# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'David Hoffman' 'van der Heide,Paul' 'Jean-Sebastien M. Lehn' 'Yongqiang Wang' _publ_contact_author_name 'Prof David Hoffman' _publ_contact_author_address ; Dept of Chemistry University of Houston Houston Texas 77204-5003 UNITED STATES OF AMERICA ; _publ_contact_author_email HOFFMAN@UH.EDU _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; A new precursor for the chemical vapor deposition of tantalum nitride films ; data_k640_Ta(NEt2)2(NCy2)2 _database_code_depnum_ccdc_archive 'CCDC 240191' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C32 H64 N4 Ta' _chemical_formula_weight 685.82 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7729(4) _cell_length_b 19.1873(9) _cell_length_c 20.5649(9) _cell_angle_alpha 63.088(1) _cell_angle_beta 83.385(1) _cell_angle_gamma 85.284(1) _cell_volume 3413.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6031 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 25.01 _exptl_crystal_description 'Flat column' _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 3.244 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0645 _exptl_absorpt_correction_T_max 0.8146 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 25 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 6031 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be -1, and the space group was shown to be either P1 or P-1. There are two independent molecules in the asymmetric unit, which differ only slightly in overall geometry. One of the ethyl ligands on the Ta2 molecule was found to be disordered over three different orientations. Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _publ_section_figure_captions ; Fig. 1 -- View of molecule 1 showing the atom numbering scheme. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens omitted. Molecule 2 is numbered similarly. Fig. 2 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(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 'Siemens SMART CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 17941 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11483 _reflns_number_gt 9073 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Bruker SAINT software (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT software (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 4sigma(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^)+(0.0375P)^2^+1.9148P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00034(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11483 _refine_ls_number_parameters 674 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.003 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 0.134264(13) 0.245598(8) 0.061326(7) 0.02952(5) Uani 1 1 d . . . Ta2 Ta 0.316610(15) 0.225658(9) 0.506840(8) 0.04049(6) Uani 1 1 d . A . N1 N 0.1054(3) 0.13555(16) 0.08207(15) 0.0343(6) Uani 1 1 d . . . N2 N 0.1716(3) 0.30325(16) -0.04745(14) 0.0316(6) Uani 1 1 d . . . N3 N 0.2824(3) 0.27636(17) 0.10132(16) 0.0363(6) Uani 1 1 d . . . N4 N -0.0232(3) 0.27154(18) 0.11814(15) 0.0366(6) Uani 1 1 d . . . N5 N 0.3173(3) 0.25113(18) 0.59036(15) 0.0396(7) Uani 1 1 d . . . N6 N 0.2864(3) 0.32772(19) 0.41948(15) 0.0423(7) Uani 1 1 d . . . N7 N 0.1843(4) 0.1554(2) 0.5016(2) 0.0603(9) Uani 1 1 d . . . N8 N 0.4846(4) 0.1559(2) 0.5152(2) 0.0612(9) Uani 1 1 d D . . C1 C 0.1727(3) 0.0591(2) 0.12260(19) 0.0388(8) Uani 1 1 d . . . H1 H 0.1118 0.0187 0.1257 0.047 Uiso 1 1 calc R . . C2 C 0.1911(4) 0.0440(2) 0.2007(2) 0.0505(10) Uani 1 1 d . . . H2A H 0.1004 0.0440 0.2266 0.061 Uiso 1 1 calc R . . H2B H 0.2429 0.0865 0.1991 0.061 Uiso 1 1 calc R . . C3 C 0.2675(5) -0.0341(3) 0.2428(2) 0.0652(13) Uani 1 1 d . . . H3A H 0.2831 -0.0398 0.2912 0.078 Uiso 1 1 calc R . . H3B H 0.2103 -0.0770 0.2498 0.078 Uiso 1 1 calc R . . C4 C 0.4042(4) -0.0393(3) 0.2024(2) 0.0622(12) Uani 1 1 d . . . H4A H 0.4648 0.0004 0.1995 0.075 Uiso 1 1 calc R . . H4B H 0.4485 -0.0908 0.2295 0.075 Uiso 1 1 calc R . . C5 C 0.3851(4) -0.0271(2) 0.1262(2) 0.0535(10) Uani 1 1 d . . . H5A H 0.3321 -0.0698 0.1292 0.064 Uiso 1 1 calc R . . H5B H 0.4754 -0.0282 0.1004 0.064 Uiso 1 1 calc R . . C6 C 0.3102(4) 0.0506(2) 0.0833(2) 0.0440(9) Uani 1 1 d . . . H6A H 0.2943 0.0551 0.0354 0.053 Uiso 1 1 calc R . . H6B H 0.3689 0.0933 0.0752 0.053 Uiso 1 1 calc R . . C7 C -0.0276(3) 0.1350(2) 0.05454(19) 0.0358(8) Uani 1 1 d . . . H7A H -0.0577 0.1906 0.0283 0.043 Uiso 1 1 calc R . . C8 C -0.1417(4) 0.0964(2) 0.1147(2) 0.0446(9) Uani 1 1 d . . . H8A H -0.1524 0.1216 0.1471 0.054 Uiso 1 1 calc R . . H8B H -0.1157 0.0412 0.1438 0.054 Uiso 1 1 calc R . . C9 C -0.2788(4) 0.1019(3) 0.0835(2) 0.0565(11) Uani 1 1 d . . . H9A H -0.3479 0.0733 0.1235 0.068 Uiso 1 1 calc R . . H9B H -0.3105 0.1568 0.0595 0.068 Uiso 1 1 calc R . . C10 C -0.2657(4) 0.0687(3) 0.0289(2) 0.0553(11) Uani 1 1 d . . . H10A H -0.3539 0.0758 0.0079 0.066 Uiso 1 1 calc R . . H10B H -0.2436 0.0125 0.0540 0.066 Uiso 1 1 calc R . . C11 C -0.1542(4) 0.1085(3) -0.0320(2) 0.0504(10) Uani 1 1 d . . . H11A H -0.1816 0.1635 -0.0605 0.060 Uiso 1 1 calc R . . H11B H -0.1441 0.0837 -0.0648 0.060 Uiso 1 1 calc R . . C12 C -0.0159(4) 0.1036(2) -0.0019(2) 0.0434(9) Uani 1 1 d . . . H12A H 0.0177 0.0489 0.0206 0.052 Uiso 1 1 calc R . . H12B H 0.0514 0.1336 -0.0424 0.052 Uiso 1 1 calc R . . C13 C 0.3069(3) 0.2752(2) -0.06719(18) 0.0364(8) Uani 1 1 d . . . H13A H 0.3344 0.2304 -0.0216 0.044 Uiso 1 1 calc R . . C14 C 0.3056(4) 0.2430(2) -0.1222(2) 0.0489(9) Uani 1 1 d . . . H14A H 0.2759 0.2847 -0.1682 0.059 Uiso 1 1 calc R . . H14B H 0.2387 0.2015 -0.1036 0.059 Uiso 1 1 calc R . . C15 C 0.4471(5) 0.2102(3) -0.1370(3) 0.0665(13) Uani 1 1 d . . . H15A H 0.4716 0.1641 -0.0925 0.080 Uiso 1 1 calc R . . H15B H 0.4430 0.1937 -0.1754 0.080 Uiso 1 1 calc R . . C16 C 0.5570(4) 0.2698(3) -0.1606(3) 0.0738(15) Uani 1 1 d . . . H16A H 0.5383 0.3135 -0.2080 0.089 Uiso 1 1 calc R . . H16B H 0.6470 0.2459 -0.1667 0.089 Uiso 1 1 calc R . . C17 C 0.5604(4) 0.3002(3) -0.1041(3) 0.0667(13) Uani 1 1 d . . . H17A H 0.6292 0.3406 -0.1214 0.080 Uiso 1 1 calc R . . H17B H 0.5878 0.2574 -0.0581 0.080 Uiso 1 1 calc R . . C18 C 0.4193(3) 