# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.Ballmann A.Yeo B.A.MacKay S.v.Rjit B.O.Patrick M.D.Fryzuk _publ_contact_author_name 'Joachim Ballmann' _publ_contact_author_email mail@joachim-ballmann.de data_mf518_NPNTaS2CH2TaNPN _database_code_depnum_ccdc_archive 'CCDC 790440' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H62 N4 P2 S2 Si4 Ta2' _chemical_formula_sum 'C49 H62 N4 P2 S2 Si4 Ta2' _chemical_formula_weight 1307.35 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' Si Si 0.0817 0.0704 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bcn' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 21.9524(8) _cell_length_b 21.7688(9) _cell_length_c 24.6370(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11773.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28465 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 29.43 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5184 _exptl_absorpt_coefficient_mu 3.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22431 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.08 _reflns_number_total 13086 _reflns_number_gt 7696 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^ > 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^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13086 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3569(3) 0.8261(3) 0.1272(3) 0.0225(15) Uani 1 1 d . . . H1A H 0.3785 0.8661 0.1275 0.027 Uiso 1 1 calc R . . H1B H 0.3825 0.7957 0.1464 0.027 Uiso 1 1 calc R . . C2 C 0.4079(3) 0.8287(4) 0.0161(3) 0.0248(15) Uani 1 1 d . . . H2A H 0.4074 0.8086 -0.0199 0.030 Uiso 1 1 calc R . . H2B H 0.4470 0.8191 0.0341 0.030 Uiso 1 1 calc R . . C3 C 0.2907(4) 0.8792(4) 0.2253(3) 0.0338(18) Uani 1 1 d . . . H3A H 0.3018 0.9215 0.2160 0.051 Uiso 1 1 calc R . . H3B H 0.3228 0.8610 0.2477 0.051 Uiso 1 1 calc R . . H3C H 0.2522 0.8792 0.2455 0.051 Uiso 1 1 calc R . . C4 C 0.2494(4) 0.7569(4) 0.1780(3) 0.0338(18) Uani 1 1 d . . . H4A H 0.2082 0.7615 0.1927 0.051 Uiso 1 1 calc R . . H4B H 0.2753 0.7361 0.2047 0.051 Uiso 1 1 calc R . . H4C H 0.2478 0.7324 0.1446 0.051 Uiso 1 1 calc R . . C5 C 0.4551(3) 0.9532(4) 0.0528(4) 0.041(2) Uani 1 1 d . . . H5A H 0.4506 0.9978 0.0494 0.061 Uiso 1 1 calc R . . H5B H 0.4964 0.9412 0.0421 0.061 Uiso 1 1 calc R . . H5C H 0.4479 0.9411 0.0906 0.061 Uiso 1 1 calc R . . C6 C 0.4145(3) 0.9412(4) -0.0614(3) 0.0350(19) Uani 1 1 d . . . H6A H 0.3877 0.9196 -0.0868 0.052 Uiso 1 1 calc R . . H6B H 0.4571 0.9327 -0.0707 0.052 Uiso 1 1 calc R . . H6C H 0.4070 0.9855 -0.0637 0.052 Uiso 1 1 calc R . . C7 C 0.1773(3) 0.8911(3) 0.1406(3) 0.0259(16) Uani 1 1 d . . . C8 C 0.1283(4) 0.8506(4) 0.1437(3) 0.041(2) Uani 1 1 d . . . H8 H 0.1310 0.8109 0.1279 0.049 Uiso 1 1 calc R . . C9 C 0.0746(4) 0.8693(5) 0.1704(4) 0.055(3) Uani 1 1 d . . . H9 H 0.0410 0.8419 0.1725 0.066 Uiso 1 1 calc R . . C10 C 0.0703(4) 0.9264(5) 0.1933(4) 0.049(3) Uani 1 1 d . . . H10 H 0.0341 0.9382 0.2115 0.059 Uiso 1 1 calc R . . C11 C 0.1181(4) 0.9664(4) 0.1899(4) 0.042(2) Uani 1 1 d . . . H11 H 0.1150 1.0061 0.2056 0.051 Uiso 1 1 calc R . . C12 C 0.1715(4) 0.9487(4) 0.1634(3) 0.036(2) Uani 1 1 d . . . H12 H 0.2044 0.9769 0.1610 0.043 Uiso 1 1 calc R . . C13 C 0.3492(3) 0.7184(3) 0.0579(3) 0.0229(16) Uani 1 1 d . . . C14 C 0.3599(3) 0.6833(3) 0.1048(3) 0.0314(18) Uani 1 1 d . . . H14 H 0.3663 0.7035 0.1385 0.038 Uiso 1 1 calc R . . C15 C 0.3614(3) 0.6199(4) 0.1027(4) 0.039(2) Uani 1 1 d . . . H15 H 0.3677 0.5971 0.1351 0.047 Uiso 1 1 calc R . . C16 C 0.3539(4) 0.5892(4) 0.0544(4) 0.040(2) Uani 1 1 d . . . H16 H 0.3555 0.5456 0.0535 0.048 Uiso 1 1 calc R . . C17 C 0.3441(4) 0.6218(4) 0.0070(4) 0.042(2) Uani 1 1 d . . . H17 H 0.3390 0.6006 -0.0264 0.050 Uiso 1 1 calc R . . C18 C 0.3415(3) 0.6867(4) 0.0085(3) 0.0320(18) Uani 1 1 d . . . H18 H 0.3346 0.7091 -0.0240 0.038 Uiso 1 1 calc R . . C19 C 0.3171(3) 0.9930(3) 0.0487(3) 0.0217(14) Uani 1 1 d . . . C20 C 0.3221(4) 1.0093(4) 0.1027(3) 0.0349(19) Uani 1 1 d . . . H20 H 0.3274 0.9782 0.1293 0.042 Uiso 1 1 calc R . . C21 C 0.3194(5) 1.0704(4) 0.1185(3) 0.046(2) Uani 1 1 d . . . H21 H 0.3225 1.0806 0.1559 0.055 Uiso 1 1 calc R . . C22 C 0.3125(4) 1.1159(4) 0.0812(4) 0.043(2) Uani 1 1 d . . . H22 H 0.3113 1.1577 0.0922 0.052 Uiso 1 1 calc R . . C23 C 0.3074(4) 1.1005(4) 0.0272(4) 0.039(2) Uani 1 1 d . . . H23 H 0.3026 1.1319 0.0008 0.047 Uiso 1 1 calc R . . C24 C 0.3092(4) 1.0396(4) 0.0111(3) 0.0325(18) Uani 1 1 d . . . H24 H 0.3049 1.0297 -0.0262 0.039 Uiso 1 1 calc R . . C25 C 0.0425(4) 0.7636(4) -0.0986(3) 0.039(2) Uani 1 1 d . . . H25A H 0.0201 0.7891 -0.1252 0.047 Uiso 1 1 calc R . . H25B H 0.0137 0.7327 -0.0842 0.047 Uiso 1 1 calc R . . C26 C 0.0268(3) 0.8843(4) -0.0525(3) 0.0328(19) Uani 1 1 d . . . H26A H 0.0284 0.9096 -0.0191 0.039 Uiso 1 1 calc R . . H26B H -0.0164 0.8759 -0.0611 0.039 Uiso 1 1 calc R . . C27 C 0.1007(5) 0.6379(4) -0.1205(5) 0.058(3) Uani 1 1 d . . . H27A H 0.1332 0.6158 -0.1396 0.087 Uiso 1 1 calc R . . H27B H 0.0610 0.6226 -0.1328 0.087 Uiso 1 1 calc R . . H27C H 0.1048 0.6311 -0.0814 0.087 Uiso 1 1 calc R . . C28 C 0.0940(4) 0.7331(4) -0.2106(3) 0.047(2) Uani 1 1 d . . . H28A H 0.0752 0.7733 -0.2168 0.070 Uiso 1 1 calc R . . H28B H 0.0670 0.7007 -0.2242 0.070 Uiso 1 1 calc R . . H28C H 0.1331 0.7311 -0.2296 0.070 Uiso 1 1 calc R . . C29 C 0.0202(4) 0.9153(5) -0.1769(4) 0.052(3) Uani 1 1 d . . . H29A H 0.0416 0.9365 -0.2064 0.079 Uiso 1 1 calc R . . H29B H -0.0208 0.9324 -0.1730 0.079 Uiso 1 1 calc R . . H29C H 0.0174 0.8714 -0.1853 0.079 Uiso 1 1 calc R . . C30 C 0.0685(4) 1.0107(4) -0.0961(4) 0.048(2) Uani 1 1 d . . . H30A H 0.0867 1.0172 -0.0602 0.071 Uiso 1 1 calc R . . H30B H 0.0274 1.0283 -0.0968 0.071 Uiso 1 1 calc R . . H30C H 0.0937 1.0307 -0.1237 0.071 Uiso 1 1 calc R . . C31 C 0.2301(3) 0.7218(4) -0.1349(3) 0.0265(17) Uani 1 1 d . . . C32 C 0.2667(4) 0.7494(4) -0.1737(3) 0.036(2) Uani 1 1 d . . . H32 H 0.2561 0.7890 -0.1870 0.043 Uiso 1 1 calc R . . C33 C 0.3184(4) 0.7207(5) -0.1935(3) 0.045(2) Uani 1 1 d . . . H33 H 0.3435 0.7407 -0.2195 0.054 Uiso 1 1 calc R . . C34 C 0.3334(4) 0.6623(5) -0.1748(4) 0.054(3) Uani 1 1 d . . . H34 H 0.3686 0.6419 -0.1882 0.065 Uiso 1 1 calc R . . C35 C 0.2979(5) 0.6349(4) -0.1377(4) 0.049(3) Uani 1 1 d . . . H35 H 0.3077 0.5947 -0.1256 0.059 Uiso 1 1 calc R . . C36 C 0.2471(4) 0.6643(4) -0.1170(3) 0.040(2) Uani 1 1 d . . . H36 H 0.2235 0.6445 -0.0898 0.048 Uiso 1 1 calc R . . C37 C 0.0374(3) 0.7760(4) 0.0182(3) 0.0276(17) Uani 1 1 d . . . C38 C 0.0605(3) 0.7187(4) 0.0335(3) 0.0348(19) Uani 1 1 d . . . H38 H 0.0921 0.7001 0.0129 0.042 Uiso 1 1 calc R . . C39 C 0.0379(4) 0.6896(5) 0.0779(4) 0.049(2) Uani 1 1 d . . . H39 H 0.0545 0.6510 0.0884 0.058 Uiso 1 1 calc R . . C40 C -0.0088(4) 0.7150(5) 0.1082(4) 0.054(3) Uani 1 1 d . . . H40 H -0.0245 0.6939 0.1390 0.064 Uiso 1 1 calc R . . C41 C -0.0323(4) 0.7714(5) 0.0932(4) 0.051(3) Uani 1 1 d . . . H41 H -0.0648 0.7889 0.1134 0.062 Uiso 1 1 calc R . . C42 C -0.0088(4) 0.8024(4) 0.0490(3) 0.0347(19) Uani 1 1 d . . . H42 H -0.0242 0.8417 0.0396 0.042 Uiso 1 1 calc R . . C43 C 0.1743(4) 0.9124(4) -0.1587(3) 0.0299(18) Uani 1 1 d . . . C44 C 0.1751(4) 0.8868(4) -0.2103(3) 0.044(2) Uani 1 1 d . . . H44 H 0.1479 0.8544 -0.2191 0.053 Uiso 1 1 calc R . . C45 C 0.2167(5) 0.9091(4) -0.2496(4) 0.048(3) Uani 1 1 d . . . H45 H 0.2179 0.8911 -0.2847 0.058 Uiso 1 1 calc R . . C46 C 0.2544(5) 0.9558(4) -0.2375(4) 0.058(3) Uani 1 1 d . . . H46 H 0.2825 0.9699 -0.2641 0.069 Uiso 1 1 calc R . . C47 C 0.2529(5) 0.9839(4) -0.1868(4) 0.054(3) Uani 1 1 d . . . H47 H 0.2789 1.0177 -0.1790 0.065 Uiso 1 1 calc R . . C48 C 0.2137(4) 0.9623(4) -0.1483(3) 0.039(2) Uani 1 1 d . . . H48 H 0.2129 0.9814 -0.1136 0.046 Uiso 1 1 calc R . . N1 N 0.2339(2) 0.8713(3) 0.1161(2) 0.0181(12) Uani 1 1 d . . . N2 N 0.3255(2) 0.9294(3) 0.0315(2) 0.0203(12) Uani 1 1 d . . . N3 N 0.1768(3) 0.7528(3) -0.1146(2) 0.0239(13) Uani 1 1 d . . . N4 N 0.1354(3) 0.8904(3) -0.1161(2) 0.0270(15) Uani 1 1 d . . . C100 C 0.2007(3) 0.7905(3) 0.0116(3) 0.0202(15) Uani 1 1 d . . . Si1 Si 0.28164(9) 0.83393(10) 0.16260(7) 0.0217(4) Uani 1 1 d . . . Si2 Si 0.39903(9) 0.91450(10) 0.00823(9) 0.0253(5) Uani 1 1 d . . . Si3 Si 0.10676(10) 0.72176(11) -0.13545(9) 0.0313(5) Uani 1 1 d . . . Si4 Si 0.06422(10) 0.92614(11) -0.11047(10) 0.0345(5) Uani 1 1 d . . . P1 P 0.34426(8) 0.80133(8) 0.05717(7) 0.0194(4) Uani 1 1 d . . . P2 P 0.06747(8) 0.81309(9) -0.04230(8) 0.0247(4) Uani 1 1 d . . . S1 S 0.16775(8) 0.92863(8) 0.00359(7) 0.0222(4) Uani 1 1 d . . . S2 S 0.28538(7) 0.84924(8) -0.06878(7) 0.0212(4) Uani 1 1 d . . . Ta1 Ta 0.247842(12) 0.875461(14) 0.035563(10) 0.01456(6) Uani 1 1 d . . . Ta2 Ta 0.184326(12) 0.829976(13) -0.068290(10) 0.01732(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.022(4) 0.014(4) 0.032(4) 0.002(3) -0.010(3) -0.001(3) C2 0.015(3) 0.025(4) 0.035(4) 0.001(3) 0.006(3) 0.004(3) C3 0.042(5) 0.034(5) 0.025(4) -0.002(4) -0.009(3) 0.008(4) C4 0.038(5) 0.028(4) 0.035(4) 0.002(3) 0.010(4) -0.001(4) C5 0.018(4) 0.044(6) 0.059(6) -0.005(4) -0.004(4) -0.009(4) C6 0.026(4) 0.027(4) 0.052(5) 0.001(4) 0.014(4) -0.009(3) C7 