Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Ian Rothwell' _publ_contact_author_address ; Prof Ian Rothwell Department of Chemistry Purdue University 1393 Brown Building West Lafayette IN 47907-1393 UNITED STATES OF AMERICA ; _publ_contact_author_email 'rothwell@purdue.edu' _publ_requested_journal 'Dalton Transactions' _publ_requested_category ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Studies of the alkylation of niobium and tantalum halides containing 2,6-diarylphenoxide ancillary ligation ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name 'Fanwick, P.' 'Freeman, Emily E.' 'Pulvirenti, April L.' 'Rothwell, Ian' 'Salberg, Michelle M.' 'Schweiger, Scott W.' # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Hall S.R. & du Boulay, D. (1995) Editors U. of Western Aurtralia Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1996). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXS97, Program for the Solution of Crystal Structures. Univ. of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of G\"ottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; #====================================================================== data_MMS240 _database_code_CSD 159022 _audit_creation_date 16-12-98 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour dark _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C72 H54 O2 Nb I3' _chemical_formula_structural ? _chemical_formula_weight 1424.85 _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 25.7491(8) _cell_length_b 7.9562(3) _cell_length_c 19.5543(6) _cell_angle_alpha 90.00 _cell_angle_beta 125.8090(16) _cell_angle_gamma 90.00 _cell_volume 3248.7(4) _cell_measurement_reflns_used 14265 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.628 _cell_measurement_temperature 203 _exptl_crystal_F_000 1236 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.6091 _exptl_absorpt_correction_T_max 0.7521 _diffrn_reflns_number 14265 _reflns_number_total 5623 _reflns_number_gt 5456 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.50 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_max 27 # 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 0.051 _refine_ls_wR_factor_ref 0.139 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 5623 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+30.1281P] where P=(Fo^2^+2Fc^2^)/' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.61 _refine_diff_density_min -0.89 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.20E-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 Direct_methods_(Shelxs97,_Sheldrick,_1997) _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 ; refinement results