0.3345(2) -0.0901(2) 0.0464(9) Uani 1 1 d . . . H18A H 0.4233 0.3507 -0.0516 0.056 Uiso 1 1 calc R . . H18B H 0.3965 0.3809 -0.1348 0.056 Uiso 1 1 calc R . . C19 C 0.1043(3) 0.3676(2) -0.10730(18) 0.0341(7) Uani 1 1 d . . . H19A H 0.1710 0.3857 -0.1513 0.041 Uiso 1 1 calc R . . C20 C -0.0229(4) 0.3413(2) -0.12578(19) 0.0422(8) Uani 1 1 d . . . H20A H 0.0044 0.2999 -0.1406 0.051 Uiso 1 1 calc R . . H20B H -0.0880 0.3195 -0.0820 0.051 Uiso 1 1 calc R . . C21 C -0.0936(4) 0.4086(3) -0.1870(2) 0.0519(10) Uani 1 1 d . . . H21A H -0.0317 0.4273 -0.2322 0.062 Uiso 1 1 calc R . . H21B H -0.1768 0.3902 -0.1960 0.062 Uiso 1 1 calc R . . C22 C -0.1321(4) 0.4751(3) -0.1674(2) 0.0594(12) Uani 1 1 d . . . H22A H -0.2000 0.4576 -0.1247 0.071 Uiso 1 1 calc R . . H22B H -0.1744 0.5185 -0.2083 0.071 Uiso 1 1 calc R . . C23 C -0.0066(4) 0.5034(2) -0.1504(2) 0.0563(11) Uani 1 1 d . . . H23A H -0.0353 0.5440 -0.1347 0.068 Uiso 1 1 calc R . . H23B H 0.0567 0.5265 -0.1948 0.068 Uiso 1 1 calc R . . C24 C 0.0680(4) 0.4362(2) -0.0902(2) 0.0439(9) Uani 1 1 d . . . H24A H 0.1527 0.4553 -0.0835 0.053 Uiso 1 1 calc R . . H24B H 0.0092 0.4184 -0.0441 0.053 Uiso 1 1 calc R . . C25 C 0.2719(4) 0.3488(2) 0.1099(2) 0.0499(10) Uani 1 1 d . . . H25A H 0.2927 0.3358 0.1597 0.060 Uiso 1 1 calc R . . H25B H 0.1762 0.3689 0.1050 0.060 Uiso 1 1 calc R . . C26 C 0.3641(5) 0.4131(3) 0.0569(3) 0.0618(12) Uani 1 1 d . . . H26A H 0.3498 0.4579 0.0672 0.093 Uiso 1 1 calc R . . H26B H 0.3425 0.4282 0.0073 0.093 Uiso 1 1 calc R . . H26C H 0.4596 0.3947 0.0619 0.093 Uiso 1 1 calc R . . C27 C 0.4166(4) 0.2347(2) 0.1176(2) 0.0437(9) Uani 1 1 d . . . H27A H 0.4890 0.2710 0.0875 0.052 Uiso 1 1 calc R . . H27B H 0.4210 0.1925 0.1028 0.052 Uiso 1 1 calc R . . C28 C 0.4480(5) 0.1996(3) 0.1971(2) 0.0663(13) Uani 1 1 d . . . H28A H 0.5381 0.1732 0.2025 0.099 Uiso 1 1 calc R . . H28B H 0.3786 0.1622 0.2276 0.099 Uiso 1 1 calc R . . H28C H 0.4474 0.2408 0.2121 0.099 Uiso 1 1 calc R . . C29 C -0.1582(4) 0.3028(2) 0.0902(2) 0.0454(9) Uani 1 1 d . . . H29A H -0.2285 0.2656 0.1217 0.054 Uiso 1 1 calc R . . H29B H -0.1569 0.3064 0.0411 0.054 Uiso 1 1 calc R . . C30 C -0.2004(5) 0.3824(3) 0.0864(3) 0.0645(12) Uani 1 1 d . . . H30A H -0.2903 0.3984 0.0677 0.097 Uiso 1 1 calc R . . H30B H -0.1333 0.4203 0.0540 0.097 Uiso 1 1 calc R . . H30C H -0.2044 0.3794 0.1349 0.097 Uiso 1 1 calc R . . C31 C -0.0227(4) 0.2502(3) 0.1960(2) 0.0696(14) Uani 1 1 d . . . H31A H 0.0714 0.2330 0.2096 0.083 Uiso 1 1 calc R . . H31B H -0.0445 0.2977 0.2022 0.083 Uiso 1 1 calc R . . C32 C -0.1145(7) 0.1905(5) 0.2475(3) 0.114(2) Uani 1 1 d . . . H32A H -0.1036 0.1824 0.2968 0.171 Uiso 1 1 calc R . . H32B H -0.0923 0.1420 0.2440 0.171 Uiso 1 1 calc R . . H32C H -0.2090 0.2070 0.2364 0.171 Uiso 1 1 calc R . . C33 C 0.2311(4) 0.2415(2) 0.65675(18) 0.0404(8) Uani 1 1 d . . . H33A H 0.2868 0.2565 0.6854 0.048 Uiso 1 1 calc R . . C34 C 0.1902(5) 0.1578(2) 0.7051(2) 0.0545(10) Uani 1 1 d . . . H34A H 0.2732 0.1238 0.7179 0.065 Uiso 1 1 calc R . . H34B H 0.1358 0.1405 0.6783 0.065 Uiso 1 1 calc R . . C35 C 0.1053(5) 0.1504(3) 0.7754(2) 0.0638(12) Uani 1 1 d . . . H35A H 0.0741 0.0967 0.8036 0.077 Uiso 1 1 calc R . . H35B H 0.1641 0.1607 0.8054 0.077 Uiso 1 1 calc R . . C36 C -0.0179(5) 0.2060(3) 0.7600(2) 0.0678(13) Uani 1 1 d . . . H36A H -0.0634 0.2026 0.8063 0.081 Uiso 1 1 calc R . . H36B H -0.0837 0.1906 0.7367 0.081 Uiso 1 1 calc R . . C37 C 0.0209(5) 0.2895(3) 0.7107(2) 0.0594(11) Uani 1 1 d . . . H37A H 0.0762 0.3079 0.7364 0.071 Uiso 1 1 calc R . . H37B H -0.0628 0.3231 0.6983 0.071 Uiso 1 1 calc R . . C38 C 0.1037(4) 0.2954(2) 0.6402(2) 0.0486(9) Uani 1 1 d . . . H38A H 0.0451 0.2816 0.6124 0.058 Uiso 1 1 calc R . . H38B H 0.1315 0.3494 0.6098 0.058 Uiso 1 1 calc R . . C39 C 0.4486(4) 0.2898(2) 0.57907(19) 0.0425(9) Uani 1 1 d . . . H39A H 0.4906 0.2971 0.5303 0.051 Uiso 1 1 calc R . . C40 C 0.5521(4) 0.2392(3) 0.6328(2) 0.0570(11) Uani 1 1 d . . . H40A H 0.5149 0.2292 0.6824 0.068 Uiso 1 1 calc R . . H40B H 0.5653 0.1887 0.6313 0.068 Uiso 1 1 calc R . . C41 C 0.6907(5) 0.2771(3) 0.6161(3) 0.0770(16) Uani 1 1 d . . . H41A H 0.7517 0.2438 0.6538 0.092 Uiso 1 1 calc R . . H41B H 0.7333 0.2815 0.5689 0.092 Uiso 1 1 calc R . . C42 C 0.6756(5) 0.3570(3) 0.6134(3) 0.0773(16) Uani 1 1 d . . . H42A H 0.7656 0.3812 0.5994 0.093 Uiso 1 1 calc R . . H42B H 0.6430 0.3521 0.6622 0.093 Uiso 1 1 calc R . . C43 C 0.5742(5) 0.4089(3) 0.5587(2) 0.0636(12) Uani 1 1 d . . . H43A H 0.6123 0.4187 0.5092 0.076 Uiso 1 1 calc R . . H43B H 0.5618 0.4593 0.5603 0.076 Uiso 1 1 calc R . . C44 C 0.4343(4) 0.3714(2) 0.5750(2) 0.0520(10) Uani 1 1 d . . . H44A H 0.3906 0.3680 0.6217 0.062 Uiso 1 1 calc R . . H44B H 0.3745 0.4045 0.5366 0.062 Uiso 1 1 calc R . . C45 C 0.1418(4) 0.3520(3) 0.42907(19) 0.0477(10) Uani 1 1 d . . . H45A H 0.1071 0.3143 0.4790 0.057 Uiso 1 1 calc R . . C46 C 0.1218(4) 0.4322(3) 0.4276(2) 0.0595(12) Uani 1 1 d . . . H46A H 0.1567 0.4721 0.3795 0.071 Uiso 1 1 calc R . . H46B H 0.1754 0.4337 0.4644 0.071 Uiso 1 1 calc R . . C47 C -0.0302(5) 0.4513(4) 0.4431(3) 0.0843(18) Uani 1 1 d . . . H47A H -0.0618 0.4158 0.4936 0.101 Uiso 1 1 calc R . . H47B H -0.0399 0.5049 0.4376 0.101 Uiso 1 1 calc R . . C48 C -0.1196(5) 0.4433(4) 0.3909(3) 0.101(2) Uani 1 1 d . . . H48A H -0.2166 0.4525 0.4041 0.121 Uiso 1 1 calc R . . H48B H -0.0951 0.4831 0.3409 0.121 Uiso 1 1 calc R . . C49 C -0.1011(5) 0.3633(4) 0.3934(3) 0.096(2) Uani 1 1 d . . . H49A H -0.1558 0.3612 0.3574 0.115 Uiso 1 1 calc R . . H49B H -0.1349 0.3239 0.4420 0.115 Uiso 1 1 calc R . . C50 C 0.0494(4) 0.3448(3) 0.3773(2) 0.0685(14) Uani 1 1 d . . . H50A H 0.0800 0.3806 0.3267 0.082 Uiso 1 1 calc R . . H50B H 0.0587 0.2914 0.3822 0.082 Uiso 1 1 calc R . . C51 C 0.3625(4) 0.3793(2) 0.35027(19) 0.0434(9) Uani 1 1 d . . . H51A H 0.2955 0.4193 0.3203 0.052 Uiso 1 1 calc R . . C52 C 0.4750(4) 0.4226(2) 0.3611(2) 0.0498(10) Uani 1 1 d . . . H52A H 0.4340 0.4528 0.3865 0.060 Uiso 1 1 calc R . . H52B H 0.5419 0.3845 0.3919 0.060 Uiso 1 1 calc R . . C53 C 0.5486(5) 0.4772(3) 0.2885(2) 0.0564(11) Uani 1 1 d . . . H53A H 0.4834 0.5182 0.2596 0.068 Uiso 1 1 calc R . . H53B H 0.6226 0.5024 0.2976 0.068 Uiso 1 