0.021(4) 0.036(5) 0.020(3) -0.001(3) 0.001(3) 0.006(3) C8 0.026(4) 0.058(6) 0.039(5) -0.011(4) 0.010(4) -0.012(4) C9 0.034(5) 0.087(8) 0.045(5) -0.008(5) 0.013(4) -0.017(5) C10 0.033(5) 0.076(8) 0.038(5) -0.003(5) 0.007(4) 0.017(5) C11 0.043(5) 0.036(5) 0.048(5) -0.003(4) 0.013(4) 0.013(4) C12 0.030(5) 0.037(5) 0.040(4) 0.004(4) 0.005(4) 0.002(4) C13 0.011(3) 0.020(4) 0.038(4) -0.005(3) 0.001(3) -0.001(3) C14 0.024(4) 0.024(5) 0.046(5) 0.001(3) 0.010(3) 0.004(3) C15 0.024(4) 0.028(5) 0.066(6) 0.012(5) 0.007(4) 0.008(4) C16 0.026(4) 0.021(5) 0.073(7) -0.004(4) 0.005(4) -0.002(3) C17 0.026(4) 0.030(5) 0.069(6) -0.025(5) 0.002(4) -0.007(4) C18 0.021(4) 0.027(5) 0.048(5) -0.002(4) -0.003(4) 0.000(3) C19 0.014(3) 0.013(3) 0.038(4) -0.003(3) 0.002(3) -0.005(3) C20 0.047(5) 0.027(4) 0.031(4) 0.003(3) -0.002(4) -0.012(4) C21 0.059(6) 0.041(5) 0.037(5) -0.017(4) 0.017(5) -0.020(5) C22 0.040(5) 0.020(4) 0.070(6) -0.012(4) 0.015(5) -0.009(4) C23 0.043(5) 0.013(4) 0.062(6) 0.003(4) -0.008(4) 0.008(4) C24 0.027(4) 0.031(5) 0.039(4) -0.003(3) -0.006(4) 0.001(4) C25 0.024(4) 0.060(6) 0.034(4) -0.012(4) -0.002(4) -0.016(4) C26 0.016(4) 0.043(5) 0.039(4) 0.002(4) -0.004(3) 0.002(3) C27 0.043(6) 0.039(6) 0.091(8) -0.004(5) -0.021(5) -0.009(5) C28 0.042(5) 0.060(7) 0.037(5) -0.025(4) -0.008(4) 0.001(5) C29 0.032(5) 0.072(7) 0.054(6) 0.015(5) -0.025(5) 0.006(5) C30 0.034(5) 0.033(5) 0.076(7) 0.007(5) -0.011(5) 0.013(4) C31 0.026(4) 0.031(5) 0.022(3) -0.011(3) -0.006(3) -0.002(3) C32 0.034(5) 0.045(6) 0.029(4) -0.007(4) -0.006(4) -0.003(4) C33 0.030(5) 0.074(7) 0.032(4) -0.017(4) -0.002(4) -0.002(5) C34 0.026(5) 0.091(9) 0.047(5) -0.040(6) -0.009(4) 0.016(5) C35 0.054(6) 0.044(6) 0.050(5) -0.019(5) -0.024(5) 0.019(5) C36 0.042(5) 0.041(5) 0.037(4) -0.004(4) -0.006(4) 0.006(5) C37 0.013(4) 0.039(5) 0.031(4) -0.004(3) 0.002(3) -0.008(3) C38 0.020(4) 0.051(6) 0.033(4) 0.001(4) 0.004(3) -0.012(4) C39 0.034(5) 0.050(6) 0.062(6) 0.012(5) -0.009(5) -0.012(4) C40 0.040(6) 0.078(8) 0.043(5) 0.012(5) 0.003(4) -0.027(6) C41 0.038(5) 0.080(8) 0.037(5) -0.017(5) 0.018(4) -0.017(5) C42 0.027(4) 0.039(5) 0.039(4) -0.011(4) 0.004(3) -0.006(4) C43 0.035(5) 0.033(5) 0.022(4) 0.004(3) 0.001(3) 0.011(4) C44 0.060(6) 0.040(6) 0.034(4) 0.001(4) -0.002(4) -0.001(5) C45 0.072(7) 0.038(6) 0.035(5) 0.007(4) 0.011(5) 0.008(5) C46 0.088(8) 0.037(6) 0.048(5) 0.012(4) 0.022(6) 0.003(6) C47 0.075(7) 0.035(6) 0.053(6) 0.002(4) 0.010(5) -0.014(5) C48 0.053(6) 0.028(5) 0.034(4) 0.002(4) 0.010(4) 0.000(4) N1 0.012(3) 0.027(3) 0.015(2) -0.001(2) -0.0015(19) -0.002(3) N2 0.013(3) 0.016(3) 0.033(3) 0.001(2) -0.003(3) -0.005(2) N3 0.028(3) 0.025(3) 0.019(3) -0.008(2) -0.002(3) -0.007(3) N4 0.017(3) 0.035(4) 0.029(3) 0.006(3) 0.000(3) -0.003(3) C100 0.017(4) 0.022(4) 0.022(3) -0.002(3) 0.005(3) -0.007(3) Si1 0.0260(11) 0.0191(10) 0.0198(9) -0.0015(8) -0.0016(8) 0.0021(9) Si2 0.0132(10) 0.0267(12) 0.0359(12) 0.0012(9) 0.0024(9) -0.0051(8) Si3 0.0271(12) 0.0310(13) 0.0357(12) -0.0090(10) -0.0053(10) -0.0064(10) Si4 0.0222(12) 0.0419(15) 0.0394(13) 0.0063(11) -0.0087(10) 0.0038(10) P1 0.0131(8) 0.0176(9) 0.0275(9) -0.0002(7) -0.0002(7) 0.0004(7) P2 0.0130(9) 0.0354(12) 0.0257(9) -0.0030(8) -0.0017(7) -0.0035(8) S1 0.0175(9) 0.0213(9) 0.0278(9) -0.0033(7) -0.0047(7) 0.0045(7) S2 0.0151(8) 0.0271(9) 0.0215(8) -0.0022(7) 0.0022(7) -0.0077(7) Ta1 0.01021(11) 0.01465(12) 0.01883(11) -0.00097(11) -0.00068(11) -0.00091(11) Ta2 0.01206(12) 0.02044(13) 0.01945(12) -0.00094(12) -0.00102(12) -0.00188(12) _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 C1 P1 1.829(7) . ? C1 Si1 1.876(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 P1 1.825(7) . ? C2 Si2 1.887(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 Si1 1.842(7) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si1 1.859(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si2 1.852(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si2 1.842(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.380(11) . ? C7 C8 1.393(11) . ? C7 N1 1.448(8) . ? C8 C9 1.409(12) . ? C8 H8 0.9500 . ? C9 C10 1.368(13) . ? C9 H9 0.9500 . ? C10 C11 1.365(13) . ? C10 H10 0.9500 . ? C11 C12 1.395(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.405(10) . ? C13 C18 1.409(10) . ? C13 P1 1.809(7) . ? C14 C15 1.383(11) . ? C14 H14 0.9500 . ? C15 C16 1.375(12) . ? C15 H15 0.9500 . ? C16 C17 1.382(13) . ? C16 H16 0.9500 . ? C17 C18 1.416(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.380(10) . ? C19 C24 1.384(10) . ? C19 N2 1.461(8) . ? C20 C21 1.387(11) . ? C20 H20 0.9500 . ? C21 C22 1.359(12) . ? C21 H21 0.9500 . ? C22 C23 1.375(12) . ? C22 H22 0.9500 . ? C23 C24 1.384(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 P2 1.839(8) . ? C25 Si3 1.909(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 P2 1.807(8) . ? C26 Si4 1.883(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 Si3 1.868(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Si3 1.888(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si4 1.915(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Si4 1.877(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.380(11) . ? C31 C32 1.386(11) . ? C31 N3 1.440(9) . ? C32 C33 1.384(12) . ? C32 H32 0.9500 . ? C33 C34 1.393(14) . ? C33 H33 0.9500 . ? C34 C35 1.340(14) . ? C34 H34 0.9500 . ? C35 C36 1.384(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.390(10) . ? C37 C38 1.398(11) . ? C37 P2 1.820(8) . ? C38 C39 1.358(11) . ? C38 H38 0.9500 . ? C39 C40 1.382(13) . ? C39 H39 0.9500 . ? C40 C41 1.383(14) . ? C40 H40 0.9500 . ? C41 C42 1.382(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.387(11) . ? C43 C48 1.412(11) . ? C43 N4 1.436(9) . ? C44 C45 1.418(12) . ? C44 H44 0.9500 . ? C45 C46 1.344(14) . ? C45 H45 0.9500 . ? C46 C47 1.393(12) . ? C46 H46 0.9500 . ? C47 C48 1.365(12) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N1 Si1 1.754(6) . ? N1 Ta1 2.009(5) . ? N2 Si2 1.743(6) . ? N2 Ta1 2.073(5) . ? N3 Si3 1.756(6) . ? N3 Ta2 2.038(5) . ? N4 Si4 1.752(6) . ? N4 Ta2 2.066(6) . ? C100 Ta2 2.177(7) . ? C100 Ta1 2.200(7) . ? P1 Ta1 2.7143(18) . ? P2 Ta2 2.6694(19) . ? S1 Ta1 2.2476(17) . ? S1 Ta2 2.8073(18) . ? S2 Ta2 2.2577(16) . ? S2 Ta1 2.7591(18) . ? Ta1 Ta2 3.0775(4) . ? 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 P1 C1 Si1 109.4(3) . . ? P1 C1 H1A 109.8 . . ? Si1 C1 H1A 109.8 . . ? P1 C1 H1B 109.8 . . ? Si1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? P1 C2 Si2 107.6(4) . . ? P1 C2 H2A 110.2 . . ? Si2 C2 H2A 110.2 . . ? P1 C2 H2B 110.2 . . ? Si2 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 118.8(7) . . ? C12 C7 N1 121.3(7) . . ? C8 C7 N1 119.8(7) . . ? C7 C8 C9 119.2(9) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 120.8(9) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 120.1(9) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.9(9) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 121.2(8) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C18 117.8(7) . . ? C14 C13 P1 124.1(6) . . ? C18 C13 P1 118.2(6) . . ? C15 C14 C13 121.0(8) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 121.0(8) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.0(8) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 119.9(8) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 120.3(8) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C24 117.8(7) . . ? C20 C19 N2 120.8(6) . . ? C24 C19 N2 121.2(6) . . ? C19 C20 C21 120.8(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 120.9(8) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.1(8) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C24 120.5(8) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 120.9(7) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? P2 C25 Si3 114.7(4) . . ? P2 C25 H25A 108.6 . . ? Si3 C25 H25A 108.6 . . ? P2 C25 H25B 108.6 . . ? Si3 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? P2 C26 Si4 107.7(4) . . ? P2 C26 H26A 110.2 . . ? Si4 C26 H26A 110.2 . . ? P2 C26 H26B 110.2 . . ? Si4 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C28 H28A 109.5 . . ? Si3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.3(8) . . ? C36 C31 N3 122.3(7) . . ? C32 C31 N3 120.5(7) . . ? C33 C32 C31 121.5(9) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 119.3(9) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 119.6(9) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 121.0(9) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C31 C36 C35 121.3(9) . . ? C31 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C42 C37 C38 119.1(7) . . ? C42 C37 P2 121.9(7) . . ? C38 C37 P2 119.0(6) . . ? C39 C38 C37 120.1(8) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 121.3(9) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C41 119.2(9) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 120.3(9) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C37 120.0(9) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C44 C43 C48 118.0(7) . . ? C44 C43 N4 122.8(8) . . ? C48 C43 N4 119.2(7) . . ? C43 C44 C45 119.8(9) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 