for the other absolute structure: R = 0.000 Rw = 0.000 goodness_of_fit = 0.000 ; # 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 I(2) 0.59905(3) 0.97632(8) 0.06983(3) 0.0399(2) Uani ? I(3) 0.5000 0.42402(9) 0.0000 0.0398(4) Uani ? Nb(1) 0.5000 0.76466(11) 0.0000 0.0150(3) Uani ? O(1) 0.5027(2) 0.7527(7) 0.0980(3) 0.0157(16) Uani ? C(11) 0.5041(3) 0.7467(10) 0.1694(4) 0.016(3) Uani ? C(12) 0.5644(3) 0.7618(10) 0.2494(4) 0.015(3) Uani ? C(13) 0.5643(3) 0.7831(9) 0.3201(4) 0.019(3) Uani ? C(14) 0.5064(3) 0.7837(10) 0.3110(4) 0.019(3) Uani ? C(15) 0.4479(3) 0.7573(11) 0.2338(4) 0.019(3) Uani ? C(16) 0.4459(3) 0.7375(9) 0.1608(4) 0.015(3) Uani ? C(121) 0.6244(3) 0.7603(11) 0.2549(4) 0.017(2) Uani ? C(122) 0.6374(4) 0.6233(10) 0.2227(5) 0.023(3) Uani ? C(123) 0.6952(4) 0.6198(12) 0.2298(5) 0.033(4) Uani ? C(124) 0.7394(4) 0.7507(13) 0.2700(5) 0.035(3) Uani ? C(125) 0.7269(4) 0.8848(13) 0.3031(5) 0.033(3) Uani ? C(126) 0.6689(3) 0.8911(11) 0.2953(4) 0.025(3) Uani ? C(131) 0.6248(3) 0.8012(9) 0.4079(4) 0.021(3) Uani ? C(132) 0.6308(4) 0.9392(11) 0.4572(5) 0.031(3) Uani ? C(133) 0.6858(4) 0.9513(14) 0.5399(5) 0.041(4) Uani ? C(134) 0.7324(4) 0.8325(16) 0.5729(5) 0.044(4) Uani ? C(135) 0.7272(4) 0.6967(15) 0.5246(6) 0.043(4) Uani ? C(136) 0.6725(4) 0.6821(12) 0.4412(5) 0.030(3) Uani ? C(151) 0.3898(3) 0.7476(11) 0.2341(4) 0.024(3) Uani ? C(152) 0.3453(4) 0.6202(11) 0.1945(5) 0.028(3) Uani ? C(153) 0.2932(4) 0.6149(15) 0.2000(6) 0.036(4) Uani ? C(154) 0.2862(4) 0.7332(14) 0.2433(7) 0.048(4) Uani ? C(155) 0.3300(4) 0.8625(13) 0.2838(5) 0.036(4) Uani ? C(156) 0.3822(3) 0.8726(11) 0.2781(5) 0.026(3) Uani ? C(161) 0.3838(3) 0.7047(11) 0.0766(4) 0.021(3) Uani ? C(162) 0.3756(4) 0.5548(11) 0.0358(5) 0.029(3) Uani ? C(163) 0.3157(5) 0.5211(15) -0.0404(6) 0.047(4) Uani ? C(164) 0.2667(4) 0.6316(17) -0.0728(6) 0.051(4) Uani ? C(165) 0.2737(4) 0.7748(18) -0.0317(6) 0.049(4) Uani ? C(166) 0.3335(4) 0.8163(11) 0.0436(5) 0.030(3) Uani ? C(901) 0.0342(9) 0.7104(18) 0.2136(10) 0.069(9) Uani ? C(902) -0.0308(9) 0.6818(15) 0.1707(8) 0.069(7) Uani ? C(903) -0.0604(6) 0.7272(18) 0.2080(9) 0.067(6) Uani ? C(904) -0.0263(10) 0.8023(16) 0.2850(13) 0.080(11) Uani ? C(905) 0.0371(8) 0.8374(18) 0.3260(9) 0.071(7) Uani ? C(906) 0.0676(7) 0.7864(18) 0.2890(12) 0.073(8) Uani ? H(14) 0.5070 0.8024 0.3583 0.0250 Uiso calc H(122) 0.6083 0.5352 0.1968 0.0300 Uiso calc H(123) 0.7039 0.5299 0.2075 0.0420 Uiso calc H(124) 0.7774 0.7475 0.2745 0.0450 Uiso calc H(125) 0.7567 0.9710 0.3305 0.0430 Uiso calc H(126) 0.6603 0.9821 0.3170 0.0320 Uiso calc H(132) 0.5989 1.0204 0.4352 0.0390 Uiso calc H(133) 0.6906 1.0424 0.5730 0.0540 Uiso calc H(134) 0.7683 