1 calc R . . C54 C 0.6091(4) 0.4337(3) 0.2455(2) 0.0532(10) Uani 1 1 d . . . H54A H 0.6514 0.4708 0.1979 0.064 Uiso 1 1 calc R . . H54B H 0.6811 0.3962 0.2720 0.064 Uiso 1 1 calc R . . C55 C 0.4986(4) 0.3909(3) 0.2341(2) 0.0575(11) Uani 1 1 d . . . H55A H 0.5406 0.3604 0.2091 0.069 Uiso 1 1 calc R . . H55B H 0.4325 0.4290 0.2026 0.069 Uiso 1 1 calc R . . C56 C 0.4223(4) 0.3361(3) 0.3068(2) 0.0543(11) Uani 1 1 d . . . H56A H 0.3477 0.3119 0.2970 0.065 Uiso 1 1 calc R . . H56B H 0.4862 0.2943 0.3358 0.065 Uiso 1 1 calc R . . C57 C 0.2243(7) 0.1099(4) 0.4590(3) 0.0957(19) Uani 1 1 d . . . H57A H 0.3240 0.1135 0.4457 0.115 Uiso 1 1 calc R . . H57B H 0.2054 0.0547 0.4911 0.115 Uiso 1 1 calc R . . C58 C 0.1552(8) 0.1345(5) 0.3927(4) 0.127(3) Uani 1 1 d . . . H58A H 0.1880 0.1019 0.3689 0.191 Uiso 1 1 calc R . . H58B H 0.1749 0.1886 0.3597 0.191 Uiso 1 1 calc R . . H58C H 0.0565 0.1294 0.4051 0.191 Uiso 1 1 calc R . . C59 C 0.0442(5) 0.1441(3) 0.5351(3) 0.0716(14) Uani 1 1 d . . . H59A H -0.0182 0.1606 0.4963 0.086 Uiso 1 1 calc R . . H59B H 0.0248 0.1785 0.5588 0.086 Uiso 1 1 calc R . . C60 C 0.0113(7) 0.0613(4) 0.5911(4) 0.115(2) Uani 1 1 d . . . H60A H -0.0843 0.0597 0.6105 0.173 Uiso 1 1 calc R . . H60B H 0.0704 0.0446 0.6307 0.173 Uiso 1 1 calc R . . H60C H 0.0268 0.0267 0.5681 0.173 Uiso 1 1 calc R . . C61 C 0.6178(5) 0.1866(3) 0.4776(3) 0.0740(14) Uani 1 1 d . A . H61A H 0.6830 0.1744 0.5145 0.089 Uiso 1 1 calc R . . H61B H 0.6079 0.2437 0.4510 0.089 Uiso 1 1 calc R . . C62 C 0.6790(6) 0.1557(4) 0.4242(4) 0.107(2) Uani 1 1 d . . . H62A H 0.7670 0.1794 0.4017 0.161 Uiso 1 1 calc R A . H62B H 0.6167 0.1686 0.3866 0.161 Uiso 1 1 calc R . . H62C H 0.6925 0.0994 0.4501 0.161 Uiso 1 1 calc R . . C63 C 0.5249(12) 0.0740(5) 0.5645(6) 0.074(3) Uiso 0.50 1 d PD A 1 H63A H 0.6142 0.0733 0.5822 0.089 Uiso 0.50 1 calc PR A 1 H63B H 0.5358 0.0434 0.5368 0.089 Uiso 0.50 1 calc PR A 1 C64 C 0.4210(12) 0.0370(7) 0.6285(6) 0.079(3) Uiso 0.50 1 d P A 1 H64A H 0.4513 -0.0164 0.6591 0.119 Uiso 0.50 1 calc PR A 1 H64B H 0.3328 0.0368 0.6112 0.119 Uiso 0.50 1 calc PR A 1 H64C H 0.4114 0.0664 0.6567 0.119 Uiso 0.50 1 calc PR A 1 C63' C 0.4583(16) 0.0706(5) 0.5505(7) 0.066(4) Uiso 0.35 1 d PD A 2 H63C H 0.3593 0.0615 0.5627 0.079 Uiso 0.35 1 calc PR A 2 H63D H 0.4940 0.0472 0.5181 0.079 Uiso 0.35 1 calc PR A 2 C64' C 0.533(2) 0.0367(12) 0.6184(11) 0.098(5) Uiso 0.35 1 d P A 2 H64D H 0.5209 -0.0193 0.6440 0.147 Uiso 0.35 1 calc PR A 2 H64E H 0.4955 0.0603 0.6499 0.147 Uiso 0.35 1 calc PR A 2 H64F H 0.6300 0.0472 0.6053 0.147 Uiso 0.35 1 calc PR A 2 C63" C 0.485(3) 0.0948(13) 0.5923(8) 0.061(8) Uiso 0.15 1 d PD A 3 H63E H 0.4049 0.1041 0.6213 0.073 Uiso 0.15 1 calc PR A 3 H63F H 0.5682 0.0985 0.6126 0.073 Uiso 0.15 1 calc PR A 3 C64" C 0.479(5) 0.0143(19) 0.598(3) 0.108(14) Uiso 0.15 1 d PD A 3 H64G H 0.4800 -0.0239 0.6493 0.162 Uiso 0.15 1 calc PR A 3 H64H H 0.5587 0.0046 0.5702 0.162 Uiso 0.15 1 calc PR A 3 H64I H 0.3956 0.0100 0.5794 0.162 Uiso 0.15 1 calc PR A 3 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 0.02870(8) 0.02873(8) 0.03080(8) -0.01329(6) -0.00241(5) 0.00048(5) Ta2 0.04041(9) 0.04386(10) 0.03667(9) -0.01793(7) 0.00069(6) -0.00490(7) N1 0.0343(14) 0.0252(14) 0.0431(16) -0.0143(13) -0.0082(12) 0.0022(12) N2 0.0286(13) 0.0316(15) 0.0292(14) -0.0098(12) -0.0019(11) 0.0038(11) N3 0.0342(15) 0.0363(16) 0.0445(16) -0.0235(14) -0.0051(12) 0.0016(12) N4 0.0323(14) 0.0488(18) 0.0366(15) -0.0277(14) 0.0011(12) 0.0040(13) N5 0.0400(16) 0.0427(18) 0.0337(15) -0.0149(14) -0.0012(12) -0.0045(13) N6 0.0385(16) 0.0515(19) 0.0302(15) -0.0121(14) -0.0017(12) -0.0043(14) N7 0.062(2) 0.069(2) 0.060(2) -0.039(2) 0.0092(17) -0.0198(19) N8 0.064(2) 0.049(2) 0.060(2) -0.0193(18) 0.0042(18) 0.0050(18) C1 0.0376(18) 0.0298(18) 0.044(2) -0.0105(16) -0.0086(15) -0.0025(15) C2 0.049(2) 0.049(2) 0.042(2) -0.0099(18) -0.0037(17) 0.0003(18) C3 0.063(3) 0.057(3) 0.048(2) 0.003(2) -0.015(2) -0.003(2) C4 0.049(2) 0.045(2) 0.069(3) -0.002(2) -0.021(2) 0.0055(19) C5 0.048(2) 0.035(2) 0.070(3) -0.017(2) -0.012(2) 0.0073(18) C6 0.048(2) 0.035(2) 0.046(2) -0.0167(17) -0.0097(17) 0.0081(17) C7 0.0339(17) 0.0294(18) 0.0406(19) -0.0125(15) -0.0044(14) -0.0006(14) C8 0.041(2) 0.045(2) 0.047(2) -0.0196(18) -0.0010(16) -0.0061(17) C9 0.037(2) 0.065(3) 0.063(3) -0.025(2) 0.0021(18) -0.0089(19) C10 0.044(2) 0.060(3) 0.066(3) -0.029(2) -0.0121(19) -0.0101(19) C11 0.048(2) 0.056(3) 0.053(2) -0.027(2) -0.0132(18) 0.0002(19) C12 0.0393(19) 0.043(2) 0.051(2) -0.0236(18) -0.0070(16) -0.0002(16) C13 0.0341(17) 0.0335(19) 0.0314(17) -0.0082(15) 0.0026(13) 0.0066(15) C14 0.050(2) 0.046(2) 0.050(2) -0.0235(19) 0.0004(17) 0.0067(18) C15 0.075(3) 0.065(3) 0.055(3) -0.029(2) 0.002(2) 0.027(3) C16 0.047(2) 0.098(4) 0.055(3) -0.023(3) 0.009(2) 0.025(3) C17 0.034(2) 0.087(4) 0.068(3) -0.028(3) 0.0054(19) 0.003(2) C18 0.0336(18) 0.052(2) 0.049(2) -0.0194(19) 0.0001(16) 0.0012(17) C19 0.0337(17) 0.0344(19) 0.0305(17) -0.0121(15) -0.0020(13) 0.0029(14) C20 0.0405(19) 0.048(2) 0.0367(19) -0.0166(17) -0.0060(15) -0.0015(17) C21 0.039(2) 0.064(3) 0.040(2) -0.011(2) -0.0098(16) -0.0027(19) C22 0.040(2) 0.058(3) 0.057(2) -0.007(2) -0.0112(18) 0.0176(19) C23 0.052(2) 0.040(2) 0.065(3) -0.015(2) -0.011(2) 0.0169(19) C24 0.046(2) 0.037(2) 0.048(2) -0.0182(17) -0.0085(16) 0.0065(16) C25 0.045(2) 0.053(2) 0.070(3) -0.042(2) -0.0118(19) 0.0032(18) C26 0.073(3) 0.046(3) 0.074(3) -0.032(2) -0.013(2) -0.005(2) C27 0.0360(18) 0.045(2) 0.054(2) -0.0246(19) -0.0108(16) 0.0030(16) C28 0.072(3) 0.065(3) 0.066(3) -0.028(2) -0.031(2) 0.003(2) C29 0.040(2) 0.046(2) 0.055(2) -0.0274(19) 0.0025(17) -0.0019(17) C30 0.055(3) 0.063(3) 0.078(3) -0.038(3) -0.002(2) 0.015(2) C31 0.051(2) 0.112(4) 0.049(3) -0.042(3) 0.002(2) 0.005(3) C32 0.107(5) 0.168(7) 0.052(3) -0.038(4) 0.015(3) -0.025(5) C33 0.046(2) 0.040(2) 0.0304(18) -0.0109(16) -0.0026(15) -0.0051(16) C34 0.070(3) 0.041(2) 0.042(2) -0.0090(18) -0.0023(19) -0.007(2) C35 0.083(3) 0.057(3) 0.036(2) -0.006(2) 0.007(2) -0.024(2) C36 0.059(3) 0.095(4) 0.047(2) -0.030(3) 0.011(2) -0.022(3) C37 0.057(3) 0.076(3) 0.048(2) -0.033(2) 0.0006(19) 0.004(2) C38 0.055(2) 0.050(2) 