120.2(9) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 121.2(9) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C48 C47 C46 119.2(9) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C43 121.6(8) . . ? C47 C48 H48 119.2 . . ? C43 C48 H48 119.2 . . ? C7 N1 Si1 112.2(4) . . ? C7 N1 Ta1 122.0(4) . . ? Si1 N1 Ta1 125.1(3) . . ? C19 N2 Si2 112.9(4) . . ? C19 N2 Ta1 114.8(4) . . ? Si2 N2 Ta1 132.3(3) . . ? C31 N3 Si3 115.4(4) . . ? C31 N3 Ta2 121.0(5) . . ? Si3 N3 Ta2 123.5(3) . . ? C43 N4 Si4 116.1(5) . . ? C43 N4 Ta2 108.7(4) . . ? Si4 N4 Ta2 134.5(3) . . ? Ta2 C100 Ta1 89.4(3) . . ? N1 Si1 C3 111.3(3) . . ? N1 Si1 C4 109.0(4) . . ? C3 Si1 C4 110.7(4) . . ? N1 Si1 C1 105.3(3) . . ? C3 Si1 C1 110.1(4) . . ? C4 Si1 C1 110.4(4) . . ? N2 Si2 C6 114.7(3) . . ? N2 Si2 C5 109.6(3) . . ? C6 Si2 C5 106.6(4) . . ? N2 Si2 C2 104.2(3) . . ? C6 Si2 C2 112.9(3) . . ? C5 Si2 C2 108.7(4) . . ? N3 Si3 C27 112.4(4) . . ? N3 Si3 C28 111.5(4) . . ? C27 Si3 C28 108.0(5) . . ? N3 Si3 C25 108.9(3) . . ? C27 Si3 C25 108.7(5) . . ? C28 Si3 C25 107.1(4) . . ? N4 Si4 C30 113.9(4) . . ? N4 Si4 C26 103.6(3) . . ? C30 Si4 C26 110.6(4) . . ? N4 Si4 C29 109.1(4) . . ? C30 Si4 C29 107.9(4) . . ? C26 Si4 C29 111.7(4) . . ? C13 P1 C2 106.6(3) . . ? C13 P1 C1 106.0(3) . . ? C2 P1 C1 108.1(3) . . ? C13 P1 Ta1 129.9(2) . . ? C2 P1 Ta1 107.1(2) . . ? C1 P1 Ta1 97.3(2) . . ? C26 P2 C37 108.4(4) . . ? C26 P2 C25 104.5(4) . . ? C37 P2 C25 104.5(4) . . ? C26 P2 Ta2 108.9(3) . . ? C37 P2 Ta2 127.3(2) . . ? C25 P2 Ta2 100.7(3) . . ? Ta1 S1 Ta2 74.08(5) . . ? Ta2 S2 Ta1 74.93(5) . . ? N1 Ta1 N2 101.4(2) . . ? N1 Ta1 C100 99.0(2) . . ? N2 Ta1 C100 148.2(2) . . ? N1 Ta1 S1 104.46(16) . . ? N2 Ta1 S1 109.60(16) . . ? C100 Ta1 S1 88.32(19) . . ? N1 Ta1 P1 84.19(16) . . ? N2 Ta1 P1 72.80(16) . . ? C100 Ta1 P1 85.40(19) . . ? S1 Ta1 P1 170.04(6) . . ? N1 Ta1 S2 162.97(17) . . ? N2 Ta1 S2 80.02(16) . . ? C100 Ta1 S2 73.54(17) . . ? S1 Ta1 S2 90.78(6) . . ? P1 Ta1 S2 80.03(5) . . ? N1 Ta1 Ta2 137.51(15) . . ? N2 Ta1 Ta2 121.01(16) . . ? C100 Ta1 Ta2 45.03(17) . . ? S1 Ta1 Ta2 61.31(5) . . ? P1 Ta1 Ta2 108.97(4) . . ? S2 Ta1 Ta2 45.10(3) . . ? N3 Ta2 N4 99.4(2) . . ? N3 Ta2 C100 101.2(2) . . ? N4 Ta2 C100 148.4(2) . . ? N3 Ta2 S2 103.29(18) . . ? N4 Ta2 S2 112.90(17) . . ? C100 Ta2 S2 85.18(18) . . ? N3 Ta2 P2 86.73(18) . . ? N4 Ta2 P2 74.05(17) . . ? C100 Ta2 P2 83.53(18) . . ? S2 Ta2 P2 166.19(6) . . ? N3 Ta2 S1 166.79(18) . . ? N4 Ta2 S1 78.78(18) . . ? C100 Ta2 S1 75.69(18) . . ? S2 Ta2 S1 89.35(6) . . ? P2 Ta2 S1 80.18(6) . . ? N3 Ta2 Ta1 140.17(17) . . ? N4 Ta2 Ta1 120.30(17) . . ? C100 Ta2 Ta1 45.62(18) . . ? S2 Ta2 Ta1 59.97(5) . . ? P2 Ta2 Ta1 106.28(4) . . ? S1 Ta2 Ta1 44.61(4) . . ? 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 C12 C7 C8 C9 -0.8(12) . . . . ? N1 C7 C8 C9 176.5(7) . . . . ? C7 C8 C9 C10 -0.1(14) . . . . ? C8 C9 C10 C11 0.7(15) . . . . ? C9 C10 C11 C12 -0.4(14) . . . . ? C8 C7 C12 C11 1.1(12) . . . . ? N1 C7 C12 C11 -176.1(7) . . . . ? C10 C11 C12 C7 -0.5(13) . . . . ? C18 C13 C14 C15 -1.5(11) . . . . ? P1 C13 C14 C15 178.1(6) . . . . ? C13 C14 C15 C16 1.6(11) . . . . ? C14 C15 C16 C17 -0.7(12) . . . . ? C15 C16 C17 C18 -0.2(12) . . . . ? C14 C13 C18 C17 0.6(11) . . . . ? P1 C13 C18 C17 -179.1(6) . . . . ? C16 C17 C18 C13 0.2(12) . . . . ? C24 C19 C20 C21 -0.3(12) . . . . ? N2 C19 C20 C21 174.3(7) . . . . ? C19 C20 C21 C22 -0.7(14) . . . . ? C20 C21 C22 C23 0.8(14) . . . . ? C21 C22 C23 C24 0.0(14) . . . . ? C22 C23 C24 C19 -1.0(13) . . . . ? C20 C19 C24 C23 1.2(12) . . . . ? N2 C19 C24 C23 -173.4(7) . . . . ? C36 C31 C32 C33 -0.3(11) . . . . ? N3 C31 C32 C33 179.4(7) . . . . ? C31 C32 C33 C34 1.3(12) . . . . ? C32 C33 C34 C35 -0.5(12) . . . . ? C33 C34 C35 C36 -1.2(13) . . . . ? C32 C31 C36 C35 -1.4(11) . . . . ? N3 C31 C36 C35 178.9(7) . . . . ? C34 C35 C36 C31 2.2(13) . . . . ? C42 C37 C38 C39 -0.1(11) . . . . ? P2 C37 C38 C39 -178.7(6) . . . . ? C37 C38 C39 C40 1.2(13) . . . . ? C38 C39 C40 C41 -0.7(14) . . . . ? C39 C40 C41 C42 -1.0(14) . . . . ? C40 C41 C42 C37 2.1(13) . . . . ? C38 C37 C42 C41 -1.6(11) . . . . ? P2 C37 C42 C41 177.0(6) . . . . ? C48 C43 C44 C45 2.9(13) . . . . ? N4 C43 C44 C45 -177.1(8) . . . . ? C43 C44 C45 C46 -1.4(15) . . . . ? C44 C45 C46 C47 -1.1(16) . . . . ? C45 C46 C47 C48 2.0(16) . . . . ? C46 C47 C48 C43 -0.4(15) . . . . ? C44 C43 C48 C47 -2.0(13) . . . . ? N4 C43 C48 C47 178.0(8) . . . . ? C12 C7 N1 Si1 91.1(7) . . . . ? C8 C7 N1 Si1 -86.0(7) . . . . ? C12 C7 N1 Ta1 -97.9(7) . . . . ? C8 C7 N1 Ta1 85.0(8) . . . . ? C20 C19 N2 Si2 -96.7(7) . . . . ? C24 C19 N2 Si2 77.6(8) . . . . ? C20 C19 N2 Ta1 86.3(7) . . . . ? C24 C19 N2 Ta1 -99.3(7) . . . . ? C36 C31 N3 Si3 -71.1(8) . . . . ? C32 C31 N3 Si3 109.2(7) . . . . ? C36 C31 N3 Ta2 111.9(7) . . . . ? C32 C31 N3 Ta2 -67.8(8) . . . . ? C44 C43 N4 Si4 -91.8(8) . . . . ? C48 C43 N4 Si4 88.2(8) . . . . ? C44 C43 N4 Ta2 96.2(8) . . . . ? C48 C43 N4 Ta2 -83.8(7) . . . . ? C7 N1 Si1 C3 -50.0(6) . . . . ? Ta1 N1 Si1 C3 139.3(4) . . . . ? C7 N1 Si1 C4 72.3(6) . . . . ? Ta1 N1 Si1 C4 -98.3(4) . . . . ? C7 N1 Si1 C1 -169.3(5) . . . . ? Ta1 N1 Si1 C1 20.0(5) . . . . ? P1 C1 Si1 N1 -43.7(4) . . . . ? P1 C1 Si1 C3 -163.8(4) . . . . ? P1 C1 Si1 C4 73.7(5) . . . . ? C19 N2 Si2 C6 -78.3(5) . . . . ? Ta1 N2 Si2 C6 98.0(5) . . . . ? C19 N2 Si2 C5 41.6(6) . . . . ? Ta1 N2 Si2 C5 -142.1(5) . . . . ? C19 N2 Si2 C2 157.8(5) . . . . ? Ta1 N2 Si2 C2 -25.9(5) . . . . ? P1 C2 Si2 N2 -11.9(4) . . . . ? P1 C2 Si2 C6 -137.1(4) . . . . ? P1 C2 Si2 C5 104.8(4) . . . . ? C31 N3 Si3 C27 53.5(7) . . . . ? Ta2 N3 Si3 C27 -129.6(5) . . . . ? C31 N3 Si3 C28 -68.0(6) . . . . ? Ta2 N3 Si3 C28 108.9(4) . . . . ? C31 N3 Si3 C25 174.0(5) . . . . ? Ta2 N3 Si3 C25 -9.0(5) . . . . ? P2 C25 Si3 N3 -11.6(6) . . . . ? P2 C25 Si3 C27 111.2(5) . . . . ? P2 C25 Si3 C28 -132.3(5) . . . . ? C43 N4 Si4 C30 -61.0(7) . . . . ? Ta2 N4 Si4 C30 108.4(5) . . . . ? C43 N4 Si4 C26 178.8(6) . . . . ? Ta2 N4 Si4 C26 -11.9(6) . . . . ? C43 N4 Si4 C29 59.7(6) . . . . ? Ta2 N4 Si4 C29 -130.9(5) . . . . ? P2 C26 Si4 N4 -17.6(5) . . . . ? P2 C26 Si4 C30 -140.0(4) . . . . ? P2 C26 Si4 C29 99.7(5) . . . . ? C14 C13 P1 C2 115.8(6) . . . . ? C18 C13 P1 C2 -64.5(6) . . . . ? C14 C13 P1 C1 0.7(7) . . . . ? C18 C13 P1 C1 -179.6(5) . . . . ? C14 C13 P1 Ta1 -113.7(6) . . . . ? C18 C13 P1 Ta1 66.0(6) . . . . ? Si2 C2 P1 C13 173.9(3) . . . . ? Si2 C2 P1 C1 -72.4(4) . . . . ? Si2 C2 P1 Ta1 31.5(4) . . . . ? Si1 C1 P1 C13 -92.9(4) . . . . ? Si1 C1 P1 C2 153.0(4) . . . . ? Si1 C1 P1 Ta1 42.3(4) . . . . ? Si4 C26 P2 C37 173.8(4) . . . . ? Si4 C26 P2 C25 -75.2(5) . . . . ? Si4 C26 P2 Ta2 31.8(4) . . . . ? C42 C37 P2 C26 -0.6(7) . . . . ? C38 C37 P2 C26 177.9(6) . . . . ? C42 C37 P2 C25 -111.7(7) . . . . ? C38 C37 P2 C25 66.9(7) . . . . ? C42 C37 P2 Ta2 132.3(5) . . . . ? C38 C37 P2 Ta2 -49.1(7) . . . . ? Si3 C25 P2 C26 133.4(5) . . . . ? Si3 C25 P2 C37 -112.9(5) . . . . ? Si3 C25 P2 Ta2 20.4(5) . . . . ? C7 N1 Ta1 N2 123.0(5) . . . . ? Si1 N1 Ta1 N2 -67.2(4) . . . . ? C7 N1 Ta1 C100 -81.4(6) . . . . ? Si1 N1 Ta1 C100 88.4(4) . . . . ? C7 N1 Ta1 S1 9.1(6) . . . . ? Si1 N1 Ta1 S1 178.9(3) . . . . ? C7 N1 Ta1 P1 -165.8(5) . . . . ? Si1 N1 Ta1 P1 4.0(3) . . . . ? C7 N1 Ta1 S2 -143.8(5) . . . . ? Si1 N1 Ta1 S2 26.0(8) . . . . ? C7 N1 Ta1 Ta2 -54.0(6) . . . . ? Si1 N1 Ta1 Ta2 115.8(3) . . . . ? C19 N2 Ta1 N1 -67.1(5) . . . . ? Si2 N2 Ta1 N1 116.6(4) . . . . ? C19 N2 Ta1 C100 163.9(5) . . . . ? Si2 N2 Ta1 C100 -12.3(7) . . . . ? C19 N2 Ta1 S1 42.9(5) . . . . ? Si2 N2 Ta1 S1 -133.4(4) . . . . ? C19 N2 Ta1 P1 -147.3(5) . . . . ? Si2 N2 Ta1 P1 36.4(4) . . . . ? C19 N2 Ta1 S2 130.1(5) . . . . ? Si2 N2 Ta1 S2 -46.1(4) . . . . ? C19 N2 Ta1 Ta2 110.5(4) . . . . ? Si2 N2 Ta1 Ta2 -65.7(4) . . . . ? Ta2 C100 Ta1 N1 153.9(2) . . . . ? Ta2 C100 Ta1 N2 -76.7(5) . . . . ? Ta2 C100 Ta1 S1 49.49(18) . . . . ? Ta2 C100 Ta1 P1 -122.77(19) . . . . ? Ta2 C100 Ta1 S2 -41.83(14) . . . . ? Ta2 S1 Ta1 N1 -136.64(17) . . . . ? Ta2 S1 Ta1 N2 115.37(17) . . . . ? Ta2 S1 Ta1 C100 -37.82(17) . . . . ? Ta2 S1 Ta1 S2 35.69(4) . . . . ? C13 P1 Ta1 N1 91.5(3) . . . . ? C2 P1 Ta1 N1 -138.2(3) . . . . ? C1 P1 Ta1 N1 -26.6(3) . . . . ? C13 P1 Ta1 N2 -164.6(4) . . . . ? C2 P1 Ta1 N2 -34.3(3) . . . . ? C1 P1 Ta1 N2 77.3(3) . . . . ? C13 P1 Ta1 C100 -8.0(4) . . . . ? C2 P1 Ta1 C100 122.3(3) . . . . ? C1 P1 Ta1 C100 -126.1(3) . . . . ? C13 P1 Ta1 S2 -82.1(3) . . . . ? C2 P1 Ta1 S2 48.3(3) . . . . ? C1 P1 Ta1 S2 159.8(2) . . . . ? C13 P1 Ta1 Ta2 -47.0(3) . . . . ? C2 P1 Ta1 Ta2 83.3(3) . . . . ? C1 P1 Ta1 Ta2 -165.1(2) . . . . ? Ta2 S2 Ta1 N1 107.6(5) . . . . ? Ta2 S2 Ta1 N2 -156.02(16) . . . . ? Ta2 S2 Ta1 C100 41.8(2) . . . . ? Ta2 S2 Ta1 S1 -46.25(6) . . . . ? Ta2 S2 Ta1 P1 129.87(6) . . . . ? C31 N3 Ta2 N4 121.2(5) . . . . ? Si3 N3 Ta2 N4 -55.5(4) . . . . ? C31 N3 Ta2 C100 -82.8(5) . . . . ? Si3 N3 Ta2 C100 100.5(4) . . . . ? C31 N3 Ta2 S2 4.9(5) . . . . ? Si3 N3 Ta2 S2 -171.9(3) . . . . ? C31 N3 Ta2 P2 -165.5(5) . . . . ? Si3 N3 Ta2 P2 17.7(3) . . . . ? C31 N3 Ta2 S1 -158.0(6) . . . . ? Si3 N3 Ta2 S1 25.3(10) . . . . ? C31 N3 Ta2 Ta1 -53.8(6) . . . . ? Si3 N3 Ta2 Ta1 