0.8421 0.6285 0.0580 Uiso calc H(135) 0.7596 0.6166 0.5472 0.0550 Uiso calc H(136) 0.6684 0.5916 0.4083 0.0400 Uiso calc H(152) 0.3497 0.5382 0.1643 0.0360 Uiso calc H(153) 0.2634 0.5287 0.1735 0.0460 Uiso calc H(154) 0.2513 0.7280 0.2459 0.0620 Uiso calc H(155) 0.3252 0.9421 0.3145 0.0480 Uiso calc H(156) 0.4112 0.9611 0.3033 0.0340 Uiso calc H(162) 0.4090 0.4778 0.0582 0.0370 Uiso calc H(163) 0.3097 0.4213 -0.0690 0.0610 Uiso calc H(164) 0.2279 0.6082 -0.1239 0.0670 Uiso calc H(165) 0.2390 0.8468 -0.0529 0.0630 Uiso calc H(166) 0.3390 0.9179 0.0706 0.0380 Uiso calc H(901) 0.0549 0.6764 0.1899 0.0900 Uiso calc H(902) -0.0542 0.6327 0.1175 0.0900 Uiso calc H(903) -0.1039 0.7065 0.1804 0.0870 Uiso calc H(904) -0.0467 0.8301 0.3101 0.1040 Uiso calc H(905) 0.0597 0.8939 0.3774 0.0930 Uiso calc H(906) 0.1112 0.8055 0.3169 0.0950 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 I(2) 0.0362(3) 0.0505(4) 0.0316(3) -0.0087(3) 0.0190(2) -0.0030(3) I(3) 0.0558(5) 0.0333(5) 0.0394(4) 0.0000 0.0330(4) 0.0000 Nb(1) 0.0141(4) 0.0252(4) 0.0073(4) 0.0000 0.0072(3) 0.0000 O(1) 0.012(2) 0.026(2) 0.010(2) 0.000(2) 0.0069(17) 0.002(2) C(11) 0.016(3) 0.028(4) 0.007(3) 0.002(3) 0.009(3) -0.003(3) C(12) 0.013(3) 0.025(3) 0.008(3) 0.006(3) 0.006(3) 0.002(3) C(13) 0.016(3) 0.027(4) 0.008(3) 0.001(3) 0.004(3) -0.003(3) C(14) 0.021(4) 0.031(4) 0.011(3) 0.005(3) 0.012(3) -0.001(3) C(15) 0.015(3) 0.033(4) 0.014(3) 0.002(3) 0.011(3) 0.001(3) C(16) 0.010(3) 0.023(4) 0.011(3) 0.001(3) 0.006(3) 0.003(3) C(121) 0.013(3) 0.032(4) 0.005(3) 0.003(3) 0.004(2) 0.003(3) C(122) 0.020(3) 0.033(5) 0.018(3) 0.005(3) 0.013(3) 0.001(3) C(123) 0.031(4) 0.046(5) 0.031(4) 0.018(4) 0.024(4) 0.011(4) C(124) 0.020(4) 0.055(5) 0.033(4) 0.016(4) 0.018(3) 0.025(4) C(125) 0.020(3) 0.056(6) 0.023(4) -0.004(4) 0.012(3) 0.007(4) C(126) 0.024(3) 0.036(4) 0.015(3) -0.004(3) 0.012(3) -0.002(3) C(131) 0.017(4) 0.038(5) 0.006(3) 0.001(3) 0.005(3) 0.004(3) C(132) 0.029(4) 0.041(5) 0.014(3) -0.007(3) 0.008(3) 0.000(3) C(133) 0.044(5) 0.062(6) 0.017(4) -0.021(5) 0.018(4) -0.014(4) C(134) 0.021(4) 0.087(7) 0.009(4) -0.006(4) 0.000(3) 0.000(4) C(135) 0.023(4) 0.076(7) 0.022(4) 0.010(4) 0.009(3) 0.004(5) C(136) 0.024(4) 0.050(5) 0.019(4) 0.011(4) 0.014(3) 0.008(4) C(151) 0.023(3) 0.041(5) 0.016(3) 0.006(4) 0.016(3) 0.009(3) C(152) 0.028(4) 0.036(5) 0.031(4) -0.004(3) 0.024(3) -0.004(4) C(153) 0.026(4) 0.053(6) 0.035(4) 0.000(4) 0.022(4) 0.009(5) C(154) 0.027(4) 0.060(7) 0.064(6) 0.015(4) 0.031(4) 0.026(6) C(155) 0.038(4) 0.051(5) 0.041(5) 0.018(4) 0.035(4) 0.011(4) C(156) 0.022(3) 0.041(5) 0.025(4) 0.007(3) 0.019(3) 0.003(4) C(161) 0.013(3) 0.039(4) 0.010(3) -0.006(3) 