0.0336(19) -0.0138(18) -0.0035(16) 0.0051(19) C39 0.044(2) 0.044(2) 0.0316(18) -0.0088(16) -0.0035(15) -0.0055(17) C40 0.048(2) 0.059(3) 0.052(2) -0.013(2) -0.0104(18) -0.002(2) C41 0.050(3) 0.093(4) 0.068(3) -0.014(3) -0.019(2) -0.008(3) C42 0.066(3) 0.108(5) 0.054(3) -0.027(3) -0.003(2) -0.040(3) C43 0.071(3) 0.064(3) 0.047(2) -0.015(2) 0.001(2) -0.029(2) C44 0.058(2) 0.049(2) 0.042(2) -0.0127(19) -0.0042(18) -0.0116(19) C45 0.0369(19) 0.063(3) 0.0307(18) -0.0101(18) -0.0022(15) -0.0042(18) C46 0.050(2) 0.070(3) 0.046(2) -0.017(2) -0.0049(18) 0.013(2) C47 0.063(3) 0.101(4) 0.057(3) -0.015(3) 0.003(2) 0.027(3) C48 0.041(3) 0.139(6) 0.064(3) 0.001(4) 0.002(2) 0.016(3) C49 0.047(3) 0.154(7) 0.058(3) -0.018(4) -0.010(2) -0.017(3) C50 0.046(2) 0.108(4) 0.043(2) -0.023(3) -0.0074(18) -0.015(2) C51 0.0392(19) 0.057(2) 0.0328(18) -0.0188(18) -0.0023(15) -0.0057(17) C52 0.059(2) 0.052(2) 0.039(2) -0.0202(19) -0.0004(17) -0.012(2) C53 0.062(3) 0.054(3) 0.047(2) -0.016(2) 0.0010(19) -0.020(2) C54 0.041(2) 0.063(3) 0.043(2) -0.013(2) 0.0032(16) -0.0091(19) C55 0.055(2) 0.078(3) 0.042(2) -0.030(2) 0.0067(18) -0.012(2) C56 0.055(2) 0.070(3) 0.046(2) -0.034(2) 0.0107(18) -0.022(2) C57 0.102(4) 0.112(5) 0.104(5) -0.076(4) 0.014(4) -0.034(4) C58 0.162(7) 0.154(7) 0.104(5) -0.088(5) 0.003(5) -0.044(6) C59 0.060(3) 0.086(4) 0.072(3) -0.036(3) 0.003(2) -0.029(3) C60 0.117(5) 0.112(5) 0.109(5) -0.043(4) 0.033(4) -0.065(4) C61 0.052(3) 0.093(4) 0.077(3) -0.042(3) 0.001(2) 0.016(3) C62 0.096(4) 0.122(6) 0.104(5) -0.062(4) 0.018(4) 0.025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N4 1.992(3) . ? Ta1 N3 1.994(3) . ? Ta1 N1 1.994(3) . ? Ta1 N2 2.000(3) . ? Ta2 N7 1.987(3) . ? Ta2 N5 1.988(3) . ? Ta2 N6 1.998(3) . ? Ta2 N8 2.003(4) . ? N1 C1 1.463(4) . ? N1 C7 1.478(4) . ? N2 C19 1.466(4) . ? N2 C13 1.469(4) . ? N3 C27 1.469(4) . ? N3 C25 1.472(5) . ? N4 C31 1.462(5) . ? N4 C29 1.471(4) . ? N5 C33 1.463(4) . ? N5 C39 1.477(4) . ? N6 C51 1.470(4) . ? N6 C45 1.471(5) . ? N7 C59 1.446(5) . ? N7 C57 1.497(6) . ? N8 C61 1.457(6) . ? N8 C63 1.482(8) . ? N8 C63" 1.485(10) . ? N8 C63' 1.491(9) . ? C1 C6 1.523(5) . ? C1 C2 1.527(5) . ? C2 C3 1.532(6) . ? C3 C4 1.511(6) . ? C4 C5 1.508(6) . ? C5 C6 1.521(5) . ? C7 C8 1.520(5) . ? C7 C12 1.523(5) . ? C8 C9 1.527(5) . ? C9 C10 1.512(6) . ? C10 C11 1.515(6) . ? C11 C12 1.528(5) . ? C13 C14 1.516(5) . ? C13 C18 1.524(5) . ? C14 C15 1.528(5) . ? C15 C16 1.508(7) . ? C16 C17 1.524(7) . ? C17 C18 1.531(5) . ? C19 C24 1.515(5) . ? C19 C20 1.527(5) . ? C20 C21 1.521(5) . ? C21 C22 1.512(6) . ? C22 C23 1.517(6) . ? C23 C24 1.528(5) . ? C25 C26 1.504(6) . ? C27 C28 1.519(5) . ? C29 C30 1.518(6) . ? C31 C32 1.446(7) . ? C33 C38 1.517(5) . ? C33 C34 1.516(5) . ? C34 C35 1.534(6) . ? C35 C36 1.503(7) . ? C36 C37 1.510(6) . ? C37 C38 1.539(5) . ? C39 C40 1.520(5) . ? C39 C44 1.526(6) . ? C40 C41 1.520(6) . ? C41 C42 1.505(8) . ? C42 C43 1.523(7) . ? C43 C44 1.529(5) . ? C45 C46 1.522(6) . ? C45 C50 1.531(5) . ? C46 C47 1.533(6) . ? C47 C48 1.525(8) . ? C48 C49 1.508(9) . ? C49 C50 1.520(7) . ? C51 C56 1.516(5) . ? C51 C52 1.524(5) . ? C52 C53 1.518(5) . ? C53 C54 1.516(6) . ? C54 C55 1.508(6) . ? C55 C56 1.531(5) . ? C57 C58 1.456(8) . ? C59 C60 1.515(7) . ? C61 C62 1.516(7) . ? C63 C64 1.495(15) . ? C63' C64' 1.49(2) . ? C63" C64" 1.499(10) . ? 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 N4 Ta1 N3 96.40(11) . . ? N4 Ta1 N1 104.53(12) . . ? N3 Ta1 N1 123.55(11) . . ? N4 Ta1 N2 123.92(11) . . ? N3 Ta1 N2 105.02(11) . . ? N1 Ta1 N2 105.12(12) . . ? N7 Ta2 N5 124.42(13) . . ? N7 Ta2 N6 104.10(14) . . ? N5 Ta2 N6 105.72(13) . . ? N7 Ta2 N8 96.65(16) . . ? N5 Ta2 N8 103.97(14) . . ? N6 Ta2 N8 123.74(13) . . ? C1 N1 C7 116.1(3) . . ? C1 N1 Ta1 136.4(2) . . ? C7 N1 Ta1 107.1(2) . . ? C19 N2 C13 116.3(3) . . ? C19 N2 Ta1 136.0(2) . . ? C13 N2 Ta1 107.49(19) . . ? C27 N3 C25 113.5(3) . . ? C27 N3 Ta1 124.1(2) . . ? C25 N3 Ta1 122.1(2) . . ? C31 N4 C29 112.7(3) . . ? C31 N4 Ta1 122.7(2) . . ? C29 N4 Ta1 124.1(2) . . ? C33 N5 C39 114.7(3) . . ? C33 N5 Ta2 139.4(2) . . ? C39 N5 Ta2 105.9(2) . . ? C51 N6 C45 115.2(3) . . ? C51 N6 Ta2 138.5(3) . . ? C45 N6 Ta2 106.2(2) . . ? C59 N7 C57 113.8(4) . . ? C59 N7 Ta2 125.5(3) . . ? C57 N7 Ta2 120.7(3) . . ? C61 N8 C63 100.9(5) . . ? C61 N8 C63" 116.6(13) . . ? C63 N8 C63" 34.4(12) . . ? C61 N8 C63' 122.0(7) . . ? C63 N8 C63' 29.6(6) . . ? C63" N8 C63' 47.8(13) . . ? C61 N8 Ta2 122.0(3) . . ? C63 N8 Ta2 135.9(5) . . ? C63" N8 Ta2 108.2(13) . . ? C63' N8 Ta2 115.1(7) . . ? N1 C1 C6 111.6(3) . . ? N1 C1 C2 111.1(3) . . ? C6 C1 C2 110.7(3) . . ? C1 C2 C3 111.9(4) . . ? C4 C3 C2 111.4(3) . . ? C5 C4 C3 111.0(3) . . ? C4 C5 C6 111.2(4) . . ? C5 C6 C1 112.6(3) . . ? N1 C7 C8 113.8(3) . . ? N1 C7 C12 113.7(3) . . ? C8 C7 C12 111.5(3) . . ? C7 C8 C9 111.8(3) . . ? C10 C9 C8 111.5(3) . . ? C9 C10 C11 111.0(3) . . ? C10 C11 C12 111.6(3) . . ? C7 C12 C11 111.9(3) . . ? N2 C13 C14 114.6(3) . . ? N2 C13 C18 113.4(3) . . ? C14 C13 C18 111.1(3) . . ? C13 C14 C15 112.2(3) . . ? C16 C15 C14 111.8(4) . . ? C15 C16 C17 110.6(4) . . ? C16 C17 C18 111.2(4) . . ? C13 C18 C17 111.5(3) . . ? N2 C19 C24 111.3(3) . . ? N2 C19 C20 111.9(3) . . ? C24 C19 C20 110.7(3) . . ? C21 C20 C19 111.7(3) . . ? C22 C21 C20 110.8(3) . . ? C21 C22 C23 111.1(3) . . ? C22 C23 C24 111.1(3) . . ? C19 C24 C23 112.7(3) . . ? N3 C25 C26 115.9(3) . . ? N3 C27 C28 115.5(3) . . ? N4 C29 C30 114.9(3) . . ? C32 C31 N4 118.3(4) . . ? N5 C33 C38 112.4(3) . . ? N5 C33 C34 113.2(3) . . ? C38 C33 C34 109.9(3) . . ? C33 C34 C35 111.0(4) . . ? C36 C35 C34 112.4(3) . . ? C35 C36 C37 112.2(4) . . ? C36 C37 C38 110.3(4) . . ? C33 C38 C37 111.6(3) . . ? N5 C39 C40 113.4(3) . . ? N5 C39 C44 115.1(3) . . ? C40 C39 C44 110.7(3) . . ? C41 C40 C39 112.5(4) . . ? C42 C41 C40 111.5(4) . . ? C41 C42 C43 110.9(4) . . ? C42 C43 C44 111.8(4) . . ? C39 C44 C43 111.6(4) . . ? N6 C45 C46 114.6(3) . . ? N6 C45 C50 113.5(3) . . ? C46 C45 C50 110.9(4) . . ? C45 C46 C47 111.8(4) . . ? C48 C47 C46 111.2(4) . . ? C49 C48 C47 111.5(5) . . ? C48 C49 C50 111.2(5) . . ? C49 C50 C45 112.0(4) . . ? N6 C51 C56 112.3(3) . . ? N6 C51 C52 112.7(3) . . ? C56 C51 C52 110.2(3) . . ? C53 C52 C51 