Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email rothwell@purdue.edu _publ_contact_author_name 'Ian P. Rothwell' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name I.Rothwell P.E.Fanwick J.E.Moses S.W.Schweiger A.J.R.Son ; M.G.Thorn ; data_SS3198 _database_code_CSD 200553 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C30 H41 Cl2 N2 O2 Si2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 769.70 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6800(2) _cell_length_b 10.4416(2) _cell_length_c 16.3287(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.3445(8) _cell_angle_gamma 90.00 _cell_volume 1636.88(11) _cell_measurement_reflns_used 14721 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.56 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.583 _cell_measurement_temperature 150 _exptl_crystal_F_000 772 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.1947 _exptl_absorpt_correction_T_max 0.5587 _diffrn_reflns_number 14721 _reflns_number_total 6932 _reflns_friedl_coverage 0.8240 _reflns_number_gt 6763 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 21 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.101 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 6930 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+13.4136P] where P=(Fo^2^+2Fc^2^)/' _refine_ls_shift/su_max 0.040 _refine_diff_density_max 5.03 _refine_diff_density_min -5.31 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(10) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ta 0.80068(3) 0.49391(4) 1.151668(15) 0.02492(7) Uani ? Cl(1) 0.7781(2) 0.28476(19) 1.09205(12) 0.0287(5) Uani ? Cl(2) 0.8159(3) 0.5840(2) 1.02030(11) 0.0334(6) Uani ? Si(12) 0.9883(2) 0.89140(19) 1.17567(11) 0.0153(5) Uani ? Si(22) 0.5616(2) 0.19360(19) 1.28378(12) 0.0163(5) Uani ? O(1) 0.7928(5) 0.6615(5) 1.1986(3) 0.0177(12) Uani ? O(2) 0.7630(5) 0.4296(5) 1.2579(3) 0.0143(10) Uani ? N(3) 1.0082(6) 0.4622(7) 1.1775(4) 0.031(2) Uani ? N(4) 0.5621(7) 0.5106(11) 1.1143(4) 0.0318(19) Uani ? C(11) 0.8366(7) 0.7174(6) 1.2731(4) 0.0115(15) Uani ? C(12) 0.9373(7) 0.8166(7) 1.2736(4) 0.0125(15) Uani ? C(13) 0.9901(7) 0.8659(7) 1.3487(4) 0.0157(15) Uani ? C(14) 0.9527(7) 0.8179(6) 1.4243(4) 0.0148(15) Uani ? C(15) 1.0180(7) 0.8644(7) 1.5008(4) 0.0148(15) Uani ? C(16) 0.9885(8) 0.8140(7) 1.5744(4) 0.0172(19) Uani ? C(17) 0.8856(8) 0.7174(7) 1.5722(4) 0.0171(17) Uani ? C(18) 0.8166(8) 0.6743(7) 1.4996(4) 0.0165(17) Uani ? C(19) 0.8477(7) 0.7226(6) 1.4220(4) 0.0120(15) Uani ? C(1A) 0.7837(7) 0.6741(6) 1.3439(4) 0.0114(15) Uani ? C(21) 0.6631(6) 0.4627(5) 1.3063(4) 0.0084(15) Uani ? C(22) 0.5601(7) 0.3675(7) 1.3176(4) 0.0136(15) Uani ? C(23) 0.4522(8) 0.4042(7) 1.3604(4) 0.0156(17) Uani ? C(24) 0.4387(7) 0.5302(6) 1.3901(4) 0.0131(17) Uani ? C(25) 0.3231(9) 0.5650(7) 1.4303(5) 0.023(2) Uani ? C(26) 0.3066(8) 0.6878(7) 1.4566(5) 0.0203(19) Uani ? C(27) 0.4068(8) 0.7803(7) 1.4433(5) 0.022(2) Uani ? C(28) 0.5242(7) 0.7501(7) 1.4072(4) 0.0152(15) Uani ? C(29) 0.5432(7) 0.6219(7) 1.3799(4) 0.0125(15) Uani ? C(2A) 0.6619(7) 0.5840(7) 1.3415(4) 0.0132(17) Uani ? C(31) 0.4956(10) 0.6306(10) 1.1331(7) 0.042(3) Uani ? C(32) 0.4962(11) 0.4611(10) 1.0337(5) 0.042(3) Uani ? C(41) 1.0896(7) 0.5021(14) 1.2540(4) 0.0279(17) Uani ? C(42) 1.0940(10) 0.4107(10) 1.1178(6) 0.036(3) Uani ? C(121) 1.0823(8) 1.0446(7) 1.2044(5) 0.0227(19) Uani ? C(122) 0.8283(8) 0.9266(7) 1.1027(5) 0.022(2) Uani ? C(123) 1.1137(9) 0.7872(9) 1.1280(5) 0.026(2) Uani ? C(221) 0.4731(10) 0.1735(9) 1.1763(5) 0.030(2) Uani ? C(222) 0.7398(8) 0.1265(8) 1.2967(5) 0.024(2) Uani ? C(223) 0.4546(9) 0.0995(8) 1.3514(5) 0.025(2) Uani ? H(4) 0.5289 0.4555 1.1503 0.12(7) Uiso calc H(13) 1.0530 0.9335 1.3503 0.0200 Uiso calc H(15) 1.0825 0.9306 1.5014 0.0190 Uiso calc H(16) 1.0350 0.8427 1.6244 0.0230 Uiso calc H(17) 0.8646 0.6825 1.6215 0.0220 Uiso calc H(18) 0.7478 0.6123 1.5004 0.0220 Uiso calc H(23) 0.3858 0.3435 1.3701 0.0200 Uiso calc H(25) 0.2572 0.5033 1.4390 0.0310 Uiso calc H(26) 0.2302 0.7097 1.4830 0.0270 Uiso calc H(27) 0.3936 0.8645 1.4592 0.0290 Uiso calc H(28) 0.5904 0.8126 1.4008 0.0200 Uiso calc H(12A) 1.0979 1.0897 1.1552 0.0290 Uiso calc H(12B) 1.1701 1.0261 1.2366 0.0290 Uiso calc H(12C) 1.0271 1.0966 1.2362 0.0290 Uiso calc H(12D) 0.7584 0.9623 1.1327 0.0290 Uiso calc H(12E) 0.7941 0.8488 1.0761 0.0290 Uiso calc H(12F) 0.8503 0.9868 1.0618 0.0290 Uiso calc H(12G) 1.0677 0.7098 1.1080 0.0340 Uiso calc H(12H) 1.1911 0.7665 1.1687 0.0340 Uiso calc H(12I) 1.1468 0.8319 1.0830 0.0340 Uiso calc H(22A) 0.5259 0.2164 1.1386 0.0400 Uiso calc H(22B) 0.3813 0.2097 1.1721 0.0400 Uiso calc H(22C) 0.4666 0.0840 1.1629 0.0400 Uiso calc H(22D) 0.7357 0.0367 1.2840 0.0310 Uiso calc H(22E) 0.7815 0.1383 1.3528 0.0310 Uiso calc H(22F) 0.7947 0.1695 1.2602 0.0310 Uiso calc H(22G) 0.4628 0.0097 1.3403 0.0320 Uiso calc H(22H) 0.3588 0.1248 1.3401 0.0320 Uiso calc H(22I) 0.4879 0.1160 1.4084 0.0320 Uiso calc H(31A) 0.5355 0.6999 1.1055 0.0540 Uiso calc H(31B) 0.5100 0.6452 1.1917 0.0540 Uiso calc H(31C) 0.3975 0.6257 1.1147 0.0540 Uiso calc H(32A) 0.3973 0.4556 1.0340 0.0540 Uiso calc H(32B) 0.5327 0.3776 1.0244 0.0540 Uiso calc H(32C) 0.5160 0.5180 0.9905 0.0540 Uiso calc H(41A) 1.1435 0.4310 1.2778 0.0360 Uiso calc H(41B) 1.0283 0.5312 1.2919 0.0360 Uiso calc H(41C) 1.1509 0.5705 1.2430 0.0360 Uiso calc H(42A) 1.1562 0.4760 1.1032 0.0470 Uiso calc H(42B) 1.0351 0.3830 1.0693 0.0470 Uiso calc H(42C) 1.1471 0.3394 1.1418 0.0470 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.04528(18) 0.01823(12) 0.01404(12) -0.0068(2) 0.01450(10) -0.00400(17) Cl(1) 0.0437(12) 0.0219(9) 0.0232(9) -0.0051(8) 0.0141(8) -0.0086(7) Cl(2) 0.0608(15) 0.0276(10) 0.0123(8) -0.0062(10) 0.0067(8) -0.0008(7) Si(12) 0.0160(10) 0.0170(9) 0.0133(8) -0.0024(8) 0.0035(7) 0.0013(7) Si(22) 0.0180(10) 0.0136(9) 0.0176(9) -0.0023(8) 0.0038(7) -0.0024(7) O(1) 0.014(2) 0.026(3) 0.013(2) -0.002(2) 0.0018(18) -0.003(2) O(2) 0.013(2) 0.017(2) 0.014(2) 0.0004(19) 0.0059(18) -0.0018(18) N(3) 0.006(3) 0.055(6) 0.033(3) 0.009(3) 0.007(2) -0.007(3) N(4) 0.031(3) 0.040(5) 0.023(3) 0.000(4) -0.002(2) -0.012(4) C(11) 0.015(3) 0.008(3) 0.011(3) 0.003(2) 0.000(2) -0.003(2) C(12) 0.006(3) 0.019(3) 0.012(3) 0.001(2) -0.001(2) 0.000(2) C(13) 0.016(3) 0.014(3) 0.017(3) -0.002(3) 0.002(2) -0.002(3) C(14) 0.015(3) 0.013(3) 0.017(3) -0.005(3) 0.004(2) -0.001(3) C(15) 0.010(3) 0.019(3) 0.015(3) -0.002(3) 0.000(2) -0.001(3) C(16) 0.017(4) 0.022(4) 0.012(3) 0.002(3) -0.001(2) -0.004(3) C(17) 0.021(4) 0.017(3) 0.014(3) 0.004(3) 0.005(3) 0.002(3) C(18) 0.021(4) 0.015(3) 0.014(3) 0.000(3) 0.004(3) 0.000(3) C(19) 0.008(3) 0.014(3) 0.014(3) 0.001(2) 0.001(2) -0.003(2) C(1A) 0.011(3) 0.012(3) 0.011(3) 0.000(2) 0.001(2) -0.002(2) C(21) 0.003(3) 0.010(3) 0.012(3) 0.002(2) 0.000(2) -0.001(2) C(22) 0.007(3) 0.017(3) 0.016(3) -0.002(3) -0.002(2) -0.001(3) C(23) 0.014(4) 0.017(3) 0.017(3) -0.004(3) 0.007(3) -0.001(3) C(24) 0.013(3) 0.014(4) 0.012(3) 0.000(2) 0.001(2) 0.000(2) C(25) 0.030(4) 0.021(4) 0.021(4) 0.002(3) 0.010(3) 0.001(3) C(26) 0.014(3) 0.023(4) 0.024(4) 0.009(3) 0.003(3) -0.002(3) C(27) 0.026(4) 0.018(4) 0.023(4) 0.006(3) 0.004(3) 0.000(3) C(28) 0.012(3) 0.014(3) 0.020(3) 0.003(3) 0.004(2) -0.001(3) C(29) 0.008(3) 0.018(3) 0.011(3) 0.000(3) -0.001(2) 0.001(2) C(2A) 0.018(4) 0.014(3) 0.009(3) 0.002(3) 0.007(2) -0.004(2) C(31) 0.018(4) 0.045(6) 0.058(6) 0.014(4) -0.010(4) -0.007(5) C(32) 0.036(5) 0.058(8) 0.026(4) -0.011(4) -0.014(3) -0.002(4) C(41) 0.019(3) 0.039(4) 0.025(3) -0.002(5) 0.000(2) 0.008(5) C(42) 0.030(5) 0.045(5) 0.037(5) 0.008(4) 0.019(4) 0.001(4) C(121) 0.024(4) 0.024(3) 0.021(4) -0.007(3) 0.006(3) 0.002(3) C(122) 0.023(4) 0.020(4) 0.021(4) 0.002(3) -0.002(3) 0.004(3) C(123) 0.025(4) 0.036(5) 0.019(4) 0.006(4) 0.008(3) 0.003(3) C(221) 0.035(5) 0.031(4) 0.025(4) -0.005(4) 0.005(3) -0.004(3) C(222) 0.011(4) 0.026(4) 0.035(4) 0.006(3) 0.000(3) -0.003(3) C(223) 0.023(4) 0.021(4) 0.031(4) -0.004(3) 0.008(3) -0.003(3) # 10. MOLECULAR GEOMETRY _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_publ_flag Ta O(1) 1.916(5) ? Ta O(2) 1.938(5) ? Ta N(3) 2.027(6) ? Ta N(4) 2.318(7) ? Ta Cl(2) 2.3640(19) ? Ta Cl(1) 2.3896(19) ? Si(12) C(122) 1.865(8) ? Si(12) C(121) 1.870(8) ? Si(12) C(123) 1.872(8) ? Si(12) C(12) 1.901(7) ? Si(22) C(222) 1.848(7) ? Si(22) C(221) 1.864(9) ? Si(22) C(223) 1.884(8) ? Si(22) C(22) 1.898(7) ? O(1) C(11) 1.367(8) ? O(2) C(21) 1.370(7) ? N(3) C(41) 1.450(10) ? N(3) C(42) 1.462(10) ? N(4) C(31) 1.459(13) ? N(4) C(32) 1.481(10) ? C(11) C(1A) 1.398(9) ? C(11) C(12) 1.423(9) ? C(12) C(13) 1.366(9) ? C(13) C(14) 1.422(9) ? C(14) C(15) 1.412(10) ? C(14) C(19) 1.420(9) ? C(15) C(16) 1.375(10) ? C(16) C(17) 1.414(11) ? C(17) C(18) 1.361(10) ? C(18) C(19) 1.431(9) ? C(19) C(1A) 1.437(9) ? C(1A) C(2A) 1.506(10) ? C(21) C(2A) 1.390(9) ? C(21) C(22) 1.437(9) ? C(22) C(23) 1.383(9) ? C(23) C(24) 1.414(10) ? C(24) C(25) 1.415(10) ? C(24) C(29) 1.417(9) ? C(25) C(26) 1.369(10) ? C(26) C(27) 1.405(11) ? C(27) C(28) 1.382(10) ? C(28) C(29) 1.431(9) ? C(29) C(2A) 1.434(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ta O(2) 86.4(2) ? O(1) Ta N(3) 98.9(3) ? O(2) Ta N(3) 93.0(2) ? O(1) Ta N(4) 87.0(3) ? O(2) Ta N(4) 88.1(2) ? N(3) Ta N(4) 174.1(3) ? O(1) Ta Cl(2) 90.54(15) ? O(2) Ta Cl(2) 172.26(16) ? N(3) Ta Cl(2) 94.5(2) ? N(4) Ta Cl(2) 84.7(2) ? O(1) Ta Cl(1) 172.51(16) ? O(2) Ta Cl(1) 91.72(15) ? N(3) Ta Cl(1) 88.4(2) ? N(4) Ta Cl(1) 85.7(3) ? Cl(2) Ta Cl(1) 90.41(7) ? C(122) Si(12) C(121) 109.2(4) ? C(122) Si(12) C(123) 112.2(4) ? C(121) Si(12) C(123) 106.3(4) ? C(122) Si(12) C(12) 109.6(3) ? C(121) Si(12) C(12) 108.1(3) ? C(123) Si(12) C(12) 111.3(3) ? C(222) Si(22) C(221) 112.0(4) ? C(222) Si(22) C(223) 108.0(4) ? C(221) Si(22) C(223) 105.8(4) ? C(222) Si(22) C(22) 111.8(3) ? C(221) Si(22) C(22) 111.2(4) ? C(223) Si(22) C(22) 107.6(3) ? C(11) O(1) Ta 136.2(4) ? C(21) O(2) Ta 131.0(4) ? C(41) N(3) C(42) 112.8(7) ? C(41) N(3) Ta 123.2(5) ? C(42) N(3) Ta 123.6(6) ? C(31) N(4) C(32) 109.6(8) ? C(31) N(4) Ta 117.4(6) ? C(32) N(4) Ta 120.6(6) ? O(1) C(11) C(1A) 119.6(6) ? O(1) C(11) C(12) 116.8(6) ? C(1A) C(11) C(12) 123.6(6) ? C(13) C(12) C(11) 117.3(6) ? C(13) C(12) Si(12) 119.5(5) ? C(11) C(12) Si(12) 123.0(5) ? C(12) C(13) C(14) 122.5(6) ? C(15) C(14) C(19) 120.2(6) ? C(15) C(14) C(13) 120.8(6) ? C(19) C(14) C(13) 119.1(6) ? C(16) C(15) C(14) 121.4(7) ? C(15) C(16) C(17) 118.4(6) ? C(18) C(17) C(16) 121.5(6) ? C(17) C(18) C(19) 121.3(7) ? C(14) C(19) C(18) 117.0(6) ? C(14) C(19) C(1A) 119.7(6) ? C(18) C(19) C(1A) 123.1(6) ? C(11) C(1A) C(19) 117.3(6) ? C(11) C(1A) C(2A) 123.3(6) ? C(19) C(1A) C(2A) 119.4(6) ? O(2) C(21) C(2A) 120.8(5) ? O(2) C(21) C(22) 116.9(5) ? C(2A) C(21) C(22) 122.3(6) ? C(23) C(22) C(21) 117.0(6) ? C(23) C(22) Si(22) 116.6(5) ? C(21) C(22) Si(22) 126.4(5) ? C(22) C(23) C(24) 122.7(7) ? C(23) C(24) C(25) 120.7(6) ? C(23) C(24) C(29) 119.3(6) ? C(25) C(24) C(29) 120.0(6) ? C(26) C(25) C(24) 121.1(7) ? C(25) C(26) C(27) 119.0(7) ? C(28) C(27) C(26) 122.1(7) ? C(27) C(28) C(29) 119.4(7) ? C(24) C(29) C(28) 118.3(6) ? C(24) C(29) C(2A) 119.3(6) ? C(28) C(29) C(2A) 122.5(6) ? C(21) C(2A) C(29) 118.8(6) ? C(21) C(2A) C(1A) 122.2(6) ? C(29) C(2A) C(1A) 119.0(6) ? data_SONX05 _database_code_CSD 200554 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C60 H53 Cl2 N2 O2 Si2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 1142.13 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.1790(2) _cell_length_b 20.4517(5) _cell_length_c 13.5288(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.9264(10) _cell_angle_gamma 90.00 _cell_volume 2907.9(2) _cell_measurement_reflns_used 28371 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.30 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.039 _cell_measurement_temperature 150 _exptl_crystal_F_000 1156 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.4406 _exptl_absorpt_correction_T_max 0.7365 _diffrn_reflns_number 28371 _reflns_number_total 12603 _reflns_friedl_coverage 0.8941 _reflns_number_gt 11388 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.90 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_max 17 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.047 _refine_ls_wR_factor_ref 0.106 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10645 _refine_ls_d_res_high 0.81 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0493P)^2^+6.2670P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 2.62 _refine_diff_density_min -1.74 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(7) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ta -0.07920(2) 0.502670(12) 0.224601(19) 0.03224(8) Uani ? Cl(1) -0.30173(17) 0.49166(12) 0.14681(18) 0.0553(7) Uani ? Cl(2) -0.0528(2) 0.38684(11) 0.23226(18) 0.0476(7) Uani ? Si(12) 0.29775(18) 0.44816(11) 0.48153(15) 0.0215(5) Uani ? Si(22) -0.32527(15) 0.68416(9) 0.10798(13) 0.0220(5) Uani ? O(1) 0.0968(4) 0.51793(19) 0.3013(3) 0.0250(13) Uani ? O(2) -0.1056(4) 0.5944(2) 0.2522(3) 0.0242(13) Uani ? N(31) -0.0532(6) 0.5065(6) 0.0858(4) 0.050(2) Uani ? N(41) -0.1117(6) 0.4853(3) 0.3835(5) 0.037(2) Uani ? C(11) 0.1754(5) 0.5633(3) 0.3646(5) 0.0190(19) Uani ? C(12) 0.2715(6) 0.5375(4) 0.4559(6) 0.024(2) Uani ? C(13) 0.3463(6) 0.5834(3) 0.5274(5) 0.0223(19) Uani ? C(14) 0.3297(6) 0.6510(3) 0.5119(5) 0.0251(19) Uani ? C(15) 0.4043(7) 0.6957(4) 0.5867(5) 0.033(2) Uani ? C(16) 0.3913(7) 0.7614(4) 0.5721(6) 0.041(2) Uani ? C(17) 0.3032(7) 0.7858(4) 0.4782(6) 0.038(2) Uani ? C(18) 0.2279(6) 0.7438(3) 0.4033(5) 0.030(2) Uani ? C(19) 0.2382(5) 0.6751(3) 0.4173(5) 0.0190(17) Uani ? C(1A) 0.1624(5) 0.6293(3) 0.3405(4) 0.0187(17) Uani ? C(21) -0.0598(6) 0.6447(3) 0.2075(5) 0.0192(18) Uani ? C(22) -0.1512(5) 0.6818(3) 0.1275(5) 0.0205(17) Uani ? C(23) -0.1021(6) 0.7248(3) 0.0706(5) 0.0270(19) Uani ? C(24) 0.0279(6) 0.7295(3) 0.0854(5) 0.027(2) Uani ? C(25) 0.0735(7) 0.7695(4) 0.0201(6) 0.035(2) Uani ? C(26) 0.2008(7) 0.7748(4) 0.0359(5) 0.034(2) Uani ? C(27) 0.2885(6) 0.7392(4) 0.1199(6) 0.033(2) Uani ? C(28) 0.2486(6) 0.7012(3) 0.1856(6) 0.028(2) Uani ? C(29) 0.1167(6) 0.6958(3) 0.1728(4) 0.0210(17) Uani ? C(2A) 0.0702(5) 0.6557(3) 0.2379(4) 0.0203(17) Uani ? C(111) 0.4574(6) 0.4363(3) 0.5851(5) 0.0243(19) Uani ? C(112) 0.5688(6) 0.4612(3) 0.5736(6) 0.032(2) Uani ? C(113) 0.6895(7) 0.4502(4) 0.6482(6) 0.042(2) Uani ? C(114) 0.6997(8) 0.4126(4) 0.7360(6) 0.046(2) Uani ? C(115) 0.5938(7) 0.3887(5) 0.7504(6) 0.045(3) Uani ? C(116) 0.4744(7) 0.4001(4) 0.6767(6) 0.035(2) Uani ? C(121) 0.1767(6) 0.4184(3) 0.5393(5) 0.027(2) Uani ? C(122) 0.1504(6) 0.4587(4) 0.6135(5) 0.032(2) Uani ? C(123) 0.0720(7) 0.4392(5) 0.6666(6) 0.042(3) Uani ? C(124) 0.0133(7) 0.3789(5) 0.6475(7) 0.047(3) Uani ? C(125) 0.0339(9) 0.3377(5) 0.5743(9) 0.057(4) Uani ? C(126) 0.1151(8) 0.3581(4) 0.5186(7) 