129.4(3) . . . . ? C43 N4 Ta2 N3 -81.5(5) . . . . ? Si4 N4 Ta2 N3 108.6(5) . . . . ? C43 N4 Ta2 C100 148.2(5) . . . . ? Si4 N4 Ta2 C100 -21.7(8) . . . . ? C43 N4 Ta2 S2 27.3(5) . . . . ? Si4 N4 Ta2 S2 -142.6(4) . . . . ? C43 N4 Ta2 P2 -165.3(5) . . . . ? Si4 N4 Ta2 P2 24.7(4) . . . . ? C43 N4 Ta2 S1 111.8(5) . . . . ? Si4 N4 Ta2 S1 -58.1(5) . . . . ? C43 N4 Ta2 Ta1 94.8(5) . . . . ? Si4 N4 Ta2 Ta1 -75.1(5) . . . . ? Ta1 C100 Ta2 N3 154.3(2) . . . . ? Ta1 C100 Ta2 N4 -75.9(5) . . . . ? Ta1 C100 Ta2 S2 51.66(17) . . . . ? Ta1 C100 Ta2 P2 -120.37(19) . . . . ? Ta1 C100 Ta2 S1 -38.90(15) . . . . ? Ta1 S2 Ta2 N3 -140.80(17) . . . . ? Ta1 S2 Ta2 N4 112.86(19) . . . . ? Ta1 S2 Ta2 C100 -40.36(18) . . . . ? Ta1 S2 Ta2 P2 -5.1(3) . . . . ? Ta1 S2 Ta2 S1 35.34(5) . . . . ? C26 P2 Ta2 N3 -130.1(3) . . . . ? C37 P2 Ta2 N3 97.1(4) . . . . ? C25 P2 Ta2 N3 -20.5(4) . . . . ? C26 P2 Ta2 N4 -29.3(3) . . . . ? C37 P2 Ta2 N4 -162.1(4) . . . . ? C25 P2 Ta2 N4 80.2(4) . . . . ? C26 P2 Ta2 C100 128.2(3) . . . . ? C37 P2 Ta2 C100 -4.6(4) . . . . ? C25 P2 Ta2 C100 -122.2(4) . . . . ? C26 P2 Ta2 S2 92.9(4) . . . . ? C37 P2 Ta2 S2 -39.9(5) . . . . ? C25 P2 Ta2 S2 -157.6(4) . . . . ? C26 P2 Ta2 S1 51.7(3) . . . . ? C37 P2 Ta2 S1 -81.1(3) . . . . ? C25 P2 Ta2 S1 161.3(3) . . . . ? C26 P2 Ta2 Ta1 88.3(3) . . . . ? C37 P2 Ta2 Ta1 -44.5(3) . . . . ? C25 P2 Ta2 Ta1 -162.2(3) . . . . ? Ta1 S1 Ta2 N3 117.8(7) . . . . ? Ta1 S1 Ta2 N4 -158.99(17) . . . . ? Ta1 S1 Ta2 C100 39.72(18) . . . . ? Ta1 S1 Ta2 S2 -45.48(6) . . . . ? Ta1 S1 Ta2 P2 125.48(6) . . . . ? N1 Ta1 Ta2 N3 -81.8(4) . . . . ? N2 Ta1 Ta2 N3 101.7(3) . . . . ? C100 Ta1 Ta2 N3 -41.6(4) . . . . ? S1 Ta1 Ta2 N3 -161.6(3) . . . . ? P1 Ta1 Ta2 N3 20.8(3) . . . . ? S2 Ta1 Ta2 N3 73.8(3) . . . . ? N1 Ta1 Ta2 N4 103.9(3) . . . . ? N2 Ta1 Ta2 N4 -72.7(3) . . . . ? C100 Ta1 Ta2 N4 144.0(3) . . . . ? S1 Ta1 Ta2 N4 24.03(19) . . . . ? P1 Ta1 Ta2 N4 -153.59(19) . . . . ? S2 Ta1 Ta2 N4 -100.53(19) . . . . ? N1 Ta1 Ta2 C100 -40.1(4) . . . . ? N2 Ta1 Ta2 C100 143.3(3) . . . . ? S1 Ta1 Ta2 C100 -120.0(3) . . . . ? P1 Ta1 Ta2 C100 62.4(3) . . . . ? S2 Ta1 Ta2 C100 115.5(3) . . . . ? N1 Ta1 Ta2 S2 -155.6(3) . . . . ? N2 Ta1 Ta2 S2 27.84(19) . . . . ? C100 Ta1 Ta2 S2 -115.5(3) . . . . ? S1 Ta1 Ta2 S2 124.57(8) . . . . ? P1 Ta1 Ta2 S2 -53.06(7) . . . . ? N1 Ta1 Ta2 P2 23.2(3) . . . . ? N2 Ta1 Ta2 P2 -153.43(19) . . . . ? C100 Ta1 Ta2 P2 63.3(3) . . . . ? S1 Ta1 Ta2 P2 -56.70(7) . . . . ? P1 Ta1 Ta2 P2 125.67(6) . . . . ? S2 Ta1 Ta2 P2 178.73(7) . . . . ? N1 Ta1 Ta2 S1 79.9(3) . . . . ? N2 Ta1 Ta2 S1 -96.73(19) . . . . ? C100 Ta1 Ta2 S1 120.0(3) . . . . ? P1 Ta1 Ta2 S1 -177.63(7) . . . . ? S2 Ta1 Ta2 S1 -124.57(8) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.368 _refine_diff_density_min -0.964 _refine_diff_density_rms 0.164 # Attachment 'Ta2S2_ChemCommun.cif' data_mf821_NPNTaS2TaNPN _database_code_depnum_ccdc_archive 'CCDC 790441' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H62 N4 P2 S2 Si4 Ta2' _chemical_formula_sum 'C48 H62 N4 P2 S2 Si4 Ta2' _chemical_formula_weight 1295.34 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' Si Si 0.0817 0.0704 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9856(8) _cell_length_b 16.6498(10) _cell_length_c 35.4061(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.996(3) _cell_angle_gamma 90.00 _cell_volume 8093.2(8) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7700 _cell_measurement_theta_min 2.4465 _cell_measurement_theta_max 25.0605 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3852 _exptl_absorpt_coefficient_mu 4.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.441 _exptl_absorpt_correction_T_max 0.5959 _exptl_absorpt_process_details 'SADABS. Bruker Nonius area detector scaling and absorption correction - V2.10, Bruker AXS Inc., Madison, Wisconsin, USA (2003).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55572 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.07 _reflns_number_total 14312 _reflns_number_gt 12540 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+6.3775P] 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 14312 _refine_ls_number_parameters 850 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_gt 0.0435 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.006 _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 Ta3 Ta 0.103395(9) 0.513940(7) 0.502006(3) 0.01241(3) Uani 1 1 d . . . Ta2 Ta 0.268796(8) 0.997193(7) 0.328846(3) 0.01190(3) Uani 1 1 d . . . Ta1 Ta 0.075777(8) 1.036144(7) 0.338658(3) 0.01174(3) Uani 1 1 d . . . S3 S 0.00233(5) 0.41853(5) 0.46380(2) 0.01598(16) Uani 1 1 d . . . S1 S 0.17494(5) 0.92832(5) 0.36744(2) 0.01631(16) Uani 1 1 d . . . S2 S 0.16883(5) 1.10316(4) 0.29916(2) 0.01583(16) Uani 1 1 d . . . P1 P -0.05415(6) 1.14647(5) 0.31526(2) 0.01592(17) Uani 1 1 d . . . P3 P 0.24146(6) 0.60933(5) 0.53565(2) 0.01698(17) Uani 1 1 d . . . P2 P 0.40371(6) 0.89045(5) 0.35054(2) 0.01728(17) Uani 1 1 d . . . Si2 Si -0.16575(6) 0.99576(5) 0.31268(3) 0.01810(19) Uani 1 1 d . . . Si3 Si 0.50703(6) 1.04475(6) 0.35044(3) 0.0225(2) Uani 1 1 d . . . Si1 Si 0.03820(6) 1.19743(5) 0.39411(2) 0.01748(19) Uani 1 1 d . . . Si6 Si 0.19263(7) 0.67459(5) 0.45694(3) 0.0230(2) Uani 1 1 d . . . Si4 Si 0.30426(6) 0.83308(5) 0.27418(3) 0.01848(19) Uani 1 1 d . . . Si5 Si 0.33222(6) 0.44836(6) 0.53771(3) 0.02067(19) Uani 1 1 d . . . N1 N 0.07243(18) 1.09687(15) 0.38813(7) 0.0169(6) Uani 1 1 d . . . C49 C -0.0389(2) 0.88290(18) 0.30561(9) 0.0160(7) Uani 1 1 d . . . C69 C -0.0105(3) 0.5373(2) 0.35992(10) 0.0293(8) Uani 1 1 d . . . H69 H -0.0696 0.5530 0.3449 0.035 Uiso 1 1 calc R . . C31 C 0.2292(2) 0.97079(18) 0.24310(9) 0.0193(7) Uani 1 1 d . . . C22 C 0.5411(3) 0.8427(2) 0.47695(11) 0.0436(11) Uani 1 1 d . . . H22 H 0.5707 0.8352 0.5025 0.052 Uiso 1 1 calc R . . C15 C 0.3835(3) 0.3873(2) 0.50185(10) 0.0319(9) Uani 1 1 d . . . H15A H 0.3705 0.3314 0.5053 0.048 Uiso 1 1 calc R . . H15B H 0.4526 0.3957 0.5056 0.048 Uiso 1 1 calc R . . H15C H 0.3538 0.4035 0.4763 0.048 Uiso 1 1 calc R . . C9 C -0.2431(2) 0.9837(2) 0.26371(10) 0.0295(8) Uani 1 1 d . . . H9A H -0.2158 1.0145 0.2454 0.044 Uiso 1 1 calc R . . H9B H -0.3078 1.0023 0.2641 0.044 Uiso 1 1 calc R . . H9C H -0.2453 0.9280 0.2565 0.044 Uiso 1 1 calc R . . N2 N -0.04338(17) 0.96770(14) 0.31476(7) 0.0154(5) Uani 1 1 d . . . C29 C 0.3616(2) 1.2911(2) 0.35403(10) 0.0255(8) Uani 1 1 d . . . H29 H 0.3465 1.3325 0.3362 0.031 Uiso 1 1 calc R . . C66 C 0.1846(2) 0.3331(2) 0.57981(9) 0.0233(7) Uani 1 1 d . . . H66 H 0.1967 0.3722 0.5989 0.028 Uiso 1 1 calc R . . N5 N 0.20512(17) 0.43529(15) 0.53134(7) 0.0159(6) Uani 1 1 d . . . N6 N 0.13813(18) 0.57878(15) 0.45756(7) 0.0168(6) Uani 1 1 d . . . C45 C 0.2371(3) 1.0273(2) 0.47838(10) 0.0368(10) Uani 1 1 d . . . H45 H 0.3007 1.0351 0.4914 0.044 Uiso 1 1 calc R . . C11 C 0.5460(3) 1.1089(2) 0.31304(12) 0.0413(10) Uani 1 1 d . . . H11A H 0.4987 1.1052 0.2896 0.062 Uiso 1 1 calc R . . H11B H 0.6080 1.0908 0.3086 0.062 Uiso 1 1 calc R . . H11C H 0.5512 1.1636 0.3217 0.062 Uiso 1 1 calc R . . C23 C 0.5847(3) 0.8130(2) 0.44816(12) 0.0447(11) Uani 1 1 d . . . H23 H 0.6433 0.7853 0.4543 0.054 Uiso 1 1 calc R . . C68 C 0.0193(2) 0.57069(19) 0.39628(9) 0.0236(7) Uani 1 1 d . . . H68 H -0.0197 0.6085 0.4054 0.028 Uiso 1 1 calc R . . C41 C -0.2001(3) 1.2497(2) 0.21583(11) 0.0398(10) Uani 1 1 d . . . H41 H -0.2498 1.2870 0.2089 0.048 Uiso 1 1 calc R . . C46 C 0.1769(3) 0.9756(2) 0.49320(10) 0.0415(10) Uani 1 1 d . . . H46 H 0.1999 0.9484 0.5161 0.050 Uiso 1 1 calc R . . N3 N 0.38637(17) 1.06702(15) 0.35392(7) 0.0162(6) Uani 1 1 d . . . C18 C 0.1063(3) 0.7523(2) 0.43444(11) 0.0392(10) Uani 1 1 d . . . H18A H 0.0850 0.7401 0.4076 0.059 Uiso 1 1 calc R . . H18B H 0.1378 0.8037 0.4370 0.059 Uiso 1 1 calc R . . H18C H 0.0511 0.7534 0.4469 0.059 Uiso 1 1 calc R . . N4 N 0.27107(18) 0.93478(15) 0.27945(7) 0.0164(6) Uani 1 1 d . . . C26 C 0.4055(2) 1.16695(19) 0.40635(9) 0.0204(7) Uani 1 1 d . . . H26 H 0.4200 1.1256 0.4242 0.024 Uiso 1 1 calc R . . C59 C 0.3673(3) 0.6778(3) 0.64505(11) 0.0435(11) Uani 1 1 d . . . H59 H 0.4230 0.7052 0.6569 0.052 Uiso 1 1 calc R . . C62 C 0.1647(2) 0.29405(19) 0.51377(9) 0.0221(7) Uani 1 1 d . . . H62 H 0.1630 0.3071 0.4881 0.027 Uiso 1 1 calc R . . C53 C -0.0555(2) 0.77643(19) 0.25839(9) 0.0231(7) Uani 1 1 d . . . H53 H -0.0661 0.7604 0.2328 0.028 Uiso 1 1 calc R . . C10 C -0.2186(2) 0.9366(2) 0.34843(10) 0.0277(8) Uani 1 1 d . . . H10A H -0.2181 0.8806 0.3421 0.041 Uiso 1 1 calc R . . H10B H -0.2844 0.9537 0.3479 0.041 Uiso 1 1 calc R . . H10C H -0.1806 0.9451 0.3737 0.041 Uiso 1 1 calc R . . C39 C -0.0864(2) 1.1555(2) 0.19790(10) 0.0270(8) Uani 1 1 d . . . H39 H -0.0596 1.1299 0.1790 0.032 Uiso 1 1 calc R . . C5 C 0.2362(2) 0.70265(19) 0.50923(9) 0.0221(7) Uani 1 1 d . . . H5A H 0.3000 0.7276 0.5129 0.026 Uiso 1 1 calc R . . H5B H 0.1911 0.7398 0.5177 0.026 Uiso 1 1 calc R . . C32 C 0.1337(2) 0.9545(2) 0.22488(9) 0.0245(8) Uani 1 1 d . . . H32 H 0.0962 0.9187 0.2361 0.029 Uiso 1 1 calc R . . C6 C 0.3511(2) 0.55788(19) 0.52843(9) 0.0217(7) Uani 1 1 d . . . H6A H 0.4075 0.5782 0.5461 0.026 Uiso 