111.5(3) . . ? C54 C53 C52 111.5(4) . . ? C55 C54 C53 110.5(3) . . ? C54 C55 C56 111.6(3) . . ? C51 C56 C55 111.8(4) . . ? C58 C57 N7 115.6(6) . . ? N7 C59 C60 115.6(5) . . ? N8 C61 C62 115.1(5) . . ? N8 C63 C64 112.2(8) . . ? C64' C63' N8 105.0(12) . . ? N8 C63" C64" 112(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ta1 N1 C1 -110.3(3) . . . . ? N3 Ta1 N1 C1 -2.2(4) . . . . ? N2 Ta1 N1 C1 117.9(3) . . . . ? N4 Ta1 N1 C7 61.7(2) . . . . ? N3 Ta1 N1 C7 169.78(19) . . . . ? N2 Ta1 N1 C7 -70.1(2) . . . . ? N4 Ta1 N2 C19 -2.6(4) . . . . ? N3 Ta1 N2 C19 -111.3(3) . . . . ? N1 Ta1 N2 C19 117.0(3) . . . . ? N4 Ta1 N2 C13 171.3(2) . . . . ? N3 Ta1 N2 C13 62.6(2) . . . . ? N1 Ta1 N2 C13 -69.1(2) . . . . ? N4 Ta1 N3 C27 142.8(3) . . . . ? N1 Ta1 N3 C27 30.7(3) . . . . ? N2 Ta1 N3 C27 -89.5(3) . . . . ? N4 Ta1 N3 C25 -43.9(3) . . . . ? N1 Ta1 N3 C25 -156.0(3) . . . . ? N2 Ta1 N3 C25 83.8(3) . . . . ? N3 Ta1 N4 C31 -44.1(3) . . . . ? N1 Ta1 N4 C31 83.0(3) . . . . ? N2 Ta1 N4 C31 -157.1(3) . . . . ? N3 Ta1 N4 C29 145.5(3) . . . . ? N1 Ta1 N4 C29 -87.4(3) . . . . ? N2 Ta1 N4 C29 32.5(3) . . . . ? N7 Ta2 N5 C33 -10.6(4) . . . . ? N6 Ta2 N5 C33 109.3(4) . . . . ? N8 Ta2 N5 C33 -119.0(4) . . . . ? N7 Ta2 N5 C39 167.7(2) . . . . ? N6 Ta2 N5 C39 -72.3(2) . . . . ? N8 Ta2 N5 C39 59.4(2) . . . . ? N7 Ta2 N6 C51 -114.3(4) . . . . ? N5 Ta2 N6 C51 113.1(4) . . . . ? N8 Ta2 N6 C51 -6.2(4) . . . . ? N7 Ta2 N6 C45 60.8(3) . . . . ? N5 Ta2 N6 C45 -71.7(3) . . . . ? N8 Ta2 N6 C45 169.0(2) . . . . ? N5 Ta2 N7 C59 30.3(4) . . . . ? N6 Ta2 N7 C59 -90.4(4) . . . . ? N8 Ta2 N7 C59 142.3(4) . . . . ? N5 Ta2 N7 C57 -151.2(4) . . . . ? N6 Ta2 N7 C57 88.0(4) . . . . ? N8 Ta2 N7 C57 -39.2(4) . . . . ? N7 Ta2 N8 C61 140.6(4) . . . . ? N5 Ta2 N8 C61 -91.4(4) . . . . ? N6 Ta2 N8 C61 28.7(4) . . . . ? N7 Ta2 N8 C63 -55.1(9) . . . . ? N5 Ta2 N8 C63 72.9(9) . . . . ? N6 Ta2 N8 C63 -167.0(8) . . . . ? N7 Ta2 N8 C63" -79.8(12) . . . . ? N5 Ta2 N8 C63" 48.1(12) . . . . ? N6 Ta2 N8 C63" 168.3(12) . . . . ? N7 Ta2 N8 C63' -28.7(7) . . . . ? N5 Ta2 N8 C63' 99.3(7) . . . . ? N6 Ta2 N8 C63' -140.5(6) . . . . ? C7 N1 C1 C6 116.1(3) . . . . ? Ta1 N1 C1 C6 -72.4(4) . . . . ? C7 N1 C1 C2 -119.7(3) . . . . ? Ta1 N1 C1 C2 51.8(4) . . . . ? N1 C1 C2 C3 -177.3(3) . . . . ? C6 C1 C2 C3 -52.6(4) . . . . ? C1 C2 C3 C4 55.0(5) . . . . ? C2 C3 C4 C5 -56.4(5) . . . . ? C3 C4 C5 C6 56.3(5) . . . . ? C4 C5 C6 C1 -55.2(4) . . . . ? N1 C1 C6 C5 177.4(3) . . . . ? C2 C1 C6 C5 53.0(4) . . . . ? C1 N1 C7 C8 65.4(4) . . . . ? Ta1 N1 C7 C8 -108.5(3) . . . . ? C1 N1 C7 C12 -63.8(4) . . . . ? Ta1 N1 C7 C12 122.3(3) . . . . ? N1 C7 C8 C9 176.4(3) . . . . ? C12 C7 C8 C9 -53.3(4) . . . . ? C7 C8 C9 C10 55.1(5) . . . . ? C8 C9 C10 C11 -55.9(5) . . . . ? C9 C10 C11 C12 55.6(5) . . . . ? N1 C7 C12 C11 -176.7(3) . . . . ? C8 C7 C12 C11 52.9(4) . . . . ? C10 C11 C12 C7 -54.2(5) . . . . ? C19 N2 C13 C14 -61.0(4) . . . . ? Ta1 N2 C13 C14 123.7(3) . . . . ? C19 N2 C13 C18 68.0(4) . . . . ? Ta1 N2 C13 C18 -107.3(3) . . . . ? N2 C13 C14 C15 -176.5(3) . . . . ? C18 C13 C14 C15 53.3(4) . . . . ? C13 C14 C15 C16 -54.8(5) . . . . ? C14 C15 C16 C17 55.7(5) . . . . ? C15 C16 C17 C18 -56.3(5) . . . . ? N2 C13 C18 C17 175.3(3) . . . . ? C14 C13 C18 C17 -53.9(4) . . . . ? C16 C17 C18 C13 55.8(5) . . . . ? C13 N2 C19 C24 -124.8(3) . . . . ? Ta1 N2 C19 C24 48.7(4) . . . . ? C13 N2 C19 C20 110.7(3) . . . . ? Ta1 N2 C19 C20 -75.7(4) . . . . ? N2 C19 C20 C21 179.0(3) . . . . ? C24 C19 C20 C21 54.3(4) . . . . ? C19 C20 C21 C22 -56.7(4) . . . . ? C20 C21 C22 C23 57.1(4) . . . . ? C21 C22 C23 C24 -55.3(5) . . . . ? N2 C19 C24 C23 -178.1(3) . . . . ? C20 C19 C24 C23 -53.0(4) . . . . ? C22 C23 C24 C19 53.9(5) . . . . ? C27 N3 C25 C26 66.0(4) . . . . ? Ta1 N3 C25 C26 -107.9(3) . . . . ? C25 N3 C27 C28 67.6(4) . . . . ? Ta1 N3 C27 C28 -118.6(3) . . . . ? C31 N4 C29 C30 69.0(5) . . . . ? Ta1 N4 C29 C30 -119.7(3) . . . . ? C29 N4 C31 C32 61.0(6) . . . . ? Ta1 N4 C31 C32 -110.4(5) . . . . ? C39 N5 C33 C38 108.6(4) . . . . ? Ta2 N5 C33 C38 -73.1(5) . . . . ? C39 N5 C33 C34 -126.0(3) . . . . ? Ta2 N5 C33 C34 52.2(5) . . . . ? N5 C33 C34 C35 177.5(3) . . . . ? C38 C33 C34 C35 -55.9(4) . . . . ? C33 C34 C35 C36 54.3(5) . . . . ? C34 C35 C36 C37 -53.5(5) . . . . ? C35 C36 C37 C38 53.9(5) . . . . ? N5 C33 C38 C37 -175.1(3) . . . . ? C34 C33 C38 C37 57.8(4) . . . . ? C36 C37 C38 C33 -56.6(5) . . . . ? C33 N5 C39 C40 70.6(4) . . . . ? Ta2 N5 C39 C40 -108.2(3) . . . . ? C33 N5 C39 C44 -58.2(4) . . . . ? Ta2 N5 C39 C44 122.9(3) . . . . ? N5 C39 C40 C41 174.9(4) . . . . ? C44 C39 C40 C41 -54.0(5) . . . . ? C39 C40 C41 C42 55.6(5) . . . . ? C40 C41 C42 C43 -55.4(5) . . . . ? C41 C42 C43 C44 55.4(6) . . . . ? N5 C39 C44 C43 -176.6(3) . . . . ? C40 C39 C44 C43 53.3(4) . . . . ? C42 C43 C44 C39 -54.6(5) . . . . ? C51 N6 C45 C46 -60.0(4) . . . . ? Ta2 N6 C45 C46 123.5(3) . . . . ? C51 N6 C45 C50 68.8(5) . . . . ? Ta2 N6 C45 C50 -107.6(3) . . . . ? N6 C45 C46 C47 -176.1(3) . . . . ? C50 C45 C46 C47 53.7(5) . . . . ? C45 C46 C47 C48 -54.4(6) . . . . ? C46 C47 C48 C49 55.3(6) . . . . ? C47 C48 C49 C50 -55.9(6) . . . . ? C48 C49 C50 C45 55.6(6) . . . . ? N6 C45 C50 C49 174.9(4) . . . . ? C46 C45 C50 C49 -54.4(5) . . . . ? C45 N6 C51 C56 -122.9(4) . . . . ? Ta2 N6 C51 C56 51.9(5) . . . . ? C45 N6 C51 C52 111.9(4) . . . . ? Ta2 N6 C51 C52 -73.2(5) . . . . ? N6 C51 C52 C53 -178.2(4) . . . . ? C56 C51 C52 C53 55.4(5) . . . . ? C51 C52 C53 C54 -56.7(5) . . . . ? C52 C53 C54 C55 56.1(5) . . . . ? C53 C54 C55 C56 -55.2(5) . . . . ? N6 C51 C56 C55 178.8(3) . . . . ? C52 C51 C56 C55 -54.6(4) . . . . ? C54 C55 C56 C51 55.4(5) . . . . ? C59 N7 C57 C58 68.0(7) . . . . ? Ta2 N7 C57 C58 -110.7(5) . . . . ? C57 N7 C59 C60 62.0(6) . . . . ? Ta2 N7 C59 C60 -119.4(5) . . . . ? C63 N8 C61 C62 70.5(7) . . . . ? C63" N8 C61 C62 103.1(14) . . . . ? C63' N8 C61 C62 48.0(9) . . . . ? Ta2 N8 C61 C62 -120.5(5) . . . . ? C61 N8 C63 C64 158.4(9) . . . . ? C63" N8 C63 C64 37(2) . . . . ? C63' N8 C63 C64 -62.6(16) . . . . ? Ta2 N8 C63 C64 -8.1(15) . . . . ? C61 N8 C63' C64' 73.8(13) . . . . ? C63 N8 C63' C64' 24.2(14) . . . . ? C63" N8 C63' C64' -25(2) . . . . ? Ta2 N8 C63' C64' -117.0(11) . . . . ? C61 N8 C63" C64" -99(3) . . . . ? C63 N8 C63" C64" -30(3) . . . . ? C63' N8 C63" C64" 11(3) . . . . ? Ta2 N8 C63" C64" 119(3) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.045 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.070 #===END data_k534_Ta(NEt2)2Cl2(py-NMe2)2 _database_code_depnum_ccdc_archive 'CCDC 240192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H40 N6 Cl2 Ta, 1.5 C7 H8' _chemical_formula_sum 'C32.50 H52 N6 Cl2 Ta' _chemical_formula_weight 778.