0.047(3) Uani ? C(131) 0.3009(6) 0.4040(3) 0.3603(5) 0.0254(19) Uani ? C(132) 0.2787(10) 0.3397(5) 0.3409(8) 0.060(4) Uani ? C(133) 0.2881(10) 0.3105(5) 0.2487(10) 0.069(4) Uani ? C(134) 0.3223(9) 0.3472(6) 0.1781(8) 0.060(4) Uani ? C(135) 0.3469(15) 0.4104(7) 0.1987(10) 0.095(6) Uani ? C(136) 0.3325(10) 0.4391(5) 0.2860(8) 0.062(4) Uani ? C(211) -0.3571(6) 0.6692(3) 0.2337(5) 0.026(2) Uani ? C(212) -0.3069(14) 0.7109(6) 0.3171(8) 0.090(6) Uani ? C(213) -0.3326(17) 0.7044(7) 0.4097(10) 0.106(7) Uani ? C(214) -0.4074(11) 0.6556(6) 0.4223(8) 0.064(4) Uani ? C(215) -0.4522(8) 0.6126(5) 0.3472(7) 0.056(3) Uani ? C(216) -0.4288(7) 0.6187(5) 0.2509(6) 0.044(2) Uani ? C(221) -0.3776(6) 0.7715(4) 0.0683(5) 0.0265(19) Uani ? C(222) -0.4929(6) 0.7854(3) -0.0103(5) 0.0252(19) Uani ? C(223) -0.5348(7) 0.8487(4) -0.0329(5) 0.030(2) Uani ? C(224) -0.4626(8) 0.9014(4) 0.0211(7) 0.035(3) Uani ? C(225) -0.3448(7) 0.8875(4) 0.0998(6) 0.034(2) Uani ? C(226) -0.3055(7) 0.8243(4) 0.1230(6) 0.034(2) Uani ? C(231) -0.4209(7) 0.6288(3) -0.0010(5) 0.029(2) Uani ? C(232) -0.5494(8) 0.6151(4) -0.0211(7) 0.030(2) Uani ? C(233) -0.6185(8) 0.5778(5) -0.1055(6) 0.044(3) Uani ? C(234) -0.5620(9) 0.5506(4) -0.1717(6) 0.046(3) Uani ? C(235) -0.4375(8) 0.5640(4) -0.1561(6) 0.045(3) Uani ? C(236) -0.3653(7) 0.6028(4) -0.0709(5) 0.035(2) Uani ? C(321) -0.1297(11) 0.4695(5) -0.0055(7) 0.071(4) Uani ? C(322) 0.0639(12) 0.5293(6) 0.0705(7) 0.073(4) Uani ? C(421) -0.2194(9) 0.4433(5) 0.3840(8) 0.059(3) Uani ? C(422) -0.1070(8) 0.5432(4) 0.4487(6) 0.043(3) Uani ? H(13) 0.4094 0.5684 0.5876 0.0290 Uiso calc H(15) 0.4644 0.6798 0.6480 0.0430 Uiso calc H(16) 0.4401 0.7900 0.6236 0.0530 Uiso calc H(17) 0.2958 0.8307 0.4666 0.0490 Uiso calc H(18) 0.1690 0.7608 0.3423 0.0390 Uiso calc H(23) -0.1584 0.7516 0.0205 0.0350 Uiso calc H(25) 0.0156 0.7926 -0.0346 0.0460 Uiso calc H(26) 0.2294 0.8012 -0.0075 0.0440 Uiso calc H(27) 0.3750 0.7418 0.1303 0.0430 Uiso calc H(28) 0.3083 0.6785 0.2397 0.0360 Uiso calc H(41) -0.0420 0.4620 0.4218 0.0480 Uiso calc H(112) 0.5624 0.4858 0.5142 0.0410 Uiso calc H(113) 0.7616 0.4679 0.6391 0.0550 Uiso calc H(114) 0.7794 0.4037 0.7850 0.0600 Uiso calc H(115) 0.6013 0.3645 0.8104 0.0590 Uiso calc H(116) 0.4033 0.3830 0.6884 0.0460 Uiso calc H(122) 0.1874 0.5000 0.6269 0.0420 Uiso calc H(123) 0.0582 0.4669 0.7162 0.0550 Uiso calc H(124) -0.0400 0.3660 0.6839 0.0600 Uiso calc H(125) -0.0049 0.2969 0.5613 0.0740 Uiso calc H(126) 0.1272 0.3309 0.4678 0.0620 Uiso calc H(132) 0.2569 0.3140 0.3888 0.0780 Uiso calc H(133) 0.2709 0.2662 0.2362 0.0900 Uiso calc H(134) 0.3281 0.3285 0.1173 0.0780 Uiso calc H(135) 0.3744 0.4356 0.1533 0.1230 Uiso calc H(136) 0.3445 0.4840 0.2951 0.0800 Uiso calc H(212) -0.2540 0.7446 0.3112 0.1170 Uiso calc H(213) -0.2978 0.7340 0.4641 0.1370 Uiso calc H(214) -0.4270 0.6527 0.4837 0.0840 Uiso calc H(215) -0.5000 0.5775 0.3570 0.0740 Uiso calc H(216) -0.4627 0.5879 0.1982 0.0570 Uiso calc H(222) -0.5424 0.7513 -0.0483 0.0330 Uiso calc H(223) -0.6128 0.8566 -0.0851 0.0400 Uiso calc H(224) -0.4910 0.9442 0.0059 0.0460 Uiso calc H(225) -0.2936 0.9216 0.1361 0.0440 Uiso calc H(226) -0.2288 0.8162 0.1766 0.0440 Uiso calc H(232) -0.5891 0.6317 0.0238 0.0390 Uiso calc H(233) -0.7046 0.5708 -0.1181 0.0560 Uiso calc H(234) -0.6083 0.5235 -0.2265 0.0590 Uiso calc H(235) -0.3999 0.5472 -0.2023 0.0580 Uiso calc H(236) -0.2803 0.6113 -0.0609 0.0460 Uiso calc H(32A) 0.1160 0.4924 0.0683 0.0960 Uiso calc H(32B) 0.1098 0.5574 0.1277 0.0960 Uiso calc H(32C) 0.0425 0.5530 0.0055 0.0960 Uiso calc H(32D) -0.1432 0.4951 -0.0679 0.0920 Uiso calc H(32E) -0.2103 0.4592 0.0013 0.0920 Uiso calc H(32F) -0.0863 0.4298 -0.0104 0.0920 Uiso calc H(42A) -0.2099 0.4319 0.4551 0.0760 Uiso calc H(42B) -0.2201 0.4042 0.3444 0.0760 Uiso calc H(42C) -0.2979 0.4665 0.3527 0.0760 Uiso calc H(42D) -0.1749 0.5724 0.4123 0.0560 Uiso calc H(42E) -0.0269 0.5650 0.4626 0.0560 Uiso calc H(42F) -0.1160 0.5301 0.5139 0.0560 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02594(13) 0.02144(13) 0.03680(14) -0.00268(16) -0.00557(9) -0.00067(18) Cl(1) 0.0304(8) 0.0336(15) 0.0732(12) -0.0094(8) -0.0197(8) 0.0070(10) Cl(2) 0.0479(11) 0.0188(11) 0.0589(15) 0.0024(9) -0.0042(10) -0.0050(9) Si(12) 0.0199(9) 0.0222(10) 0.0213(9) 0.0039(8) 0.0056(7) 0.0022(9) Si(22) 0.0159(8) 0.0243(9) 0.0234(9) 0.0018(7) 0.0034(6) 0.0031(7) O(1) 0.028(2) 0.017(3) 0.025(2) 0.0009(16) 0.0027(17) -0.0009(16) O(2) 0.019(2) 0.021(3) 0.031(2) -0.0071(18) 0.0066(18) 0.0081(19) N(31) 0.056(4) 0.051(4) 0.040(3) -0.013(5) 0.012(3) -0.019(5) N(41) 0.023(3) 0.033(5) 0.051(4) -0.002(2) 0.008(3) 0.009(3) C(11) 0.010(3) 0.025(4) 0.021(3) -0.002(2) 0.004(2) -0.002(2) C(12) 0.016(3) 0.030(4) 0.024(4) -0.003(3) 0.006(3) 0.006(3) C(13) 0.021(3) 0.027(4) 0.017(3) 0.001(3) 0.004(2) -0.002(3) C(14) 0.019(3) 0.029(4) 0.022(3) -0.001(3) 0.000(2) -0.001(3) C(15) 0.030(4) 0.031(4) 0.030(4) -0.002(3) 0.000(3) -0.005(3) C(16) 0.034(4) 0.036(5) 0.043(4) -0.003(3) 0.002(3) -0.010(3) C(17) 0.038(4) 0.022(4) 0.051(5) 0.004(3) 0.013(3) 0.001(3) C(18) 0.025(4) 0.033(4) 0.033(4) 0.005(3) 0.011(3) 0.001(3) C(19) 0.017(3) 0.019(3) 0.022(3) -0.001(2) 0.008(2) 0.000(2) C(1A) 0.013(3) 0.024(3) 0.018(3) 0.004(2) 0.004(2) 0.003(2) C(21) 0.022(3) 0.011(3) 0.024(3) 0.002(3) 0.007(3) 0.006(3) C(22) 0.017(3) 0.022(3) 0.022(3) 0.004(2) 0.006(2) 0.003(2) C(23) 0.028(3) 0.031(4) 0.021(3) 0.004(3) 0.007(3) 0.010(3) C(24) 0.022(3) 0.030(4) 0.028(4) 0.003(3) 0.008(3) 0.009(3) C(25) 0.025(4) 0.042(5) 0.039(4) 0.002(3) 0.011(3) 0.016(3) C(26) 0.033(4) 0.041(4) 0.031(4) 0.002(3) 0.013(3) 0.011(3) C(27) 0.020(3) 0.038(4) 0.042(4) -0.001(3) 0.013(3) 0.005(3) C(28) 0.023(3) 0.027(4) 0.033(4) 0.003(3) 0.010(3) 0.005(3) C(29) 0.023(3) 0.021(3) 0.019(3) -0.002(2) 0.007(2) 0.004(2) C(2A) 0.017(3) 0.025(3) 0.014(3) 0.003(2) -0.001(2) 0.002(2) C(111) 0.024(3) 0.026(4) 0.025(3) 0.010(3) 0.011(3) -0.002(3) C(112) 0.026(4) 0.035(4) 0.033(4) 0.006(3) 0.009(3) 0.005(3) C(113) 0.027(4) 0.051(5) 0.046(4) 0.002(3) 0.008(3) -0.010(4) C(114) 0.037(4) 0.058(5) 0.030(4) 0.021(4) -0.005(3) -0.010(4) C(115) 0.035(4) 0.065(6) 0.030(4) 0.017(4) 0.004(3) 0.019(4) C(116) 0.036(4) 0.038(4) 0.035(4) 0.009(3) 0.017(3) 0.014(3) C(121) 0.023(3) 0.026(3) 0.030(4) 0.002(3) 0.007(3) 0.007(3) C(122) 0.023(3) 0.042(5) 0.032(4) -0.001(3) 0.009(3) 0.004(3) C(123) 0.025(4) 0.065(6) 0.039(4) 0.001(4) 0.013(3) 0.003(4) C(124) 0.030(4) 0.059(6) 0.057(5) -0.001(4) 0.023(4) 0.010(4) C(125) 0.047(5) 0.041(5) 0.098(8) -0.005(4) 0.044(5) 0.006(5) C(126) 0.043(5) 0.034(5) 0.076(6) -0.001(4) 0.035(4) -0.003(4) C(131) 0.023(3) 0.027(4) 0.026(3) 0.008(3) 0.008(3) -0.001(3) C(132) 0.082(7) 0.036(5) 0.077(7) 0.000(5) 0.047(6) -0.006(5) C(133) 0.058(6) 0.047(6) 0.109(9) -0.012(5) 0.038(6) -0.054(6) C(134) 0.052(6) 0.076(7) 0.058(6) -0.008(5) 0.026(5) -0.030(5) C(135) 0.156(13) 0.086(9) 0.086(8) -0.029(9) 0.097(9) -0.032(7) C(136) 0.095(8) 0.045(5) 0.071(6) -0.011(5) 0.061(6) -0.021(5) C(211) 0.022(3) 0.029(4) 0.030(4) -0.001(3) 0.012(3) 0.005(3) C(212) 0.165(13) 0.076(8) 0.064(7) -0.069(8) 0.084(8) -0.041(6) C(213) 0.202(17) 0.079(9) 0.070(8) -0.059(10) 0.091(10) -0.031(6) C(214) 0.083(8) 0.075(7) 0.052(6) 0.001(6) 0.045(6) 0.002(5) C(215) 0.028(4) 0.081(7) 0.061(6) 0.000(4) 0.016(4) 0.043(5) C(216) 0.039(4) 0.055(5) 0.032(4) -0.009(4) 0.005(3) 0.010(4) C(221) 0.015(3) 0.042(4) 0.023(3) 0.005(3) 0.007(2) 0.001(3) C(222) 0.016(3) 0.031(4) 0.029(3) 0.004(3) 0.008(2) 0.007(3) C(223) 0.024(3) 0.037(4) 0.028(4) 0.006(3) 0.006(3) 0.006(3) C(224) 0.035(5) 0.031(5) 0.037(5) 0.009(3) 0.008(4) 0.001(3) C(225) 0.033(4) 0.028(4) 0.035(4) 0.003(3) 0.004(3) -0.005(3) C(226) 0.026(4) 0.039(4) 0.033(4) 0.002(3) 0.004(3) -0.002(3) C(231) 0.029(4) 0.026(4) 0.027(4) 0.004(3) 0.002(3) 0.008(3) C(232) 0.025(4) 0.025(4) 0.036(4) -0.002(3) 0.006(3) -0.002(3) C(233) 0.032(4) 0.047(5) 0.046(5) -0.010(4) 0.006(3) 0.000(4) C(234) 0.058(5) 0.042(5) 0.026(4) -0.010(4) 0.000(4) -0.006(3) C(235) 0.049(5) 0.050(5) 0.028(4) 0.009(4) 0.004(3) -0.005(3) C(236) 0.033(4) 0.040(5) 0.027(4) 0.004(3) 0.003(3) -0.006(3) C(321) 0.084(8) 0.071(7) 0.042(5) 0.005(6) 0.000(5) -0.025(5) C(322) 0.102(9) 0.082(8) 0.039(5) 0.000(6) 0.028(5) -0.013(5) C(421) 0.043(5) 0.059(6) 0.073(6) -0.013(4) 0.019(4) 0.024(5) C(422) 0.039(4) 0.054(5) 0.038(4) 0.006(4) 0.016(4) 0.009(4) # 10. MOLECULAR GEOMETRY _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_publ_flag Ta O(1) 1.911(4) ? Ta O(2) 1.956(5) ? Ta N(31) 1.998(6) ? Ta N(41) 2.326(7) ? Ta Cl(1) 2.3584(17) ? Ta Cl(2) 2.385(2) ? Si(12) C(12) 1.863(8) ? Si(12) C(111) 1.872(7) ? Si(12) C(121) 1.881(7) ? Si(12) C(131) 1.883(7) ? Si(22) C(22) 1.873(6) ? Si(22) C(231) 1.877(7) ? Si(22) C(211) 1.878(6) ? Si(22) C(221) 1.899(7) ? O(1) C(11) 1.362(7) ? O(2) C(21) 1.376(8) ? N(31) C(321) 1.452(11) ? N(31) C(322) 1.469(13) ? N(41) C(422) 1.467(10) ? N(41) C(421) 1.481(10) ? C(11) C(1A) 1.385(9) ? C(11) C(12) 1.433(9) ? C(12) C(13) 1.403(9) ? C(13) C(14) 1.401(9) ? C(14) C(15) 1.407(9) ? C(14) C(19) 1.427(8) ? C(15) C(16) 1.359(11) ? C(16) C(17) 1.407(11) ? C(17) C(18) 1.376(10) ? C(18) C(19) 1.416(9) ? C(19) C(1A) 1.440(8) ? C(1A) C(2A) 1.519(8) ? C(21) C(2A) 1.387(9) ? C(21) C(22) 1.428(8) ? C(22) C(23) 1.399(9) ? C(23) C(24) 1.401(9) ? C(24) C(25) 1.420(9) ? C(24) C(29) 1.435(8) ? C(25) C(26) 1.370(10) ? C(26) C(27) 1.423(10) ? C(27) C(28) 1.365(10) ? C(28) C(29) 1.429(9) ? C(29) C(2A) 1.425(8) ? C(111) C(116) 1.400(9) ? C(111) C(112) 1.402(10) ? C(112) C(113) 1.400(10) ? C(113) C(114) 1.387(12) ? C(114) C(115) 1.354(12) ? C(115) C(116) 1.387(10) ? C(121) C(126) 1.391(11) ? C(121) C(122) 1.406(10) ? C(122) C(123) 1.369(10) ? C(123) C(124) 1.380(12) ? C(124) C(125) 1.378(13) ? C(125) C(126) 1.426(11) ? C(131) C(132) 1.348(11) ? C(131) C(136) 1.375(11) ? C(132) C(133) 1.418(14) ? C(133) C(134) 1.367(15) ? C(134) C(135) 1.331(16) ? C(135) C(136) 1.377(12) ? C(211) C(212) 1.372(12) ? C(211) C(216) 1.374(10) ? C(212) C(213) 1.384(13) ? C(213) C(214) 1.349(15) ? C(214) C(215) 1.309(15) ? C(215) C(216) 1.420(12) ? C(221) C(222) 1.392(9) ? C(221) C(226) 1.399(10) ? C(222) C(223) 1.375(10) ? C(223) C(224) 1.394(12) ? C(224) C(225) 1.411(11) ? C(225) C(226) 1.367(11) ? C(231) C(232) 1.396(10) ? C(231) C(236) 1.401(10) ? C(232) C(233) 1.371(12) ? C(233) C(234) 1.377(13) ? C(234) C(235) 1.362(12) ? C(235) C(236) 1.406(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ta O(2) 86.22(17) ? O(1) Ta N(31) 92.9(2) ? O(2) Ta N(31) 102.8(4) ? O(1) Ta N(41) 88.83(19) ? O(2) Ta N(41) 83.61(19) ? N(31) Ta N(41) 173.4(4) ? O(1) Ta Cl(1) 172.71(14) ? O(2) Ta Cl(1) 88.40(14) ? N(31) Ta Cl(1) 93.08(19) ? N(41) Ta Cl(1) 85.67(16) ? O(1) Ta Cl(2) 92.82(13) ? O(2) Ta Cl(2) 165.80(15) ? N(31) Ta Cl(2) 91.4(3) ? N(41) Ta Cl(2) 82.20(15) ? Cl(1) Ta Cl(2) 91.18(8) ? C(12) Si(12) C(111) 108.4(3) ? C(12) Si(12) C(121) 107.8(3) ? C(111) Si(12) C(121) 106.5(3) ? C(12) Si(12) C(131) 110.9(3) ? C(111) Si(12) C(131) 107.1(3) ? C(121) Si(12) C(131) 115.9(3) ? C(22) Si(22) C(231) 112.4(3) ? C(22) Si(22) C(211) 112.1(3) ? C(231) Si(22) C(211) 112.3(3) ? C(22) Si(22) C(221) 105.6(3) ? C(231) Si(22) C(221) 107.9(3) ? C(211) Si(22) C(221) 105.9(3) ? C(11) O(1) Ta 141.0(4) ? C(21) O(2) Ta 122.0(4) ? C(321) N(31) C(322) 109.9(7) ? C(321) N(31) Ta 123.1(7) ? C(322) N(31) Ta 124.5(5) ? C(422) N(41) C(421) 109.2(7) ? C(422) N(41) Ta 116.6(4) ? C(421) N(41) Ta 118.4(5) ? O(1) C(11) C(1A) 121.5(5) ? O(1) C(11) C(12) 115.1(5) ? C(1A) C(11) C(12) 123.3(6) ? C(13) C(12) C(11) 116.3(6) ? C(13) C(12) Si(12) 120.7(5) ? C(11) C(12) Si(12) 123.1(5) ? C(14) C(13) C(12) 122.8(6) ? C(13) C(14) C(15) 121.2(6) ? C(13) C(14) C(19) 119.5(6) ? C(15) C(14) C(19) 119.3(6) ? C(16) C(15) C(14) 122.0(7) ? C(15) C(16) C(17) 119.3(7) ? C(18) C(17) C(16) 120.6(7) ? C(17) C(18) C(19) 121.3(6) ? C(18) C(19) C(14) 117.6(6) ? C(18) C(19) C(1A) 123.2(6) ? C(14) C(19) C(1A) 119.2(5) ? C(11) C(1A) C(19) 118.4(5) ? C(11) C(1A) C(2A) 123.1(5) ? C(19) C(1A) C(2A) 118.5(5) ? O(2) C(21) C(2A) 120.0(6) ? O(2) C(21) C(22) 117.0(5) ? C(2A) C(21) C(22) 123.0(6) ? C(23) C(22) C(21) 116.0(6) ? C(23) C(22) Si(22) 119.4(5) ? C(21) C(22) Si(22) 124.1(5) ? C(22) C(23) C(24) 123.1(6) ? C(23) C(24) C(25) 121.7(6) ? C(23) C(24) C(29) 118.6(6) ? C(25) C(24) C(29) 119.7(6) ? C(26) C(25) C(24) 121.6(6) ? C(25) C(26) C(27) 118.7(6) ? C(28) C(27) C(26) 121.5(6) ? C(27) C(28) C(29) 121.2(6) ? C(2A) C(29) C(28) 123.3(6) ? C(2A) C(29) C(24) 119.3(6) ? C(28) C(29) C(24) 117.2(5) ? C(21) C(2A) C(29) 118.5(5) ? C(21) C(2A) C(1A) 122.0(5) ? C(29) C(2A) C(1A) 119.5(5) ? C(116) C(111) C(112) 115.6(6) ? C(116) C(111) Si(12) 122.6(5) ? C(112) C(111) Si(12) 121.8(5) ? C(113) C(112) C(111) 122.4(7) ? C(114) C(113) C(112) 119.0(7) ? C(115) C(114) C(113) 120.1(7) ? C(114) C(115) C(116) 120.7(7) ? C(115) C(116) C(111) 122.2(7) ? C(126) C(121) C(122) 117.0(6) ? C(126) C(121) Si(12) 125.4(6) ? C(122) C(121) Si(12) 117.5(5) ? C(123) C(122) C(121) 122.0(7) ? C(122) C(123) C(124) 120.8(8) ? C(125) C(124) C(123) 119.7(7) ? C(124) C(125) C(126) 119.6(8) ? C(121) C(126) C(125) 120.8(8) ? C(132) C(131) C(136) 116.2(7) ? C(132) C(131) Si(12) 125.5(6) ? C(136) C(131) Si(12) 118.2(6) ? C(131) C(132) C(133) 121.2(9) ? C(134) C(133) C(132) 120.3(9) ? C(135) C(134) C(133) 118.4(9) ? C(134) C(135) C(136) 121.1(10) ? C(131) C(136) C(135) 122.7(10) ? C(212) C(211) C(216) 115.3(7) ? C(212) C(211) Si(22) 119.5(6) ? C(216) C(211) Si(22) 125.2(6) ? C(211) C(212) C(213) 122.1(9) ? C(214) C(213) C(212) 120.9(11) ? C(215) C(214) C(213) 119.3(9) ? C(214) C(215) C(216) 120.8(9) ? C(211) C(216) C(215) 121.5(8) ? C(222) C(221) C(226) 117.5(7) ? C(222) C(221) Si(22) 121.6(5) ? C(226) C(221) Si(22) 120.7(5) ? C(223) C(222) C(221) 121.3(7) ? C(222) C(223) C(224) 121.2(7) ? C(223) C(224) C(225) 117.7(8) ? C(226) C(225) C(224) 120.5(7) ? C(225) C(226) C(221) 121.8(7) ? C(232) C(231) C(236) 117.1(7) ? C(232) C(231) Si(22) 123.1(6) ? C(236) C(231) Si(22) 119.6(5) ? C(233) C(232) C(231) 121.6(8) ? C(232) C(233) C(234) 120.9(8) ? C(235) C(234) C(233) 119.3(7) ? C(234) C(235) C(236) 120.7(8) ? C(231) C(236) C(235) 120.3(7) ? #============================================================================== data_MT14I _database_code_CSD 200555 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C31 H39 Cl4 N O2 Si2 Ta' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 836.59 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 27.604(2) _cell_length_b 12.7559(7) _cell_length_c 11.5492(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.591(3) _cell_angle_gamma 90.00 _cell_volume 3997.4(9) _cell_measurement_reflns_used 16547 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.39 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.071 _cell_measurement_temperature 173 _exptl_crystal_F_000 1668 # 6. DATA