0.007(3) -0.002(3) C(162) 0.022(4) 0.047(5) 0.020(3) -0.010(3) 0.014(3) -0.007(3) C(163) 0.042(5) 0.075(7) 0.025(4) -0.035(5) 0.021(4) -0.027(5) C(164) 0.022(4) 0.103(10) 0.017(4) -0.019(5) 0.006(4) -0.005(5) C(165) 0.017(4) 0.100(9) 0.024(4) 0.003(5) 0.009(4) 0.014(5) C(166) 0.017(4) 0.049(5) 0.021(4) 0.001(3) 0.010(3) 0.007(3) C(901) 0.112(12) 0.052(7) 0.084(10) 0.029(8) 0.080(10) 0.025(7) C(902) 0.107(12) 0.033(6) 0.043(7) 0.006(7) 0.030(7) 0.004(5) C(903) 0.050(6) 0.064(8) 0.070(8) -0.008(6) 0.026(6) 0.010(7) C(904) 0.114(13) 0.054(8) 0.118(14) 0.029(8) 0.093(13) 0.024(8) C(905) 0.090(10) 0.054(7) 0.060(8) 0.002(7) 0.038(7) -0.002(7) C(906) 0.060(8) 0.060(8) 0.100(12) 0.002(6) 0.047(8) 0.018(7) # 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 Nb(1) O(1) 1.879(4) ? Nb(1) O(1) 1.879(4) ? Nb(1) I(2) 2.6701(8) ? Nb(1) I(2) 2.6702(8) ? Nb(1) I(3) 2.7102(11) ? O(1) C(11) 1.375(7) ? C(11) C(16) 1.410(9) ? C(11) C(12) 1.425(9) ? C(12) C(13) 1.395(9) ? C(12) C(121) 1.484(9) ? C(13) C(14) 1.392(10) ? C(13) C(131) 1.506(9) ? C(14) C(15) 1.390(10) ? C(15) C(16) 1.405(9) ? C(15) C(151) 1.501(9) ? C(16) C(161) 1.501(9) ? C(121) C(122) 1.394(11) ? C(121) C(126) 1.401(11) ? C(122) C(123) 1.412(11) ? C(123) C(124) 1.397(15) ? C(124) C(125) 1.381(14) ? C(125) C(126) 1.409(10) ? C(131) C(136) 1.377(11) ? C(131) C(132) 1.408(11) ? C(132) C(133) 1.396(11) ? C(133) C(134) 1.358(16) ? C(134) C(135) 1.389(16) ? C(135) C(136) 1.403(12) ? C(151) C(152) 1.378(12) ? C(151) C(156) 1.402(12) ? C(152) C(153) 1.408(11) ? C(153) C(154) 1.347(16) ? C(154) C(155) 1.383(16) ? C(155) C(156) 1.413(10) ? C(161) C(166) 1.379(12) ? C(161) C(162) 1.381(12) ? C(162) C(163) 1.408(11) ? C(163) C(164) 1.353(17) ? C(164) C(165) 1.344(18) ? C(166) C(165) 1.412(12) ? C(901) C(906) 1.34(2) ? C(901) C(902) 1.38(2) ? C(903) C(904) 1.36(2) ? C(903) C(902) 1.37(2) ? C(905) C(904) 1.36(2) ? C(905) C(906) 1.40(2) ? 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) Nb(1) O(1) 174.2(3) ? O(1) Nb(1) I(2) 93.21(14) ? O(1) Nb(1) I(2) 90.45(14) ? O(1) Nb(1) I(2) 90.45(14) ? O(1) Nb(1) I(2) 93.21(14) ? I(2) Nb(1) I(2) 101.80(4) ? O(1) Nb(1) I(3) 87.09(16) ? O(1) Nb(1) I(3) 87.09(16) ? I(2) Nb(1) I(3) 129.10(2) ? I(2) Nb(1) I(3) 129.10(2) ? C(11) O(1) Nb(1) 178.9(5) ? O(1) C(11) C(16) 119.2(6) ? O(1) C(11) C(12) 118.4(6) ? C(16) C(11) C(12) 122.3(6) ? C(13) C(12) C(11) 117.7(6) ? C(13) C(12) C(121) 122.4(6) ? C(11) C(12) C(121) 119.9(5) ? C(12) C(13) C(14) 119.8(6) ? C(12) C(13) C(131) 122.8(6) ? C(14) C(13) C(131) 117.4(6) ? C(15) C(14) C(13) 122.5(6) ? C(14) C(15) C(16) 119.4(6) ? C(14) C(15) C(151) 117.0(6) ? C(16) C(15) C(151) 123.6(6) ? C(15) C(16) C(11) 