1 1 calc R . . H6B H 0.3612 0.5658 0.5023 0.026 Uiso 1 1 calc R . . C52 C -0.0404(2) 0.71934(19) 0.28734(10) 0.0251(8) Uani 1 1 d . . . H52 H -0.0412 0.6649 0.2813 0.030 Uiso 1 1 calc R . . C8 C 0.1475(2) 1.26082(19) 0.41074(9) 0.0228(7) Uani 1 1 d . . . H8A H 0.1836 1.2398 0.4345 0.034 Uiso 1 1 calc R . . H8B H 0.1276 1.3148 0.4147 0.034 Uiso 1 1 calc R . . H8C H 0.1879 1.2606 0.3916 0.034 Uiso 1 1 calc R . . C24 C 0.5411(3) 0.8244(2) 0.41016(11) 0.0342(9) Uani 1 1 d . . . H24 H 0.5702 0.8036 0.3907 0.041 Uiso 1 1 calc R . . C16 C 0.3980(2) 0.4227(2) 0.58729(10) 0.0337(9) Uani 1 1 d . . . H16A H 0.3724 0.4543 0.6057 0.051 Uiso 1 1 calc R . . H16B H 0.4661 0.4338 0.5894 0.051 Uiso 1 1 calc R . . H16C H 0.3891 0.3667 0.5922 0.051 Uiso 1 1 calc R . . C57 C 0.2250(2) 0.6023(2) 0.64970(9) 0.0267(8) Uani 1 1 d . . . H57 H 0.1840 0.5796 0.6646 0.032 Uiso 1 1 calc R . . C72 C 0.1650(3) 0.4921(2) 0.40405(10) 0.0257(8) Uani 1 1 d . . . H72 H 0.2249 0.4770 0.4186 0.031 Uiso 1 1 calc R . . C28 C 0.3872(2) 1.3088(2) 0.39281(10) 0.0281(8) Uani 1 1 d . . . H28 H 0.3899 1.3618 0.4012 0.034 Uiso 1 1 calc R . . C55 C 0.2647(2) 0.62725(19) 0.58736(9) 0.0200(7) Uani 1 1 d . . . C60 C 0.3464(3) 0.6700(2) 0.60528(10) 0.0351(9) Uani 1 1 d . . . H60 H 0.3873 0.6934 0.5905 0.042 Uiso 1 1 calc R . . C35 C 0.2434(3) 1.0607(2) 0.19066(10) 0.0328(9) Uani 1 1 d . . . H35 H 0.2805 1.0963 0.1792 0.039 Uiso 1 1 calc R . . C65 C 0.1682(2) 0.2538(2) 0.58956(10) 0.0296(8) Uani 1 1 d . . . H65 H 0.1693 0.2403 0.6151 0.035 Uiso 1 1 calc R . . C3 C 0.5056(2) 0.93713(19) 0.33417(10) 0.0224(7) Uani 1 1 d . . . H3A H 0.4971 0.9342 0.3064 0.027 Uiso 1 1 calc R . . H3B H 0.5661 0.9106 0.3454 0.027 Uiso 1 1 calc R . . C43 C 0.1084(2) 1.05692(18) 0.42438(8) 0.0179(7) Uani 1 1 d . . . C50 C -0.0235(2) 0.82548(18) 0.33444(9) 0.0199(7) Uani 1 1 d . . . H50 H -0.0128 0.8414 0.3601 0.024 Uiso 1 1 calc R . . C54 C -0.0547(2) 0.85761(19) 0.26749(9) 0.0186(7) Uani 1 1 d . . . H54 H -0.0649 0.8955 0.2478 0.022 Uiso 1 1 calc R . . C20 C 0.4103(3) 0.8962(2) 0.42981(9) 0.0289(8) Uani 1 1 d . . . H20 H 0.3519 0.9244 0.4238 0.035 Uiso 1 1 calc R . . C33 C 0.0941(3) 0.9911(2) 0.19022(10) 0.0338(9) Uani 1 1 d . . . H33 H 0.0303 0.9795 0.1784 0.041 Uiso 1 1 calc R . . C64 C 0.1502(3) 0.1953(2) 0.56150(11) 0.0318(9) Uani 1 1 d . . . H64 H 0.1390 0.1425 0.5681 0.038 Uiso 1 1 calc R . . C14 C 0.1966(2) 0.76616(19) 0.26233(10) 0.0262(8) Uani 1 1 d . . . H14A H 0.1602 0.7682 0.2827 0.039 Uiso 1 1 calc R . . H14B H 0.2179 0.7121 0.2594 0.039 Uiso 1 1 calc R . . H14C H 0.1562 0.7836 0.2387 0.039 Uiso 1 1 calc R . . C63 C 0.1489(2) 0.2154(2) 0.52362(10) 0.0289(8) Uani 1 1 d . . . H63 H 0.1373 0.1760 0.5047 0.035 Uiso 1 1 calc R . . C58 C 0.3058(3) 0.6450(2) 0.66702(10) 0.0344(9) Uani 1 1 d . . . H58 H 0.3189 0.6517 0.6936 0.041 Uiso 1 1 calc R . . C21 C 0.4536(3) 0.8838(2) 0.46812(11) 0.0414(10) Uani 1 1 d . . . H21 H 0.4239 0.9029 0.4877 0.050 Uiso 1 1 calc R . . C30 C 0.3582(2) 1.21239(19) 0.34154(9) 0.0211(7) Uani 1 1 d . . . H30 H 0.3404 1.2015 0.3154 0.025 Uiso 1 1 calc R . . C70 C 0.0463(3) 0.4810(2) 0.34572(10) 0.0329(9) Uani 1 1 d . . . H70 H 0.0254 0.4583 0.3216 0.039 Uiso 1 1 calc R . . C56 C 0.2047(2) 0.5932(2) 0.61003(9) 0.0229(7) Uani 1 1 d . . . H56 H 0.1503 0.5639 0.5985 0.028 Uiso 1 1 calc R . . C2 C -0.1639(2) 1.10471(18) 0.32757(9) 0.0192(7) Uani 1 1 d . . . H2A H -0.2211 1.1325 0.3139 0.023 Uiso 1 1 calc R . . H2B H -0.1624 1.1093 0.3550 0.023 Uiso 1 1 calc R . . C38 C -0.0535(2) 1.13717(19) 0.23649(9) 0.0226(7) Uani 1 1 d . . . H38 H -0.0047 1.0990 0.2433 0.027 Uiso 1 1 calc R . . C61 C 0.1830(2) 0.35409(18) 0.54161(9) 0.0177(7) Uani 1 1 d . . . C37 C -0.0926(2) 1.17512(18) 0.26480(9) 0.0184(7) Uani 1 1 d . . . C7 C -0.0495(2) 1.2031(2) 0.42770(9) 0.0245(8) Uani 1 1 d . . . H7A H -0.1077 1.1741 0.4170 0.037 Uiso 1 1 calc R . . H7B H -0.0655 1.2582 0.4314 0.037 Uiso 1 1 calc R . . H7C H -0.0205 1.1798 0.4520 0.037 Uiso 1 1 calc R . . C44 C 0.2036(2) 1.0679(2) 0.44410(9) 0.0266(8) Uani 1 1 d . . . H44 H 0.2450 1.1025 0.4343 0.032 Uiso 1 1 calc R . . C48 C 0.0476(3) 1.0051(2) 0.43996(10) 0.0280(8) Uani 1 1 d . . . H48 H -0.0166 0.9979 0.4275 0.034 Uiso 1 1 calc R . . C51 C -0.0240(2) 0.74405(19) 0.32531(10) 0.0249(8) Uani 1 1 d . . . H51 H -0.0133 0.7060 0.3449 0.030 Uiso 1 1 calc R . . C25 C 0.3808(2) 1.14905(18) 0.36727(9) 0.0178(7) Uani 1 1 d . . . C36 C 0.2838(3) 1.0242(2) 0.22511(10) 0.0267(8) Uani 1 1 d . . . H36 H 0.3481 1.0352 0.2365 0.032 Uiso 1 1 calc R . . C40 C -0.1596(3) 1.2124(2) 0.18771(10) 0.0359(9) Uani 1 1 d . . . H40 H -0.1813 1.2254 0.1620 0.043 Uiso 1 1 calc R . . C4 C 0.3746(2) 0.79963(18) 0.32272(9) 0.0217(7) Uani 1 1 d . . . H4A H 0.3353 0.7640 0.3352 0.026 Uiso 1 1 calc R . . H4B H 0.4336 0.7716 0.3198 0.026 Uiso 1 1 calc R . . C47 C 0.0825(3) 0.9643(2) 0.47408(11) 0.0389(10) Uani 1 1 d . . . H47 H 0.0419 0.9291 0.4840 0.047 Uiso 1 1 calc R . . C67 C 0.1073(2) 0.54752(18) 0.41896(8) 0.0187(7) Uani 1 1 d . . . C1 C -0.0217(2) 1.23484(18) 0.34495(9) 0.0206(7) Uani 1 1 d . . . H1A H -0.0794 1.2659 0.3466 0.025 Uiso 1 1 calc R . . H1B H 0.0228 1.2685 0.3341 0.025 Uiso 1 1 calc R . . C13 C 0.3814(3) 0.8249(2) 0.23681(10) 0.0289(8) Uani 1 1 d . . . H13A H 0.3472 0.8472 0.2131 0.043 Uiso 1 1 calc R . . H13B H 0.3957 0.7694 0.2330 0.043 Uiso 1 1 calc R . . H13C H 0.4411 0.8538 0.2451 0.043 Uiso 1 1 calc R . . C34 C 0.1483(3) 1.0448(2) 0.17304(10) 0.0368(10) Uani 1 1 d . . . H34 H 0.1212 1.0697 0.1500 0.044 Uiso 1 1 calc R . . C71 C 0.1345(3) 0.4592(2) 0.36791(10) 0.0323(9) Uani 1 1 d . . . H71 H 0.1738 0.4221 0.3585 0.039 Uiso 1 1 calc R . . C42 C -0.1669(2) 1.2315(2) 0.25412(10) 0.0310(9) Uani 1 1 d . . . H42 H -0.1941 1.2570 0.2729 0.037 Uiso 1 1 calc R . . C12 C 0.5937(2) 1.0580(2) 0.39681(11) 0.0417(10) Uani 1 1 d . . . H12A H 0.5954 1.1136 0.4042 0.063 Uiso 1 1 calc R . . H12B H 0.6576 1.0413 0.3939 0.063 Uiso 1 1 calc R . . H12C H 0.5729 1.0260 0.4163 0.063 Uiso 1 1 calc R . . C27 C 0.4086(2) 1.2467(2) 0.41886(10) 0.0269(8) Uani 1 1 d . . . H27 H 0.4253 1.2581 0.4450 0.032 Uiso 1 1 calc R . . C19 C 0.4537(2) 0.86688(19) 0.40058(9) 0.0220(7) Uani 1 1 d . . . C17 C 0.2969(3) 0.6701(2) 0.43067(11) 0.0415(10) Uani 1 1 d . . . H17A H 0.3412 0.6285 0.4416 0.062 Uiso 1 1 calc R . . H17B H 0.3302 0.7208 0.4330 0.062 Uiso 1 1 calc R . . H17C H 0.2726 0.6587 0.4040 0.062 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 Ta3 0.01233(7) 0.01246(6) 0.01243(6) -0.00065(5) 0.00232(5) -0.00153(5) Ta2 0.01042(7) 0.01179(7) 0.01373(6) 0.00060(5) 0.00293(5) 0.00166(5) Ta1 0.01008(6) 0.01198(7) 0.01331(6) -0.00081(5) 0.00262(5) 0.00107(5) S3 0.0156(4) 0.0153(4) 0.0172(4) -0.0038(3) 0.0035(3) -0.0020(3) S1 0.0142(4) 0.0157(4) 0.0196(4) 0.0038(3) 0.0047(3) 0.0015(3) S2 0.0141(4) 0.0154(4) 0.0185(4) 0.0040(3) 0.0045(3) 0.0032(3) P1 0.0135(4) 0.0151(4) 0.0191(4) -0.0004(3) 0.0031(3) 0.0031(3) P3 0.0140(4) 0.0181(4) 0.0188(4) -0.0030(3) 0.0030(3) -0.0036(3) P2 0.0140(4) 0.0158(4) 0.0215(4) 0.0011(3) 0.0020(3) 0.0037(3) Si2 0.0122(4) 0.0186(5) 0.0228(5) -0.0017(4) 0.0016(4) 0.0003(4) Si3 0.0120(5) 0.0208(5) 0.0350(5) -0.0025(4) 0.0052(4) -0.0008(4) Si1 0.0189(5) 0.0166(5) 0.0179(4) -0.0036(4) 0.0061(4) 0.0007(4) Si6 0.0298(6) 0.0198(5) 0.0202(5) 0.0012(4) 0.0071(4) -0.0077(4) Si4 0.0206(5) 0.0162(5) 0.0198(5) -0.0016(4) 0.0066(4) 0.0035(4) Si5 0.0150(5) 0.0240(5) 0.0224(5) -0.0007(4) 0.0020(4) 0.0025(4) N1 0.0173(14) 0.0179(14) 0.0158(13) -0.0025(11) 0.0041(11) -0.0004(11) C49 0.0096(16) 0.0156(16) 0.0214(16) -0.0003(13) -0.0006(12) -0.0020(12) C69 0.037(2) 0.026(2) 0.0224(18) 0.0073(15) -0.0013(15) -0.0086(16) C31 0.0248(18) 0.0179(17) 0.0166(16) -0.0036(13) 0.0075(13) 0.0078(13) C22 0.050(3) 0.043(3) 0.030(2) 0.0096(19) -0.014(2) 0.004(2) C15 0.028(2) 0.030(2) 0.041(2) -0.0016(18) 0.0153(17) 0.0052(16) C9 0.0164(18) 0.033(2) 0.035(2) -0.0075(17) -0.0039(15) 0.0034(15) N2 0.0149(14) 0.0143(14) 0.0169(13) 0.0018(11) 0.0023(10) -0.0016(10) C29 0.0222(19) 0.0214(18) 0.034(2) 0.0071(16) 0.0081(15) -0.0023(14) C66 0.0200(18) 0.0261(19) 0.0232(18) 0.0008(15) 0.0029(14) -0.0003(14) N5 0.0177(14) 0.0148(14) 0.0145(13) 0.0000(11) 0.0015(11) -0.0001(11) N6 0.0207(15) 0.0189(14) 0.0120(13) 0.0021(11) 0.0060(11) -0.0026(11) C45 0.040(2) 0.034(2) 0.029(2) -0.0055(17) -0.0107(17) 0.0121(18) C11 0.031(2) 0.031(2) 0.070(3) 0.004(2) 0.032(2) -0.0001(17) C23 0.033(2) 0.043(3) 0.051(3) 0.018(2) -0.010(2) 0.0106(19) C68 0.032(2) 0.0180(18) 0.0213(17) 0.0024(14) 0.0063(15) -0.0007(14) C41 0.040(2) 0.042(2) 0.037(2) 0.0145(19) 0.0055(18) 0.0253(19) C46 0.073(3) 0.035(2) 0.0174(18) 0.0066(17) 0.0095(19) 0.015(2) N3 0.0121(13) 0.0174(14) 0.0192(14) 0.0003(11) 0.0032(11) 0.0001(11) C18 0.058(3) 0.022(2) 0.031(2) 0.0053(17) -0.0065(19) -0.0052(18) N4 0.0201(14) 0.0164(14) 0.0136(13) -0.0009(11) 0.0051(11) 0.0036(11) C26 0.0169(17) 0.0204(18) 0.0232(17) 0.0017(14) 0.0025(14) -0.0003(13) C59 0.035(2) 0.058(3) 0.034(2) -0.020(2) -0.0024(18) -0.018(2) C62 0.0242(19) 0.0189(18) 0.0214(17) 0.0018(14) -0.0006(14) 0.0043(14) C53 0.0221(19) 0.0240(19) 0.0222(18) -0.0054(15) 0.0018(14) -0.0003(14) C10 