COLLECTION _diffrn_ambient_temperature 173 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.2923 _exptl_absorpt_correction_T_max 0.6309 _diffrn_reflns_number 16547 _reflns_number_total 8683 _reflns_friedl_coverage 0.8331 _reflns_number_gt 7859 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.93 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 15 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.130 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 8683 _refine_ls_number_parameters 372 _refine_ls_number_restraints 1 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.26 _refine_diff_density_min -2.94 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.35E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(10) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 1.101729(9) 0.99738(3) 0.84081(2) 0.03411(13) Uani 1 1 d . . . Cl(3) Cl 1.04545(10) 0.8792(2) 0.9130(3) 0.0467(7) Uani 1 1 d . . . Cl(4) Cl 1.05713(10) 1.1410(2) 0.9115(3) 0.0444(6) Uani 1 1 d . . . Cl(5) Cl 1.04522(7) 0.9984(4) 0.66046(16) 0.0490(4) Uani 1 1 d . . . Cl(6) Cl 1.15177(7) 1.0068(3) 1.03164(17) 0.0431(5) Uani 1 1 d . . . Si(12) Si 1.12350(10) 1.2983(2) 0.6433(2) 0.0464(6) Uani 1 1 d . . . Si(22) Si 1.17134(10) 0.67626(19) 0.9469(2) 0.0406(6) Uani 1 1 d . . . O(1) O 1.1387(2) 0.8814(5) 0.8043(6) 0.0326(14) Uani 1 1 d . . . O(2) O 1.1434(2) 1.0884(5) 0.7745(6) 0.0368(16) Uani 1 1 d . . . N(7) N 0.9431(3) 1.0203(7) 0.8147(7) 0.055(3) Uani 1 1 d . . . C(11) C 1.1635(3) 1.0871(7) 0.6738(7) 0.0378(19) Uani 1 1 d . . . C(12) C 1.1547(3) 1.1748(7) 0.5996(8) 0.042(2) Uani 1 1 d . . . C(13) C 1.1707(4) 1.1674(9) 0.4932(9) 0.054(3) Uani 1 1 d . . . C(14) C 1.1937(4) 1.0769(8) 0.4582(8) 0.044(2) Uani 1 1 d . . . C(15) C 1.2063(4) 1.0711(9) 0.3453(9) 0.051(2) Uani 1 1 d . . . C(16) C 1.2242(3) 0.9772(12) 0.3093(7) 0.060(4) Uani 1 1 d . . . C(17) C 1.2314(4) 0.8933(10) 0.3814(8) 0.054(3) Uani 1 1 d . . . C(18) C 1.2211(3) 0.8986(9) 0.4951(8) 0.045(2) Uani 1 1 d . . . C(19) C 1.2021(2) 0.9934(12) 0.5346(6) 0.0410(16) Uani 1 1 d . . . C(1A) C 1.1915(2) 1.0024(11) 0.6519(6) 0.0354(15) Uani 1 1 d . . . C(21) C 1.1875(3) 0.8611(6) 0.8063(7) 0.0292(15) Uani 1 1 d . . . C(22) C 1.2087(3) 0.7757(7) 0.8790(7) 0.0345(17) Uani 1 1 d . . . C(23) C 1.2591(3) 0.7624(7) 0.8915(8) 0.0395(19) Uani 1 1 d . . . C(24) C 1.2885(3) 0.8297(7) 0.8385(7) 0.0383(18) Uani 1 1 d . . . C(25) C 1.3406(3) 0.8183(8) 0.8632(8) 0.0404(19) Uani 1 1 d . . . C(26) C 1.3704(3) 0.8914(8) 0.8181(9) 0.050(2) Uani 1 1 d . . . C(27) C 1.3484(3) 0.9701(7) 0.7441(8) 0.045(3) Uani 1 1 d . . . C(28) C 1.2987(3) 0.9819(10) 0.7178(7) 0.042(2) Uani 1 1 d . . . C(29) C 1.2668(3) 0.9109(7) 0.7637(7) 0.0352(17) Uani 1 1 d . . . C(2A) C 1.2140(3) 0.9230(7) 0.7428(7) 0.0326(17) Uani 1 1 d . . . C(71) C 0.9342(4) 1.1246(11) 0.7584(11) 0.065(3) Uani 1 1 d . . . C(72) C 0.9217(4) 0.9309(10) 0.7411(12) 0.067(3) Uani 1 1 d . . . C(121) C 1.1336(5) 1.4058(10) 0.5412(12) 0.073(4) Uani 1 1 d . . . C(122) C 1.0560(4) 1.2787(11) 0.6201(14) 0.080(4) Uani 1 1 d . . . C(123) C 1.1508(5) 1.3344(9) 0.7972(10) 0.065(3) Uani 1 1 d . . . C(221) C 1.1520(5) 0.7265(9) 1.0815(9) 0.062(3) Uani 1 1 d . . . C(222) C 1.1177(4) 0.6367(9) 0.8346(10) 0.056(3) Uani 1 1 d . . . C(223) C 1.2113(4) 0.5614(7) 0.9862(9) 0.050(2) Uani 1 1 d . . . C(901) C 0.0000 0.394(3) 0.0000 0.117(10) Uiso 1 2 d S . . C(902) C 0.0091(12) 0.485(4) -0.055(3) 0.112(10) Uiso 0.50 1 d P . . C(903) C 0.0000 0.588(3) 0.0000 0.163(15) Uiso 1 2 d S . . C(904) C 0.0152(15) 0.595(3) 0.121(4) 0.108(11) Uiso 0.50 1 d P . . C(905) C 0.0010(12) 0.492(4) -0.183(3) 0.111(9) Uiso 0.50 1 d P . . C(906) C -0.0074(12) 0.409(3) 0.127(3) 0.084(8) Uiso 0.50 1 d P . . H(13) H 1.1661 1.2246 0.4425 0.070 Uiso 1 1 calc R . . H(15) H 1.2026 1.1292 0.2958 0.067 Uiso 1 1 calc R . . H(16) H 1.2314 0.9720 0.2339 0.078 Uiso 1 1 calc R . . H(17) H 1.2434 0.8312 0.3552 0.071 Uiso 1 1 calc R . . H(18) H 1.2265 0.8407 0.5447 0.058 Uiso 1 1 calc R . . H(23) H 1.2740 0.7067 0.9366 0.051 Uiso 1 1 calc R . . H(25) H 1.3550 0.7627 0.9090 0.053 Uiso 1 1 calc R . . H(26) H 1.4045 0.8871 0.8379 0.065 Uiso 1 1 calc R . . H(27) H 1.3682 1.0162 0.7113 0.059 Uiso 1 1 calc R . . H(28) H 1.2852 1.0368 0.6695 0.055 Uiso 1 1 calc R . . H(7A) H 0.9758 1.0105 0.8350 0.071 Uiso 1 1 calc R . . H(7B) H 0.9306 1.0203 0.8815 0.071 Uiso 1 1 calc R . . H(12A) H 1.1238 1.4714 0.5706 0.095 Uiso 1 1 calc R . . H(12B) H 1.1143 1.3926 0.4646 0.095 Uiso 1 1 calc R . . H(12C) H 1.1678 1.4087 0.5358 0.095 Uiso 1 1 calc R . . H(12D) H 1.0484 1.2272 0.6747 0.105 Uiso 1 1 calc R . . H(12E) H 1.0443 1.2550 0.5410 0.105 Uiso 1 1 calc R . . H(12F) H 1.0402 1.3438 0.6326 0.105 Uiso 1 1 calc R . . H(12G) H 1.1345 1.3957 0.8197 0.085 Uiso 1 1 calc R . . H(12H) H 1.1852 1.3489 0.8027 0.085 Uiso 1 1 calc R . . H(12I) H 1.1466 1.2775 0.8489 0.085 Uiso 1 1 calc R . . H(22A) H 1.1385 0.6701 1.1207 0.081 Uiso 1 1 calc R . . H(22B) H 1.1274 0.7798 1.0605 0.081 Uiso 1 1 calc R . . H(22C) H 1.1800 0.7556 1.1332 0.081 Uiso 1 1 calc R . . H(22D) H 1.1289 0.6132 0.7650 0.073 Uiso 1 1 calc R . . H(22E) H 1.0960 0.6955 0.8155 0.073 Uiso 1 1 calc R . . H(22F) H 1.1004 0.5808 0.8651 0.073 Uiso 1 1 calc R . . H(22G) H 1.1925 0.5057 1.0122 0.065 Uiso 1 1 calc R . . H(22H) H 1.2380 0.5799 1.0484 0.065 Uiso 1 1 calc R . . H(22I) H 1.2241 0.5388 0.9186 0.065 Uiso 1 1 calc R . . H(71A) H 0.9603 1.1408 0.7169 0.084 Uiso 1 1 calc R . . H(71B) H 0.9331 1.1767 0.8178 0.084 Uiso 1 1 calc R . . H(71C) H 0.9034 1.1238 0.7040 0.084 Uiso 1 1 calc R . . H(72A) H 0.8869 0.9418 0.7159 0.087 Uiso 1 1 calc R . . H(72B) H 0.9270 0.8674 0.7862 0.087 Uiso 1 1 calc R . . H(72C) H 0.9372 0.9254 0.6734 0.087 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02725(16) 0.04159(19) 0.03622(18) 0.0001(2) 0.01304(10) 0.0041(2) Cl(3) 0.0342(13) 0.0481(14) 0.0639(17) -0.0013(10) 0.0254(12) 0.0073(12) Cl(4) 0.0418(14) 0.0418(13) 0.0535(15) 0.0052(10) 0.0191(11) 0.0009(11) Cl(5) 0.0385(9) 0.0635(11) 0.0429(9) 0.001(2) 0.0022(7) 0.004(2) Cl(6) 0.0389(9) 0.0555(15) 0.0358(9) -0.0016(13) 0.0090(7) 0.0038(14) Si(12) 0.0416(14) 0.0498(15) 0.0492(15) 0.0012(10) 0.0121(12) 0.0159(11) Si(22) 0.0451(14) 0.0388(13) 0.0427(14) 0.0058(10) 0.0201(11) 0.0044(10) O(1) 0.028(3) 0.039(3) 0.034(3) 0.000(2) 0.015(3) 0.007(3) O(2) 0.033(3) 0.048(4) 0.032(3) 0.013(3) 0.014(3) 0.005(3) N(7) 0.053(5) 0.069(8) 0.046(4) 0.005(4) 0.017(4) -0.007(4) C(11) 0.032(4) 0.060(5) 0.026(4) -0.008(4) 0.015(3) 0.011(4) C(12) 0.038(5) 0.052(5) 0.035(5) -0.004(4) 0.007(4) 0.010(4) C(13) 0.038(5) 0.089(8) 0.035(5) -0.007(5) 0.009(4) 0.027(5) C(14) 0.037(5) 0.061(6) 0.037(5) -0.011(4) 0.014(4) -0.001(4) C(15) 0.038(5) 0.085(8) 0.035(5) 0.003(5) 0.015(4) 0.013(5) C(16) 0.037(4) 0.122(13) 0.022(4) 0.004(6) 0.008(3) 0.000(6) C(17) 0.047(6) 0.088(8) 0.029(5) 0.008(5) 0.010(4) -0.007(5) C(18) 0.034(5) 0.070(6) 0.031(5) 0.003(4) 0.009(4) 0.002(4) C(19) 0.024(3) 0.070(5) 0.029(3) 0.000(6) 0.006(2) 0.004(7) C(1A) 0.029(3) 0.052(4) 0.029(3) -0.005(5) 0.013(3) 0.005(6) C(21) 0.026(4) 0.033(4) 0.032(4) 0.004(3) 0.014(3) 0.000(3) C(22) 0.035(4) 0.042(5) 0.028(4) -0.002(3) 0.010(3) -0.003(3) C(23) 0.039(5) 0.044(5) 0.036(5) 0.010(4) 0.011(4) 0.001(3) C(24) 0.037(4) 0.048(5) 0.030(4) 0.000(4) 0.008(3) -0.012(3) C(25) 0.027(4) 0.058(6) 0.036(5) 0.009(4) 0.006(3) -0.003(4) C(26) 0.023(4) 0.077(7) 0.051(6) 0.005(4) 0.008(4) -0.008(5) C(27) 0.033(4) 0.064(8) 0.042(5) -0.013(4) 0.015(4) -0.006(4) C(28) 0.031(4) 0.067(8) 0.029(3) -0.007(4) 0.008(3) -0.004(4) C(29) 0.031(4) 0.044(5) 0.031(4) 0.001(3) 0.007(3) -0.002(3) C(2A) 0.023(4) 0.047(5) 0.030(4) 0.003(3) 0.010(3) -0.004(3) C(71) 0.038(6) 0.088(9) 0.064(8) 0.006(5) 0.000(5) 0.011(6) C(72) 0.056(7) 0.070(8) 0.080(9) -0.005(6) 0.027(6) -0.014(6) C(121) 0.071(8) 0.074(8) 0.079(9) 0.002(6) 0.023(7) 0.037(7) C(122) 0.038(6) 0.083(9) 0.123(12) 0.009(5) 0.023(7) 0.040(8) C(123) 0.092(9) 0.050(6) 0.057(7) -0.005(6) 0.023(6) 0.001(5) C(221) 0.089(9) 0.062(7) 0.045(6) 0.019(6) 0.034(6) 0.009(5) C(222) 0.050(6) 0.052(6) 0.068(7) -0.007(5) 0.012(5) 0.004(5) C(223) 0.064(6) 0.041(5) 0.050(6) 0.003(4) 0.026(5) 0.012(4) # 10. MOLECULAR GEOMETRY _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. ; #============================================================================== data_MT11I _database_code_CSD 200556 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C34 H53 N4 O2 Si2 Ta' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 786.95 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0515(3) _cell_length_b 15.2435(4) _cell_length_c 21.8989(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3689.2(3) _cell_measurement_reflns_used 22873 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.42 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.040 _cell_measurement_temperature 193 _exptl_crystal_F_000 1608 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.4752 _exptl_absorpt_correction_T_max 0.7378 _diffrn_reflns_number 22873 _reflns_number_total 0 _reflns_number_gt 0 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.098 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_max 28 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.088 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 8380 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.05 _refine_diff_density_min -1.31 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.19E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(9) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.99021(2) 0.925389(16) 0.844745(10) 0.02788(9) Uani 1 1 d . . . Si(12) Si 1.35388(18) 0.97258(13) 0.93807(8) 0.0326(4) Uani 1 1 d . . . Si(22) Si 0.82949(15) 0.89834(12) 0.64803(8) 0.0315(4) Uani 1 1 d . . . O(1) O 1.1733(3) 0.9121(3) 0.8398(2) 0.0272(9) Uani 1 1 d . . . O(2) O 1.0017(4) 0.9585(2) 0.75471(16) 0.0269(8) Uani 1 1 d . . . N(3) N 0.8088(4) 0.9284(4) 0.8462(3) 0.0385(13) Uani 1 1 d . . . N(4) N 0.9923(6) 0.8614(3) 0.9249(2) 0.0377(12) Uani 1 1 d . . . N(5) N 0.9948(5) 1.0515(3) 0.8698(2) 0.0363(12) Uani 1 1 d . . . N(6) N 0.9966(5) 0.7796(3) 0.7972(2) 0.0355(12) Uani 1 1 d . . . C(11) C 1.2585(5) 0.9658(4) 0.8147(3) 0.0226(14) Uani 1 1 d . . . C(12) C 1.3412(5) 1.0068(4) 0.8563(3) 0.0250(13) Uani 1 1 d . . . C(13) C 1.4183(5) 1.0689(4) 0.8325(3) 0.0290(13) Uani 1 1 d . . . C(14) C 1.4211(5) 1.0924(4) 0.7704(3) 0.0278(14) Uani 1 1 d . . . C(15) C 1.5000(8) 1.1588(4) 0.7481(3) 0.0340(14) Uani 1 1 d . . . C(16) C 1.4989(7) 1.1820(4) 0.6882(3) 0.0426(16) Uani 1 1 d . . . C(17) C 1.4192(6) 1.1403(4) 0.6478(3) 0.0386(16) Uani 1 1 d . . . C(18) C 1.3425(5) 1.0753(4) 0.6674(2) 0.0276(12) Uani 1 1 d . . . C(19) C 1.3411(5) 1.0486(4) 0.7296(3) 0.0242(13) Uani 1 1 d . . . C(1A) C 1.2628(5) 0.9818(4) 0.7524(3) 0.0228(13) Uani 1 1 d . . . C(21) C 1.0647(5) 0.9245(4) 0.7078(2) 0.0203(11) Uani 1 1 d . . . C(22) C 0.9994(5) 0.8863(3) 0.6583(2) 0.0243(10) Uani 1 1 d . . . C(23) C 1.0633(6) 0.8442(4) 0.6133(3) 0.0257(14) Uani 1 1 d . . . C(24) C 1.1916(5) 0.8361(4) 0.6145(3) 0.0245(13) Uani 1 1 d . . . C(25) C 1.2553(6) 0.7876(4) 0.5691(3) 0.0276(14) Uani 1 1 d . . . C(26) C 1.3768(6) 0.7788(4) 0.5716(3) 0.0334(15) Uani 1 1 d . . . C(27) C 1.4411(6) 0.8184(4) 0.6194(3) 0.0330(15) Uani 1 1 d . . . C(28) C 1.3831(5) 0.8673(4) 0.6635(3) 0.0266(13) Uani 1 1 d . . . C(29) C 1.2552(5) 0.8778(4) 0.6619(3) 0.0227(12) Uani 1 1 d . . . C(2A) C 1.1909(5) 0.9275(4) 0.7071(2) 0.0216(11) Uani 1 1 d . . . C(31) C 0.7215(7) 0.8696(6) 0.8747(4) 0.060(2) Uani 1 1 d . . . C(32) C 0.7440(7) 1.0015(6) 0.8179(4) 0.057(2) Uani 1 1 d . . . C(41) C 1.0792(7) 0.7922(5) 0.9419(4) 0.051(2) Uani 1 1 d . . . C(42) C 0.9169(7) 0.8814(6) 0.9787(3) 0.052(2) Uani 1 1 d . . . C(51) C 1.0720(6) 1.1192(4) 0.8430(4) 0.0415(16) Uani 1 1 d . . . C(52) C 0.9257(9) 1.0908(5) 0.9189(4) 0.064(3) Uani 1 1 d . . . C(61) C 1.1169(7) 0.7369(5) 0.7847(4) 0.0450(19) Uani 1 1 d . . . C(62) C 0.9136(7) 0.7097(5) 0.8211(4) 0.048(2) Uani 1 1 d . . . C(121) C 1.3886(7) 0.8536(5) 0.9421(4) 0.050(2) Uani 1 1 d . . . C(122) C 1.4830(7) 1.0345(6) 0.9735(3) 0.054(2) Uani 1 1 d . . . C(123) C 1.2166(7) 0.9988(5) 0.9844(3) 0.0418(18) Uani 1 1 d . . . C(221) C 0.7903(7) 1.0169(5) 0.6486(4) 0.053(2) Uani 1 1 d . . . C(222) C 0.7849(6) 0.8504(5) 0.5718(3) 0.0394(17) Uani 1 1 d . . . C(223) C 0.7456(6) 0.8364(5) 0.7069(3) 0.045(2) Uani 1 1 d . . . H(6) H 0.9672 0.7898 0.7590 0.046 Uiso 1 1 calc R . . H(13) H 1.4717 1.0968 0.8590 0.038 Uiso 1 1 calc R . . H(15) H 1.5529 1.1867 0.7748 0.044 Uiso 1 1 calc R . . H(16) H 1.5509 1.2254 0.6740 0.055 Uiso 1 1 calc R . . H(17) H 1.4181 1.1570 0.6070 0.050 Uiso 1 1 calc R . . H(18) H 1.2909 1.0484 0.6396 0.036 Uiso 1 1 calc R . . H(23) H 1.0211 0.8200 0.5806 0.033 Uiso 1 1 calc R . . H(25) H 1.2126 0.7617 0.5372 0.036 Uiso 1 1 calc R . . H(26) H 1.4175 0.7467 0.5419 0.043 Uiso 1 1 calc R . . H(27) H 1.5246 0.8117 0.6214 0.043 Uiso 1 1 calc R . . H(28) H 1.4277 0.8934 0.6946 0.035 Uiso 1 1 calc R . . H(12A) H 1.4681 0.8432 0.9259 0.065 Uiso 1 1 calc R . . H(12B) H 1.3301 0.8215 0.9186 0.065 Uiso 1 1 calc R . . H(12C) H 1.3857 0.8345 0.9838 0.065 Uiso 1 1 calc R . . H(12D) H 1.4705 1.0963 0.9681 0.071 Uiso 1 1 calc R . . H(12E) H 1.5573 1.0175 0.9542 0.071 Uiso 1 1 calc R . . H(12F) H 1.4870 1.0212 1.0163 0.071 Uiso 1 1 calc R . . H(12G) H 1.2220 0.9700 1.0233 0.054 Uiso 1 1 calc R . . H(12H) H 1.1457 0.9788 0.9632 0.054 Uiso 1 1 calc R . . H(12I) H 1.2116 1.0611 0.9904 0.054 Uiso 1 1 calc R . . H(22A) H 0.7041 1.0235 0.6462 0.069 Uiso 1 1 calc R . . H(22B) H 0.8273 1.0452 0.6141 0.069 Uiso 1 1 calc R . . H(22C) H 0.8194 1.0431 0.6856 0.069 Uiso 1 1 calc R . . H(22D) H 0.7983 0.7882 0.5722 0.051 Uiso 1 1 calc R . . H(22E) H 0.8329 0.8766 0.5401 0.051 Uiso 1 1 calc R . . H(22F) H 0.7009 0.8620 0.5642 0.051 Uiso 1 1 calc R . . H(22G) H 0.7735 0.8535 0.7467 0.058 Uiso 1 1 calc R . . H(22H) H 0.7591 0.7747 0.7013 0.058 Uiso 1 1 calc R . . H(22I) H 0.6607 0.8487 0.7034 0.058 Uiso 1 1 calc R . . H(31A) H 0.6684 0.9029 0.9006 0.078 Uiso 1 1 calc R . . H(31B) H 0.7636 0.8267 0.8987 0.078 Uiso 1 1 calc R . . H(31C) H 0.6751 0.8407 0.8437 0.078 Uiso 1 1 calc R . . H(32A) H 0.6880 0.9792 0.7882 0.074 Uiso 1 1 calc R . . H(32B) H 0.8009 1.0398 0.7982 0.074 Uiso 1 1 calc R . . H(32C) H 0.7006 1.0334 0.8487 0.074 Uiso 1 1 calc R . . H(41A) H 1.1165 0.8069 0.9802 0.066 Uiso 1 1 calc R . . H(41B) H 1.1402 0.7874 0.9109 0.066 Uiso 1 1 calc R . . H(41C) H 1.0374 0.7373 0.9458 0.066 Uiso 1 1 calc R . . H(42A) H 0.8704 0.8305 0.9896 0.068 Uiso 1 1 calc R . . H(42B) H 0.8632 0.9290 0.9693 0.068 Uiso 1 1 calc R . . H(42C) H 0.9680 0.8976 1.0123 0.068 Uiso 1 1 calc R . . H(51A) H 1.0231 1.1681 0.8307 0.054 Uiso 1 1 calc R . . H(51B) H 1.1134 1.0957 0.8081 0.054 Uiso 1 1 calc R . . H(51C) H 1.1302 1.1383 0.8727 0.054 Uiso 1 1 calc R . . H(52A) H 0.9770 1.0988 0.9539 0.083 Uiso 1 1 calc R . . H(52B) H 0.8595 1.0529 0.9295 0.083 Uiso 1 1 calc R . . H(52C) H 0.8948 1.1466 0.9059 0.083 Uiso 1 1 calc R . . H(61A) H 1.1554 0.7225 0.8228 0.059 Uiso 1 1 calc R . . H(61B) H 1.1673 0.7765 0.7621 0.059 Uiso 1 1 calc R . . H(61C) H 1.1047 0.6843 0.7614 0.059 Uiso 1 1 calc R . . H(62A) H 0.9217 0.6579 0.7966 0.063 Uiso 1 1 calc R . . H(62B) H 0.8316 0.7302 0.8194 0.063 Uiso 1 1 calc R . . H(62C) H 0.9346 0.6965 0.8626 0.063 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02458(13) 0.03380(14) 0.02524(12) -0.00373(12) 0.00569(12) -0.00202(11) Si(12) 0.0348(10) 0.0397(11) 0.0234(9) -0.0017(9) -0.0029(8) -0.0016(8) Si(22) 0.0203(8) 0.0415(11) 0.0327(10) -0.0031(7) -0.0016(8) -0.0049(8) O(1) 0.028(2) 0.028(2) 0.026(2) -0.0061(17) 0.0016(19) 0.003(2) O(2) 0.021(2) 0.031(2) 0.0286(18) 0.003(2) 0.006(2) -0.0056(16) N(3) 0.033(3) 0.050(3) 0.033(3) 0.000(3) 0.009(3) -0.002(4) N(4) 0.038(3) 0.039(3) 0.036(3) 0.001(3) 0.004(3) 0.008(2) N(5) 0.038(3) 0.035(3) 0.036(3) 0.001(3) 0.008(3) -0.002(2) N(6) 0.029(3) 0.034(3) 0.044(3) -0.011(3) 0.007(3) -0.002(2) C(11) 0.020(3) 0.027(3) 0.021(3) 0.001(3) 0.005(2) 0.002(3) C(12) 0.028(3) 0.026(3) 0.021(3) 0.002(3) -0.001(2) -0.003(2) C(13) 0.025(3) 0.032(3) 0.030(3) -0.001(3) -0.003(2) -0.009(3) C(14) 0.022(3) 0.022(4) 0.040(4) -0.004(2) 0.000(3) -0.006(3) C(15) 0.032(3) 0.032(3) 0.037(3) -0.013(4) 0.003(3) -0.003(3) C(16) 0.042(4) 0.032(3) 0.054(4) -0.010(4) 0.017(4) 0.005(3) C(17) 0.045(4) 0.040(4) 0.030(4) 0.005(3) 0.010(3) 0.008(3) C(18) 0.024(3) 0.033(3) 0.025(3) 0.004(3) 0.003(2) -0.001(3) C(19) 0.018(3) 0.028(3) 0.026(3) 0.004(2) 0.001(2) -0.004(3) C(1A) 0.021(3) 0.022(3) 0.026(3) -0.002(2) 0.000(2) 0.002(3) C(21) 0.021(3) 0.022(3) 0.018(3) 0.001(3) -0.002(2) 0.004(3) C(22) 0.021(3) 0.027(3) 0.024(2) -0.004(2) 0.001(4) 0.005(2) C(23) 0.032(3) 0.023(3) 0.022(3) -0.005(3) -0.005(3) -0.005(3) C(24) 0.024(3) 0.029(3) 0.021(3) 0.000(3) 0.006(2) -0.006(3) C(25) 0.030(3) 0.025(3) 0.028(3) -0.004(3) 0.001(3) -0.007(3) C(26) 0.035(4) 0.032(4) 0.033(3) -0.003(3) 0.010(3) -0.006(3) C(27) 0.023(3) 0.041(4) 0.035(4) 0.001(3) 0.009(3) -0.006(3) C(28) 0.022(3) 0.026(3) 0.031(3) -0.001(2) -0.004(3) -0.005(3) C(29) 0.026(3) 0.024(3) 0.018(3) -0.006(2) 0.002(3) -0.002(3) C(2A) 0.020(3) 0.026(3) 0.019(3) -0.002(3) -0.001(2) 0.005(3) C(31) 0.036(4) 0.079(6) 0.065(5) -0.025(4) 0.022(4) -0.024(5) C(32) 0.034(4) 0.075(7) 0.062(5) 0.007(4) 0.002(4) -0.008(5) C(41) 0.046(5) 0.051(5) 0.055(5) -0.003(4) -0.001(4) 0.011(4) C(42) 0.064(6) 0.055(5) 0.038(4) -0.008(4) 0.022(4) 0.005(4) C(51) 0.044(4) 0.026(3) 0.054(4) -0.001(3) 0.010(4) 0.004(4) C(52) 0.098(7) 0.040(5) 0.053(5) 0.011(4) 0.027(5) -0.013(4) C(61) 0.050(5) 0.032(4) 0.053(5) -0.002(4) 0.000(4) -0.003(4) C(62) 0.049(5) 0.043(5) 0.053(5) -0.022(4) 0.012(4) 0.000(4) C(121) 0.053(5) 0.051(5) 0.045(4) -0.002(4) 0.006(4) 0.003(4) C(122) 0.052(5) 0.090(5) 0.022(3) -0.001(5) -0.012(4) -0.022(3) C(123) 0.048(4) 0.054(5) 0.023(3) -0.012(4) 0.004(3) -0.014(3) C(221) 0.043(4) 0.054(5) 0.062(5) 0.005(4) -0.006(4) -0.008(4) C(222) 0.025(4) 0.060(5) 0.033(4) -0.006(3) -0.004(3) -0.006(4) C(223) 0.023(4) 0.072(6) 0.040(4) -0.010(4) -0.001(3) -0.012(4) # 10. MOLECULAR GEOMETRY _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. ; data_JMI11 _database_code_CSD 200557 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.20 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C72 H79 N4 O2 Si2 Ta' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 1269.58 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.4866(2) _cell_length_b 20.5325(4) _cell_length_c 26.7517(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6309.4(4) _cell_measurement_reflns_used 30323 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.804 _cell_measurement_temperature 173 _exptl_crystal_F_000 2624 # 6. DATA COLLECTION _diffrn_ambient_temperature 173 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.2013 _exptl_absorpt_correction_T_max 0.6971 _diffrn_reflns_number 30323 _reflns_number_total 7930 _reflns_friedl_coverage 0.8398 _reflns_number_gt 7039 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 28.71 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_max 36 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.040 _refine_ls_wR_factor_ref 0.073 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7915 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+17.2409P] where P=(Fo^2^+2Fc^2^)/' _refine_ls_shift/su_max 0.020 _refine_diff_density_max 0.48 _refine_diff_density_min -0.93 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(7) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.88106(2) 0.99776(11) 0.99221(4) 0.0235(2) Uani 0.50 1 d P . . Si(2) Si 0.73577(9) 0.81701(5) 1.08103(4) 0.0249(2) Uani 1 1 d . . . O(1) O 0.75215(18) 0.93243(11) 1.00811(12) 0.0238(6) Uani 1 1 d . . . N(3) N 1.0044(2) 0.93106(13) 1.00385(19) 0.0308(7) Uani 1 1 d . . . N(4) N 0.8601(3) 0.98208(15) 0.91879(12) 0.0358(8) Uani 1 1 d . . . C(1) C 0.6533(3) 0.93576(16) 1.03502(13) 0.0201(7) Uani 1 1 d . . . C(2) C 0.6379(3) 0.88989(15) 1.07544(13) 0.0225(7) Uani 1 1 d . . . C(3) C 0.5457(3) 0.89956(17) 1.10752(14) 0.0244(8) Uani 1 1 d . . . C(4) C 0.4662(3) 0.95225(17) 1.10219(13) 0.0235(8) Uani 1 1 d . . . C(5) C 0.3776(4) 0.96505(17) 1.13750(14) 0.0287(8) Uani 1 1 d . . . C(6) C 0.3050(4) 1.01672(18) 1.13214(15) 0.0332(10) Uani 1 1 d . . . C(7) C 0.3154(3) 1.0578(2) 1.09054(15) 0.0328(9) Uani 1 1 d . . . C(8) C 0.3973(3) 1.04547(18) 1.05471(14) 0.0285(8) Uani 1 1 d . . . C(9) C 0.4764(3) 0.9929(2) 1.05928(12) 0.0233(8) Uani 1 1 d . . . C(10) C 0.5679(3) 0.98123(15) 1.02401(13) 0.0221(8) Uani 1 1 d . . . C(21) C 0.7443(4) 0.77441(18) 1.01886(14) 0.0290(9) Uani 1 1 d . . . C(22) C 0.8251(3) 0.72384(19) 1.01231(16) 0.0346(11) Uani 1 1 d . . . C(23) C 0.8375(4) 0.6918(2) 0.96740(17) 0.0406(11) Uani 1 1 d . . . C(24) C 0.7689(4) 0.7087(2) 0.92732(17) 0.0437(11) Uani 1 1 d . . . C(25) C 0.6872(4) 0.7588(2) 0.93274(18) 0.0395(11) Uani 1 1 d . . . C(26) C 0.6753(4) 0.7905(2) 0.97806(15) 0.0330(9) Uani 1 1 d . . . C(27) C 0.6727(4) 0.75625(18) 1.12622(16) 0.0295(9) Uani 1 1 d . . . C(28) C 0.5557(4) 0.7372(2) 1.12458(19) 0.0406(11) Uani 1 1 d . . . C(29) C 0.5126(5) 0.6906(2) 1.1572(2) 0.0545(14) Uani 1 1 d . . . C(31) C 1.1169(4) 0.9342(2) 1.02894(16) 0.0386(9) Uani 1 1 d . . . C(32) C 0.9917(4) 0.86716(19) 0.97965(17) 0.0422(11) Uani 1 1 d . . . C(41) C 0.9589(4) 0.9856(2) 0.88431(16) 0.0400(12) Uani 1 1 d . . . C(42) C 0.7660(4) 0.9433(2) 0.89739(17) 0.0442(11) Uani 1 1 d . . . C(210) C 0.5878(6) 0.6600(2) 1.19065(19) 0.0593(16) Uani 1 1 d . . . C(211) C 0.7018(6) 0.6762(3) 1.1929(2) 0.0544(15) Uani 1 1 d . . . C(212) C 0.7443(4) 0.7247(2) 1.16119(16) 0.0399(10) Uani 1 1 d . . . C(213) C 0.8838(4) 0.84011(18) 1.10354(15) 0.0350(9) Uani 1 1 d . . . C(901) C 1.0000 0.7022(4) 1.2500 0.072(2) Uani 1 2 d S . . C(902) C 0.9716(5) 0.6694(4) 1.2922(2) 0.0773(19) Uani 1 1 d . . . C(903) C 0.9721(6) 0.6019(4) 1.2920(3) 0.083(2) Uani 1 1 d . . . C(904) C 1.0000 0.5699(5) 1.2500 0.093(3) Uani 1 2 d S . . C(911) C 0.7521(10) 0.1740(4) 0.7234(3) 0.107(3) Uani 1 1 d . . . C(912) C 0.6752(7) 0.1461(5) 0.7571(3) 0.097(3) Uani 1 1 d . . . C(913) C 0.6961(8) 0.0824(5) 0.7728(2) 0.095(3) Uani 1 1 d . . . C(914) C 0.7899(10) 0.0504(5) 0.7552(3) 0.126(4) Uani 1 1 d . . . C(915) C 0.8612(9) 0.0773(8) 0.7210(4) 0.147(6) Uani 1 1 d . . . C(916) C 0.8428(10) 0.1383(8) 0.7074(4) 0.144(6) Uani 1 1 d . . . H(3) H 0.5350 0.8705 1.1338 0.032 Uiso 1 1 calc R . . H(4) H 0.8296 1.0218 0.9113 0.047 Uiso 0.50 1 calc PR . . H(5) H 0.3689 0.9376 1.1649 0.037 Uiso 1 1 calc R . . H(6) H 0.2482 1.0249 1.1561 0.043 Uiso 1 1 calc R . . H(7) H 0.2664 1.0937 1.0873 0.043 Uiso 1 1 calc R . . H(8) H 0.4012 1.0722 1.0267 0.037 Uiso 1 1 calc R . . H(22) H 0.8718 0.7116 1.0391 0.045 Uiso 1 1 calc R . . H(23) H 0.8923 0.6588 0.9642 0.053 Uiso 1 1 calc R . . H(24) H 0.7766 0.6871 0.8970 0.057 Uiso 1 1 calc R . . H(25) H 0.6408 0.7708 0.9058 0.051 Uiso 1 1 calc R . . H(26) H 0.6199 0.8233 0.9813 0.043 Uiso 1 1 calc R . . H(28) H 0.5061 0.7561 1.1012 0.053 Uiso 1 1 calc R . . H(29) H 0.4340 0.6798 1.1568 0.071 Uiso 1 1 calc R . . H(210) H 0.5592 0.6278 1.2118 0.077 Uiso 1 1 calc R . . H(211) H 0.7513 0.6554 1.2153 0.071 Uiso 1 1 calc R . . H(212) H 0.8224 0.7365 1.1633 0.052 Uiso 1 1 calc R . . H(21A) H 0.9173 0.8713 1.0810 0.045 Uiso 1 1 calc R . . H(21B) H 0.9322 0.8021 1.1048 0.045 Uiso 1 1 calc R . . H(21C) H 0.8779 0.8588 1.1363 0.045 Uiso 1 1 calc R . . H(31A) H 1.1182 0.9036 1.0561 0.050 Uiso 1 1 calc R . . H(31B) H 1.1290 0.9773 1.0417 0.050 Uiso 1 1 calc R . . H(31C) H 1.1775 0.9237 1.0056 0.050 Uiso 1 1 calc R . . H(32A) H 1.0461 0.8637 0.9526 0.055 Uiso 1 1 calc R . . H(32B) H 0.9139 0.8627 0.9670 0.055 Uiso 1 1 calc R . . H(32C) H 1.0068 0.8334 1.0036 0.055 Uiso 1 1 calc R . . H(41A) H 1.0020 0.9455 0.8857 0.052 Uiso 1 1 calc R . . H(41B) H 1.0087 1.0211 0.8937 0.052 Uiso 1 1 calc R . . H(41C) H 0.9309 0.9923 0.8509 0.052 Uiso 1 1 calc R . . H(42A) H 0.7394 0.9633 0.8671 0.058 Uiso 1 1 calc R . . H(42B) H 0.7028 0.9408 0.9208 0.058 Uiso 1 1 calc R . . H(42C) H 0.7940 0.9002 0.8902 0.058 Uiso 1 1 calc R . . H(901) H 1.0000 0.7475 1.2500 0.094 Uiso 1 2 calc SR . . H(902) H 0.9519 0.6920 1.3211 0.100 Uiso 1 1 calc R . . H(903) H 0.9533 0.5790 1.3208 0.108 Uiso 1 1 calc R . . H(904) H 1.0000 0.5246 1.2500 0.120 Uiso 1 2 calc SR . . H(911) H 0.7411 0.2164 0.7122 0.139 Uiso 1 1 calc R . . H(912) H 0.6113 0.1693 0.7689 0.126 Uiso 1 1 calc R . . H(913) H 0.6458 0.0623 0.7952 0.124 Uiso 1 1 calc R . . H(914) H 0.8059 0.0087 0.7670 0.164 Uiso 1 1 calc R . . H(915) H 0.9220 0.0535 0.7072 0.191 Uiso 1 1 calc R . . H(916) H 0.8956 0.1576 0.6856 0.188 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.01719(9) 0.0212(3) 0.0321(7) 0.0008(3) 0.00018(14) 0.0052(6) Si(2) 0.0248(5) 0.0195(5) 0.0303(6) 0.0019(4) -0.0020(4) 0.0031(4) O(1) 0.0171(10) 0.0211(10) 0.0332(18) 0.0001(8) 0.0042(13) 0.0025(13) N(3) 0.0255(13) 0.0245(13) 0.042(2) 0.0006(10) -0.002(2) 0.003(2) N(4) 0.0295(17) 0.039(2) 0.0387(19) -0.0029(13) 0.0079(14) -0.0042(14) C(1) 0.0169(16) 0.0180(16) 0.026(2) -0.0020(12) -0.0005(13) -0.0025(14) C(2) 0.0246(18) 0.0161(15) 0.027(2) -0.0014(13) -0.0021(15) 0.0007(13) C(3) 0.0282(19) 0.0223(18) 0.023(2) -0.0027(14) -0.0033(15) 0.0038(15) C(4) 0.0252(18) 0.0230(18) 0.022(2) 0.0002(14) -0.0013(15) -0.0004(15) C(5) 0.030(2) 0.0302(19) 0.026(2) 0.0035(18) 0.0052(19) 0.0040(15) C(6) 0.031(2) 0.035(3) 0.034(2) 0.0057(16) 0.0064(17) -0.0004(17) C(7) 0.030(2) 0.033(2) 0.035(2) 0.0065(16) 0.0008(17) 0.0014(18) C(8) 0.0242(19) 0.0294(18) 0.032(2) 0.0035(15) 0.0002(16) 0.0058(15) C(9) 0.0214(14) 0.025(2) 0.0239(17) 0.0009(17) -0.0009(12) -0.0018(17) C(10) 0.0193(16) 0.0188(18) 0.0282(18) 0.0000(11) 0.0001(13) 0.0029(13) C(21) 0.027(2) 0.0225(19) 0.038(2) -0.0018(15) 0.0037(16) 0.0038(15) C(22) 0.037(2) 0.0270(19) 0.040(3) 0.0009(15) 0.0104(18) 0.0036(18) C(23) 0.051(3) 0.027(2) 0.044(3) -0.0024(19) 0.016(2) 0.0026(19) C(24) 0.053(3) 0.039(2) 0.039(3) -0.010(2) 0.013(2) -0.009(2) C(25) 0.041(2) 0.041(2) 0.036(3) -0.0117(19) -0.004(2) 0.0014(19) C(26) 0.032(2) 0.028(2) 0.038(2) -0.0042(16) -0.0024(17) -0.0026(17) C(27) 0.038(2) 0.0220(19) 0.028(2) 0.0035(15) 0.0035(18) 0.0016(15) C(28) 0.045(3) 0.029(2) 0.047(3) -0.0017(19) 0.005(2) 0.004(2) C(29) 0.060(3) 0.038(3) 0.066(3) -0.012(2) 0.021(3) 0.002(2) C(31) 0.0243(19) 0.040(2) 0.052(3) 0.0045(19) -0.001(2) 0.0105(19) C(32) 0.040(2) 0.029(2) 0.057(3) 0.0037(18) 0.0011(19) 0.0026(18) C(41) 0.044(2) 0.033(3) 0.043(3) -0.0043(18) 0.0123(19) -0.0005(19) C(42) 0.040(3) 0.056(3) 0.037(3) -0.006(2) 0.000(2) -0.008(2) C(210) 0.102(5) 0.033(2) 0.043(3) -0.006(3) 0.017(3) 0.012(2) C(211) 0.081(4) 0.043(3) 0.040(3) 0.003(3) -0.005(3) 0.012(2) C(212) 0.052(3) 0.029(2) 0.038(2) 0.004(2) -0.003(2) 0.0105(19) C(213) 0.032(2) 0.0301(19) 0.043(2) 0.0071(18) -0.006(2) 0.0017(17) C(901) 0.069(6) 0.049(5) 0.098(7) 0.0000 0.006(5) 0.0000 C(902) 0.059(4) 0.110(6) 0.063(4) -0.002(4) -0.002(3) -0.017(4) C(903) 0.062(4) 0.101(6) 0.087(5) 0.008(4) 0.006(3) 0.039(4) C(904) 0.070(6) 0.056(6) 0.152(11) 0.0000 0.034(7) 0.0000 C(911) 0.148(8) 0.089(6) 0.085(6) -0.051(6) 0.012(6) -0.039(4) C(912) 0.081(5) 0.126(7) 0.083(5) -0.016(5) 0.014(4) -0.070(5) C(913) 0.111(6) 0.128(7) 0.046(4) -0.037(6) 0.010(4) -0.036(4) C(914) 0.148(9) 0.191(10) 0.039(4) 0.066(8) -0.031(5) -0.042(5) C(915) 0.072(6) 0.273(16) 0.095(8) 0.036(9) -0.035(6) -0.113(10) C(916) 0.091(8) 0.220(14) 0.122(9) -0.085(9) 0.046(7) -0.092(11) # 10. MOLECULAR GEOMETRY _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 Ta 0.427(2) 4_577 ? Ta N3 1.995(3) . ? Ta N4 2.005(3) . ? Ta N3 2.038(3) 4_577 ? Ta O1 2.043(3) . ? Ta O1 2.061(3) 4_577 ? Ta N4 2.428(4) 4_577 ? Si2 C213 1.865(4) . ? Si2 C2 1.878(3) . ? Si2 C21 1.882(4) . ? Si2 C27 1.882(4) . ? O1 C1 1.346(4) . ? O1 Ta 2.061(3) 4_577 ? N3 C31 1.457(5) . ? N3 C32 1.470(5) . ? N3 Ta 2.038(3) 4_577 ? N4 C42 1.460(5) . ? N4 C41 1.464(5) . ? N4 Ta 2.428(4) 4_577 ? C1 C10 1.386(5) . ? C1 C2 1.445(5) . ? C2 C3 1.377(5) . ? C3 C4 1.423(5) . ? C4 C5 1.414(5) . ? C4 C9 1.424(5) . ? C5 C6 1.357(5) . ? C6 C7 1.402(6) . ? C7 C8 1.367(5) . ? C8 C9 1.416(5) . ? C9 C10 1.433(5) . ? C10 C10 1.498(7) 4_577 ? C21 C26 1.389(5) . ? C21 C22 1.404(6) . ? C22 C23 1.377(6) . ? C23 C24 1.375(7) . ? C24 C25 1.400(6) . ? C25 C26 1.383(6) . ? C27 C28 1.400(6) . ? C27 C212 1.404(6) . ? C28 C29 1.387(6) . ? C29 C210 1.393(8) . ? C210 C211 1.352(8) . ? C211 C212 1.395(7) . ? C901 C902 1.354(8) . ? C901 C902 1.355(8) 3_757 ? C902 C903 1.385(10) . ? C903 C904 1.340(9) . ? C911 C916 1.344(15) . ? C911 C912 1.384(11) . ? C904 C903 1.340(9) 3_757 ? C913 C914 1.348(11) . ? C913 C912 1.395(11) . ? C915 C916 1.320(16) . ? C915 C914 1.347(16) . ? 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 Ta Ta N3 89.7(5) 4_577 . ? Ta Ta N4 172.4(3) 4_577 . ? N3 Ta N4 97.35(18) . . ? Ta Ta N3 78.2(5) 4_577 4_577 ? N3 Ta N3 89.45(15) . 4_577 ? N4 Ta N3 104.43(18) . 4_577 ? Ta Ta O1 86.5(4) 4_577 . ? N3 Ta O1 91.81(13) . . ? N4 Ta O1 90.67(14) . . ? N3 Ta O1 164.6(2) 4_577 . ? Ta Ta O1 81.6(4) 4_577 4_577 ? N3 Ta O1 171.3(2) . 4_577 ? N4 Ta O1 91.23(13) . 4_577 ? N3 Ta O1 90.05(13) 4_577 4_577 ? O1 Ta O1 86.38(12) . 4_577 ? Ta Ta N4 6.2(3) 4_577 4_577 ? N3 Ta N4 91.96(17) . 4_577 ? N4 Ta N4 167.42(17) . 4_577 ? N3 Ta N4 84.02(17) 4_577 4_577 ? O1 Ta N4 80.56(12) . 4_577 ? O1 Ta N4 79.31(12) 4_577 4_577 ? C213 Si2 C2 111.65(16) . . ? C213 Si2 C21 110.87(19) . . ? C2 Si2 C21 109.33(17) . . ? C213 Si2 C27 108.18(19) . . ? C2 Si2 C27 110.42(17) . . ? C21 Si2 C27 106.23(18) . . ? C1 O1 Ta 133.6(2) . . ? C1 O1 Ta 125.0(2) . 4_577 ? Ta O1 Ta 11.93(6) . 