118.0(6) ? C(15) C(16) C(161) 121.1(6) ? C(11) C(16) C(161) 121.0(6) ? C(122) C(121) C(126) 120.1(6) ? C(122) C(121) C(12) 119.3(7) ? C(126) C(121) C(12) 120.6(7) ? C(121) C(122) C(123) 119.3(8) ? C(124) C(123) C(122) 120.4(8) ? C(125) C(124) C(123) 120.2(7) ? C(124) C(125) C(126) 120.0(8) ? C(121) C(126) C(125) 120.0(7) ? C(136) C(131) C(132) 120.1(7) ? C(136) C(131) C(13) 121.0(7) ? C(132) C(131) C(13) 118.8(7) ? C(133) C(132) C(131) 118.6(8) ? C(134) C(133) C(132) 121.2(9) ? C(133) C(134) C(135) 120.7(8) ? C(134) C(135) C(136) 119.1(9) ? C(131) C(136) C(135) 120.3(8) ? C(152) C(151) C(156) 119.9(7) ? C(152) C(151) C(15) 122.5(7) ? C(156) C(151) C(15) 117.6(7) ? C(151) C(152) C(153) 119.6(8) ? C(154) C(153) C(152) 120.8(9) ? C(153) C(154) C(155) 121.0(8) ? C(154) C(155) C(156) 119.4(8) ? C(151) C(156) C(155) 119.2(8) ? C(166) C(161) C(162) 120.1(7) ? C(166) C(161) C(16) 120.5(7) ? C(162) C(161) C(16) 119.2(7) ? C(161) C(162) C(163) 118.6(8) ? C(164) C(163) C(162) 121.0(10) ? C(165) C(164) C(163) 120.6(8) ? C(161) C(166) C(165) 119.3(9) ? C(164) C(165) C(166) 120.3(10) ? C(906) C(901) C(902) 120.8(13) ? C(904) C(903) C(902) 120.3(13) ? C(903) C(902) C(901) 118.9(12) ? C(904) C(905) C(906) 118.4(15) ? C(901) C(906) C(905) 120.4(14) ? C(905) C(904) C(903) 121.2(14) ? #===END #============================================================================== data_SS287 _database_code_CSD 164008 _audit_creation_date 1-10-99 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C72 H54 Br3 O2 Ta' _chemical_formula_structural ? _chemical_formula_weight 1371.91 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5985(7) _cell_length_b 13.8730(8) _cell_length_c 17.8161(6) _cell_angle_alpha 87.288(3) _cell_angle_beta 73.317(3) _cell_angle_gamma 76.722(2) _cell_volume 2902.5(4) _cell_measurement_reflns_used 22999 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.962 _cell_measurement_temperature 193 _exptl_crystal_F_000 1360 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.2154 _exptl_absorpt_correction_T_max 0.2760 _diffrn_reflns_number 22999 _reflns_number_total 12171 _reflns_number_gt 9608 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 18 _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 0.043 _refine_ls_wR_factor_ref 0.098 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 12171 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+2.0207P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.008 _refine_diff_density_max 0.98 _refine_diff_density_min -1.88 _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 0.163415(16) 0.450000(14) 0.217300(11) 0.02380(6) Uani ? Br(1) -0.01021(4) 0.40044(4) 0.20557(3) 