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.8606(9) _cell_length_b 14.5760(8) _cell_length_c 30.2633(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.938(1) _cell_angle_gamma 90.00 _cell_volume 7868.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 23.29 _exptl_crystal_description 'Flat column' _exptl_crystal_colour 'Very dark blue' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 2.957 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5449 _exptl_absorpt_correction_T_max 0.8969 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 35 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 8192 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was shown to be either Ia or I2/a. All of the toluene solvent molecules are disordered over several different orientations, with some being disordered about inversion centers or two-fold axes. Therefore all solvent molecules were treated as ideal rigid bodies, with occupancy factors based on refined isotropic thermal parameters. Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens as spheres of arbitrary diameter. Fig. 2 -- Packing of the molecules in the unit cell. Only one orientation of the disordered solvent is shown at each site. ; _diffrn_ambient_temperature 223(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 'Siemens SMART CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 16992 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 23.29 _reflns_number_total 5811 _reflns_number_gt 4129 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'Siemens SMART software (Siemens, 1996)' _computing_cell_refinement 'Siemens SAINT software (Siemens, 1996)' _computing_data_reduction 'Siemens SAINT software (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 4sigma(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^)+(0.0513P)^2^+41.4734P] 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_number_reflns 5599 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.256 _refine_ls_shift/su_mean 0.015 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 Ta Ta 0.496251(16) 0.42282(2) 0.362668(10) 0.03623(14) Uani 1 1 d . . . Cl1 Cl 0.47035(12) 0.26040(15) 0.37156(7) 0.0524(5) Uani 1 1 d . . . Cl2 Cl 0.50912(11) 0.57580(14) 0.33044(7) 0.0452(5) Uani 1 1 d . . . N1 N 0.5925(4) 0.4247(5) 0.3988(2) 0.0445(16) Uani 1 1 d . . . N2 N 0.4358(3) 0.4615(5) 0.4129(2) 0.0418(15) Uani 1 1 d . . . N3 N 0.3903(3) 0.4153(4) 0.3143(2) 0.0414(16) Uani 1 1 d . . . N4 N 0.2057(4) 0.3697(5) 0.2256(2) 0.0536(18) Uani 1 1 d . . . N5 N 0.5624(3) 0.3760(4) 0.3019(2) 0.0387(15) Uani 1 1 d . . . N6 N 0.6956(4) 0.2859(5) 0.2000(2) 0.0540(19) Uani 1 1 d . . . C1 C 0.6509(5) 0.3536(7) 0.3970(3) 0.057(2) Uani 1 1 d . . . H1A H 0.6988 0.3832 0.3914 0.068 Uiso 1 1 calc R . . H1B H 0.6383 0.3127 0.3720 0.068 Uiso 1 1 calc R . . C2 C 0.6610(7) 0.2963(9) 0.4387(4) 0.101(4) Uani 1 1 d . . . H2A H 0.6994 0.2504 0.4348 0.151 Uiso 1 1 calc R . . H2B H 0.6141 0.2662 0.4445 0.151 Uiso 1 1 calc R . . H2C H 0.6759 0.3356 0.4634 0.151 Uiso 1 1 calc R . . C3 C 0.6149(4) 0.4985(6) 0.4291(3) 0.052(2) Uani 1 1 d . . . H3A H 0.6379 0.4717 0.4562 0.062 Uiso 1 1 calc R . . H3B H 0.5701 0.5322 0.4371 0.062 Uiso 1 1 calc R . . C4 C 0.6705(5) 0.5661(7) 0.4098(4) 0.071(3) Uani 1 1 d . . . H4A H 0.6833 0.6133 0.4315 0.106 Uiso 1 1 calc R . . H4B H 0.6477 0.5943 0.3834 0.106 Uiso 1 1 calc R . . H4C H 0.7155 0.5336 0.4024 0.106 Uiso 1 1 calc R . . C5 C 0.4434(5) 0.4182(6) 0.4571(3) 0.051(2) Uani 1 1 d . . . H5A H 0.4476 0.4664 0.4796 0.061 Uiso 1 1 calc R . . H5B H 0.4897 0.3821 0.4592 0.061 Uiso 1 1 calc R . . C6 C 0.3766(6) 0.3553(8) 0.4668(3) 0.074(3) Uani 1 1 d . . . H6A H 0.3843 0.3293 0.4962 0.111 Uiso 1 1 calc R . . H6B H 0.3730 0.3063 0.4451 0.111 Uiso 1 1 calc R . . H6C H 0.3307 0.3908 0.4653 0.111 Uiso 1 1 calc R . . C7 C 0.3804(4) 0.5363(6) 0.4117(3) 0.051(2) Uani 1 1 d . . . H7A H 0.3351 0.5148 0.4254 0.061 Uiso 1 1 calc R . . H7B H 0.3667 0.5509 0.3807 0.061 Uiso 1 1 calc R . . C8 C 0.4073(6) 0.6222(7) 0.4347(3) 0.070(3) Uani 1 1 d . . . H8A H 0.3678 0.6680 0.4329 0.105 Uiso 1 1 calc R . . H8B H 0.4510 0.6456 0.4206 0.105 Uiso 1 1 calc R . . H8C H 0.4205 0.6087 0.4655 0.105 Uiso 1 1 calc R . . C9 C 0.3911(4) 0.4384(5) 0.2715(3) 0.0407(19) Uani 1 1 d . . . H9 H 0.4349 0.4654 0.2614 0.049 Uiso 1 1 calc R . . C10 C 0.3321(4) 0.4253(5) 0.2414(3) 0.0430(19) Uani 1 1 d . . . H10 H 0.3367 0.4426 0.2117 0.052 Uiso 1 1 calc R . . C11 C 0.2643(4) 0.3859(6) 0.2547(3) 0.0423(19) Uani 1 1 d . . . C12 C 0.2637(4) 0.3664(5) 0.3002(3) 0.042(2) Uani 1 1 d . . . H12 H 0.2200 0.3428 0.3120 0.051 Uiso 1 1 calc R . . C13 C 0.3256(4) 0.3812(6) 0.3275(3) 0.0437(19) Uani 1 1 d . . . H13 H 0.3226 0.3664 0.3576 0.052 Uiso 1 1 calc R . . C14 C 0.2096(6) 0.3853(8) 0.1792(3) 0.072(3) Uani 1 1 d . . . H14A H 0.2589 0.4088 0.1732 0.108 Uiso 1 1 calc R . . H14B H 0.1718 0.4296 0.1696 0.108 Uiso 1 1 calc R . . H14C H 0.2010 0.3281 0.1634 0.108 Uiso 1 1 calc R . . C15 C 0.1348(4) 0.3331(7) 0.2409(3) 0.062(3) Uani 1 1 d . . . H15A H 0.1391 0.3243 0.2727 0.092 Uiso 1 1 calc R . . H15B H 0.1240 0.2747 0.2265 0.092 Uiso 1 1 calc R . . H15C H 0.0946 0.3759 0.2335 0.092 Uiso 1 1 calc R . . C16 C 0.6253(4) 0.4194(5) 0.2922(3) 0.0393(18) Uani 1 1 d . . . H16 H 0.6395 0.4714 0.3089 0.047 Uiso 1 1 calc R . . C17 C 0.6707(4) 0.3924(5) 0.2589(3) 0.0422(19) Uani 1 1 d . . . H17 H 0.7145 0.4256 0.2538 0.051 Uiso 1 1 calc R . . C18 C 0.6517(4) 0.3161(5) 0.2330(3) 0.0425(19) Uani 1 1 d . . . C19 C 0.5854(4) 0.2701(6) 0.2429(3) 0.0426(19) Uani 1 1 d . . . H19 H 0.5694 0.2181 0.2266 0.051 Uiso 1 1 calc R . . C20 C 0.5445(4) 0.3024(5) 0.2768(3) 0.0409(19) Uani 1 1 d . . . H20 