4_577 ? C31 N3 C32 109.3(3) . . ? C31 N3 Ta 132.2(3) . . ? C32 N3 Ta 118.2(3) . . ? C31 N3 Ta 124.1(3) . 4_577 ? C32 N3 Ta 126.4(3) . 4_577 ? Ta N3 Ta 12.09(6) . 4_577 ? C42 N4 C41 110.7(3) . . ? C42 N4 Ta 124.1(3) . . ? C41 N4 Ta 121.1(3) . . ? C42 N4 Ta 123.4(3) . 4_577 ? C41 N4 Ta 122.2(3) . 4_577 ? Ta N4 Ta 1.33(6) . 4_577 ? O1 C1 C10 121.2(3) . . ? O1 C1 C2 118.1(3) . . ? C10 C1 C2 120.7(3) . . ? C3 C2 C1 117.8(3) . . ? C3 C2 Si2 121.7(3) . . ? C1 C2 Si2 120.4(3) . . ? C2 C3 C4 122.7(3) . . ? C5 C4 C3 122.5(3) . . ? C5 C4 C9 119.3(3) . . ? C3 C4 C9 118.3(3) . . ? C6 C5 C4 121.1(3) . . ? C5 C6 C7 120.2(4) . . ? C8 C7 C6 120.2(4) . . ? C7 C8 C9 121.5(3) . . ? C8 C9 C4 117.6(3) . . ? C8 C9 C10 122.8(3) . . ? C4 C9 C10 119.5(3) . . ? C1 C10 C9 119.5(3) . . ? C1 C10 C10 121.9(3) . 4_577 ? C9 C10 C10 118.6(3) . 4_577 ? C26 C21 C22 117.1(4) . . ? C26 C21 Si2 123.7(3) . . ? C22 C21 Si2 119.2(3) . . ? C23 C22 C21 122.0(4) . . ? C24 C23 C22 120.1(4) . . ? C23 C24 C25 119.2(4) . . ? C26 C25 C24 120.2(4) . . ? C25 C26 C21 121.4(4) . . ? C28 C27 C212 117.0(4) . . ? C28 C27 Si2 122.3(3) . . ? C212 C27 Si2 120.5(3) . . ? C29 C28 C27 121.0(5) . . ? C28 C29 C210 119.6(5) . . ? C211 C210 C29 121.2(5) . . ? C210 C211 C212 119.2(5) . . ? C211 C212 C27 121.9(5) . . ? C902 C901 C902 120.2(9) . 3_757 ? C901 C902 C903 119.6(7) . . ? C904 C903 C902 119.7(7) . . ? C916 C911 C912 118.5(10) . . ? C903 C904 C903 121.2(10) 3_757 . ? C914 C913 C912 119.3(9) . . ? C916 C915 C914 118.6(10) . . ? C911 C912 C913 118.3(8) . . ? C915 C914 C913 121.5(11) . . ? C915 C916 C911 123.6(11) . . ? data_MTSIP3 _database_code_CSD 200558 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C70 H71 N4 O2 Si2 Ta' _chemical_formula_structural ? _chemical_formula_weight 1237.49 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 11.6987(2) _cell_length_b 18.2575(4) _cell_length_c 28.1025(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.7591(12) _cell_angle_gamma 90.00 _cell_volume 5981.7(4) _cell_measurement_reflns_used 35703 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.37 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.901 _cell_measurement_temperature 173 _exptl_crystal_F_000 2544 # 6. DATA COLLECTION _diffrn_ambient_temperature 173 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.5872 _exptl_absorpt_correction_T_max 0.7885 _diffrn_reflns_number 35703 _reflns_number_total 14457 _reflns_number_gt 11250 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.85 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_max 36 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.077 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 14031 _refine_ls_number_parameters 720 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.62 _refine_diff_density_min -1.00 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ta 0.028257(13) 0.105831(8) 0.325534(5) 0.02159(5) Uani ? Si(1) 0.29627(9) 0.22726(6) 0.22965(4) 0.0236(3) Uani ? Si(2) -0.18937(9) 0.20150(6) 0.45210(4) 0.0218(3) Uani ? O(1) 0.1629(2) 0.17121(12) 0.31459(8) 0.0211(7) Uani ? O(2) -0.0304(2) 0.19022(13) 0.36658(8) 0.0209(7) Uani ? N(3) -0.1259(3) 0.06035(17) 0.32738(11) 0.0291(10) Uani ? N(4) 0.0679(3) 0.03064(16) 0.27732(11) 0.0270(9) Uani ? N(5) 0.1241(3) 0.05576(16) 0.37728(11) 0.0291(9) Uani ? N(6) -0.0525(3) 0.18539(16) 0.26176(10) 0.0274(9) Uani ? C(11) 0.1961(3) 0.24177(19) 0.32159(12) 0.0190(10) Uani ? C(12) 0.2539(3) 0.27585(19) 0.28417(12) 0.0198(10) Uani ? C(13) 0.2767(3) 0.3498(2) 0.28822(12) 0.0220(10) Uani ? C(14) 0.2450(3) 0.3927(2) 0.32679(12) 0.0205(10) Uani ? C(15) 0.2606(3) 0.46974(19) 0.32801(13) 0.0239(10) Uani ? C(16) 0.2259(3) 0.5102(2) 0.36482(13) 0.0292(12) Uani ? C(17) 0.1750(3) 0.4758(2) 0.40215(13) 0.0286(12) Uani ? C(18) 0.1608(3) 0.4014(2) 0.40226(13) 0.0249(10) Uani ? C(19) 0.1957(3) 0.35667(19) 0.36499(12) 0.0198(10) Uani ? C(1A) 0.1775(3) 0.27879(19) 0.36341(12) 0.0189(10) Uani ? C(21) 0.0259(3) 0.21449(18) 0.40697(12) 0.0196(10) Uani ? C(22) -0.0306(3) 0.21175(18) 0.45092(12) 0.0204(10) Uani ? C(23) 0.0355(3) 0.22403(19) 0.49326(13) 0.0228(10) Uani ? C(24) 0.1537(3) 0.23916(19) 0.49539(13) 0.0223(10) Uani ? C(25) 0.2240(3) 0.2456(2) 0.53873(13) 0.0288(12) Uani ? C(26) 0.3381(4) 0.2595(2) 0.53916(14) 0.0323(12) Uani ? C(27) 0.3887(4) 0.2686(2) 0.49625(14) 0.0332(10) Uani ? C(28) 0.3235(3) 0.2657(2) 0.45370(13) 0.0273(10) Uani ? C(29) 0.2044(3) 0.25067(19) 0.45143(12) 0.0209(10) Uani ? C(2A) 0.1347(3) 0.24511(19) 0.40719(12) 0.0204(10) Uani ? C(31) -0.2327(3) 0.1008(2) 0.33332(15) 0.0413(12) Uani ? C(32) -0.1558(4) -0.0173(2) 0.32169(16) 0.0468(15) Uani ? C(41) -0.0015(4) -0.0007(2) 0.23639(14) 0.0424(15) Uani ? C(42) 0.1814(4) -0.0032(2) 0.27845(15) 0.0387(14) Uani ? C(51) 0.2362(4) 0.0782(2) 0.39943(15) 0.0364(12) Uani ? C(52) 0.0971(4) -0.0169(2) 0.39496(15) 0.0417(14) Uani ? C(61) -0.0711(4) 0.2631(2) 0.27417(15) 0.0405(15) Uani ? C(62) -0.1537(4) 0.1625(3) 0.22979(15) 0.0511(15) Uani ? C(111) 0.1679(3) 0.2114(2) 0.18634(13) 0.0265(10) Uani ? C(112) 0.0968(3) 0.2701(2) 0.17181(14) 0.0327(12) Uani ? C(113) 0.0044(4) 0.2618(2) 0.13796(15) 0.0397(15) Uani ? C(114) -0.0197(4) 0.1936(3) 0.11817(14) 0.0415(14) Uani ? C(115) 0.0472(4) 0.1344(3) 0.13246(14) 0.0392(14) Uani ? C(116) 0.1393(4) 0.1430(2) 0.16578(13) 0.0329(14) Uani ? C(121) 0.4006(3) 0.2885(2) 0.20102(13) 0.0263(10) Uani ? C(122) 0.3746(4) 0.3322(2) 0.16108(13) 0.0307(12) Uani ? C(123) 0.4563(4) 0.3775(2) 0.14329(16) 0.0431(15) Uani ? C(124) 0.5658(4) 0.3805(2) 0.16510(17) 0.0430(15) Uani ? C(125) 0.5942(4) 0.3376(2) 0.20399(16) 0.0400(15) Uani ? C(126) 0.5132(4) 0.2919(2) 0.22170(14) 0.0337(14) Uani ? C(131) 0.3786(3) 0.1411(2) 0.24315(14) 0.0262(10) Uani ? C(132) 0.4148(4) 0.0998(2) 0.20503(16) 0.0362(14) Uani ? C(133) 0.4781(4) 0.0372(2) 0.21304(18) 0.0451(15) Uani ? C(134) 0.5099(4) 0.0147(2) 0.25911(19) 0.0452(16) Uani ? C(135) 0.4786(3) 0.0557(2) 0.29724(17) 0.0392(12) Uani ? C(136) 0.4134(3) 0.1186(2) 0.28944(15) 0.0299(10) Uani ? C(211) -0.2667(3) 0.2575(2) 0.40317(13) 0.0258(10) Uani ? C(212) -0.3818(4) 0.2458(2) 0.38842(15) 0.0388(15) Uani ? C(213) -0.4411(5) 0.2923(3) 0.35661(16) 0.0544(17) Uani ? C(214) -0.3875(5) 0.3517(3) 0.33913(16) 0.0531(17) Uani ? C(215) -0.2737(5) 0.3658(2) 0.35294(15) 0.0468(17) Uani ? C(216) -0.2132(4) 0.3182(2) 0.38480(14) 0.0360(12) Uani ? C(221) -0.2288(3) 0.1020(2) 0.45438(13) 0.0263(10) Uani ? C(222) -0.3402(4) 0.0782(2) 0.46012(14) 0.0361(14) Uani ? C(223) -0.3657(4) 0.0043(3) 0.46406(15) 0.0452(15) Uani ? C(224) -0.2797(5) -0.0468(2) 0.46363(15) 0.0450(16) Uani ? C(225) -0.1690(4) -0.0256(2) 0.45946(15) 0.0421(14) Uani ? C(226) -0.1442(4) 0.0486(2) 0.45444(13) 0.0341(12) Uani ? C(231) -0.2407(3) 0.2426(2) 0.50797(12) 0.0223(10) Uani ? C(232) -0.2470(4) 0.2012(2) 0.54946(14) 0.0372(14) Uani ? C(233) -0.2932(4) 0.2289(3) 0.58967(15) 0.0502(17) Uani ? C(234) -0.3331(4) 0.2994(3) 0.58946(16) 0.0457(15) Uani ? C(235) -0.3271(4) 0.3424(2) 0.54981(15) 0.0391(15) Uani ? C(236) -0.2818(3) 0.3143(2) 0.50970(14) 0.0299(10) Uani ? C(901) 0.0713(4) 0.4463(3) 0.52031(15) 0.0438(15) Uani ? C(902) 0.0978(4) 0.5203(3) 0.52723(15) 0.0425(15) Uani ? C(903) 0.0261(4) 0.5726(2) 0.50630(16) 0.0431(15) Uani ? C(911) 0.5378(5) 0.9564(3) 0.0378(2) 0.064(2) Uani ? C(912) 0.5985(5) 0.9587(3) -0.0015(2) 0.0654(19) Uani ? C(913) 0.4395(5) 0.9966(3) 0.0398(2) 0.0648(19) Uani ? H(6) 0.0045 0.1879 0.2417 0.0360 Uiso calc H(13) 0.3147 0.3725 0.2644 0.0290 Uiso calc H(15) 0.2949 0.4928 0.3034 0.0310 Uiso calc H(16) 0.2361 0.5607 0.3651 0.0380 Uiso calc H(17) 0.1505 0.5037 0.4271 0.0370 Uiso calc H(18) 0.1272 0.3796 0.4276 0.0320 Uiso calc H(23) 0.0001 0.2222 0.5217 0.0300 Uiso calc H(25) 0.1913 0.2403 0.5676 0.0370 Uiso calc H(26) 0.3826 0.2628 0.5681 0.0420 Uiso calc H(27) 0.4673 0.2767 0.4967 0.0430 Uiso calc H(28) 0.3580 0.2738 0.4255 0.0360 Uiso calc H(112) 0.1117 0.3161 0.1852 0.0420 Uiso calc H(113) -0.0411 0.3019 0.1286 0.0510 Uiso calc H(114) -0.0811 0.1877 0.0952 0.0540 Uiso calc H(115) 0.0302 0.0884 0.1196 0.0510 Uiso calc H(116) 0.1838 0.1024 0.1750 0.0430 Uiso calc H(122) 0.3008 0.3311 0.1460 0.0400 Uiso calc H(123) 0.4369 0.4060 0.1164 0.0560 Uiso calc H(124) 0.6200 0.4116 0.1535 0.0560 Uiso calc H(125) 0.6683 0.3390 0.2187 0.0520 Uiso calc H(126) 0.5344 0.2627 0.2481 0.0440 Uiso calc H(132) 0.3954 0.1152 0.1738 0.0470 Uiso calc H(133) 0.4998 0.0099 0.1874 0.0580 Uiso calc H(134) 0.5522 -0.0281 0.2645 0.0590 Uiso calc H(135) 0.5014 0.0410 0.3283 0.0510 Uiso calc H(136) 0.3928 0.1460 0.3153 0.0390 Uiso calc H(212) -0.4195 0.2057 0.4003 0.0500 Uiso calc H(213) -0.5178 0.2833 0.3470 0.0710 Uiso calc H(214) -0.4280 0.3829 0.3177 0.0690 Uiso calc H(215) -0.2376 0.4066 0.3412 0.0610 Uiso calc H(216) -0.1362 0.3271 0.3939 0.0460 Uiso calc H(222) -0.3986 0.1126 0.4613 0.0470 Uiso calc H(223) -0.4408 -0.0105 0.4670 0.0590 Uiso calc H(224) -0.2970 -0.0963 0.4662 0.0590 Uiso calc H(225) -0.1107 -0.0603 0.4600 0.0550 Uiso calc H(226) -0.0689 0.0627 0.4510 0.0450 Uiso calc H(232) -0.2193 0.1534 0.5502 0.0490 Uiso calc H(233) -0.2970 0.1997 0.6166 0.0650 Uiso calc H(234) -0.3644 0.3181 0.6163 0.0590 Uiso calc H(235) -0.3535 0.3905 0.5499 0.0510 Uiso calc H(236) -0.2785 0.3441 0.4830 0.0390 Uiso calc H(31A) -0.2854 0.0936 0.3057 0.0540 Uiso calc H(31B) -0.2159 0.1521 0.3370 0.0540 Uiso calc H(31C) -0.2664 0.0832 0.3612 0.0540 Uiso calc H(32A) -0.1824 -0.0356 0.3509 0.0610 Uiso calc H(32B) -0.0894 -0.0445 0.3142 0.0610 Uiso calc H(32C) -0.2153 -0.0228 0.2963 0.0610 Uiso calc H(41A) 0.0270 0.0162 0.2073 0.0550 Uiso calc H(41B) -0.0799 0.0144 0.2374 0.0550 Uiso calc H(41C) 0.0029 -0.0532 0.2377 0.0550 Uiso calc H(42A) 0.1736 -0.0555 0.2792 0.0500 Uiso calc H(42B) 0.2273 0.0128 0.3064 0.0500 Uiso calc H(42C) 0.2179 0.0109 0.2505 0.0500 Uiso calc H(51A) 0.2315 0.0852 0.4331 0.0470 Uiso calc H(51B) 0.2589 0.1233 0.3853 0.0470 Uiso calc H(51C) 0.2918 0.0409 0.3944 0.0470 Uiso calc H(52A) 0.1478 -0.0523 0.3828 0.0540 Uiso calc H(52B) 0.0192 -0.0291 0.3845 0.0540 Uiso calc H(52C) 0.1066 -0.0171 0.4292 0.0540 Uiso calc H(61A) -0.0891 0.2908 0.2455 0.0530 Uiso calc H(61B) -0.0027 0.2824 0.2909 0.0530 Uiso calc H(61C) -0.1335 0.2665 0.2942 0.0530 Uiso calc H(62A) -0.2206 0.1622 0.2474 0.0660 Uiso calc H(62B) -0.1410 0.1143 0.2177 0.0660 Uiso calc H(62C) -0.1648 0.1963 0.2036 0.0660 Uiso calc H(901) 0.1201 0.4104 0.5338 0.0570 Uiso calc H(902) 0.1636 0.5340 0.5459 0.0550 Uiso calc H(903) 0.0447 0.6219 0.5104 0.0560 Uiso calc H(911) 0.5634 0.9272 0.0636 0.0820 Uiso calc H(912) 0.6646 0.9307 -0.0028 0.0850 Uiso calc H(913) 0.3982 0.9941 0.0666 0.0840 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02264(9) 0.01992(9) 0.02210(9) -0.00216(8) 0.00116(6) -0.00236(7) Si(1) 0.0251(6) 0.0251(6) 0.0209(5) -0.0004(5) 0.0039(5) -0.0029(5) Si(2) 0.0211(6) 0.0237(6) 0.0207(5) 0.0001(5) 0.0026(5) 0.0013(5) O(1) 0.0214(14) 0.0195(13) 0.0227(13) -0.0015(11) 0.0038(11) -0.0046(11) O(2) 0.0193(14) 0.0249(14) 0.0182(13) -0.0044(11) -0.0010(11) -0.0043(11) N(3) 0.030(2) 0.0303(19) 0.0270(18) -0.0070(16) 0.0032(15) -0.0051(15) N(4) 0.027(2) 0.0263(18) 0.0271(18) -0.0008(15) -0.0017(15) -0.0063(15) N(5) 0.032(2) 0.0242(18) 0.0307(18) 0.0013(15) 0.0006(16) -0.0023(15) N(6) 0.0277(19) 0.0281(18) 0.0264(17) 0.0015(15) 0.0028(15) 0.0003(15) C(11) 0.015(2) 0.021(2) 0.0203(19) 0.0008(16) -0.0033(15) 0.0018(17) C(12) 0.015(2) 0.025(2) 0.0195(19) 0.0011(16) 0.0022(16) -0.0014(17) C(13) 0.021(2) 0.026(2) 0.0192(19) -0.0007(17) 0.0021(16) 0.0044(17) C(14) 0.0155(19) 0.026(2) 0.0197(18) 0.0023(17) -0.0004(15) -0.0046(18) C(15) 0.026(2) 0.024(2) 0.022(2) -0.0019(17) 0.0041(17) 0.0034(18) C(16) 0.036(3) 0.023(2) 0.028(2) 0.0015(19) -0.0013(19) -0.0049(19) C(17) 0.034(3) 0.030(2) 0.022(2) 0.0045(19) 0.0033(18) -0.0072(18) C(18) 0.025(2) 0.029(2) 0.0212(19) -0.0034(18) 0.0055(16) -0.0026(18) C(19) 0.019(2) 0.022(2) 0.0185(19) 0.0018(16) 0.0018(16) -0.0021(17) C(1A) 0.017(2) 0.021(2) 0.0182(19) 0.0003(16) -0.0013(16) -0.0045(16) C(21) 0.025(2) 0.0171(19) 0.0165(19) 0.0034(16) 0.0008(16) -0.0019(16) C(22) 0.024(2) 0.0135(18) 0.024(2) -0.0001(16) 0.0040(17) 0.0005(16) C(23) 0.027(2) 0.021(2) 0.021(2) 0.0028(17) 0.0049(17) 0.0041(17) C(24) 0.026(2) 0.018(2) 0.023(2) 0.0018(16) 0.0022(17) 0.0034(16) C(25) 0.031(3) 0.035(2) 0.020(2) 0.0007(19) -0.0003(18) 0.0030(18) C(26) 0.038(3) 0.033(2) 0.024(2) -0.004(2) -0.0081(19) -0.0017(19) C(27) 0.025(2) 0.039(2) 0.035(2) -0.0033(19) -0.0014(19) 0.000(2) C(28) 0.025(2) 0.032(2) 0.025(2) -0.0041(18) 0.0021(18) 0.0015(18) C(29) 0.022(2) 0.0174(19) 0.023(2) -0.0022(16) 0.0009(17) -0.0034(16) C(2A) 0.020(2) 0.0191(19) 0.022(2) -0.0020(16) 0.0018(16) 0.0001(16) C(31) 0.028(2) 0.060(3) 0.036(2) -0.012(2) 0.004(2) -0.014(2) C(32) 0.058(3) 0.039(3) 0.043(3) -0.022(2) 0.001(2) -0.001(2) C(41) 0.049(3) 0.040(3) 0.037(3) 0.003(2) -0.004(2) -0.015(2) C(42) 0.038(3) 0.034(2) 0.044(3) 0.001(2) 0.003(2) -0.013(2) C(51) 0.039(3) 0.031(2) 0.037(2) 0.007(2) -0.010(2) -0.002(2) C(52) 0.051(3) 0.031(2) 0.042(3) 0.004(2) -0.003(2) 0.017(2) C(61) 0.043(3) 0.037(3) 0.040(3) 0.004(2) -0.005(2) 0.001(2) C(62) 0.060(3) 0.051(3) 0.039(3) -0.003(3) -0.016(2) -0.003(2) C(111) 0.028(2) 0.034(2) 0.018(2) -0.0041(19) 0.0050(17) -0.0035(18) C(112) 0.031(3) 0.035(2) 0.032(2) 0.000(2) 0.002(2) -0.003(2) C(113) 0.034(3) 0.049(3) 0.035(3) 0.001(2) -0.003(2) 0.012(2) C(114) 0.036(3) 0.061(3) 0.026(2) -0.014(2) -0.006(2) 0.003(2) C(115) 0.040(3) 0.048(3) 0.030(2) -0.013(2) 0.005(2) -0.008(2) C(116) 0.034(3) 0.039(3) 0.026(2) -0.002(2) 0.0039(19) -0.002(2) C(121) 0.031(2) 0.026(2) 0.023(2) 0.0018(18) 0.0096(18) -0.0101(18) C(122) 0.033(3) 0.034(2) 0.025(2) 0.001(2) 0.0021(19) -0.0027(19) C(123) 0.056(3) 0.040(3) 0.035(3) -0.006(2) 0.014(2) 0.007(2) C(124) 0.046(3) 0.038(3) 0.048(3) -0.005(2) 0.022(2) 0.004(2) C(125) 0.030(3) 0.036(3) 0.055(3) -0.004(2) 0.010(2) -0.005(2) C(126) 0.032(3) 0.040(3) 0.029(2) 0.004(2) 0.0024(19) 0.000(2) C(131) 0.017(2) 0.027(2) 0.035(2) -0.0009(17) 0.0054(18) -0.0074(19) C(132) 0.033(3) 0.035(2) 0.041(3) 0.003(2) 0.006(2) -0.009(2) C(133) 0.037(3) 0.039(3) 0.061(3) 0.002(2) 0.015(2) -0.018(3) C(134) 0.027(3) 0.026(2) 0.084(4) 0.005(2) 0.013(3) -0.001(3) C(135) 0.022(2) 0.034(2) 0.062(3) 0.002(2) 0.005(2) 0.006(2) C(136) 0.022(2) 0.029(2) 0.039(2) -0.0009(18) 0.0043(18) -0.0028(19) C(211) 0.030(2) 0.027(2) 0.021(2) 0.0060(18) 0.0055(18) -0.0013(17) C(212) 0.032(3) 0.045(3) 0.038(3) 0.006(2) -0.005(2) 0.007(2) C(213) 0.054(3) 0.065(4) 0.041(3) 0.014(3) -0.015(3) -0.005(3) C(214) 0.076(4) 0.048(3) 0.032(3) 0.025(3) -0.015(3) 0.004(2) C(215) 0.073(4) 0.034(3) 0.034(3) 0.014(3) 0.008(3) 0.006(2) C(216) 0.044(3) 0.033(2) 0.031(2) 0.009(2) 0.004(2) 0.001(2) C(221) 0.034(2) 0.026(2) 0.0193(19) -0.002(2) 0.0041(17) 0.0000(18) C(222) 0.034(3) 0.039(3) 0.037(2) -0.006(2) 0.013(2) -0.006(2) C(223) 