0.03579(17) Uani ? Br(2) 0.33100(4) 0.52338(4) 0.16974(3) 0.03561(17) Uani ? Br(3) 0.04507(5) 0.62310(4) 0.23273(4) 0.04073(19) Uani ? O(1) 0.2445(3) 0.3330(2) 0.16140(19) 0.0288(11) Uani ? O(2) 0.1602(3) 0.4207(2) 0.31875(19) 0.0274(10) Uani ? C(11) 0.2682(4) 0.2659(3) 0.1012(3) 0.0257(14) Uani ? C(12) 0.2840(4) 0.1654(4) 0.1194(3) 0.0278(14) Uani ? C(13) 0.3051(4) 0.0968(3) 0.0583(3) 0.0283(16) Uani ? C(14) 0.3151(4) 0.1318(4) -0.0175(3) 0.0314(16) Uani ? C(15) 0.3052(4) 0.2316(4) -0.0355(3) 0.0293(16) Uani ? C(16) 0.2791(4) 0.3017(4) 0.0248(3) 0.0282(16) Uani ? C(21) 0.1647(4) 0.3686(3) 0.3871(3) 0.0236(12) Uani ? C(22) 0.0643(4) 0.3455(3) 0.4343(3) 0.0239(14) Uani ? C(23) 0.0724(4) 0.2857(3) 0.4997(3) 0.0252(12) Uani ? C(24) 0.1775(4) 0.2563(4) 0.5147(3) 0.0294(17) Uani ? C(25) 0.2767(4) 0.2823(4) 0.4686(3) 0.0277(16) Uani ? C(26) 0.2705(4) 0.3403(3) 0.4020(3) 0.0249(12) Uani ? C(121) 0.2850(4) 0.1321(4) 0.2005(3) 0.0289(16) Uani ? C(122) 0.1885(5) 0.1587(4) 0.2644(3) 0.0310(16) Uani ? C(123) 0.1913(5) 0.1238(4) 0.3381(3) 0.041(2) Uani ? C(124) 0.2887(5) 0.0631(4) 0.3493(3) 0.043(2) Uani ? C(125) 0.3846(6) 0.0360(4) 0.2863(3) 0.046(2) Uani ? C(126) 0.3825(5) 0.0710(4) 0.2123(3) 0.0389(17) Uani ? C(131) 0.3144(5) -0.0117(4) 0.0703(3) 0.0331(17) Uani ? C(132) 0.2396(5) -0.0493(4) 0.1317(3) 0.040(2) Uani ? C(133) 0.2492(6) -0.1511(5) 0.1384(4) 0.051(2) Uani ? C(134) 0.3309(6) -0.2153(4) 0.0844(4) 0.052(3) Uani ? C(135) 0.4054(6) -0.1803(4) 0.0235(4) 0.048(2) Uani ? C(136) 0.3978(5) -0.0792(4) 0.0163(3) 0.0390(17) Uani ? C(151) 0.3237(4) 0.2610(4) -0.1197(3) 0.0300(17) Uani ? C(152) 0.4257(5) 0.2170(4) -0.1746(3) 0.0367(17) Uani ? C(153) 0.4442(5) 0.2397(4) -0.2533(3) 0.0371(17) Uani ? C(154) 0.3617(5) 0.3060(4) -0.2782(3) 0.0352(17) Uani ? C(155) 0.2603(5) 0.3506(4) -0.2237(3) 0.0378(17) Uani ? C(156) 0.2423(5) 0.3276(4) -0.1452(3) 0.0352(17) Uani ? C(161) 0.2692(4) 0.4094(4) 0.0090(3) 0.0285(16) Uani ? C(162) 0.3652(5) 0.4448(4) -0.0277(3) 0.0344(17) Uani ? C(163) 0.3558(5) 0.5442(4) -0.0439(3) 0.0407(17) Uani ? C(164) 0.2514(6) 0.6100(4) -0.0244(4) 0.048(2) Uani ? C(165) 0.1562(5) 0.5753(4) 0.0123(4) 0.045(2) Uani ? C(166) 0.1639(5) 0.4756(4) 0.0285(3) 0.0364(17) Uani ? C(221) -0.0453(4) 0.3814(4) 0.4153(3) 0.0253(14) Uani ? C(222) -0.0909(4) 0.4828(4) 0.4136(3) 0.0293(15) Uani ? C(223) -0.1947(4) 0.5184(4) 0.3985(3) 0.0355(17) Uani ? C(224) -0.2551(5) 0.4524(5) 0.3851(3) 0.0413(19) Uani ? C(225) -0.2098(5) 0.3515(5) 0.3861(3) 0.0400(19) Uani ? C(226) -0.1066(4) 0.3159(4) 0.4016(3) 0.0333(17) Uani ? C(231) -0.0266(4) 0.2510(4) 0.5517(3) 0.0294(17) Uani ? C(232) -0.1239(4) 0.3150(4) 0.5939(3) 0.0358(17) Uani ? C(233) -0.2123(5) 0.2783(5) 0.6439(3) 0.0437(19) Uani ? C(234) -0.2042(5) 0.1781(5) 0.6513(3) 0.0461(19) Uani ? C(235) -0.1084(5) 0.1137(5) 0.6078(4) 0.052(2) Uani ? C(236) -0.0189(5) 0.1496(4) 0.5590(4) 0.0440(19) Uani ? C(251) 0.3837(4) 0.2492(4) 0.4918(3) 0.0300(15) Uani ? C(252) 0.4129(5) 0.1514(4) 0.5164(3) 0.0418(18) Uani ? C(253) 0.5091(5) 0.1190(5) 0.5408(4) 0.050(2) Uani ? C(254) 0.5794(5) 0.1809(5) 0.5411(4) 0.049(2) Uani ? C(255) 0.5515(5) 0.2783(5) 0.5190(3) 0.0424(19) Uani ? C(256) 0.4541(4) 0.3121(5) 0.4945(3) 0.0377(19) Uani ? C(261) 0.3730(4) 0.3678(4) 0.3483(3) 0.0300(15) Uani ? C(262) 0.4541(5) 0.2994(5) 0.2959(4) 0.046(2) Uani ? C(263) 0.5523(6) 0.3247(6) 0.2484(4) 0.063(3) Uani ? C(264) 0.5693(6) 0.4180(7) 0.2535(4) 0.065(3) Uani ? C(265) 0.4900(6) 0.4872(6) 0.3046(4) 0.053(3) Uani ? C(266) 0.3914(5) 0.4617(4) 0.3519(3) 0.0387(17) Uani ? C(901) -0.0558(9) 0.1223(8) 0.9784(8) 0.102(5) Uani ? C(902) 0.0180(8) 0.1686(6) 0.9905(6) 0.077(4) Uani ? C(903) 0.0079(7) 0.1975(6) 1.0644(6) 0.077(4) Uani ? C(904) -0.0727(8) 0.1773(7) 1.1269(6) 0.082(4) Uani ? C(905) -0.1502(8) 0.1260(7) 1.1146(8) 0.098(5) Uani ? C(906) -0.1391(10) 0.0989(7) 1.0373(8) 0.098(5) Uani ? C(911) 0.1754(10) 0.1027(7) 0.7403(6) 0.088(4) Uani ? C(912) 0.2807(10) 0.0548(9) 0.7180(9) 0.128(6) Uani ? C(913) 0.3146(11) -0.0311(10) 0.6802(9) 0.145(7) Uani ? C(914) 0.2419(16) -0.0732(9) 0.6604(8) 0.130(7) Uani ? C(915) 0.1295(16) -0.0259(12) 0.6812(10) 0.142(8) Uani ? C(916) 0.0958(10) 0.0653(11) 0.7232(7) 0.123(6) Uani ? H(14) 0.3290 0.0863 -0.0579 0.0410 Uiso calc H(24) 0.1820 0.2170 0.5580 0.0380 Uiso calc H(122) 0.1226 0.1999 0.2575 0.0400 Uiso calc H(123) 0.1268 0.1414 0.3806 0.0530 Uiso calc H(124) 0.2898 0.0404 0.3991 0.0550 Uiso calc H(125) 0.4502 -0.0054 0.2935 0.0590 Uiso calc H(126) 0.4473 0.0533 0.1701 0.0500 Uiso calc H(132) 0.1831 -0.0062 0.1684 0.0520 Uiso calc H(133) 0.1995 -0.1757 0.1799 0.0670 Uiso calc H(134) 0.3358 -0.2831 0.0892 0.0680 Uiso calc H(135) 0.4612 -0.2242 -0.0129 0.0630 Uiso calc H(136) 0.4489 -0.0558 -0.0251 0.0510 Uiso calc H(152) 0.4815 0.1722 -0.1582 0.0480 Uiso calc H(153) 0.5123 0.2102 -0.2894 0.0480 Uiso calc H(154) 0.3739 0.3208 -0.3310 0.0460 Uiso calc H(155) 0.2047 0.3957 -0.2401 0.0490 Uiso calc H(156) 0.1743 0.3575 -0.1091 0.0460 Uiso calc H(162) 0.4362 0.4014 -0.0415 0.0450 Uiso calc H(163) 0.4209 0.5672 -0.0684 0.0530 Uiso calc H(164) 0.2456 0.6768 -0.0358 0.0620 Uiso calc H(165) 0.0855 0.6193 0.0265 0.0580 Uiso calc H(166) 0.0984 0.4530 0.0525 0.0470 Uiso calc H(222) -0.0509 0.5274 0.4228 0.0380 Uiso calc H(223) -0.2238 0.5863 0.3975 0.0460 Uiso calc H(224) -0.3252 0.4756 0.3754 0.0540 