16) 0.0226(12) -0.0018(11) 0.0010(11) 0.0225(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N3 1.9656(19) . ? Ta1 N1 1.976(2) . ? Ta1 N2 1.9914(19) . ? Ta1 C17 2.200(2) . ? Ta1 P1 2.5312(6) . ? P1 C41 1.831(2) . ? P1 C51 1.841(2) . ? N1 C11 1.401(3) . ? N1 C17 1.418(3) . ? N2 C21 1.433(3) . ? N2 C27 1.473(3) . ? N3 C31 1.443(3) . ? N3 C37 1.487(3) . ? C11 C12 1.397(3) . ? C11 C16 1.407(3) . ? C12 C13 1.399(3) . ? C13 C14 1.389(4) . ? C13 C131 1.510(4) . ? C14 C15 1.391(4) . ? C15 C16 1.387(3) . ? C15 C151 1.515(4) . ? C17 H17 1.015(17) . ? C17 C18 1.546(3) . ? C18 C183 1.524(3) . ? C18 C182 1.531(3) . ? C18 C181 1.541(3) . ? C21 C26 1.394(3) . ? C21 C22 1.398(3) . ? C22 C23 1.394(3) . ? C23 C24 1.391(4) . ? C23 C231 1.507(4) . ? C24 C25 1.391(4) . ? C25 C26 1.395(3) . ? C25 C251 1.501(3) . ? C27 C28 1.551(3) . ? C28 C283 1.526(4) . ? C28 C282 1.531(4) . ? C28 C281 1.538(4) . ? C31 C32 1.387(3) . ? C31 C36 1.399(3) . ? C32 C33 1.399(3) . ? C33 C34 1.384(4) . ? C33 C331 1.508(3) . ? C34 C35 1.395(3) . ? C35 C36 1.388(3) . ? C35 C351 1.506(3) . ? C37 C38 1.547(3) . ? C38 C383 1.520(4) . ? C38 C382 1.540(3) . ? C38 C381 1.543(4) . ? C41 C46 1.402(3) . ? C41 C42 1.407(3) . ? C42 C43 1.383(3) . ? C43 C44 1.389(4) . ? C44 C45 1.387(4) . ? C45 C46 1.398(3) . ? C51 C56 1.403(3) . ? C51 C52 1.408(3) . ? C52 C55 1.385(3) . ? C53 C54 1.384(3) . ? C53 C56 1.393(3) . ? C54 C55 1.395(3) . ? 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 N3 Ta1 N1 103.07(8) . . ? N3 Ta1 N2 122.68(8) . . ? N1 Ta1 N2 106.97(8) . . ? N3 Ta1 C17 103.59(8) . . ? N1 Ta1 C17 39.25(8) . . ? N2 Ta1 C17 130.19(8) . . ? N3 Ta1 P1 106.41(6) . . ? N1 Ta1 P1 124.97(6) . . ? N2 Ta1 P1 94.56(6) . . ? C17 Ta1 P1 88.62(6) . . ? C41 P1 C51 102.90(10) . . ? C41 P1 Ta1 112.01(7) . . ? C51 P1 Ta1 104.45(7) . . ? C11 N1 C17 130.6(2) . . ? C11 N1 Ta1 133.44(15) . . ? C17 N1 Ta1 78.94(13) . . ? C21 N2 C27 116.76(18) . . ? C21 N2 Ta1 118.91(14) . . ? C27 N2 Ta1 123.26(14) . . ? C31 N3 C37 114.52(18) . . ? C31 N3 Ta1 119.44(14) . . ? C37 N3 Ta1 122.79(14) . . ? C12 C11 N1 122.6(2) . . ? C12 C11 C16 118.8(2) . . ? N1 C11 C16 118.6(2) . . ? C11 C12 C13 120.4(2) . . ? C14 C13 C12 119.4(2) . . ? C14 C13 C131 121.2(2) . . ? C12 C13 C131 119.4(3) . . ? C13 C14 C15 121.3(2) . . ? C16 C15 C14 118.9(2) . . ? C16 C15 C151 120.2(2) . . ? C14 C15 C151 120.8(2) . . ? C15 C16 C11 121.2(2) . . ? H17 C17 N1 113.4(15) . . ? H17 C17 C18 109.5(15) . . ? N1 C17 C18 118.7(2) . . ? H17 C17 Ta1 112.2(15) . . ? N1 C17 Ta1 61.81(11) . . ? C18 C17 Ta1 132.81(16) . . ? C183 C18 C182 109.3(2) . . ? C183 C18 C181 108.8(2) . . ? C182 C18 C181 108.51(19) . . ? C183 C18 C17 112.12(19) . . ? C182 C18 C17 108.6(2) . . ? C181 C18 C17 109.39(19) . . ? C26 C21 C22 119.4(2) . . ? C26 C21 N2 122.1(2) . . ? C22 C21 N2 118.5(2) . . ? C23 C22 C21 120.9(2) . . ? C24 C23 C22 118.3(2) . . ? C24 C23 C231 121.4(2) . . ? C22 C23 C231 120.2(2) . . ? C25 C24 C23 122.1(2) . . ? C24 C25 C26 118.7(2) . . ? C24 C25 C251 121.2(2) . . ? C26 C25 C251 120.2(2) . . ? C21 C26 C25 120.6(2) . . ? N2 C27 C28 118.33(19) . . ? C283 C28 C282 109.9(2) . . ? C283 C28 C281 109.0(2) . . ? C282 C28 C281 108.6(2) . . ? C283 C28 C27 110.8(2) . . ? C282 C28 C27 106.3(2) . . ? C281 C28 C27 112.1(2) . . ? C32 C31 C36 119.4(2) . . ? C32 C31 N3 121.4(2) . . ? C36 C31 N3 119.2(2) . . ? C31 C32 C33 120.4(2) . . ? C34 C33 C32 119.0(2) . . ? C34 C33 C331 120.5(2) . . ? C32 C33 C331 120.4(2) . . ? C33 C34 C35 121.7(2) . . ? C36 C35 C34 118.4(2) . . ? C36 C35 C351 120.1(2) . . ? C34 C35 C351 121.5(2) . . ? C35 C36 C31 121.1(2) . . ? N3 C37 C38 116.56(19) . . ? C383 C38 C382 110.1(2) . . ? C383 C38 C381 110.3(2) . . ? C382 C38 C381 108.0(2) . . ? C383 C38 C37 110.6(2) . . ? C382 C38 C37 112.3(2) . . ? C381 C38 C37 105.4(2) . . ? C46 C41 C42 117.7(2) . . ? C46 C41 P1 121.72(18) . . ? C42 C41 P1 120.38(17) . . ? C43 C42 C41 121.3(2) . . ? C42 C43 C44 120.5(2) . . ? C45 C44 C43 119.3(2) . . ? C44 C45 C46 120.5(2) . . ? C45 C46 C41 120.7(2) . . ? C56 C51 C52 117.8(2) . . ? C56 C51 P1 117.32(17) . . ? C52 C51 P1 124.92(17) . . ? C55 C52 C51 121.1(2) . . ? C54 C53 C56 120.5(2) . . ? C53 C54 C55 119.5(2) . . ? C52 C55 C54 120.3(2) . . ? C53 C56 C51 120.9(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.585 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.104