0.049(3) 0.046(3) 0.043(3) -0.025(3) 0.018(2) -0.012(2) C(224) 0.073(4) 0.026(2) 0.037(3) -0.017(3) 0.010(3) -0.004(2) C(225) 0.058(3) 0.028(2) 0.041(3) 0.001(2) 0.008(2) 0.000(2) C(226) 0.042(3) 0.029(2) 0.031(2) -0.004(2) 0.001(2) 0.000(2) C(231) 0.017(2) 0.029(2) 0.021(2) -0.0062(17) 0.0023(16) -0.0025(17) C(232) 0.050(3) 0.035(3) 0.028(2) -0.006(2) 0.011(2) 0.002(2) C(233) 0.069(4) 0.055(3) 0.029(3) -0.021(3) 0.019(2) -0.004(2) C(234) 0.035(3) 0.066(3) 0.038(3) -0.011(2) 0.014(2) -0.024(3) C(235) 0.030(3) 0.044(3) 0.042(3) 0.008(2) -0.005(2) -0.021(2) C(236) 0.024(2) 0.032(2) 0.033(2) 0.0013(19) -0.0015(18) -0.004(2) C(901) 0.054(3) 0.042(3) 0.038(3) 0.015(2) 0.019(3) 0.009(2) C(902) 0.041(3) 0.050(3) 0.038(3) -0.005(2) 0.012(2) -0.009(2) C(903) 0.052(3) 0.034(3) 0.047(3) -0.006(2) 0.026(3) -0.007(2) C(911) 0.044(4) 0.047(3) 0.096(5) -0.006(3) -0.016(3) 0.008(3) C(912) 0.042(3) 0.049(3) 0.104(5) 0.005(3) -0.001(4) -0.003(3) C(913) 0.048(4) 0.058(3) 0.087(4) -0.013(3) -0.003(3) -0.006(3) # 10. MOLECULAR GEOMETRY _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_publ_flag Ta N(5) 1.984(3) ? Ta N(3) 1.990(3) ? Ta N(4) 2.010(3) ? Ta O(1) 2.020(2) ? Ta O(2) 2.075(2) ? Ta N(6) 2.436(3) ? Si(1) C(131) 1.867(4) ? Si(1) C(12) 1.873(3) ? Si(1) C(111) 1.875(4) ? Si(1) C(121) 1.885(4) ? Si(2) C(22) 1.870(4) ? Si(2) C(221) 1.877(4) ? Si(2) C(231) 1.883(4) ? Si(2) C(211) 1.883(4) ? O(1) C(11) 1.355(4) ? O(2) C(21) 1.339(4) ? N(3) C(32) 1.467(5) ? N(3) C(31) 1.473(5) ? N(4) C(42) 1.462(5) ? N(4) C(41) 1.468(5) ? N(5) C(52) 1.460(5) ? N(5) C(51) 1.463(5) ? N(6) C(61) 1.481(5) ? N(6) C(62) 1.485(5) ? C(11) C(1A) 1.388(5) ? C(11) C(12) 1.438(5) ? C(12) C(13) 1.380(5) ? C(13) C(14) 1.411(5) ? C(14) C(15) 1.419(5) ? C(14) C(19) 1.421(5) ? C(15) C(16) 1.360(5) ? C(16) C(17) 1.398(5) ? C(17) C(18) 1.369(5) ? C(18) C(19) 1.415(5) ? C(19) C(1A) 1.438(5) ? C(1A) C(2A) 1.498(5) ? C(21) C(2A) 1.390(5) ? C(21) C(22) 1.449(5) ? C(22) C(23) 1.382(5) ? C(23) C(24) 1.406(5) ? C(24) C(25) 1.418(5) ? C(24) C(29) 1.429(5) ? C(25) C(26) 1.357(5) ? C(26) C(27) 1.397(5) ? C(27) C(28) 1.365(5) ? C(28) C(29) 1.416(5) ? C(29) C(2A) 1.433(5) ? C(111) C(112) 1.397(5) ? C(111) C(116) 1.405(5) ? C(112) C(113) 1.388(6) ? C(113) C(114) 1.384(6) ? C(114) C(115) 1.374(6) ? C(115) C(116) 1.376(6) ? C(121) C(122) 1.390(5) ? C(121) C(126) 1.396(5) ? C(122) C(123) 1.388(5) ? C(123) C(124) 1.375(6) ? C(124) C(125) 1.363(6) ? C(125) C(126) 1.386(5) ? C(131) C(136) 1.393(5) ? C(131) C(132) 1.404(5) ? C(132) C(133) 1.370(6) ? C(133) C(134) 1.380(6) ? C(134) C(135) 1.381(6) ? C(135) C(136) 1.387(5) ? C(211) C(216) 1.393(5) ? C(211) C(212) 1.393(5) ? C(212) C(213) 1.378(6) ? C(213) C(214) 1.364(7) ? C(214) C(215) 1.380(7) ? C(215) C(216) 1.398(6) ? C(221) C(226) 1.389(5) ? C(221) C(222) 1.396(5) ? C(222) C(223) 1.389(6) ? C(223) C(224) 1.374(6) ? C(224) C(225) 1.366(6) ? C(225) C(226) 1.395(5) ? C(231) C(232) 1.397(5) ? C(231) C(236) 1.397(5) ? C(232) C(233) 1.388(6) ? C(233) C(234) 1.369(6) ? C(234) C(235) 1.370(6) ? C(235) C(236) 1.384(5) ? C(901) C(903) 1.355(6) ? C(901) C(902) 1.396(6) ? C(902) C(903) 1.371(6) ? C(903) C(901) 1.355(6) ? C(911) C(912) 1.362(7) ? C(911) C(913) 1.369(7) ? C(912) C(913) 1.393(7) ? C(913) C(912) 1.393(7) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N(5) Ta N(3) 104.29(13) ? N(5) Ta N(4) 91.79(12) ? N(3) Ta N(4) 89.61(12) ? N(5) Ta O(1) 89.05(11) ? N(3) Ta O(1) 166.00(11) ? N(4) Ta O(1) 94.26(11) ? N(5) Ta O(2) 97.32(11) ? N(3) Ta O(2) 87.32(11) ? N(4) Ta O(2) 170.85(11) ? O(1) Ta O(2) 86.77(9) ? N(5) Ta N(6) 167.19(12) ? N(3) Ta N(6) 88.33(12) ? N(4) Ta N(6) 90.49(11) ? O(1) Ta N(6) 78.20(10) ? O(2) Ta N(6) 80.81(9) ? C(131) Si(1) C(12) 113.59(17) ? C(131) Si(1) C(111) 111.95(17) ? C(12) Si(1) C(111) 110.60(16) ? C(131) Si(1) C(121) 104.19(17) ? C(12) Si(1) C(121) 107.04(16) ? C(111) Si(1) C(121) 109.07(17) ? C(22) Si(2) C(221) 110.18(17) ? C(22) Si(2) C(231) 111.17(16) ? C(221) Si(2) C(231) 105.11(16) ? C(22) Si(2) C(211) 110.50(17) ? C(221) Si(2) C(211) 116.47(17) ? C(231) Si(2) C(211) 103.03(16) ? C(11) O(1) Ta 139.2(2) ? C(21) O(2) Ta 123.7(2) ? C(32) N(3) C(31) 107.5(3) ? C(32) N(3) Ta 127.5(3) ? C(31) N(3) Ta 124.9(2) ? C(42) N(4) C(41) 107.1(3) ? C(42) N(4) Ta 122.3(2) ? C(41) N(4) Ta 130.6(3) ? C(52) N(5) C(51) 108.7(3) ? C(52) N(5) Ta 122.9(3) ? C(51) N(5) Ta 127.9(2) ? C(61) N(6) C(62) 106.7(3) ? C(61) N(6) Ta 117.0(2) ? C(62) N(6) Ta 121.2(2) ? O(1) C(11) C(1A) 121.5(3) ? O(1) C(11) C(12) 116.8(3) ? C(1A) C(11) C(12) 121.6(3) ? C(13) C(12) C(11) 117.6(3) ? C(13) C(12) Si(1) 118.0(3) ? C(11) C(12) Si(1) 124.5(3) ? C(12) C(13) C(14) 123.0(3) ? C(13) C(14) C(15) 121.8(3) ? C(13) C(14) C(19) 118.2(3) ? C(15) C(14) C(19) 120.0(3) ? C(16) C(15) C(14) 120.7(3) ? C(15) C(16) C(17) 120.0(4) ? C(18) C(17) C(16) 120.4(4) ? C(17) C(18) C(19) 121.9(3) ? C(18) C(19) C(14) 116.9(3) ? C(18) C(19) C(1A) 122.9(3) ? C(14) C(19) C(1A) 120.2(3) ? C(11) C(1A) C(19) 118.3(3) ? C(11) C(1A) C(2A) 125.6(3) ? C(19) C(1A) C(2A) 116.0(3) ? O(2) C(21) C(2A) 121.5(3) ? O(2) C(21) C(22) 119.0(3) ? C(2A) C(21) C(22) 119.5(3) ? C(23) C(22) C(21) 117.8(3) ? C(23) C(22) Si(2) 119.1(3) ? C(21) C(22) Si(2) 122.8(3) ? C(22) C(23) C(24) 123.1(3) ? C(23) C(24) C(25) 123.5(3) ? C(23) C(24) C(29) 118.0(3) ? C(25) C(24) C(29) 118.5(3) ? C(26) C(25) C(24) 121.6(4) ? C(25) C(26) C(27) 120.1(4) ? C(28) C(27) C(26) 120.3(4) ? C(27) C(28) C(29) 121.6(4) ? C(28) C(29) C(24) 117.8(3) ? C(28) C(29) C(2A) 122.6(3) ? C(24) C(29) C(2A) 119.5(3) ? C(21) C(2A) C(29) 119.1(3) ? C(21) C(2A) C(1A) 122.0(3) ? C(29) C(2A) C(1A) 118.6(3) ? C(112) C(111) C(116) 116.5(4) ? C(112) C(111) Si(1) 119.8(3) ? C(116) C(111) Si(1) 123.7(3) ? C(113) C(112) C(111) 121.8(4) ? C(114) C(113) C(112) 119.7(4) ? C(115) C(114) C(113) 119.9(4) ? C(114) C(115) C(116) 120.2(4) ? C(115) C(116) C(111) 121.9(4) ? C(122) C(121) C(126) 116.5(4) ? C(122) C(121) Si(1) 125.4(3) ? C(126) C(121) Si(1) 118.1(3) ? C(123) C(122) C(121) 121.4(4) ? C(124) C(123) C(122) 120.5(4) ? C(125) C(124) C(123) 119.3(4) ? C(124) C(125) C(126) 120.4(4) ? C(125) C(126) C(121) 121.8(4) ? C(136) C(131) C(132) 118.1(4) ? C(136) C(131) Si(1) 123.0(3) ? C(132) C(131) Si(1) 118.7(3) ? C(133) C(132) C(131) 121.1(4) ? C(132) C(133) C(134) 120.2(4) ? C(133) C(134) C(135) 119.9(4) ? C(134) C(135) C(136) 120.3(4) ? C(135) C(136) C(131) 120.4(4) ? C(216) C(211) C(212) 117.7(4) ? C(216) C(211) Si(2) 119.9(3) ? C(212) C(211) Si(2) 121.9(3) ? C(213) C(212) C(211) 121.4(4) ? C(214) C(213) C(212) 120.1(5) ? C(213) C(214) C(215) 120.6(4) ? C(214) C(215) C(216) 119.3(4) ? C(211) C(216) C(215) 120.9(4) ? C(226) C(221) C(222) 117.0(4) ? C(226) C(221) Si(2) 120.1(3) ? C(222) C(221) Si(2) 122.6(3) ? C(223) C(222) C(221) 121.3(4) ? C(224) C(223) C(222) 119.9(4) ? C(225) C(224) C(223) 120.5(4) ? C(224) C(225) C(226) 119.4(4) ? C(221) C(226) C(225) 121.8(4) ? C(232) C(231) C(236) 115.8(3) ? C(232) C(231) Si(2) 121.6(3) ? C(236) C(231) Si(2) 122.5(3) ? C(233) C(232) C(231) 122.3(4) ? C(234) C(233) C(232) 119.7(4) ? C(233) C(234) C(235) 120.2(4) ? C(234) C(235) C(236) 119.9(4) ? C(235) C(236) C(231) 122.2(4) ? C(903) C(901) C(902) 119.4(4) ? C(903) C(902) C(901) 119.6(4) ? C(901) C(903) C(902) 121.0(4) ? C(912) C(911) C(913) 120.8(5) ? C(911) C(912) C(913) 119.3(5) ? C(911) C(913) C(912) 119.9(5) ? C(911) C(913) C(912) 120.0(6) ? data_SS4243 _database_code_CSD 200559 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.35 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C40 H45 Cl2 N2 O2 Si2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 893.84 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.21600(10) _cell_length_b 12.59880(10) _cell_length_c 31.0769(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3999.89(12) _cell_measurement_reflns_used 23184 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.48 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.943 _cell_measurement_temperature 150 _exptl_crystal_F_000 1800 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.2976 _exptl_absorpt_correction_T_max 0.3569 _diffrn_reflns_number 23184 _reflns_number_total 9012 _reflns_friedl_coverage 0.8755 _reflns_number_gt 8461 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 40 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.048 _refine_ls_wR_factor_ref 0.091 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 9011 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.7958P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.93 _refine_diff_density_min -3.05 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(8) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ta 0.95818(3) 0.90360(2) 0.839517(9) 0.03122(7) Uani ? Cl(1) 1.17054(16) 0.83304(14) 0.82639(5) 0.0328(5) Uani ? Cl(2) 0.86497(17) 0.76406(14) 0.79805(5) 0.0318(4) Uani ? Si(1) 0.55631(18) 0.97873(14) 0.78767(5) 0.0240(4) Uani ? Si(2) 1.25482(18) 0.98541(14) 0.94597(6) 0.0234(4) Uani ? O(1) 0.7862(4) 0.9510(3) 0.85633(14) 0.0250(10) Uani ? O(2) 1.0277(5) 1.0079(3) 0.87804(12) 0.0240(10) Uani ? N(3) 0.9749(7) 1.0009(5) 0.78616(19) 0.0440(18) Uani ? N(4) 0.9484(7) 0.7875(4) 0.89426(17) 0.0353(15) Uani ? C(11) 0.7377(6) 1.0527(5) 0.85528(18) 0.0193(15) Uani ? C(12) 0.6401(6) 1.0780(5) 0.82412(18) 0.0217(15) Uani ? C(13) 0.6036(7) 1.1824(6) 0.8208(2) 0.0280(17) Uani ? C(14) 0.6623(7) 1.2648(5) 0.8455(2) 0.0303(18) Uani ? C(15) 0.6307(8) 1.3730(5) 0.8387(3) 0.045(2) Uani ? C(16) 0.6915(10) 1.4515(7) 0.8612(3) 0.054(3) Uani ? C(17) 0.7863(9) 1.4241(6) 0.8923(2) 0.048(2) Uani ? C(18) 0.8147(8) 1.3197(5) 0.9011(2) 0.033(2) Uani ? C(19) 0.7550(7) 1.2366(5) 0.8782(2) 0.0260(17) Uani ? C(1A) 0.7872(6) 1.1271(5) 0.88455(18) 0.0207(15) Uani ? C(21) 0.9920(6) 1.0487(5) 0.91716(18) 0.0210(15) Uani ? C(22) 1.0834(6) 1.0390(5) 0.95175(19) 0.0223(15) Uani ? C(23) 1.0424(7) 1.0728(4) 0.99203(17) 0.0207(15) Uani ? C(24) 0.9172(5) 1.1140(4) 0.99984(18) 0.0183(15) Uani ? C(25) 0.8766(7) 1.1452(5) 1.04158(19) 0.0257(17) Uani ? C(26) 0.7526(7) 1.1819(5) 1.0489(2) 0.0273(17) Uani ? C(27) 0.6630(6) 1.1870(5) 1.0148(2) 0.0247(15) Uani ? C(28) 0.6994(6) 1.1607(5) 0.97388(19) 0.0227(15) Uani ? C(29) 0.8291(6) 1.1244(4) 0.96457(18) 0.0180(15) Uani ? C(2A) 0.8713(5) 1.0964(5) 0.92191(17) 0.0190(15) Uani ? C(31) 0.9896(8) 1.1156(6) 0.7903(2) 0.048(2) Uani ? C(32) 1.0169(8) 0.9639(7) 0.7440(2) 0.046(2) Uani ? C(41) 0.8448(8) 0.7988(7) 0.9269(2) 0.041(2) Uani ? C(42) 0.9745(8) 0.6738(6) 0.8871(3) 0.043(2) Uani ? C(121) 0.6496(6) 0.9661(5) 0.7355(2) 0.0260(17) Uani ? C(122) 0.6847(7) 0.8699(6) 0.7167(2) 0.0323(18) Uani ? C(123) 0.7416(8) 0.8658(6) 0.6760(2) 0.041(2) Uani ? C(124) 0.7599(8) 0.9572(6) 0.6531(2) 0.043(2) Uani ? C(125) 0.7248(8) 1.0532(6) 0.6704(2) 0.041(2) Uani ? C(126) 0.6708(7) 1.0581(6) 0.7114(2) 0.0313(18) Uani ? C(127) 0.3946(7) 1.0371(6) 0.7723(2) 0.035(2) Uani ? C(128) 0.5299(7) 0.8468(5) 0.8134(2) 0.0327(17) Uani ? C(221) 1.2458(7) 0.8373(5) 0.9525(2) 0.0273(18) Uani ? C(222) 1.3303(7) 0.7664(6) 0.9331(2) 0.036(2) Uani ? C(223) 1.3241(9) 0.6569(6) 0.9412(3) 0.043(2) Uani ? C(224) 1.2326(8) 0.6175(6) 0.9694(2) 0.043(2) Uani ? C(225) 1.1466(8) 0.6861(6) 0.9889(2) 0.037(2) Uani ? C(226) 1.1513(7) 0.7952(5) 0.9811(2) 0.032(2) Uani ? C(227) 1.3542(7) 1.0357(6) 0.9917(2) 0.039(2) Uani ? C(228) 1.3369(7) 1.0280(6) 0.8952(2) 0.038(2) Uani ? H(4) 1.0203 0.8066 0.9097 0.0460 Uiso calc H(13) 0.5375 1.2002 0.8015 0.0360 Uiso calc H(15) 0.5674 1.3908 0.8184 0.0580 Uiso calc H(16) 0.6708 1.5223 0.8562 0.0710 Uiso calc H(17) 0.8303 1.4775 0.9071 0.0620 Uiso calc H(18) 0.8746 1.3037 0.9227 0.0440 Uiso calc H(23) 1.1007 1.0680 1.0149 0.0270 Uiso calc H(25) 0.9353 1.1407 1.0644 0.0330 Uiso calc H(26) 0.7279 1.2034 1.0763 0.0350 Uiso calc H(27) 0.5775 1.2086 1.0201 0.0320 Uiso calc H(28) 0.6388 1.1664 0.9517 0.0290 Uiso calc H(122) 0.6698 0.8071 0.7316 0.0420 Uiso calc H(123) 0.7672 0.8010 0.6644 0.0530 Uiso calc H(124) 0.7963 0.9543 0.6257 0.0560 Uiso calc H(125) 0.7371 1.1152 0.6546 0.0530 Uiso calc H(126) 0.6483 1.1237 0.7229 0.0410 Uiso calc H(12A) 0.3448 0.9856 0.7565 0.0460 Uiso calc H(12B) 0.4084 1.0988 0.7548 0.0460 Uiso calc H(12C) 0.3476 1.0568 0.7979 0.0460 Uiso calc H(12D) 0.4777 0.8554 0.8388 0.0420 Uiso calc H(12E) 0.6129 0.8164 0.8209 0.0420 Uiso calc H(12F) 0.4854 0.8007 0.7936 0.0420 Uiso calc H(222) 1.3933 0.7920 0.9141 0.0470 Uiso calc H(223) 1.3819 0.6110 0.9274 0.0560 Uiso calc H(224) 1.2290 0.5452 0.9753 0.0560 Uiso calc H(225) 1.0838 0.6593 1.0076 0.0490 Uiso calc H(226) 1.0924 0.8402 0.9948 0.0420 Uiso calc H(22A) 1.3483 1.1117 0.9928 0.0510 Uiso calc H(22B) 1.4439 1.0151 0.9878 0.0510 Uiso calc H(22C) 1.3217 1.0062 1.0181 0.0510 Uiso calc H(22D) 1.2940 0.9956 0.8711 0.0490 Uiso calc H(22E) 1.4270 1.0065 0.8958 0.0490 Uiso calc H(22F) 1.3319 1.1038 0.8926 0.0490 Uiso calc H(31A) 1.0782 1.1352 0.7837 0.0620 Uiso calc H(31B) 0.9692 1.1366 0.8192 0.0620 Uiso calc H(31C) 0.9311 1.1505 0.7707 0.0620 Uiso calc H(32A) 0.9662 0.9986 0.7221 0.0600 Uiso calc H(32B) 1.0042 0.8886 0.7420 0.0600 Uiso calc H(32C) 1.1079 0.9802 0.7400 0.0600 Uiso calc H(41A) 0.7660 0.7658 0.9167 0.0540 Uiso calc H(41B) 0.8288 0.8728 0.9321 0.0540 Uiso calc H(41C) 0.8721 0.7653 0.9531 0.0540 Uiso calc H(42A) 1.0015 0.6415 0.9136 0.0560 Uiso calc H(42B) 1.0428 0.6661 0.8660 0.0560 Uiso calc H(42C) 0.8964 0.6398 0.8768 0.0560 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02143(12) 0.03621(14) 0.03603(14) 0.00652(13) -0.00758(13) -0.01834(13) Cl(1) 0.0215(8) 0.0402(10) 0.0368(9) 0.0001(7) 0.0068(6) -0.0075(7) Cl(2) 0.0290(9) 0.0356(9) 0.0307(8) 0.0015(7) -0.0031(7) -0.0129(7) Si(1) 0.0203(9) 0.0301(9) 0.0217(8) -0.0050(8) -0.0040(7) -0.0027(7) Si(2) 0.0186(9) 0.0244(9) 0.0272(9) 0.0000(7) -0.0027(7) -0.0021(7) O(1) 0.024(2) 0.025(2) 0.026(2) -0.0063(19) -0.0006(18) -0.0044(18) O(2) 0.023(2) 0.027(2) 0.022(2) 0.002(2) 0.0024(19) -0.0010(17) N(3) 0.053(4) 0.048(4) 0.031(3) 0.005(4) 0.014(3) 0.010(3) N(4) 0.044(3) 0.029(3) 0.033(3) -0.004(3) 0.007(3) 0.001(2) C(11) 0.023(3) 0.019(3) 0.016(3) 0.000(2) 0.001(2) 0.000(2) C(12) 0.019(3) 0.025(3) 0.021(3) -0.003(3) -0.003(2) 0.002(2) C(13) 0.027(3) 0.038(4) 0.019(3) 0.005(3) -0.007(3) 0.001(3) C(14) 0.039(4) 0.022(3) 0.030(4) 0.003(3) -0.014(3) 0.001(3) C(15) 0.063(5) 0.032(4) 0.039(4) 0.005(3) -0.027(4) 0.001(4) C(16) 0.087(7) 0.026(4) 0.050(5) -0.009(4) -0.034(5) 0.006(4) C(17) 0.075(6) 0.025(4) 0.043(4) -0.016(4) -0.030(4) 0.006(3) C(18) 0.047(4) 0.027(4) 0.026(4) -0.006(3) -0.015(3) 0.005(3) C(19) 0.032(4) 0.024(3) 0.022(3) -0.004(3) -0.004(3) 0.003(3) C(1A) 0.019(3) 0.024(3) 0.019(3) -0.001(2) -0.003(2) 0.000(2) C(21) 0.026(3) 0.023(3) 0.014(3) -0.001(2) 0.003(2) -0.004(2) C(22) 0.023(3) 0.022(3) 0.022(3) -0.001(2) 0.002(2) 0.001(2) C(23) 0.024(3) 0.018(3) 0.020(3) 0.000(3) -0.009(3) -0.002(2) C(24) 0.021(3) 0.012(3) 