H 0.5005 0.2704 0.2829 0.049 Uiso 1 1 calc R . . C21 C 0.7603(5) 0.3365(7) 0.1873(3) 0.065(3) Uani 1 1 d . . . H21A H 0.7706 0.3858 0.2082 0.097 Uiso 1 1 calc R . . H21B H 0.7506 0.3619 0.1579 0.097 Uiso 1 1 calc R . . H21C H 0.8032 0.2957 0.1871 0.097 Uiso 1 1 calc R . . C22 C 0.6706(5) 0.2091(7) 0.1725(3) 0.075(3) Uani 1 1 d . . . H22A H 0.6265 0.1818 0.1845 0.112 Uiso 1 1 calc R . . H22B H 0.7102 0.1637 0.1719 0.112 Uiso 1 1 calc R . . H22C H 0.6584 0.2307 0.1426 0.112 Uiso 1 1 calc R . . C31 C 0.9166(6) 0.6195(7) 0.1187(3) 0.108(3) Uiso 0.65 1 d PG A 1 C32 C 0.9718(7) 0.6255(8) 0.1527(4) 0.108(3) Uiso 0.65 1 d PG A 1 H32 H 0.9924 0.6842 0.1611 0.130 Uiso 0.65 1 d PG A 1 C33 C 0.9971(7) 0.5466(9) 0.1745(4) 0.108(3) Uiso 0.65 1 d PG A 1 H33 H 1.0352 0.5508 0.1979 0.130 Uiso 0.65 1 d PG A 1 C34 C 0.9672(8) 0.4617(8) 0.1623(5) 0.108(3) Uiso 0.65 1 d PG A 1 H34 H 0.9847 0.4072 0.1774 0.130 Uiso 0.65 1 d PG A 1 C35 C 0.9120(8) 0.4557(7) 0.1283(5) 0.108(3) Uiso 0.65 1 d PG A 1 H35 H 0.8914 0.3971 0.1199 0.130 Uiso 0.65 1 d PG A 1 C36 C 0.8867(7) 0.5346(8) 0.1065(4) 0.108(3) Uiso 0.65 1 d PG A 1 H36 H 0.8486 0.5305 0.0830 0.130 Uiso 0.65 1 d PG A 1 C37 C 0.8893(9) 0.7047(9) 0.0952(5) 0.108(3) Uiso 0.65 1 d PG A 1 H37A H 0.9155 0.7570 0.1075 0.162 Uiso 0.65 1 d PG A 1 H37B H 0.8985 0.6998 0.0643 0.162 Uiso 0.65 1 d PG A 1 H37C H 0.8365 0.7118 0.0986 0.162 Uiso 0.65 1 d PG A 1 C41 C 0.9554(16) 0.5372(19) 0.1470(10) 0.112(7) Uiso 0.25 1 d PG B 2 C42 C 0.9001(19) 0.4934(18) 0.1208(13) 0.112(7) Uiso 0.25 1 d PG B 2 H42 H 0.8981 0.4276 0.1198 0.135 Uiso 0.25 1 d PG B 2 C43 C 0.8478(19) 0.545(2) 0.0958(13) 0.112(7) Uiso 0.25 1 d PG B 2 H43 H 0.8097 0.5145 0.0777 0.135 Uiso 0.25 1 d PG B 2 C44 C 0.8507(19) 0.640(2) 0.0972(11) 0.112(7) Uiso 0.25 1 d PG B 2 H44 H 0.8146 0.6756 0.0799 0.135 Uiso 0.25 1 d PG B 2 C45 C 0.906(2) 0.6839(18) 0.1234(13) 0.112(7) Uiso 0.25 1 d PG B 2 H45 H 0.9080 0.7497 0.1244 0.135 Uiso 0.25 1 d PG B 2 C46 C 0.958(2) 0.6324(19) 0.1483(12) 0.112(7) Uiso 0.25 1 d PG B 2 H46 H 0.9964 0.6627 0.1665 0.135 Uiso 0.25 1 d PG B 2 C47 C 1.012(2) 0.482(3) 0.1739(14) 0.112(7) Uiso 0.25 1 d PG B 2 H47A H 1.0020 0.4176 0.1693 0.168 Uiso 0.25 1 d PG B 2 H47B H 1.0613 0.4959 0.1650 0.168 Uiso 0.25 1 d PG B 2 H47C H 1.0083 0.4960 0.2047 0.168 Uiso 0.25 1 d PG B 2 C51 C 0.2110(17) 0.4352(18) 0.0304(9) 0.106(8) Uiso 0.22 1 d PG C -3 C52 C 0.154(2) 0.418(2) 0.0586(12) 0.106(8) Uiso 0.22 1 d PG C -3 H52 H 0.1430 0.3557 0.0671 0.128 Uiso 0.22 1 d PG C -3 C53 C 0.1116(19) 0.490(3) 0.0744(13) 0.106(8) Uiso 0.22 1 d PG C -3 H53 H 0.0719 0.4775 0.0938 0.128 Uiso 0.22 1 d PG C -3 C54 C 0.127(2) 0.579(2) 0.0621(13) 0.106(8) Uiso 0.22 1 d PG C -3 H54 H 0.0979 0.6290 0.0730 0.128 Uiso 0.22 1 d PG C -3 C55 C 0.184(2) 0.5969(18) 0.0339(13) 0.106(8) Uiso 0.22 1 d PG C -3 H55 H 0.1949 0.6588 0.0254 0.128 Uiso 0.22 1 d PG C -3 C56 C 0.2263(19) 0.525(2) 0.0181(11) 0.106(8) Uiso 0.22 1 d PG C -3 H56 H 0.2660 0.5370 -0.0014 0.128 Uiso 0.22 1 d PG C -3 C57 C 0.256(3) 0.358(2) 0.0133(14) 0.106(8) Uiso 0.22 1 d PG C -3 H57A H 0.2934 0.3812 -0.0055 0.159 Uiso 0.22 1 d PG C -3 H57B H 0.2808 0.3255 0.0378 0.159 Uiso 0.22 1 d PG C -3 H57C H 0.2239 0.3160 -0.0032 0.159 Uiso 0.22 1 d PG C -3 C61 C 0.0450(17) 0.461(2) 0.0313(10) 0.114(8) Uiso 0.22 1 d PG D -4 C62 C 0.0276(19) 0.549(2) 0.0158(11) 0.114(8) Uiso 0.22 1 d PG D -4 H62 H -0.0158 0.5582 -0.0037 0.136 Uiso 0.22 1 d PG D -4 C63 C 0.073(2) 0.622(2) 0.0285(14) 0.114(8) Uiso 0.22 1 d PG D -4 H63 H 0.0612 0.6828 0.0179 0.136 Uiso 0.22 1 d PG D -4 C64 C 0.136(2) 0.608(3) 0.0567(14) 0.114(8) Uiso 0.22 1 d PG D -4 H64 H 0.1675 0.6592 0.0655 0.136 Uiso 0.22 1 d PG D -4 C65 C 0.1534(19) 0.521(3) 0.0722(14) 0.114(8) Uiso 0.22 1 d PG D -4 H65 H 0.1969 0.5110 0.0916 0.136 Uiso 0.22 1 d PG D -4 C66 C 0.1079(19) 0.447(2) 0.0594(12) 0.114(8) Uiso 0.22 1 d PG D -4 H66 H 0.1199 0.3864 0.0701 0.136 Uiso 0.22 1 d PG D -4 C67 C -0.004(2) 0.381(3) 0.0175(16) 0.114(8) Uiso 0.22 1 d PG D -4 H67A H 0.0155 0.3262 0.0310 0.170 Uiso 0.22 1 d PG D -4 H67B H -0.0540 0.3918 0.0268 0.170 Uiso 0.22 1 d PG D -4 H67C H -0.0054 0.3751 -0.0141 0.170 Uiso 0.22 1 d PG D -4 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 Ta 0.02970(19) 0.0480(2) 0.0312(2) -0.00246(15) 0.00372(12) 0.00223(15) Cl1 0.0591(12) 0.0500(12) 0.0486(12) 0.0027(10) 0.0067(10) -0.0009(10) Cl2 0.0408(10) 0.0470(11) 0.0482(11) 0.0001(9) 0.0070(9) 0.0026(9) N1 0.037(4) 0.060(4) 0.036(4) -0.010(3) 0.002(3) 0.008(3) N2 0.031(3) 0.054(4) 0.041(4) 0.005(3) 0.002(3) 0.002(3) N3 0.034(4) 0.057(4) 0.033(4) 0.003(3) 0.004(3) -0.001(3) N4 0.038(4) 0.060(5) 0.062(5) -0.004(4) -0.009(3) -0.005(3) N5 0.030(3) 0.044(4) 0.042(4) -0.004(3) 0.005(3) -0.002(3) N6 0.045(4) 0.062(5) 0.057(5) -0.021(4) 0.020(3) -0.002(4) C1 0.045(5) 0.076(7) 0.048(5) -0.005(5) -0.005(4) 0.018(5) C2 0.120(10) 0.107(10) 0.074(8) 0.018(7) -0.001(7) 0.060(8) C3 0.035(4) 0.080(7) 0.040(5) -0.010(4) 0.005(4) 0.008(4) C4 0.045(5) 0.089(8) 0.078(7) -0.012(6) -0.004(5) -0.010(5) C5 0.042(5) 0.074(6) 0.037(5) 0.003(4) 0.001(4) 0.012(4) C6 0.079(7) 0.094(8) 0.049(6) 0.013(5) 0.018(5) -0.010(6) C7 0.039(5) 0.066(6) 0.049(5) 0.001(5) 0.010(4) 0.011(4) C8 0.083(7) 0.071(7) 0.056(6) -0.015(5) 0.007(5) 0.021(6) C9 0.030(4) 0.051(5) 0.042(5) -0.004(4) 0.007(3) 0.000(3) C10 0.040(4) 0.048(5) 0.041(5) 0.001(4) 0.004(4) 0.001(4) C11 0.033(4) 0.044(4) 0.049(5) -0.007(4) -0.003(4) 0.003(4) C12 0.022(4) 0.050(5) 0.056(5) -0.005(4) 0.011(4) -0.001(3) C13 0.037(4) 0.057(5) 0.038(5) -0.003(4) 0.009(4) 0.003(4) C14 0.071(7) 0.089(7) 0.055(6) 0.005(6) -0.018(5) -0.015(6) C15 0.032(4) 0.078(7) 0.075(7) -0.012(5) 0.003(4) -0.006(4) C16 0.037(4) 0.041(4) 0.040(4) -0.007(4) 0.005(3) 0.000(4) C17 0.033(4) 0.047(5) 0.047(5) -0.005(4) 0.009(4) -0.005(4) C18 0.043(5) 0.040(4) 0.045(5) -0.004(4) 0.007(4) 0.004(4) C19 0.039(4) 0.044(5) 0.045(5) -0.014(4) 0.004(4) -0.008(4) C20 0.031(4) 0.046(5) 0.046(5) -0.002(4) 0.002(4) -0.005(3) C21 0.059(6) 0.064(6) 0.073(7) -0.010(5) 0.030(5) -0.002(5) C22 0.061(6) 0.096(8) 0.069(7) -0.049(6) 0.019(5) 0.000(5) _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 Ta N2 1.990(6) . ? Ta N1 1.990(6) . ? Ta N3 