0.0192(18) 0.029(2) 0.037(2) 0.0017(17) 0.0096(15) -0.0043(15) C39 0.027(2) 0.031(2) 0.0226(18) 0.0002(16) 0.0038(15) 0.0042(16) C5 0.0238(19) 0.0172(17) 0.0260(18) -0.0030(14) 0.0068(14) -0.0075(14) C32 0.0279(19) 0.0204(18) 0.0238(18) -0.0064(15) 0.0012(15) 0.0037(15) C6 0.0159(17) 0.0257(19) 0.0238(17) -0.0024(15) 0.0048(13) -0.0013(14) C52 0.026(2) 0.0137(17) 0.034(2) -0.0035(15) 0.0016(15) 0.0004(14) C8 0.0250(19) 0.0207(18) 0.0236(18) -0.0039(14) 0.0070(14) -0.0015(14) C24 0.031(2) 0.034(2) 0.036(2) 0.0097(18) -0.0003(17) 0.0107(17) C16 0.0206(19) 0.044(2) 0.034(2) 0.0049(18) -0.0024(16) -0.0010(16) C57 0.0247(19) 0.035(2) 0.0188(17) -0.0005(15) 0.0001(14) 0.0015(16) C72 0.029(2) 0.0239(19) 0.0261(18) -0.0003(15) 0.0112(15) -0.0014(15) C28 0.0239(19) 0.0194(18) 0.043(2) -0.0082(17) 0.0106(16) -0.0057(15) C55 0.0165(17) 0.0197(17) 0.0222(17) -0.0044(14) -0.0001(13) 0.0006(13) C60 0.028(2) 0.047(2) 0.030(2) -0.0079(18) 0.0056(16) -0.0149(18) C35 0.051(3) 0.028(2) 0.0242(19) 0.0064(16) 0.0191(18) 0.0099(18) C65 0.031(2) 0.033(2) 0.0233(19) 0.0117(16) 0.0030(15) 0.0004(16) C3 0.0102(16) 0.0248(19) 0.0323(19) -0.0017(15) 0.0042(14) 0.0034(13) C43 0.0237(18) 0.0161(16) 0.0143(15) -0.0044(13) 0.0048(13) 0.0034(13) C50 0.0194(18) 0.0228(18) 0.0164(16) -0.0005(14) 0.0002(13) -0.0036(14) C54 0.0151(17) 0.0221(18) 0.0184(16) 0.0007(14) 0.0023(13) 0.0012(13) C20 0.031(2) 0.029(2) 0.0232(18) 0.0004(16) -0.0047(15) 0.0059(16) C33 0.034(2) 0.033(2) 0.029(2) -0.0114(17) -0.0056(17) 0.0138(17) C64 0.034(2) 0.0183(18) 0.041(2) 0.0085(17) 0.0000(17) 0.0003(15) C14 0.029(2) 0.0211(18) 0.0281(19) -0.0044(15) 0.0048(15) 0.0026(15) C63 0.030(2) 0.0212(19) 0.032(2) -0.0043(16) -0.0045(16) 0.0036(15) C58 0.033(2) 0.046(2) 0.0206(19) -0.0101(17) -0.0037(16) -0.0025(18) C21 0.054(3) 0.040(2) 0.027(2) 0.0023(18) -0.0026(19) 0.004(2) C30 0.0165(17) 0.0223(18) 0.0240(18) 0.0009(14) 0.0027(14) -0.0019(13) C70 0.055(3) 0.026(2) 0.0182(17) -0.0040(15) 0.0084(17) -0.0138(18) C56 0.0185(18) 0.0266(19) 0.0215(17) -0.0022(15) -0.0019(14) -0.0013(14) C2 0.0094(16) 0.0206(17) 0.0288(18) -0.0037(14) 0.0068(13) 0.0012(13) C38 0.0205(18) 0.0203(18) 0.0256(18) -0.0001(15) 0.0008(14) 0.0050(14) C61 0.0124(16) 0.0170(17) 0.0226(17) 0.0007(13) 0.0002(13) 0.0020(13) C37 0.0165(17) 0.0167(17) 0.0206(17) 0.0032(13) -0.0001(13) 0.0016(13) C7 0.0256(19) 0.0233(19) 0.0265(18) -0.0058(15) 0.0095(15) -0.0004(15) C44 0.028(2) 0.0231(19) 0.0265(19) -0.0042(15) 0.0008(15) 0.0010(15) C48 0.032(2) 0.027(2) 0.0282(19) 0.0016(16) 0.0137(16) 0.0023(16) C51 0.0260(19) 0.0186(18) 0.0283(19) 0.0067(15) 0.0005(15) -0.0008(14) C25 0.0106(16) 0.0173(17) 0.0263(18) -0.0035(14) 0.0059(13) -0.0034(13) C36 0.030(2) 0.028(2) 0.0256(18) 0.0008(15) 0.0123(15) 0.0057(15) C40 0.035(2) 0.044(2) 0.025(2) 0.0117(18) -0.0027(17) 0.0080(18) C4 0.0228(18) 0.0150(17) 0.0269(18) 0.0016(14) 0.0034(14) 0.0053(13) C47 0.057(3) 0.034(2) 0.032(2) 0.0098(18) 0.023(2) 0.0074(19) C67 0.0267(18) 0.0144(16) 0.0161(16) 0.0021(13) 0.0070(13) -0.0041(14) C1 0.0199(18) 0.0169(17) 0.0260(18) -0.0023(14) 0.0066(14) 0.0012(13) C13 0.034(2) 0.0230(19) 0.033(2) -0.0036(16) 0.0153(16) 0.0076(15) C34 0.055(3) 0.038(2) 0.0167(18) 0.0006(17) 0.0042(17) 0.020(2) C71 0.048(2) 0.026(2) 0.0279(19) -0.0035(16) 0.0209(18) -0.0023(17) C42 0.030(2) 0.033(2) 0.030(2) 0.0052(17) 0.0066(16) 0.0129(16) C12 0.020(2) 0.041(2) 0.058(3) -0.019(2) -0.0061(18) 0.0059(17) C27 0.0249(19) 0.028(2) 0.0282(19) -0.0077(16) 0.0066(15) -0.0046(15) C19 0.0183(18) 0.0172(17) 0.0272(18) 0.0024(14) -0.0041(14) 0.0004(13) C17 0.045(3) 0.046(3) 0.039(2) -0.0031(19) 0.0215(19) -0.020(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta3 N6 2.042(2) . ? Ta3 N5 2.062(2) . ? Ta3 S3 2.3661(8) 3_566 ? Ta3 S3 2.3710(8) . ? Ta3 P3 2.6062(8) . ? Ta3 Ta3 2.9057(3) 3_566 ? Ta2 N4 2.040(2) . ? Ta2 N3 2.070(2) . ? Ta2 S1 2.3641(8) . ? Ta2 S2 2.3689(7) . ? Ta2 P2 2.5993(8) . ? Ta2 Ta1 2.8612(2) . ? Ta1 N1 2.031(2) . ? Ta1 N2 2.062(2) . ? Ta1 S2 2.3641(8) . ? Ta1 S1 2.3760(8) . ? Ta1 P1 2.6054(8) . ? S3 Ta3 2.3661(8) 3_566 ? P1 C2 1.813(3) . ? P1 C1 1.815(3) . ? P1 C37 1.828(3) . ? P3 C5 1.808(3) . ? P3 C6 1.817(3) . ? P3 C55 1.822(3) . ? P2 C4 1.808(3) . ? P2 C3 1.813(3) . ? P2 C19 1.819(3) . ? Si2 N2 1.762(3) . ? Si2 C10 1.864(3) . ? Si2 C9 1.871(3) . ? Si2 C2 1.888(3) . ? Si3 N3 1.755(3) . ? Si3 C12 1.859(4) . ? Si3 C11 1.861(4) . ? Si3 C3 1.881(3) . ? Si1 N1 1.765(3) . ? Si1 C8 1.859(3) . ? Si1 C7 1.867(3) . ? Si1 C1 1.888(3) . ? Si6 N6 1.770(3) . ? Si6 C18 1.843(4) . ? Si6 C17 1.875(4) . ? Si6 C5 1.894(3) . ? Si4 N4 1.775(3) . ? Si4 C14 1.855(3) . ? Si4 C13 1.865(3) . ? Si4 C4 1.894(3) . ? Si5 N5 1.762(3) . ? Si5 C16 1.869(3) . ? Si5 C15 1.873(3) . ? Si5 C6 1.880(3) . ? N1 C43 1.448(4) . ? C49 C50 1.385(4) . ? C49 C54 1.391(4) . ? C49 N2 1.453(4) . ? C69 C70 1.383(5) . ? C69 C68 1.391(4) . ? C69 H69 0.9300 . ? C31 C32 1.394(4) . ? C31 C36 1.402(5) . ? C31 N4 1.439(4) . ? C22 C23 1.375(6) . ? C22 C21 1.385(5) . ? C22 H22 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C29 C30 1.381(4) . ? C29 C28 1.383(5) . ? C29 H29 0.9300 . ? C66 C61 1.393(4) . ? C66 C65 1.395(5) . ? C66 H66 0.9300 . ? N5 C61 1.449(4) . ? N6 C67 1.449(4) . ? C45 C46 1.375(6) . ? C45 C44 1.390(5) . ? C45 H45 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C23 C24 1.380(5) . ? C23 H23 0.9300 . ? C68 C67 1.390(4) . ? C68 H68 0.9300 . ? C41 C42 1.380(5) . ? C41 C40 1.383(5) . ? C41 H41 0.9300 . ? C46 C47 1.377(6) . ? C46 H46 0.9300 . ? N3 C25 1.452(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C26 C25 1.393(4) . ? C26 C27 1.398(4) . ? C26 H26 0.9300 . ? C59 C58 1.379(5) . ? C59 C60 1.388(5) . ? C59 H59 0.9300 . ? C62 C63 1.384(5) . ? C62 C61 1.393(4) . ? C62 H62 0.9300 . ? C53 C52 1.384(4) . ? C53 C54 1.389(4) . ? C53 H53 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C39 C38 1.390(4) . ? C39 C40 1.391(5) . ? C39 H39 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C32 C33 1.388(5) . ? C32 H32 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C52 C51 1.383(5) . ? C52 H52 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C24 C19 1.396(5) . ? C24 H24 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C57 C58 1.375(5) . ? C57 C56 1.387(4) . ? C57 H57 0.9300 . ? C72 C71 1.382(5) . ? C72 C67 1.395(4) . ? C72 H72 0.9300 . ? C28 C27 1.379(5) . ? C28 H28 0.9300 . ? C55 C56 1.388(4) . ? C55 C60 1.392(4) . ? C60 H60 0.9300 . ? C35 C34 1.382(5) . ? C35 C36 1.384(5) . ? C35 H35 0.9300 . ? C65 C64 1.380(5) . ? C65 H65 0.9300 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C43 C44 1.393(4) . ? C43 C48 1.397(4) . ? C50 C51 1.393(4) . ? C50 H50 0.9300 . ? C54 H54 0.9300 . ? C20 C19 1.385(5) . ? C20 C21 1.392(5) . ? C20 H20 0.9300 . ? C33 C34 1.386(5) . ? C33 H33 0.9300 . ? C64 C63 1.379(5) . ? C64 H64 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C63 H63 0.9300 . ? C58 H58 0.9300 . ? C21 H21 0.9300 . ? C30 C25 1.390(4) . ? C30 H30 0.9300 . ? C70 C71 1.378(5) . ? C70 H70 0.9300 . ? C56 H56 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C38 C37 1.383(4) . ? C38 H38 0.9300 . ? C37 C42 1.398(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C44 H44 0.9300 . ? C48 C47 1.391(5) . ? C48 H48 0.9300 . ? C51 H51 0.9300 . ? C36 H36 0.9300 . ? C40 H40 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C47 H47 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C34 H34 0.9300 . ? C71 H71 0.9300 . ? C42 H42 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C27 H27 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ta3 N5 118.76(10) . . ? N6 Ta3 S3 114.00(7) . 3_566 ? N5 Ta3 S3 118.84(7) . 3_566 ? N6 Ta3 S3 96.79(7) . . ? N5 Ta3 S3 98.09(7) . . ? S3 Ta3 S3 104.33(2) 3_566 . ? N6 Ta3 P3 76.44(7) . . ? N5 Ta3 P3 77.12(7) . . ? S3 Ta3 P3 87.56(3) 3_566 . ? S3 Ta3 P3 167.99(3) . . ? N6 Ta3 Ta3 115.32(7) . 3_566 ? N5 Ta3 Ta3 120.51(7) . 3_566 ? S3 Ta3 Ta3 52.240(19) 3_566 3_566 ? S3 Ta3 Ta3 52.089(19) . 3_566 ? P3 Ta3 Ta3 139.770(19) . 