0.022(3) 0.000(2) -0.003(2) 0.001(2) C(25) 0.036(4) 0.024(3) 0.017(3) 0.001(3) -0.007(3) 0.001(2) C(26) 0.035(4) 0.023(3) 0.024(3) 0.000(3) 0.005(3) -0.004(3) C(27) 0.022(3) 0.022(3) 0.030(3) 0.000(3) 0.006(3) 0.001(3) C(28) 0.024(3) 0.026(3) 0.018(3) -0.001(3) -0.002(2) -0.003(3) C(29) 0.020(3) 0.012(3) 0.022(3) -0.003(2) -0.002(2) 0.003(2) C(2A) 0.021(3) 0.018(3) 0.018(3) -0.002(3) 0.000(2) 0.002(3) C(31) 0.053(5) 0.048(5) 0.043(4) -0.001(4) 0.008(3) 0.024(4) C(32) 0.041(5) 0.078(6) 0.018(3) -0.007(4) 0.001(3) 0.005(3) C(41) 0.046(5) 0.047(5) 0.031(4) -0.007(4) 0.011(3) 0.013(3) C(42) 0.043(5) 0.029(4) 0.058(5) 0.001(4) -0.001(4) 0.009(3) C(121) 0.025(3) 0.033(4) 0.020(3) -0.006(3) -0.007(3) -0.003(3) C(122) 0.038(4) 0.034(4) 0.025(3) -0.007(3) -0.008(3) -0.004(3) C(123) 0.045(5) 0.044(5) 0.034(4) -0.006(4) -0.004(3) -0.011(3) C(124) 0.058(5) 0.051(5) 0.021(4) -0.009(4) 0.004(3) -0.004(3) C(125) 0.058(5) 0.040(4) 0.026(4) -0.011(4) 0.002(3) 0.003(3) C(126) 0.038(4) 0.030(4) 0.026(3) -0.007(3) -0.005(3) -0.003(3) C(127) 0.026(4) 0.047(5) 0.033(4) -0.006(3) -0.004(3) -0.006(3) C(128) 0.023(3) 0.043(4) 0.032(3) -0.009(3) 0.004(3) -0.003(3) C(221) 0.027(4) 0.028(4) 0.027(3) 0.000(3) -0.005(3) -0.004(3) C(222) 0.037(4) 0.032(4) 0.039(4) 0.008(3) -0.003(3) 0.000(3) C(223) 0.055(5) 0.027(4) 0.047(5) 0.014(4) -0.020(4) -0.009(3) C(224) 0.060(5) 0.026(4) 0.043(4) 0.005(4) -0.015(4) 0.004(3) C(225) 0.046(5) 0.028(4) 0.038(4) 0.000(3) -0.009(3) 0.005(3) C(226) 0.035(4) 0.026(4) 0.034(4) -0.001(3) -0.013(3) 0.003(3) C(227) 0.025(4) 0.043(4) 0.050(5) 0.004(3) -0.012(3) -0.005(4) C(228) 0.026(4) 0.043(4) 0.045(4) -0.009(3) 0.004(3) -0.001(4) # 10. MOLECULAR GEOMETRY _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_publ_flag Ta O(2) 1.914(4) ? Ta O(1) 1.928(4) ? Ta N(3) 2.069(6) ? Ta N(4) 2.246(5) ? Ta Cl(2) 2.3787(16) ? Ta Cl(1) 2.3798(17) ? Si(1) C(128) 1.864(7) ? Si(1) C(127) 1.870(7) ? Si(1) C(121) 1.886(7) ? Si(1) C(12) 1.892(6) ? Si(2) C(227) 1.858(7) ? Si(2) C(228) 1.866(7) ? Si(2) C(221) 1.879(7) ? Si(2) C(22) 1.885(6) ? O(1) C(11) 1.375(7) ? O(2) C(21) 1.369(7) ? N(3) C(32) 1.455(9) ? N(3) C(31) 1.459(10) ? N(4) C(41) 1.472(9) ? N(4) C(42) 1.474(9) ? C(11) C(1A) 1.400(8) ? C(11) C(12) 1.426(8) ? C(12) C(13) 1.371(9) ? C(13) C(14) 1.424(9) ? C(14) C(15) 1.418(9) ? C(14) C(19) 1.433(9) ? C(15) C(16) 1.362(10) ? C(16) C(17) 1.411(11) ? C(17) C(18) 1.374(10) ? C(18) C(19) 1.405(9) ? C(19) C(1A) 1.432(9) ? C(1A) C(2A) 1.495(8) ? C(21) C(2A) 1.380(8) ? C(21) C(22) 1.429(8) ? C(22) C(23) 1.387(8) ? C(23) C(24) 1.401(9) ? C(24) C(25) 1.418(8) ? C(24) C(29) 1.424(8) ? C(25) C(26) 1.367(10) ? C(26) C(27) 1.402(9) ? C(27) C(28) 1.365(9) ? C(28) C(29) 1.431(8) ? C(29) C(2A) 1.438(8) ? C(121) C(122) 1.392(10) ? C(121) C(126) 1.399(10) ? C(122) C(123) 1.393(10) ? C(123) C(124) 1.367(11) ? C(124) C(125) 1.371(11) ? C(125) C(126) 1.389(10) ? C(221) C(222) 1.381(10) ? C(221) C(226) 1.416(10) ? C(222) C(223) 1.404(11) ? C(223) C(224) 1.376(12) ? C(224) C(225) 1.372(11) ? C(225) C(226) 1.396(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(2) Ta O(1) 87.47(19) ? O(2) Ta N(3) 93.7(2) ? O(1) Ta N(3) 96.3(2) ? O(2) Ta N(4) 89.42(19) ? O(1) Ta N(4) 87.5(2) ? N(3) Ta N(4) 175.2(2) ? O(2) Ta Cl(2) 174.09(13) ? O(1) Ta Cl(2) 90.63(13) ? N(3) Ta Cl(2) 92.1(2) ? N(4) Ta Cl(2) 84.90(16) ? O(2) Ta Cl(1) 91.46(14) ? O(1) Ta Cl(1) 173.22(14) ? N(3) Ta Cl(1) 90.5(2) ? N(4) Ta Cl(1) 85.81(18) ? Cl(2) Ta Cl(1) 89.77(6) ? C(128) Si(1) C(127) 109.4(4) ? C(128) Si(1) C(121) 111.4(3) ? C(127) Si(1) C(121) 105.1(3) ? C(128) Si(1) C(12) 113.5(3) ? C(127) Si(1) C(12) 107.0(3) ? C(121) Si(1) C(12) 110.0(3) ? C(227) Si(2) C(228) 107.7(4) ? C(227) Si(2) C(221) 106.4(3) ? C(228) Si(2) C(221) 113.5(3) ? C(227) Si(2) C(22) 108.2(3) ? C(228) Si(2) C(22) 113.3(3) ? C(221) Si(2) C(22) 107.4(3) ? C(11) O(1) Ta 127.7(4) ? C(21) O(2) Ta 135.6(4) ? C(32) N(3) C(31) 111.5(6) ? C(32) N(3) Ta 123.8(5) ? C(31) N(3) Ta 121.7(5) ? C(41) N(4) C(42) 109.2(6) ? C(41) N(4) Ta 119.3(5) ? C(42) N(4) Ta 120.7(4) ? O(1) C(11) C(1A) 118.6(5) ? O(1) C(11) C(12) 118.5(5) ? C(1A) C(11) C(12) 123.0(5) ? C(13) C(12) C(11) 117.1(5) ? C(13) C(12) Si(1) 117.7(4) ? C(11) C(12) Si(1) 125.1(5) ? C(12) C(13) C(14) 122.9(6) ? C(15) C(14) C(13) 121.6(6) ? C(15) C(14) C(19) 119.7(6) ? C(13) C(14) C(19) 118.7(6) ? C(16) C(15) C(14) 121.1(7) ? C(15) C(16) C(17) 119.2(7) ? C(18) C(17) C(16) 121.0(7) ? C(17) C(18) C(19) 121.4(6) ? C(18) C(19) C(1A) 123.2(6) ? C(18) C(19) C(14) 117.5(6) ? C(1A) C(19) C(14) 119.2(6) ? C(11) C(1A) C(19) 118.2(5) ? C(11) C(1A) C(2A) 122.6(5) ? C(19) C(1A) C(2A) 119.2(5) ? O(2) C(21) C(2A) 119.7(5) ? O(2) C(21) C(22) 117.5(5) ? C(2A) C(21) C(22) 122.7(5) ? C(23) C(22) C(21) 117.1(6) ? C(23) C(22) Si(2) 118.5(5) ? C(21) C(22) Si(2) 124.5(4) ? C(22) C(23) C(24) 123.1(5) ? C(23) C(24) C(25) 121.9(5) ? C(23) C(24) C(29) 118.5(5) ? C(25) C(24) C(29) 119.6(5) ? C(26) C(25) C(24) 121.1(6) ? C(25) C(26) C(27) 119.7(6) ? C(28) C(27) C(26) 121.0(6) ? C(27) C(28) C(29) 121.2(6) ? C(24) C(29) C(28) 117.3(5) ? C(24) C(29) C(2A) 119.8(5) ? C(28) C(29) C(2A) 122.8(5) ? C(21) C(2A) C(29) 118.2(5) ? C(21) C(2A) C(1A) 122.9(5) ? C(29) C(2A) C(1A) 118.7(5) ? C(122) C(121) C(126) 117.1(6) ? C(122) C(121) Si(1) 124.4(5) ? C(126) C(121) Si(1) 118.0(5) ? C(121) C(122) C(123) 121.4(7) ? C(124) C(123) C(122) 119.9(7) ? C(123) C(124) C(125) 120.2(7) ? C(124) C(125) C(126) 120.2(7) ? C(125) C(126) C(121) 121.1(7) ? C(222) C(221) C(226) 117.3(7) ? C(222) C(221) Si(2) 124.3(6) ? C(226) C(221) Si(2) 118.3(5) ? C(221) C(222) C(223) 121.9(8) ? C(224) C(223) C(222) 120.0(7) ? C(225) C(224) C(223) 119.2(7) ? C(224) C(225) C(226) 121.5(8) ? C(225) C(226) C(221) 120.1(7) ? data_SONX15 _database_code_CSD 203123 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C80 H70 Cl1 N2 O2 S4 Si2 Ta1' _chemical_formula_moiety 'C62 H52 Cl1 N2 O2 S4 Si2 Ta1,3(C6 H6)' _chemical_formula_structural ? _chemical_formula_weight 1492.29 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.99840(10) _cell_length_b 19.1501(3) _cell_length_c 18.4535(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.3520(10) _cell_angle_gamma 90.00 _cell_volume 3523.11(15) _cell_measurement_reflns_used 29703 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.773 _cell_measurement_temperature 150 _exptl_crystal_F_000 1524 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.2420 _exptl_absorpt_correction_T_max 0.6140 _diffrn_reflns_number 29703 _diffrn_measured_fraction_theta_max 0.9114 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9985 _reflns_number_total 15214 _reflns_friedl_coverage 0.8651 _reflns_number_gt 14575 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_max 24 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.032 _refine_ls_wR_factor_ref 0.075 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 15207 _refine_ls_number_parameters 833 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.005 _refine_diff_density_max 0.75 _refine_diff_density_min -1.39 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(4) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ta 0.208554(11) 0.501956(8) 0.241693(6) 0.02230(3) Uani ? Cl 0.16736(9) 0.39520(5) 0.30227(5) 0.0302(2) Uani ? S(1) 0.40345(9) 0.44185(5) 0.18559(5) 0.0298(2) Uani ? S(2) 0.13836(9) 0.44749(5) 0.11840(6) 0.0315(2) Uani ? S(3) 0.08994(9) 0.56451(5) 0.34342(5) 0.0294(2) Uani ? S(4) -0.04252(8) 0.51344(5) 0.21183(5) 0.0296(2) Uani ? Si(1) 0.45949(10) 0.46805(5) 0.46703(6) 0.0246(3) Uani ? Si(2) 0.22047(11) 0.65179(6) 0.04539(6) 0.0281(3) Uani ? O(1) 0.3736(2) 0.52360(13) 0.30720(14) 0.0240(6) Uani ? O(2) 0.2345(2) 0.59093(14) 0.19852(14) 0.0265(6) Uani ? N(12) 0.3229(4) 0.3639(2) 0.0680(2) 0.0373(10) Uani ? N(34) -0.1744(3) 0.57941(18) 0.3131(2) 0.0315(9) Uani ? C(12) 0.2942(4) 0.4111(2) 0.1170(2) 0.0293(9) Uani ? C(13) 0.4564(5) 0.3312(3) 0.0707(3) 0.0470(14) Uani ? C(14) 0.2229(5) 0.3406(3) 0.0119(3) 0.0454(15) Uani ? C(34) -0.0588(3) 0.5555(2) 0.2919(2) 0.0274(9) Uani ? C(35) -0.3020(4) 0.5668(3) 0.2694(3) 0.0378(10) Uani ? C(36) -0.1817(4) 0.6178(3) 0.3806(3) 0.0402(14) Uani ? C(111) 0.3790(3) 0.57565(19) 0.35755(19) 0.0216(8) Uani ? C(112) 0.3915(3) 0.55511(19) 0.4327(2) 0.0234(9) Uani ? C(113) 0.3642(4) 0.6052(3) 0.4829(3) 0.0310(10) Uani ? C(114) 0.3253(4) 0.6731(2) 0.4637(2) 0.0253(10) Uani ? C(115) 0.2825(4) 0.7208(2) 0.5157(2) 0.0308(10) Uani ? C(116) 0.2460(4) 0.7878(2) 0.4970(2) 0.0342(10) Uani ? C(117) 0.2509(4) 0.8099(2) 0.4250(2) 0.0339(10) Uani ? C(118) 0.2930(4) 0.7652(2) 0.3729(2) 0.0296(9) Uani ? C(119) 0.3309(3) 0.69519(19) 0.3901(2) 0.0250(9) Uani ? C(11A) 0.3671(3) 0.64534(19) 0.33708(19) 0.0224(8) Uani ? C(121) 0.5940(4) 0.4349(2) 0.4106(2) 0.0273(9) Uani ? C(122) 0.7296(4) 0.4514(2) 0.4260(2) 0.0312(10) Uani ? C(123) 0.8276(4) 0.4265(3) 0.3831(3) 0.0378(12) Uani ? C(124) 0.7932(4) 0.3832(3) 0.3251(3) 0.0392(14) Uani ? C(125) 0.6598(4) 0.3658(3) 0.3089(2) 0.0378(12) Uani ? C(126) 0.5623(4) 0.3918(2) 0.3507(2) 0.0310(10) Uani ? C(131) 0.3304(4) 0.3987(2) 0.4756(2) 0.0280(10) Uani ? C(132) 0.1976(4) 0.4159(2) 0.4891(2) 0.0355(10) Uani ? C(133) 0.1049(4) 0.3656(3) 0.5041(3) 0.0465(14) Uani ? C(134) 0.1396(5) 0.2956(3) 0.5036(3) 0.0501(15) Uani ? C(135) 0.2684(5) 0.2766(3) 0.4899(3) 0.0447(15) Uani ? C(136) 0.3631(5) 0.3271(3) 0.4762(3) 0.0354(12) Uani ? C(141) 0.5351(4) 0.48524(19) 0.5621(2) 0.0292(9) Uani ? C(142) 0.6177(4) 0.5428(3) 0.5799(3) 0.0402(12) Uani ? C(143) 0.6692(5) 0.5546(3) 0.6504(3) 0.0525(15) Uani ? C(144) 0.6401(5) 0.5091(4) 0.7052(2) 0.0528(14) Uani ? C(145) 0.5603(5) 0.4524(3) 0.6899(3) 0.0510(14) Uani ? C(146) 0.5082(4) 0.4399(2) 0.6188(2) 0.0373(10) Uani ? C(211) 0.3182(3) 0.64577(18) 0.19834(19) 0.0214(8) Uani ? C(212) 0.3287(3) 0.6784(2) 0.1289(2) 0.0253(9) Uani ? C(213) 0.4198(4) 0.7313(2) 0.1237(2) 0.0277(9) Uani ? C(214) 0.5037(3) 0.75390(19) 0.1849(2) 0.0265(9) Uani ? C(215) 0.6029(4) 0.8061(2) 0.1772(2) 0.0321(10) Uani ? C(216) 0.6852(4) 0.8272(2) 0.2352(2) 0.0366(12) Uani ? C(217) 0.6731(4) 0.7967(2) 0.3036(2) 0.0334(10) Uani ? C(218) 0.5776(4) 0.7467(2) 0.3131(2) 0.0289(9) Uani ? C(219) 0.4884(3) 0.72388(19) 0.2540(2) 0.0242(8) Uani ? C(21A) 0.3888(3) 0.67042(18) 0.26160(19) 0.0223(8) Uani ? C(221) 0.0419(4) 0.6374(2) 0.0668(2) 0.0344(10) Uani ? C(222) -0.0162(4) 0.6815(3) 0.1162(3) 0.0431(12) Uani ? C(223) -0.1511(5) 0.6788(3) 0.1256(4) 0.0552(19) Uani ? C(224) -0.2315(5) 0.6309(4) 0.0869(4) 0.0667(19) Uani ? C(225) -0.1764(5) 0.5861(4) 0.0396(3) 0.0638(18) Uani ? C(226) -0.0405(5) 0.5889(3) 0.0293(3) 0.0494(14) Uani ? C(231) 0.2990(4) 0.5770(2) -0.0015(2) 0.0333(10) Uani ? C(232) 0.4203(4) 0.5491(2) 0.0276(3) 0.0378(10) Uani ? C(233) 0.4893(4) 0.4993(4) -0.0100(3) 0.0507(12) Uani ? C(234) 0.4384(6) 0.4762(3) -0.0779(4) 0.0577(16) Uani ? C(235) 0.3165(5) 0.5027(4) -0.1072(3) 0.0562(14) Uani ? C(236) 0.2484(5) 0.5520(3) -0.0690(3) 0.0457(14) Uani ? C(241) 0.2137(4) 0.7289(2) -0.0194(2) 0.0328(10) Uani ? C(242) 0.2529(5) 0.7248(3) -0.0894(3) 0.0493(14) Uani ? C(243) 0.2368(6) 0.7816(3) -0.1363(3) 0.0612(19) Uani ? C(244) 0.1867(5) 0.8429(3) -0.1147(3) 0.0504(17) Uani ? C(245) 0.1502(5) 0.8486(3) -0.0448(3) 0.0566(17) Uani ? C(246) 0.1628(5) 0.7922(3) 0.0019(3) 0.0473(15) Uani ? C(901) 0.9249(6) 0.3718(4) 0.7528(4) 0.071(2) Uani ? C(902) 0.8449(7) 0.3656(4) 0.8081(4) 0.073(2) Uani ? C(903) 0.8294(8) 0.4223(6) 0.8558(4) 0.093(3) Uani ? C(904) 0.8993(8) 0.4853(4) 0.8429(4) 0.087(3) Uani ? C(905) 0.9738(7) 0.4899(5) 0.7852(5) 0.085(3) Uani ? C(906) 0.9898(6) 0.4338(4) 0.7406(4) 0.077(2) Uani ? C(911) 0.7627(10) 0.0869(6) 0.3147(5) 0.098(3) Uani ? C(912) 0.8071(10) 0.1426(6) 0.2846(5) 0.103(4) Uani ? C(913) 0.9222(12) 0.1766(6) 0.3094(8) 0.132(5) Uani ? C(914) 1.0005(8) 0.1459(9) 0.3749(9) 0.162(7) Uani ? C(915) 0.9387(10) 0.0813(7) 0.4004(6) 0.112(4) Uani ? C(916) 0.8272(8) 0.0548(6) 0.3678(5) 0.100(3) Uani ? C(921) 0.4392(7) 0.1990(3) 0.2386(4) 0.0666(19) Uani ? C(922) 0.4456(7) 0.1521(3) 0.1831(4) 0.067(2) Uani ? C(923) 0.3432(7) 0.1475(3) 0.1298(4) 0.0701(19) Uani ? C(924) 0.2328(7) 0.1902(4) 0.1324(4) 0.074(2) Uani ? C(925) 0.2248(7) 0.2373(4) 0.1881(5) 0.074(2) Uani ? C(926) 0.3302(7) 0.2421(3) 0.2417(4) 0.0673(19) Uani ? H(113) 0.3721 0.5930 0.5330 0.0370 Uiso calc H(115) 0.2791 0.7061 0.5647 0.0370 Uiso calc H(116) 0.2175 0.8190 0.5328 0.0410 Uiso calc H(117) 0.2250 0.8562 0.4119 0.0410 Uiso calc H(118) 0.2967 0.7815 0.3244 0.0360 Uiso calc H(122) 0.7552 0.4802 0.4666 0.0370 Uiso calc H(123) 0.9187 0.4395 0.3938 0.0450 Uiso calc H(124) 0.8605 0.3654 0.2965 0.0470 Uiso calc H(125) 0.6353 0.3359 0.2689 0.0460 Uiso calc H(126) 0.4711 0.3800 0.3384 0.0370 Uiso calc H(132) 0.1712 0.4636 0.4879 0.0430 Uiso calc H(133) 0.0170 0.3790 0.5149 0.0560 Uiso calc H(134) 0.0752 0.2608 0.5126 0.0600 Uiso calc H(135) 0.2926 0.2286 0.4898 0.0540 Uiso calc H(136) 0.4514 0.3131 0.4670 0.0430 Uiso calc H(13A) 0.5152 0.3532 0.1090 0.0710 Uiso calc H(13B) 0.4947 0.3373 0.0238 0.0710 Uiso calc H(13C) 0.4482 0.2812 0.0811 0.0710 Uiso calc H(142) 0.6386 0.5744 0.5427 0.0480 Uiso calc H(143) 0.7248 0.5941 0.6612 0.0630 Uiso calc H(144) 0.6758 0.5174 0.7536 0.0630 Uiso calc H(145) 0.5401 0.4214 0.7278 0.0610 Uiso calc H(146) 0.4535 0.4000 0.6087 0.0450 Uiso calc H(14A) 0.1348 0.3387 0.0318 0.0680 Uiso calc H(14B) 0.2468 0.2940 -0.0048 0.0680 Uiso calc H(14C) 0.2196 0.3733 -0.0290 0.0680 Uiso calc H(213) 0.4270 0.7535 0.0781 0.0330 Uiso calc H(215) 0.6117 0.8267 0.1310 0.0390 Uiso calc H(216) 0.7507 0.8623 0.2295 0.0440 Uiso calc H(217) 0.7316 0.8110 0.3439 0.0400 Uiso calc H(218) 0.5710 0.7269 0.3599 0.0350 Uiso calc H(222) 0.0387 0.7140 0.1437 0.0510 Uiso calc H(223) -0.1891 0.7097 0.1587 0.0660 Uiso calc H(224) -0.3249 0.6291 0.0931 0.0800 Uiso calc H(225) -0.2318 0.5528 0.0136 0.0770 Uiso calc H(226) -0.0035 0.5574 -0.0036 0.0590 Uiso calc H(232) 0.4565 0.5643 0.0740 0.0450 Uiso calc H(233) 0.5718 0.4811 0.0109 0.0610 Uiso calc H(234) 0.4861 0.4429 -0.1039 0.0690 Uiso calc H(235) 0.2799 0.4871 -0.1534 0.0670 Uiso calc H(236) 0.1648 0.5692 -0.0895 0.0550 Uiso calc H(242) 0.2913 0.6828 -0.1056 0.0590 Uiso calc H(243) 0.2617 0.7770 -0.1847 0.0730 Uiso calc H(244) 0.1769 0.8813 -0.1472 0.0600 Uiso calc H(245) 0.1160 0.8916 -0.0284 0.0680 Uiso calc H(246) 0.1359 0.7970 0.0499 0.0570 Uiso calc H(35A) -0.2835 0.5455 0.2229 0.0560 Uiso calc H(35B) -0.3490 0.6113 0.2604 0.0560 Uiso calc H(35C) -0.3583 0.5353 0.2958 0.0560 Uiso calc H(36A) -0.1110 0.6013 0.4162 0.0600 Uiso calc H(36B) -0.2695 0.6101 0.3994 0.0600 Uiso calc H(36C) -0.1693 0.6677 0.3716 0.0600 Uiso calc H(901) 0.9367 0.3330 0.7219 0.0860 Uiso calc H(902) 0.7987 0.3230 0.8149 0.0880 Uiso calc H(903) 0.7742 0.4184 0.8953 0.1110 Uiso calc H(904) 0.8933 0.5240 0.8747 0.1050 Uiso calc H(905) 1.0161 0.5329 0.7753 0.1020 Uiso calc H(906) 