2.336(6) . ? Ta N5 2.339(6) . ? Ta Cl1 2.430(2) . ? Ta Cl2 2.449(2) . ? N1 C3 1.457(10) . ? N1 C1 1.474(10) . ? N2 C7 1.472(10) . ? N2 C5 1.478(10) . ? N3 C9 1.339(10) . ? N3 C13 1.339(10) . ? N4 C11 1.352(10) . ? N4 C14 1.428(12) . ? N4 C15 1.470(11) . ? N5 C16 1.335(9) . ? N5 C20 1.344(10) . ? N6 C18 1.371(10) . ? N6 C21 1.440(11) . ? N6 C22 1.452(11) . ? C1 C2 1.515(13) . ? C3 C4 1.535(12) . ? C5 C6 1.545(12) . ? C7 C8 1.501(13) . ? C9 C10 1.370(11) . ? C10 C11 1.418(11) . ? C11 C12 1.409(11) . ? C12 C13 1.361(11) . ? C16 C17 1.381(11) . ? C17 C18 1.394(11) . ? C18 C19 1.407(11) . ? C19 C20 1.372(11) . ? C31 C32 1.3898 . ? C31 C36 1.3900 . ? C31 C37 1.5000 . ? C32 C33 1.3902 . ? C33 C34 1.3899 . ? C34 C35 1.3900 . ? C35 C36 1.3897 . ? C41 C46 1.3901 . ? C41 C42 1.3903 . ? C41 C47 1.4996 . ? C42 C43 1.3901 . ? C43 C44 1.3901 . ? C44 C45 1.3898 . ? C45 C46 1.3898 . ? C51 C56 1.3898 . ? C51 C52 1.3901 . ? C51 C57 1.5000 . ? C52 C53 1.3898 . ? C53 C54 1.3900 . ? C54 C55 1.3899 . ? C55 C56 1.3901 . ? C61 C66 1.3900 . ? C61 C62 1.3901 . ? C61 C67 1.5000 . ? C62 C63 1.3901 . ? C63 C64 1.3900 . ? C64 C65 1.3902 . ? C65 C66 1.3900 . ? 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 Ta N1 93.7(2) . . ? N2 Ta N3 92.2(2) . . ? N1 Ta N3 174.1(2) . . ? N2 Ta N5 177.5(2) . . ? N1 Ta N5 88.8(2) . . ? N3 Ta N5 85.3(2) . . ? N2 Ta Cl1 94.4(2) . . ? N1 Ta Cl1 96.7(2) . . ? N3 Ta Cl1 82.58(17) . . ? N5 Ta Cl1 84.80(17) . . ? N2 Ta Cl2 96.4(2) . . ? N1 Ta Cl2 96.3(2) . . ? N3 Ta Cl2 83.26(16) . . ? N5 Ta Cl2 83.74(17) . . ? Cl1 Ta Cl2 162.44(7) . . ? C3 N1 C1 111.7(6) . . ? C3 N1 Ta 123.9(5) . . ? C1 N1 Ta 124.3(5) . . ? C7 N2 C5 111.6(6) . . ? C7 N2 Ta 125.5(5) . . ? C5 N2 Ta 122.9(5) . . ? C9 N3 C13 115.8(7) . . ? C9 N3 Ta 123.1(5) . . ? C13 N3 Ta 121.0(5) . . ? C11 N4 C14 122.4(7) . . ? C11 N4 C15 120.6(8) . . ? C14 N4 C15 117.0(7) . . ? C16 N5 C20 115.6(6) . . ? C16 N5 Ta 120.0(5) . . ? C20 N5 Ta 124.2(5) . . ? C18 N6 C21 121.7(7) . . ? C18 N6 C22 119.7(7) . . ? C21 N6 C22 117.9(7) . . ? N1 C1 C2 114.3(8) . . ? N1 C3 C4 113.4(7) . . ? N2 C5 C6 113.0(7) . . ? N2 C7 C8 114.1(7) . . ? N3 C9 C10 124.2(7) . . ? C9 C10 C11 120.5(8) . . ? N4 C11 C12 123.8(7) . . ? N4 C11 C10 122.1(8) . . ? C12 C11 C10 114.1(7) . . ? C13 C12 C11 121.0(7) . . ? N3 C13 C12 124.4(8) . . ? N5 C16 C17 123.9(7) . . ? C16 C17 C18 120.2(7) . . ? N6 C18 C17 122.3(7) . . ? N6 C18 C19 121.4(7) . . ? C17 C18 C19 116.2(7) . . ? C20 C19 C18 118.9(7) . . ? N5 C20 C19 125.1(7) . . ? C32 C31 C36 120.0 . . ? C32 C31 C37 120.0 . . ? C36 C31 C37 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C46 C41 C42 120.0 . . ? C46 C41 C47 120.0 . . ? C42 C41 C47 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C56 C51 C52 120.0 . . ? C56 C51 C57 120.0 . . ? C52 C51 C57 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C51 C56 C55 120.0 . . ? C66 C61 C62 120.0 . . ? C66 C61 C67 120.0 . . ? C62 C61 C67 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C65 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ta N1 C3 -45.2(6) . . . . ? N3 Ta N1 C3 137(2) . . . . ? N5 Ta N1 C3 135.3(6) . . . . ? Cl1 Ta N1 C3 -140.1(6) . . . . ? Cl2 Ta N1 C3 51.7(6) . . . . ? N2 Ta N1 C1 137.0(7) . . . . ? N3 Ta N1 C1 -40(3) . . . . ? N5 Ta N1 C1 -42.5(7) . . . . ? Cl1 Ta N1 C1 42.1(7) . . . . ? Cl2 Ta N1 C1 -126.1(6) . . . . ? N1 Ta N2 C7 130.5(6) . . . . ? N3 Ta N2 C7 -49.8(6) . . . . ? N5 Ta N2 C7 -60(6) . . . . ? Cl1 Ta N2 C7 -132.5(6) . . . . ? Cl2 Ta N2 C7 33.7(6) . . . . ? N1 Ta N2 C5 -47.9(6) . . . . ? N3 Ta N2 C5 131.8(6) . . . . ? N5 Ta N2 C5 121(5) . . . . ? Cl1 Ta N2 C5 49.1(6) . . . . ? Cl2 Ta N2 C5 -144.7(6) . . . . ? N2 Ta N3 C9 144.2(6) . . . . ? N1 Ta N3 C9 -38(3) . . . . ? N5 Ta N3 C9 -36.2(6) . . . . ? Cl1 Ta N3 C9 -121.6(6) . . . . ? Cl2 Ta N3 C9 48.0(6) . . . . ? N2 Ta N3 C13 -40.3(6) . . . . ? N1 Ta N3 C13 137(2) . . . . ? N5 Ta N3 C13 139.3(6) . . . . ? Cl1 Ta N3 C13 53.9(6) . . . . ? Cl2 Ta N3 C13 -136.5(6) . . . . ? N2 Ta N5 C16 143(5) . . . . ? N1 Ta N5 C16 -47.2(6) . . . . ? N3 Ta N5 C16 133.0(6) . . . . ? Cl1 Ta N5 C16 -144.0(6) . . . . ? Cl2 Ta N5 C16 49.3(5) . . . . ? N2 Ta N5 C20 -42(6) . . . . ? N1 Ta N5 C20 127.8(6) . . . . ? N3 Ta N5 C20 -52.0(6) . . . . ? Cl1 Ta N5 C20 31.0(6) . . . . ? Cl2 Ta N5 C20 -135.7(6) . . . . ? C3 N1 C1 C2 70.2(11) . . . . ? Ta N1 C1 C2 -111.8(9) . . . . ? C1 N1 C3 C4 77.8(9) . . . . ? Ta N1 C3 C4 -100.3(7) . . . . ? C7 N2 C5 C6 74.9(9) . . . . ? Ta N2 C5 C6 -106.5(7) . . . . ? C5 N2 C7 C8 74.4(9) . . . . ? Ta N2 C7 C8 -104.1(8) . . . . ? C13 N3 C9 C10 -3.1(11) . . . . ? Ta N3 C9 C10 172.7(6) . . . . ? N3 C9 C10 C11 0.7(12) . . . . ? C14 N4 C11 C12 -176.2(9) . . . . ? C15 N4 C11 C12 2.6(13) . . . . ? C14 N4 C11 C10 4.2(13) . . . . ? C15 N4 C11 C10 -176.9(8) . . . . ? C9 C10 C11 N4 -178.1(8) . . . . ? C9 C10 C11 C12 2.3(11) . . . . ? N4 C11 C12 C13 177.5(8) . . . . ? C10 C11 C12 C13 -2.9(11) . . . . ? C9 N3 C13 C12 2.4(12) . . . . ? Ta N3 C13 C12 -173.4(6) . . . . ? C11 C12 C13 N3 0.7(13) . . . . ? C20 N5 C16 C17 -0.3(11) . . . . ? Ta N5 C16 C17 175.2(6) . . . . ? N5 C16 C17 C18 0.4(12) . . . . ? C21 N6 C18 C17 -6.3(13) . . . . ? C22 N6 C18 C17 -176.5(9) . . . . ? C21 N6 C18 C19 175.0(8) . . . . ? C22 N6 C18 C19 4.9(13) . . . . ? C16 C17 C18 N6 -179.0(8) . . . . ? C16 C17 C18 C19 -0.3(12) . . . . ? N6 C18 C19 C20 178.7(8) . . . . ? C17 C18 C19 C20 0.0(12) . . . . ? C16 N5 C20 C19 -0.1(12) . . . . ? Ta N5 C20 C19 -175.3(6) . . . . ? C18 C19 C20 N5 0.2(13) . . . . ? C36 C31 C32 C33 0.0 . . . . ? C37 C31 C32 C33 180.0 . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? C37 C31 C36 C35 180.0 . . . . ? C46 C41 C42 C43 0.0 . . . . ? C47 C41 C42 C43 -180.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? C47 C41 C46 C45 180.0 . . . . ? C56 C51 C52 C53 0.0 . . . . ? C57 C51 C52 C53 -180.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C57 C51 C56 C55 180.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C66 C61 C62 C63 0.0 . . . . ? C67 C61 C62 C63 -180.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? C67 C61 C66 C65 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.133 _refine_diff_density_min -1.023 _refine_diff_density_rms 0.182