3_566 ? N4 Ta2 N3 120.85(10) . . ? N4 Ta2 S1 110.46(7) . . ? N3 Ta2 S1 120.51(7) . . ? N4 Ta2 S2 95.93(7) . . ? N3 Ta2 S2 97.20(7) . . ? S1 Ta2 S2 105.78(3) . . ? N4 Ta2 P2 77.05(7) . . ? N3 Ta2 P2 77.57(7) . . ? S1 Ta2 P2 87.10(3) . . ? S2 Ta2 P2 166.93(3) . . ? N4 Ta2 Ta1 112.89(7) . . ? N3 Ta2 Ta1 120.74(7) . . ? S1 Ta2 Ta1 53.061(18) . . ? S2 Ta2 Ta1 52.730(18) . . ? P2 Ta2 Ta1 140.142(19) . . ? N1 Ta1 N2 118.63(10) . . ? N1 Ta1 S2 112.40(7) . . ? N2 Ta1 S2 120.73(7) . . ? N1 Ta1 S1 96.54(7) . . ? N2 Ta1 S1 96.79(7) . . ? S2 Ta1 S1 105.55(3) . . ? N1 Ta1 P1 78.10(7) . . ? N2 Ta1 P1 78.41(7) . . ? S2 Ta1 P1 84.74(3) . . ? S1 Ta1 P1 169.64(3) . . ? N1 Ta1 Ta2 113.27(7) . . ? N2 Ta1 Ta2 122.15(7) . . ? S2 Ta1 Ta2 52.884(18) . . ? S1 Ta1 Ta2 52.681(18) . . ? P1 Ta1 Ta2 137.574(19) . . ? Ta3 S3 Ta3 75.67(2) 3_566 . ? Ta2 S1 Ta1 74.26(2) . . ? Ta1 S2 Ta2 74.39(2) . . ? C2 P1 C1 107.53(15) . . ? C2 P1 C37 103.33(15) . . ? C1 P1 C37 110.43(14) . . ? C2 P1 Ta1 102.97(10) . . ? C1 P1 Ta1 107.77(10) . . ? C37 P1 Ta1 123.49(10) . . ? C5 P3 C6 106.55(15) . . ? C5 P3 C55 111.16(15) . . ? C6 P3 C55 102.99(15) . . ? C5 P3 Ta3 109.50(11) . . ? C6 P3 Ta3 102.71(11) . . ? C55 P3 Ta3 122.26(11) . . ? C4 P2 C3 107.05(15) . . ? C4 P2 C19 110.79(15) . . ? C3 P2 C19 102.97(15) . . ? C4 P2 Ta2 109.60(10) . . ? C3 P2 Ta2 100.54(11) . . ? C19 P2 Ta2 123.91(11) . . ? N2 Si2 C10 109.83(14) . . ? N2 Si2 C9 113.29(14) . . ? C10 Si2 C9 109.78(16) . . ? N2 Si2 C2 106.36(12) . . ? C10 Si2 C2 107.69(15) . . ? C9 Si2 C2 109.68(15) . . ? N3 Si3 C12 112.75(15) . . ? N3 Si3 C11 110.15(15) . . ? C12 Si3 C11 109.29(19) . . ? N3 Si3 C3 105.58(13) . . ? C12 Si3 C3 110.53(16) . . ? C11 Si3 C3 108.41(17) . . ? N1 Si1 C8 110.55(14) . . ? N1 Si1 C7 110.51(14) . . ? C8 Si1 C7 111.75(15) . . ? N1 Si1 C1 106.57(13) . . ? C8 Si1 C1 107.37(15) . . ? C7 Si1 C1 109.92(15) . . ? N6 Si6 C18 112.92(15) . . ? N6 Si6 C17 110.35(15) . . ? C18 Si6 C17 108.72(19) . . ? N6 Si6 C5 105.61(13) . . ? C18 Si6 C5 108.15(16) . . ? C17 Si6 C5 111.06(16) . . ? N4 Si4 C14 112.30(14) . . ? N4 Si4 C13 110.03(14) . . ? C14 Si4 C13 110.48(16) . . ? N4 Si4 C4 106.63(13) . . ? C14 Si4 C4 106.70(15) . . ? C13 Si4 C4 110.58(15) . . ? N5 Si5 C16 113.29(14) . . ? N5 Si5 C15 110.71(14) . . ? C16 Si5 C15 109.22(17) . . ? N5 Si5 C6 105.62(13) . . ? C16 Si5 C6 109.01(16) . . ? C15 Si5 C6 108.84(15) . . ? C43 N1 Si1 112.69(19) . . ? C43 N1 Ta1 118.33(19) . . ? Si1 N1 Ta1 128.84(14) . . ? C50 C49 C54 118.7(3) . . ? C50 C49 N2 120.9(3) . . ? C54 C49 N2 120.3(3) . . ? C70 C69 C68 121.0(3) . . ? C70 C69 H69 119.5 . . ? C68 C69 H69 119.5 . . ? C32 C31 C36 118.1(3) . . ? C32 C31 N4 121.5(3) . . ? C36 C31 N4 120.4(3) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? Si5 C15 H15A 109.5 . . ? Si5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C49 N2 Si2 109.33(18) . . ? C49 N2 Ta1 124.25(18) . . ? Si2 N2 Ta1 124.97(13) . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C61 C66 C65 120.3(3) . . ? C61 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C61 N5 Si5 109.97(19) . . ? C61 N5 Ta3 123.99(18) . . ? Si5 N5 Ta3 124.63(13) . . ? C67 N6 Si6 111.29(19) . . ? C67 N6 Ta3 117.74(19) . . ? Si6 N6 Ta3 130.73(14) . . ? C46 C45 C44 120.6(4) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C22 C23 C24 119.8(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C67 C68 C69 120.0(3) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C45 C46 C47 119.8(3) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C25 N3 Si3 109.46(19) . . ? C25 N3 Ta2 125.48(19) . . ? Si3 N3 Ta2 123.15(13) . . ? Si6 C18 H18A 109.5 . . ? Si6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C31 N4 Si4 111.94(19) . . ? C31 N4 Ta2 118.96(18) . . ? Si4 N4 Ta2 128.55(13) . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C63 C62 C61 121.2(3) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C52 C53 C54 120.2(3) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C38 C39 C40 119.6(3) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? P3 C5 Si6 105.52(16) . . ? P3 C5 H5A 110.6 . . ? Si6 C5 H5A 110.6 . . ? P3 C5 H5B 110.6 . . ? Si6 C5 H5B 110.6 . . ? H5A C5 H5B 108.8 . . ? C33 C32 C31 120.6(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? P3 C6 Si5 106.40(16) . . ? P3 C6 H6A 110.4 . . ? Si5 C6 H6A 110.4 . . ? P3 C6 H6B 110.4 . . ? Si5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? C51 C52 C53 119.3(3) . . ? C51 C52 H52 120.4 . . ? C53 C52 H52 120.4 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C23 C24 C19 120.7(4) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? Si5 C16 H16A 109.5 . . ? Si5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C58 C57 C56 120.0(3) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C71 C72 C67 120.9(3) . . ? C71 C72 H72 119.6 . . ? C67 C72 H72 119.6 . . ? C27 C28 C29 119.1(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C56 C55 C60 118.6(3) . . ? C56 C55 P3 120.2(2) . . ? C60 C55 P3 121.0(3) . . ? C59 C60 C55 120.4(4) . . ? C59 C60 H60 119.8 . . ? C55 C60 H60 119.8 . . ? C34 C35 C36 120.7(3) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C64 C65 C66 120.4(3) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? P2 C3 Si3 105.88(16) . . ? P2 C3 H3A 110.6 . . ? Si3 C3 H3A 110.6 . . ? P2 C3 H3B 110.6 . . ? Si3 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? C44 C43 C48 118.6(3) . . ? C44 C43 N1 121.4(3) . . ? C48 C43 N1 119.9(3) . . ? C49 C50 C51 120.5(3) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C53 C54 C49 120.8(3) . . ? C53 C54 H54 119.6 . . ? C49 C54 H54 119.6 . . ? C19 C20 C21 120.3(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C63 C64 C65 119.7(3) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C64 C63 C62 120.1(3) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C57 C58 C59 120.1(3) . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C29 C30 C25 121.4(3) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? C71 C70 C69 119.0(3) . . ? C71 C70 H70 120.5 . . ? C69 C70 H70 120.5 . . ? C57 C56 C55 120.7(3) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? P1 C2 Si2 105.57(15) . . ? P1 C2 H2A 110.6 . . ? Si2 C2 H2A 110.6 . . ? P1 C2 H2B 110.6 . . ? Si2 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? C37 C38 C39 120.6(3) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C62 C61 C66 118.3(3) . . ? C62 C61 N5 120.8(3) . . ? C66 C61 N5 120.9(3) . . ? C38 C37 C42 119.2(3) . . ? C38 C37 P1 120.4(2) . . ? C42 C37 P1 120.3(3) . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C47 C48 C43 120.4(3) . . ? C47 C48 H48 119.8 . . ? C43 C48 H48 119.8 . . ? C52 C51 C50 120.5(3) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C30 C25 C26 118.1(3) . . ? C30 C25 N3 121.3(3) . . ? C26 C25 N3 120.4(3) . . ? C35 C36 C31 120.8(3) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C41 C40 C39 120.1(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? P2 C4 Si4 105.81(15) . . ? P2 C4 H4A 110.6 . . ? Si4 C4 H4A 110.6 . . ? P2 C4 H4B 110.6 . . ? Si4 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? C46 C47 C48 120.3(4) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C68 C67 C72 118.5(3) . . ? C68 C67 N6 121.1(3) . . ? C72 C67 N6 120.4(3) . . ? P1 C1 Si1 106.54(16) . . ? P1 C1 H1A 110.4 . . ? Si1 C1 H1A 110.4 . . ? P1 C1 H1B 110.4 . . ? Si1 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C35 C34 C33 119.1(3) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C70 C71 C72 120.6(3) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.7 . . ? C41 C42 C37 120.4(3) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C28 C27 C26 120.7(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C20 C19 C24 119.0(3) . . ? C20 C19 P2 120.6(2) . . ? C24 C19 P2 120.1(3) . . ? Si6 C17 H17A 109.5 . . ? Si6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ta2 Ta1 N1 179.15(11) . . . . ? N3 Ta2 Ta1 N1 -26.87(11) . . . . ? S1 Ta2 Ta1 N1 80.10(8) . . . . ? S2 Ta2 Ta1 N1 -101.23(8) . . . . ? P2 Ta2 Ta1 N1 81.90(8) . . . . ? N4 Ta2 Ta1 N2 26.72(11) . . . . ? N3 Ta2 Ta1 N2 -179.30(11) . . . . ? S1 Ta2 Ta1 N2 -72.33(8) . . . . ? S2 Ta2 Ta1 N2 106.33(8) . . . . ? P2 Ta2 Ta1 N2 -70.53(8) . . . . ? N4 Ta2 Ta1 S2 -79.61(8) . . . . ? N3 Ta2 Ta1 S2 74.37(8) . . . . ? S1 Ta2 Ta1 S2 -178.67(3) . . . . ? P2 Ta2 Ta1 S2 -176.86(4) . . . . ? N4 Ta2 Ta1 S1 99.05(8) . . . . ? N3 Ta2 Ta1 S1 -106.96(8) . . . . ? S2 Ta2 Ta1 S1 178.67(3) . . . . ? P2 Ta2 Ta1 S1 1.80(4) . . . . ? N4 Ta2 Ta1 P1 -82.92(8) . . . . ? N3 Ta2 Ta1 P1 71.06(8) . . . . ? S1 Ta2 Ta1 P1 178.03(4) . . . . ? S2 Ta2 Ta1 P1 -3.31(4) . . . . ? P2 Ta2 Ta1 P1 179.83(4) . . . . ? N6 Ta3 S3 Ta3 -116.95(7) . . . 3_566 ? N5 Ta3 S3 Ta3 122.63(7) . . . 3_566 ? S3 Ta3 S3 Ta3 0.0 3_566 . . 3_566 ? P3 Ta3 S3 Ta3 -171.82(12) . . . 3_566 ? N4 Ta2 S1 Ta1 -103.82(7) . . . . ? N3 Ta2 S1 Ta1 107.41(8) . . . . ? S2 Ta2 S1 Ta1 -1.10(3) . . . . ? P2 Ta2 S1 Ta1 -178.84(2) . . . . ? N1 Ta1 S1 Ta2 -114.37(7) . . . . ? N2 Ta1 S1 Ta2 125.67(7) . . . . ? S2 Ta1 S1 Ta2 1.10(3) . . . . ? P1 Ta1 S1 Ta2 -172.58(14) . . . . ? N1 Ta1 S2 Ta2 102.94(8) . . . . ? N2 Ta1 S2 Ta2 -109.06(8) . . . . ? S1 Ta1 S2 Ta2 -1.10(3) . . . . ? P1 Ta1 S2 Ta2 177.76(2) . . . . ? N4 Ta2 S2 Ta1 114.35(7) . . . . ? N3 Ta2 S2 Ta1 -123.46(7) . . . . ? S1 Ta2 S2 Ta1 1.11(3) . . . . ? P2 Ta2 S2 Ta1 171.08(11) . . . . ? N1 Ta1 P1 C2 -82.16(13) . . . . ? N2 Ta1 P1 C2 40.73(13) . . . . ? S2 Ta1 P1 C2 163.60(11) . . . . ? S1 Ta1 P1 C2 -22.5(2) . . . . ? Ta2 Ta1 P1 C2 166.25(10) . . . . ? N1 Ta1 P1 C1 31.31(13) . . . . ? N2 Ta1 P1 C1 154.21(13) . . . . ? S2 Ta1 P1 C1 -82.92(11) . . . . ? S1 Ta1 P1 C1 90.96(18) . . . . ? Ta2 Ta1 P1 C1 -80.28(11) . . . . ? N1 Ta1 P1 C37 161.98(14) . . . . ? N2 Ta1 P1 C37 -75.13(14) . . . . ? S2 Ta1 P1 C37 47.74(12) . . . . ? S1 Ta1 P1 C37 -138.37(17) . . . . ? Ta2 Ta1 P1 C37 50.39(13) . . . . ? N6 Ta3 P3 C5 31.34(14) . . . . ? N5 Ta3 P3 C5 155.59(14) . . . . ? S3 Ta3 P3 C5 -84.07(12) 3_566 . . . ? S3 Ta3 P3 C5 88.00(17) . . . . ? Ta3 Ta3 P3 C5 -81.99(12) 3_566 . . . ? N6 Ta3 P3 C6 -81.58(13) . . . . ? N5 Ta3 P3 C6 42.67(13) . . . . ? S3 Ta3 P3 C6 163.00(11) 3_566 . . . ? S3 Ta3 P3 C6 -24.93(18) . . . . ? Ta3 Ta3 P3 C6 165.08(11) 3_566 . . . ? N6 Ta3 P3 C55 163.91(14) . . . . ? N5 Ta3 P3 C55 -71.84(14) . . . . ? S3 Ta3 P3 C55 48.49(12) 3_566 . . . ? S3 Ta3 P3 C55 -139.44(16) . . . . ? Ta3 Ta3 P3 C55 50.57(13) 3_566 . . . ? N4 Ta2 P2 C4 -31.92(14) . . . . ? N3 Ta2 P2 C4 -158.03(14) . . . . ? S1 Ta2 P2 C4 79.85(12) . . . . ? S2 Ta2 P2 C4 -90.48(17) . . . . ? Ta1 Ta2 P2 C4 78.41(12) . . . . ? N4 Ta2 P2 C3 80.59(13) . . . . ? N3 Ta2 P2 C3 -45.52(13) . . . . ? S1 Ta2 P2 C3 -167.64(11) . . . . ? S2 Ta2 P2 C3 22.02(17) . . . . ? Ta1 Ta2 P2 C3 -169.08(11) . . . . ? N4 Ta2 P2 C19 -165.81(15) . . . . ? N3 Ta2 P2 C19 68.07(15) . . . . ? S1 Ta2 P2 C19 -54.05(13) . . . . ? S2 Ta2 P2 C19 135.62(16) . . . . ? Ta1 Ta2 P2 C19 -55.49(14) . . . . ? C8 Si1 N1 C43 71.0(2) . . . . ? C7 Si1 N1 C43 -53.2(2) . . . . ? C1 Si1 N1 C43 -172.6(2) . . . . ? C8 Si1 N1 Ta1 -104.52(19) . . . . ? C7 Si1 N1 Ta1 131.24(18) . . . . ? C1 Si1 N1 Ta1 11.8(2) . . . . ? N2 Ta1 N1 C43 90.0(2) . . . . ? S2 Ta1 N1 C43 -121.3(2) . . . . ? S1 Ta1 N1 C43 -11.5(2) . . . . ? P1 Ta1 N1 C43 159.5(2) . . . . ? Ta2 Ta1 N1 C43 -63.5(2) . . . . ? N2 Ta1 N1 Si1 -94.73(18) . . . . ? S2 Ta1 N1 Si1 54.00(18) . . . . ? S1 Ta1 N1 Si1 163.83(16) . . . . ? P1 Ta1 N1 Si1 -25.15(15) . . . . ? Ta2 Ta1 N1 Si1 111.78(15) . . . . ? C50 C49 N2 Si2 -94.0(3) . . . . ? C54 C49 N2 Si2 82.9(3) . . . . ? C50 C49 N2 Ta1 72.8(3) . . . . ? C54 C49 N2 Ta1 -110.3(3) . . . . ? C10 Si2 N2 C49 60.7(2) . . . . ? C9 Si2 N2 C49 -62.5(2) . . . . ? C2 Si2 N2 C49 176.9(2) . . . . ? C10 Si2 N2 Ta1 -106.04(18) . . . . ? C9 Si2 N2 Ta1 130.80(17) . . . . ? C2 Si2 N2 Ta1 10.2(2) . . . . ? N1 Ta1 N2 C49 -125.0(2) . . . . ? S2 Ta1 N2 C49 89.0(2) . . . . ? S1 Ta1 N2 C49 -23.7(2) . . . . ? P1 Ta1 N2 C49 165.6(2) . . . . ? Ta2 Ta1 N2 C49 26.1(2) . . . . ? N1 Ta1 N2 Si2 39.82(19) . . . . ? S2 Ta1 N2 Si2 -106.25(14) . . . . ? S1 Ta1 N2 Si2 141.11(14) . . . . ? P1 Ta1 N2 Si2 -29.59(13) . . . . ? Ta2 Ta1 N2 Si2 -169.15(11) . . . . ? C16 Si5 N5 C61 -55.1(2) . . . . ? C15 Si5 N5 C61 68.0(2) . . . . ? C6 Si5 N5 C61 -174.3(2) . . . . ? C16 Si5 N5 Ta3 138.02(18) . . . . ? C15 Si5 N5 Ta3 -98.88(19) . . . . ? C6 Si5 N5 Ta3 18.78(19) . . . . ? N6 Ta3 N5 C61 -134.7(2) . . . . ? S3 Ta3 N5 C61 79.0(2) 3_566 . . . ? S3 Ta3 N5 C61 -32.4(2) . . . . ? P3 Ta3 N5 C61 158.8(2) . . . . ? Ta3 Ta3 N5 C61 18.1(3) 3_566 . . . ? N6 Ta3 N5 Si5 30.36(19) . . . . ? S3 Ta3 N5 Si5 -115.94(14) 3_566 . . . ? S3 Ta3 N5 Si5 132.73(14) . . . . ? P3 Ta3 N5 Si5 -36.06(14) . . . . ? Ta3 Ta3 N5 Si5 -176.80(11) 3_566 . . . ? C18 Si6 N6 C67 66.0(3) . . . . ? C17 Si6 N6 C67 -55.9(3) . . . . ? C5 Si6 N6 C67 -176.0(2) . . . . ? C18 Si6 N6 Ta3 -108.1(2) . . . . ? C17 Si6 N6 Ta3 130.0(2) . . . . ? C5 Si6 N6 Ta3 9.9(2) . . . . ? N5 Ta3 N6 C67 95.6(2) . . . . ? S3 Ta3 N6 C67 -116.6(2) 3_566 . . . ? S3 Ta3 N6 C67 -7.5(2) . . . . ? P3 Ta3 N6 C67 162.4(2) . . . . ? Ta3 Ta3 N6 C67 -58.6(2) 3_566 . . . ? N5 Ta3 N6 Si6 -90.63(19) . . . . ? S3 Ta3 N6 Si6 57.23(19) 3_566 . . . ? S3 Ta3 N6 Si6 166.25(17) . . . . ? P3 Ta3 N6 Si6 -23.83(16) . . . . ? Ta3 Ta3 N6 Si6 115.17(16) 3_566 . . . ? C21 C22 C23 C24 0.3(6) . . . . ? C70 C69 C68 C67 -0.1(5) . . . . ? C44 C45 C46 C47 -0.4(6) . . . . ? C12 Si3 N3 C25 57.9(3) . . . . ? C11 Si3 N3 C25 -64.5(2) . . . . ? C3 Si3 N3 C25 178.7(2) . . . . ? C12 Si3 N3 Ta2 -137.02(18) . . . . ? C11 Si3 N3 Ta2 100.6(2) . . . . ? C3 Si3 N3 Ta2 -16.2(2) . . . . ? N4 Ta2 N3 C25 132.4(2) . . . . ? S1 Ta2 N3 C25 -82.1(2) . . . . ? S2 Ta2 N3 C25 31.0(2) . . . . ? P2 Ta2 N3 C25 -161.1(2) . . . . ? Ta1 Ta2 N3 C25 -19.6(3) . . . . ? N4 Ta2 N3 Si3 -30.3(2) . . . . ? S1 Ta2 N3 Si3 115.27(14) . . . . ? S2 Ta2 N3 Si3 -131.62(14) . . . . ? P2 Ta2 N3 Si3 36.22(14) . . . . ? Ta1 Ta2 N3 Si3 177.80(11) . . . . ? C32 C31 N4 Si4 76.6(3) . . . . ? C36 C31 N4 Si4 -103.9(3) . . . . ? C32 C31 N4 Ta2 -95.6(3) . . . . ? C36 C31 N4 Ta2 84.0(3) . . . . ? C14 Si4 N4 C31 -71.8(2) . . . . ? C13 Si4 N4 C31 51.7(2) . . . . ? C4 Si4 N4 C31 171.7(2) . . . . ? C14 Si4 N4 Ta2 99.45(19) . . . . ? C13 Si4 N4 Ta2 -137.05(18) . . . . ? C4 Si4 N4 Ta2 -17.1(2) . . . . ? N3 Ta2 N4 C31 -94.3(2) . . . . ? S1 Ta2 N4 C31 117.1(2) . . . . ? S2 Ta2 N4 C31 7.8(2) . . . . ? P2 Ta2 N4 C31 -161.0(2) . . . . ? Ta1 Ta2 N4 C31 59.7(2) . . . . ? N3 Ta2 N4 Si4 95.04(18) . . . . ? S1 Ta2 N4 Si4 -53.61(18) . . . . ? S2 Ta2 N4 Si4 -162.91(16) . . . . ? P2 Ta2 N4 Si4 28.27(15) . . . . ? Ta1 Ta2 N4 Si4 -111.01(15) . . . . ? C6 P3 C5 Si6 77.03(18) . . . . ? C55 P3 C5 Si6 -171.47(15) . . . . ? Ta3 P3 C5 Si6 -33.37(17) . . . . ? N6 Si6 C5 P3 18.90(19) . . . . ? C18 Si6 C5 P3 140.05(18) . . . . ? C17 Si6 C5 P3 -100.73(19) . . . . ? C36 C31 C32 C33 -0.9(5) . . . . ? N4 C31 C32 C33 178.7(3) . . . . ? C5 P3 C6 Si5 -157.61(15) . . . . ? C55 P3 C6 Si5 85.32(18) . . . . ? Ta3 P3 C6 Si5 -42.53(15) . . . . ? N5 Si5 C6 P3 21.83(19) . . . . ? C16 Si5 C6 P3 -100.22(18) . . . . ? C15 Si5 C6 P3 140.74(17) . . . . ? C54 C53 C52 C51 -0.4(5) . . . . ? C22 C23 C24 C19 0.9(6) . . . . ? C30 C29 C28 C27 -0.5(5) . . . . ? C5 P3 C55 C56 128.3(3) . . . . ? C6 P3 C55 C56 -118.0(3) . . . . ? Ta3 P3 C55 C56 -3.6(3) . . . . ? C5 P3 C55 C60 -56.6(3) . . . . ? C6 P3 C55 C60 57.2(3) . . . . ? Ta3 P3 C55 C60 171.6(2) . . . . ? C58 C59 C60 C55 -1.7(6) . . . . ? C56 C55 C60 C59 0.3(6) . . . . ? P3 C55 C60 C59 -174.9(3) . . . . ? C61 C66 C65 C64 0.0(5) . . . . ? C4 P2 C3 Si3 161.36(15) . . . . ? C19 P2 C3 Si3 -81.80(18) . . . . ? Ta2 P2 C3 Si3 46.90(15) . . . . ? N3 Si3 C3 P2 -26.32(19) . . . . ? C12 Si3 C3 P2 95.9(2) . . . . ? C11 Si3 C3 P2 -144.34(17) . . . . ? Si1 N1 C43 C44 -80.5(3) . . . . ? Ta1 N1 C43 C44 95.6(3) . . . . ? Si1 N1 C43 C48 100.6(3) . . . . ? Ta1 N1 C43 C48 -83.4(3) . . . . ? C54 C49 C50 C51 -0.1(5) . . . . ? N2 C49 C50 C51 176.9(3) . . . . ? C52 C53 C54 C49 0.0(5) . . . . ? C50 C49 C54 C53 0.3(5) . . . . ? N2 C49 C54 C53 -176.7(3) . . . . ? C31 C32 C33 C34 -0.2(5) . . . . ? C66 C65 C64 C63 0.2(5) . . . . ? C65 C64 C63 C62 -0.6(5) . . . . ? C61 C62 C63 C64 0.6(5) . . . . ? C56 C57 C58 C59 -0.8(6) . . . . ? C60 C59 C58 C57 1.9(6) . . . . ? C23 C22 C21 C20 -1.1(6) . . . . ? C19 C20 C21 C22 0.8(6) . . . . ? C28 C29 C30 C25 -0.5(5) . . . . ? C68 C69 C70 C71 -1.1(5) . . . . ? C58 C57 C56 C55 -0.5(5) . . . . ? C60 C55 C56 C57 0.8(5) . . . . ? P3 C55 C56 C57 176.1(3) . . . . ? C1 P1 C2 Si2 -157.47(15) . . . . ? C37 P1 C2 Si2 85.72(17) . . . . ? Ta1 P1 C2 Si2 -43.81(15) . . . . ? N2 Si2 C2 P1 26.90(19) . . . . ? C10 Si2 C2 P1 144.60(16) . . . . ? C9 Si2 C2 P1 -95.97(18) . . . . ? C40 C39 C38 C37 -0.2(5) . . . . ? C63 C62 C61 C66 -0.3(5) . . . . ? C63 C62 C61 N5 176.3(3) . . . . ? C65 C66 C61 C62 0.0(5) . . . . ? C65 C66 C61 N5 -176.7(3) . . . . ? Si5 N5 C61 C62 -93.5(3) . . . . ? Ta3 N5 C61 C62 73.5(3) . . . . ? Si5 N5 C61 C66 83.1(3) . . . . ? Ta3 N5 C61 C66 -110.0(3) . . . . ? C39 C38 C37 C42 0.9(5) . . . . ? C39 C38 C37 P1 176.3(3) . . . . ? C2 P1 C37 C38 -114.8(3) . . . . ? C1 P1 C37 C38 130.4(3) . . . . ? Ta1 P1 C37 C38 0.8(3) . . . . ? C2 P1 C37 C42 60.5(3) . . . . ? C1 P1 C37 C42 -54.2(3) . . . . ? Ta1 P1 C37 C42 176.2(2) . . . . ? C46 C45 C44 C43 0.2(5) . . . . ? C48 C43 C44 C45 0.6(5) . . . . ? N1 C43 C44 C45 -178.4(3) . . . . ? C44 C43 C48 C47 -1.3(5) . . . . ? N1 C43 C48 C47 177.7(3) . . . . ? C53 C52 C51 C50 0.6(5) . . . . ? C49 C50 C51 C52 -0.3(5) . . . . ? C29 C30 C25 C26 1.2(5) . . . . ? C29 C30 C25 N3 -174.0(3) . . . . ? C27 C26 C25 C30 -1.0(5) . . . . ? C27 C26 C25 N3 174.2(3) . . . . ? Si3 N3 C25 C30 93.1(3) . . . . ? Ta2 N3 C25 C30 -71.6(3) . . . . ? Si3 N3 C25 C26 -82.0(3) . . . . ? Ta2 N3 C25 C26 113.4(3) . . . . ? C34 C35 C36 C31 -0.6(5) . . . . ? C32 C31 C36 C35 1.2(5) . . . . ? N4 C31 C36 C35 -178.3(3) . . . . ? C42 C41 C40 C39 1.1(6) . . . . ? C38 C39 C40 C41 -0.8(6) . . . . ? C3 P2 C4 Si4 -77.94(18) . . . . ? C19 P2 C4 Si4 170.49(15) . . . . ? Ta2 P2 C4 Si4 30.25(18) . . . . ? N4 Si4 C4 P2 -13.4(2) . . . . ? C14 Si4 C4 P2 -133.61(16) . . . . ? C13 Si4 C4 P2 106.21(18) . . . . ? C45 C46 C47 C48 -0.3(6) . . . . ? C43 C48 C47 C46 1.2(5) . . . . ? C69 C68 C67 C72 1.4(5) . . . . ? C69 C68 C67 N6 -177.3(3) . . . . ? C71 C72 C67 C68 -1.6(5) . . . . ? C71 C72 C67 N6 177.2(3) . . . . ? Si6 N6 C67 C68 -82.2(3) . . . . ? Ta3 N6 C67 C68 92.8(3) . . . . ? Si6 N6 C67 C72 99.1(3) . . . . ? Ta3 N6 C67 C72 -86.0(3) . . . . ? C2 P1 C1 Si1 78.23(18) . . . . ? C37 P1 C1 Si1 -169.70(15) . . . . ? Ta1 P1 C1 Si1 -32.16(17) . . . . ? N1 Si1 C1 P1 17.54(19) . . . . ? C8 Si1 C1 P1 136.01(16) . . . . ? C7 Si1 C1 P1 -102.23(18) . . . . ? C36 C35 C34 C33 -0.5(5) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C69 C70 C71 C72 1.0(5) . . . . ? C67 C72 C71 C70 0.3(5) . . . . ? C40 C41 C42 C37 -0.4(6) . . . . ? C38 C37 C42 C41 -0.6(5) . . . . ? P1 C37 C42 C41 -176.0(3) . . . . ? C29 C28 C27 C26 0.6(5) . . . . ? C25 C26 C27 C28 0.1(5) . . . . ? C21 C20 C19 C24 0.3(5) . . . . ? C21 C20 C19 P2 -174.4(3) . . . . ? C23 C24 C19 C20 -1.2(5) . . . . ? C23 C24 C19 P2 173.6(3) . . . . ? C4 P2 C19 C20 -122.8(3) . . . . ? C3 P2 C19 C20 123.0(3) . . . . ? Ta2 P2 C19 C20 10.6(3) . . . . ? C4 P2 C19 C24 62.5(3) . . . . ? C3 P2 C19 C24 -51.7(3) . . . . ? Ta2 P2 C19 C24 -164.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.800 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.086