1.0455 0.4376 0.7013 0.0920 Uiso calc H(911) 0.6782 0.0689 0.2967 0.1180 Uiso calc H(912) 0.7570 0.1608 0.2431 0.1240 Uiso calc H(913) 0.9514 0.2176 0.2864 0.1580 Uiso calc H(914) 1.0803 0.1659 0.3971 0.1950 Uiso calc H(915) 0.9802 0.0578 0.4416 0.1340 Uiso calc H(916) 0.7944 0.0114 0.3839 0.1190 Uiso calc H(921) 0.5109 0.2018 0.2753 0.0800 Uiso calc H(922) 0.5216 0.1225 0.1816 0.0810 Uiso calc H(923) 0.3483 0.1151 0.0912 0.0840 Uiso calc H(924) 0.1616 0.1870 0.0954 0.0880 Uiso calc H(925) 0.1481 0.2664 0.1900 0.0890 Uiso calc H(926) 0.3266 0.2750 0.2801 0.0810 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02085(6) 0.02171(6) 0.02434(6) -0.00183(7) 0.00172(4) -0.00208(8) Cl 0.0316(4) 0.0256(4) 0.0337(5) -0.0034(4) 0.0040(4) 0.0022(4) S(1) 0.0261(4) 0.0350(5) 0.0284(5) 0.0004(4) 0.0020(3) -0.0057(4) S(2) 0.0262(4) 0.0354(5) 0.0325(5) -0.0014(4) -0.0009(4) -0.0077(4) S(3) 0.0230(4) 0.0327(5) 0.0328(5) -0.0020(4) 0.0034(3) -0.0069(4) S(4) 0.0236(3) 0.0329(7) 0.0322(4) -0.0017(4) 0.0015(3) -0.0024(4) Si(1) 0.0259(5) 0.0236(5) 0.0242(5) -0.0017(4) 0.0018(4) 0.0017(4) Si(2) 0.0269(5) 0.0333(6) 0.0238(5) 0.0005(4) 0.0001(4) 0.0018(5) O(1) 0.0234(11) 0.0231(12) 0.0251(12) -0.0019(9) -0.0007(9) -0.0001(9) O(2) 0.0214(11) 0.0297(14) 0.0282(13) -0.0052(10) 0.0003(10) -0.0034(11) N(12) 0.0370(18) 0.041(2) 0.0344(19) -0.0008(15) 0.0057(15) -0.0106(16) N(34) 0.0244(15) 0.0302(18) 0.0406(19) 0.0031(13) 0.0068(13) 0.0006(15) C(12) 0.0322(18) 0.0282(19) 0.0277(19) -0.0057(15) 0.0041(15) -0.0023(16) C(13) 0.043(2) 0.050(3) 0.049(3) 0.009(2) 0.010(2) -0.017(2) C(14) 0.048(3) 0.047(3) 0.041(3) -0.006(2) 0.003(2) -0.021(2) C(34) 0.0194(15) 0.0283(19) 0.036(2) 0.0031(14) 0.0117(14) 0.0011(16) C(35) 0.0196(17) 0.047(2) 0.047(2) 0.0076(16) 0.0038(16) 0.001(2) C(36) 0.032(2) 0.044(3) 0.046(3) 0.0067(19) 0.0115(18) -0.008(2) C(111) 0.0207(15) 0.0235(17) 0.0201(16) -0.0045(13) -0.0010(12) -0.0053(14) C(112) 0.0225(16) 0.0256(18) 0.0225(17) -0.0032(14) 0.0039(13) 0.0017(14) C(113) 0.036(2) 0.033(2) 0.024(2) -0.0033(18) 0.0014(17) -0.0014(17) C(114) 0.0278(19) 0.0255(19) 0.0227(19) -0.0053(15) 0.0026(15) -0.0061(15) C(115) 0.036(2) 0.030(2) 0.027(2) -0.0002(17) 0.0058(17) -0.0051(17) C(116) 0.038(2) 0.026(2) 0.039(2) 0.0001(16) 0.0046(17) -0.0119(17) C(117) 0.037(2) 0.0240(19) 0.041(2) 0.0009(16) 0.0058(17) -0.0034(17) C(118) 0.0309(18) 0.0269(19) 0.0315(19) 0.0016(15) 0.0056(15) 0.0013(16) C(119) 0.0234(16) 0.0219(17) 0.0293(19) -0.0015(13) -0.0003(14) -0.0023(15) C(11A) 0.0217(15) 0.0221(17) 0.0233(17) -0.0009(13) 0.0009(13) -0.0023(14) C(121) 0.0279(17) 0.0272(18) 0.0271(18) 0.0022(15) 0.0031(14) 0.0042(15) C(122) 0.0255(17) 0.034(2) 0.034(2) -0.0027(15) 0.0012(15) 0.0077(17) C(123) 0.0278(19) 0.039(2) 0.047(3) 0.0000(17) 0.0049(17) 0.016(2) C(124) 0.038(2) 0.040(3) 0.041(3) 0.0106(19) 0.0122(18) 0.013(2) C(125) 0.039(2) 0.044(3) 0.031(2) 0.0082(19) 0.0074(17) 0.0008(19) C(126) 0.0278(18) 0.033(2) 0.032(2) 0.0040(16) 0.0014(15) 0.0013(17) C(131) 0.0279(19) 0.029(2) 0.027(2) -0.0001(16) 0.0016(15) 0.0037(17) C(132) 0.0302(19) 0.040(2) 0.036(2) -0.0011(17) 0.0008(16) 0.0065(19) C(133) 0.032(2) 0.062(3) 0.045(3) -0.010(2) -0.0002(18) 0.014(2) C(134) 0.044(3) 0.056(3) 0.049(3) -0.022(2) -0.005(2) 0.014(2) C(135) 0.052(3) 0.037(3) 0.044(3) -0.009(2) -0.004(2) 0.002(2) C(136) 0.035(2) 0.031(2) 0.040(3) -0.0006(18) 0.0008(19) 0.0043(19) C(141) 0.0319(17) 0.029(2) 0.0265(17) 0.0007(14) 0.0005(14) 0.0020(14) C(142) 0.040(2) 0.043(3) 0.037(2) -0.0077(19) -0.0011(18) 0.0000(19) C(143) 0.045(3) 0.064(3) 0.047(3) -0.016(2) -0.007(2) -0.014(3) C(144) 0.055(2) 0.067(4) 0.034(2) 0.001(3) -0.0115(17) -0.008(3) C(145) 0.056(3) 0.062(3) 0.034(2) 0.002(3) -0.004(2) 0.005(2) C(146) 0.045(2) 0.039(2) 0.027(2) -0.0007(19) -0.0022(17) 0.0050(18) C(211) 0.0206(15) 0.0196(16) 0.0237(17) -0.0021(13) 0.0006(13) 0.0003(13) C(212) 0.0240(16) 0.0266(18) 0.0253(17) 0.0030(14) 0.0024(13) 0.0026(15) C(213) 0.0311(18) 0.0271(18) 0.0251(18) -0.0020(15) 0.0041(14) 0.0049(15) C(214) 0.0253(17) 0.0247(18) 0.0298(19) 0.0025(14) 0.0042(14) 0.0012(15) C(215) 0.0325(19) 0.0272(19) 0.037(2) -0.0048(16) 0.0048(16) 0.0055(17) C(216) 0.0267(18) 0.033(2) 0.050(3) -0.0070(16) 0.0028(17) 0.0031(18) C(217) 0.0296(18) 0.035(2) 0.035(2) -0.0061(16) -0.0015(16) -0.0024(17) C(218) 0.0265(17) 0.0257(18) 0.034(2) -0.0043(14) -0.0015(15) -0.0003(16) C(219) 0.0215(15) 0.0225(17) 0.0286(18) 0.0004(13) 0.0012(13) 0.0008(14) C(21A) 0.0219(15) 0.0201(16) 0.0250(17) -0.0018(13) 0.0016(13) -0.0028(14) C(221) 0.0305(19) 0.039(2) 0.033(2) 0.0021(17) -0.0030(16) 0.0087(18) C(222) 0.035(2) 0.042(2) 0.053(3) 0.0059(19) 0.0072(19) 0.007(2) C(223) 0.038(3) 0.059(4) 0.071(4) 0.018(2) 0.020(3) 0.019(3) C(224) 0.024(2) 0.101(5) 0.074(4) 0.000(3) -0.004(2) 0.035(4) C(225) 0.035(2) 0.098(5) 0.056(3) -0.020(3) -0.013(2) 0.013(3) C(226) 0.038(2) 0.070(4) 0.039(2) -0.017(2) -0.0042(19) 0.005(2) C(231) 0.0343(19) 0.036(2) 0.030(2) -0.0006(17) 0.0054(16) -0.0027(17) C(232) 0.034(2) 0.034(2) 0.046(2) -0.0022(17) 0.0073(18) -0.0032(19) C(233) 0.0402(19) 0.038(2) 0.076(3) -0.006(3) 0.0179(19) -0.014(4) C(234) 0.060(3) 0.038(2) 0.079(4) -0.009(2) 0.031(3) -0.018(3) C(235) 0.072(3) 0.050(3) 0.048(2) -0.011(4) 0.014(2) -0.020(4) C(236) 0.051(3) 0.046(3) 0.040(2) -0.005(2) 0.003(2) -0.007(2) C(241) 0.0279(18) 0.040(2) 0.030(2) 0.0007(17) -0.0020(15) 0.0045(17) C(242) 0.065(3) 0.049(3) 0.035(2) -0.009(2) 0.011(2) 0.005(2) C(243) 0.088(4) 0.059(4) 0.038(3) -0.017(3) 0.013(3) 0.013(3) C(244) 0.044(3) 0.056(4) 0.050(3) -0.006(2) -0.005(2) 0.023(3) C(245) 0.052(3) 0.053(3) 0.065(4) 0.021(2) 0.006(3) 0.019(3) C(246) 0.052(3) 0.051(3) 0.040(3) 0.014(2) 0.010(2) 0.011(2) C(901) 0.059(3) 0.072(4) 0.080(5) 0.001(3) -0.015(3) -0.002(4) C(902) 0.069(4) 0.072(4) 0.077(5) -0.007(3) -0.005(3) 0.015(4) C(903) 0.083(5) 0.135(8) 0.060(4) 0.027(5) -0.003(4) 0.024(5) C(904) 0.099(5) 0.083(7) 0.073(5) 0.011(4) -0.040(4) -0.013(4) C(905) 0.068(4) 0.080(7) 0.101(5) -0.009(4) -0.027(4) 0.011(5) C(906) 0.050(3) 0.087(5) 0.090(5) -0.001(3) -0.012(3) 0.012(4) C(911) 0.114(6) 0.116(8) 0.067(5) 0.018(6) 0.026(5) 0.009(5) C(912) 0.108(7) 0.128(9) 0.078(5) 0.000(6) 0.030(5) 0.014(6) C(913) 0.115(8) 0.087(7) 0.204(14) -0.007(6) 0.085(8) -0.014(8) C(914) 0.046(4) 0.218(16) 0.226(16) 0.008(7) 0.028(7) -0.124(13) C(915) 0.084(6) 0.153(10) 0.098(7) 0.026(6) 0.001(5) -0.024(7) C(916) 0.083(5) 0.139(8) 0.079(5) 0.043(5) 0.019(4) -0.008(5) C(921) 0.079(4) 0.049(3) 0.073(4) -0.003(3) 0.014(3) -0.006(3) C(922) 0.077(4) 0.040(3) 0.088(5) 0.005(3) 0.024(4) -0.001(3) C(923) 0.091(4) 0.047(3) 0.074(4) -0.009(3) 0.018(4) -0.016(3) C(924) 0.070(4) 0.060(4) 0.089(5) -0.014(3) -0.005(4) -0.001(4) C(925) 0.063(4) 0.054(4) 0.107(6) -0.003(3) 0.020(4) -0.008(4) C(926) 0.083(4) 0.046(3) 0.076(4) -0.004(3) 0.027(4) -0.006(3) # 10. MOLECULAR GEOMETRY _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_publ_flag Ta O(2) 1.907(3) YES Ta O(1) 2.014(2) YES Ta Cl 2.3809(9) YES Ta S(4) 2.5385(8) YES Ta S(1) 2.5495(9) YES Ta S(2) 2.5523(10) YES Ta S(3) 2.5891(10) YES S(1) C(12) 1.713(4) YES S(2) C(12) 1.709(4) YES S(3) C(34) 1.712(4) YES S(4) C(34) 1.701(4) YES Si(1) C(131) 1.868(5) YES Si(1) C(121) 1.873(4) YES Si(1) C(141) 1.886(4) YES Si(1) C(112) 1.891(4) YES Si(2) C(231) 1.876(4) YES Si(2) C(221) 1.878(4) YES Si(2) C(212) 1.885(4) YES Si(2) C(241) 1.898(4) YES O(1) C(111) 1.361(4) YES O(2) C(211) 1.344(4) YES N(12) C(12) 1.325(5) YES N(12) C(14) 1.454(6) YES N(12) C(13) 1.472(6) YES N(34) C(34) 1.330(5) YES N(34) C(36) 1.452(6) YES N(34) C(35) 1.477(5) YES C(111) C(11A) 1.390(5) YES C(111) C(112) 1.438(5) YES C(112) C(113) 1.375(6) YES C(113) C(114) 1.397(7) YES C(114) C(115) 1.415(6) YES C(114) C(119) 1.426(6) YES C(115) C(116) 1.370(6) YES C(116) C(117) 1.400(6) YES C(117) C(118) 1.376(6) YES C(118) C(119) 1.423(5) YES C(119) C(11A) 1.433(5) YES C(11A) C(21A) 1.504(5) YES C(121) C(126) 1.397(6) YES C(121) C(122) 1.400(5) YES C(122) C(123) 1.389(6) YES C(123) C(124) 1.376(7) YES C(124) C(125) 1.386(6) YES C(125) C(126) 1.381(6) YES C(131) C(132) 1.408(6) YES C(131) C(136) 1.409(7) YES C(132) C(133) 1.379(6) YES C(133) C(134) 1.386(8) YES C(134) C(135) 1.380(8) YES C(135) C(136) 1.390(7) YES C(141) C(142) 1.402(6) YES C(141) C(146) 1.402(6) YES C(142) C(143) 1.380(6) YES C(143) C(144) 1.383(9) YES C(144) C(145) 1.364(9) YES C(145) C(146) 1.396(6) YES C(211) C(21A) 1.399(5) YES C(211) C(212) 1.436(5) YES C(212) C(213) 1.371(5) YES C(213) C(214) 1.422(5) YES C(214) C(219) 1.418(5) YES C(214) C(215) 1.423(5) YES C(215) C(216) 1.361(6) YES C(216) C(217) 1.404(6) YES C(217) C(218) 1.373(5) YES C(218) C(219) 1.424(5) YES C(219) C(21A) 1.443(5) YES C(221) C(226) 1.390(7) YES C(221) C(222) 1.402(7) YES C(222) C(223) 1.374(7) YES C(223) C(224) 1.382(9) YES C(224) C(225) 1.368(10) YES C(225) C(226) 1.388(7) YES C(231) C(236) 1.394(6) YES C(231) C(232) 1.394(6) YES C(232) C(233) 1.392(7) YES C(233) C(234) 1.388(8) YES C(234) C(235) 1.391(8) YES C(235) C(236) 1.386(8) YES C(241) C(242) 1.380(6) YES C(241) C(246) 1.382(7) YES C(242) C(243) 1.391(8) YES C(243) C(244) 1.349(9) YES C(244) C(245) 1.371(8) YES C(245) C(246) 1.382(7) YES C(901) C(902) 1.348(10) YES C(901) C(906) 1.381(10) YES C(902) C(903) 1.413(12) YES C(903) C(904) 1.424(12) YES C(904) C(905) 1.347(11) YES C(905) C(906) 1.370(12) YES C(911) C(916) 1.288(11) YES C(911) C(912) 1.295(13) YES C(912) C(913) 1.371(14) YES C(913) C(914) 1.507(18) YES C(914) C(915) 1.477(19) YES C(915) C(916) 1.326(12) YES C(921) C(922) 1.368(9) YES C(921) C(926) 1.372(9) YES C(922) C(923) 1.367(9) YES C(923) C(924) 1.377(9) YES C(924) C(925) 1.375(10) YES C(925) C(926) 1.393(10) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(2) Ta O(1) 86.32(10) YES O(2) Ta Cl 175.73(8) YES O(1) Ta Cl 93.32(7) YES O(2) Ta S(4) 89.73(8) YES O(1) Ta S(4) 149.83(8) YES Cl Ta S(4) 88.45(3) YES O(2) Ta S(1) 95.83(8) YES O(1) Ta S(1) 73.73(7) YES Cl Ta S(1) 88.15(3) YES S(4) Ta S(1) 136.45(3) YES O(2) Ta S(2) 91.70(8) YES O(1) Ta S(2) 140.96(8) YES Cl Ta S(2) 91.26(3) YES S(4) Ta S(2) 68.99(3) YES S(1) Ta S(2) 67.70(3) YES O(2) Ta S(3) 88.49(8) YES O(1) Ta S(3) 82.48(7) YES Cl Ta S(3) 87.24(3) YES S(4) Ta S(3) 67.51(3) YES S(1) Ta S(3) 155.45(3) YES S(2) Ta S(3) 136.49(3) YES C(12) S(1) Ta 89.49(14) YES C(12) S(2) Ta 89.48(13) YES C(34) S(3) Ta 88.68(13) YES C(34) S(4) Ta 90.61(12) YES C(131) Si(1) C(121) 109.63(19) YES C(131) Si(1) C(141) 106.04(18) YES C(121) Si(1) C(141) 108.78(17) YES C(131) Si(1) C(112) 114.99(17) YES C(121) Si(1) C(112) 111.58(17) YES C(141) Si(1) C(112) 105.42(16) YES C(231) Si(2) C(221) 115.0(2) YES C(231) Si(2) C(212) 110.41(17) YES C(221) Si(2) C(212) 111.35(18) YES C(231) Si(2) C(241) 107.5(2) YES C(221) Si(2) C(241) 104.91(18) YES C(212) Si(2) C(241) 107.18(18) YES C(111) O(1) Ta 123.3(2) YES C(211) O(2) Ta 143.5(2) YES C(12) N(12) C(14) 121.5(4) YES C(12) N(12) C(13) 120.7(4) YES C(14) N(12) C(13) 117.8(4) YES C(34) N(34) C(36) 121.8(3) YES C(34) N(34) C(35) 121.1(4) YES C(36) N(34) C(35) 117.0(3) YES N(12) C(12) S(2) 122.2(3) YES N(12) C(12) S(1) 125.4(3) YES S(2) C(12) S(1) 112.3(2) YES N(34) C(34) S(4) 124.1(3) YES N(34) C(34) S(3) 122.7(3) YES S(4) C(34) S(3) 113.19(19) YES O(1) C(111) C(11A) 121.3(3) YES O(1) C(111) C(112) 117.0(3) YES C(11A) C(111) C(112) 121.6(3) YES C(113) C(112) C(111) 116.9(4) YES C(113) C(112) Si(1) 118.3(3) YES C(111) C(112) Si(1) 124.5(3) YES C(112) C(113) C(114) 122.9(4) YES C(113) C(114) C(115) 121.4(4) YES C(113) C(114) C(119) 119.2(4) YES C(115) C(114) C(119) 119.4(4) YES C(116) C(115) C(114) 121.4(4) YES C(115) C(116) C(117) 119.6(4) YES C(118) C(117) C(116) 120.7(4) YES C(117) C(118) C(119) 121.3(4) YES C(118) C(119) C(114) 117.6(4) YES C(118) C(119) C(11A) 123.5(4) YES C(114) C(119) C(11A) 118.9(3) YES C(111) C(11A) C(119) 118.3(3) YES C(111) C(11A) C(21A) 122.9(3) YES C(119) C(11A) C(21A) 118.8(3) YES C(126) C(121) C(122) 116.8(4) YES C(126) C(121) Si(1) 120.7(3) YES C(122) C(121) Si(1) 122.4(3) YES C(123) C(122) C(121) 121.4(4) YES C(124) C(123) C(122) 120.3(4) YES C(123) C(124) C(125) 119.5(4) YES C(126) C(125) C(124) 120.0(4) YES C(125) C(126) C(121) 121.9(4) YES C(132) C(131) C(136) 116.6(4) YES C(132) C(131) Si(1) 121.0(3) YES C(136) C(131) Si(1) 122.1(3) YES C(133) C(132) C(131) 121.9(4) YES C(132) C(133) C(134) 120.1(5) YES C(135) C(134) C(133) 119.6(5) YES C(134) C(135) C(136) 120.5(5) YES C(135) C(136) C(131) 121.1(5) YES C(142) C(141) C(146) 117.1(4) YES C(142) C(141) Si(1) 122.9(3) YES C(146) C(141) Si(1) 120.0(3) YES C(143) C(142) C(141) 121.4(5) YES C(142) C(143) C(144) 120.1(5) YES C(145) C(144) C(143) 120.2(4) YES C(144) C(145) C(146) 120.1(5) YES C(145) C(146) C(141) 121.1(4) YES O(2) C(211) C(21A) 122.4(3) YES O(2) C(211) C(212) 115.5(3) YES C(21A) C(211) C(212) 122.1(3) YES C(213) C(212) C(211) 118.6(3) YES C(213) C(212) Si(2) 119.1(3) YES C(211) C(212) Si(2) 122.4(3) YES C(212) C(213) C(214) 121.6(3) YES C(219) C(214) C(213) 119.6(3) YES C(219) C(214) C(215) 119.8(3) YES C(213) C(214) C(215) 120.6(4) YES C(216) C(215) C(214) 121.0(4) YES C(215) C(216) C(217) 119.7(4) YES C(218) C(217) C(216) 120.8(4) YES C(217) C(218) C(219) 121.1(4) YES C(214) C(219) C(218) 117.4(3) YES C(214) C(219) C(21A) 119.8(3) YES C(218) C(219) C(21A) 122.7(3) YES C(211) C(21A) C(219) 117.8(3) YES C(211) C(21A) C(11A) 124.5(3) YES C(219) C(21A) C(11A) 117.8(3) YES C(226) C(221) C(222) 117.9(4) YES C(226) C(221) Si(2) 122.0(4) YES C(222) C(221) Si(2) 119.7(3) YES C(223) C(222) C(221) 121.2(5) YES C(222) C(223) C(224) 119.9(6) YES C(225) C(224) C(223) 120.0(5) YES C(224) C(225) C(226) 120.6(6) YES C(225) C(226) C(221) 120.5(6) YES C(236) C(231) C(232) 117.3(4) YES C(236) C(231) Si(2) 122.5(3) YES C(232) C(231) Si(2) 119.8(3) YES C(233) C(232) C(231) 121.4(4) YES C(234) C(233) C(232) 120.3(5) YES C(233) C(234) C(235) 119.1(5) YES C(236) C(235) C(234) 120.0(5) YES C(235) C(236) C(231) 121.9(5) YES C(242) C(241) C(246) 116.9(4) YES C(242) C(241) Si(2) 123.1(4) YES C(246) C(241) Si(2) 120.0(3) YES C(241) C(242) C(243) 120.7(5) YES C(244) C(243) C(242) 121.6(5) YES C(243) C(244) C(245) 118.7(5) YES C(244) C(245) C(246) 120.3(6) YES C(245) C(246) C(241) 121.8(5) YES C(902) C(901) C(906) 120.8(8) YES C(901) C(902) C(903) 120.2(7) YES C(902) C(903) C(904) 117.9(7) YES C(905) C(904) C(903) 119.7(8) YES C(904) C(905) C(906) 121.4(9) YES C(905) C(906) C(901) 119.9(8) YES C(916) C(911) C(912) 123.4(11) YES C(911) C(912) C(913) 123.7(11) YES C(912) C(913) C(914) 117.0(11) YES C(915) C(914) C(913) 112.2(9) YES C(916) C(915) C(914) 122.2(11) YES C(911) C(916) C(915) 121.2(12) YES C(922) C(921) C(926) 120.6(7) YES C(923) C(922) C(921) 120.3(6) YES C(922) C(923) C(924) 119.8(6) YES C(925) C(924) C(923) 120.5(7) YES C(924) C(925) C(926) 119.4(6) YES C(921) C(926) C(925) 119.4(6) YES