Uiso calc H(225) -0.2495 0.3070 0.3762 0.0520 Uiso calc H(226) -0.0781 0.2479 0.4029 0.0430 Uiso calc H(232) -0.1308 0.3830 0.5890 0.0460 Uiso calc H(233) -0.2775 0.3221 0.6726 0.0570 Uiso calc H(234) -0.2630 0.1541 0.6854 0.0600 Uiso calc H(235) -0.1035 0.0458 0.6110 0.0680 Uiso calc H(236) 0.0467 0.1055 0.5311 0.0570 Uiso calc H(252) 0.3667 0.1080 0.5161 0.0540 Uiso calc H(253) 0.5265 0.0542 0.5573 0.0650 Uiso calc H(254) 0.6455 0.1576 0.5561 0.0640 Uiso calc H(255) 0.5977 0.3212 0.5205 0.0550 Uiso calc H(256) 0.4359 0.3776 0.4797 0.0490 Uiso calc H(262) 0.4431 0.2359 0.2923 0.0600 Uiso calc H(263) 0.6064 0.2782 0.2131 0.0820 Uiso calc H(264) 0.6353 0.4344 0.2220 0.0850 Uiso calc H(265) 0.5016 0.5505 0.3079 0.0690 Uiso calc H(266) 0.3371 0.5089 0.3865 0.0500 Uiso calc H(901) -0.0501 0.1052 0.9273 0.1320 Uiso calc H(902) 0.0767 0.1815 0.9487 0.1000 Uiso calc H(903) 0.0587 0.2326 1.0721 0.0990 Uiso calc H(904) -0.0770 0.1968 1.1771 0.1060 Uiso calc H(905) -0.2072 0.1104 1.1564 0.1270 Uiso calc H(906) -0.1892 0.0649 1.0270 0.1270 Uiso calc H(911) 0.1552 0.1625 0.7679 0.1140 Uiso calc H(912) 0.3352 0.0825 0.7292 0.1660 Uiso calc H(913) 0.3912 -0.0630 0.6672 0.1890 Uiso calc H(914) 0.2667 -0.1335 0.6330 0.1680 Uiso calc H(915) 0.0762 -0.0532 0.6680 0.1850 Uiso calc H(916) 0.0197 0.0987 0.7386 0.1600 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 0.02622(11) 0.02056(10) 0.02308(11) -0.00409(7) -0.00579(7) 0.00213(7) Br(1) 0.0332(3) 0.0425(3) 0.0338(3) -0.0124(2) -0.0095(2) -0.0010(2) Br(2) 0.0360(3) 0.0364(3) 0.0363(3) -0.0154(2) -0.0090(2) 0.0104(2) Br(3) 0.0419(3) 0.0255(3) 0.0517(4) 0.0020(2) -0.0159(2) -0.0003(2) O(1) 0.0343(19) 0.0259(18) 0.0257(18) -0.0092(15) -0.0068(14) 0.0061(13) O(2) 0.0244(17) 0.0288(18) 0.0279(19) -0.0073(14) -0.0044(13) 0.0001(14) C(11) 0.027(2) 0.023(2) 0.024(3) -0.0042(19) -0.0037(18) 0.0007(18) C(12) 0.028(2) 0.025(2) 0.028(3) -0.004(2) -0.0064(19) 0.0042(19) C(13) 0.032(3) 0.019(2) 0.030(3) -0.0017(19) -0.006(2) 0.0012(19) C(14) 0.041(3) 0.023(2) 0.025(3) -0.002(2) -0.005(2) -0.0011(19) C(15) 0.032(3) 0.023(2) 0.029(3) -0.002(2) -0.006(2) 0.0024(19) C(16) 0.029(3) 0.022(2) 0.032(3) -0.0022(19) -0.009(2) 0.0006(19) C(21) 0.029(2) 0.020(2) 0.022(2) -0.0060(18) -0.0075(18) 0.0018(17) C(22) 0.024(2) 0.022(2) 0.026(3) -0.0047(18) -0.0077(18) -0.0026(18) C(23) 0.028(2) 0.026(2) 0.021(2) -0.0081(19) -0.0046(18) 0.0010(18) C(24) 0.031(3) 0.029(3) 0.028(3) -0.009(2) -0.007(2) 0.004(2) C(25) 0.030(3) 0.024(2) 0.029(3) -0.004(2) -0.010(2) 0.0005(19) C(26) 0.027(2) 0.023(2) 0.024(2) -0.0069(19) -0.0056(18) 0.0024(18) C(121) 0.032(3) 0.024(2) 0.029(3) -0.005(2) -0.007(2) 0.0014(19) C(122) 0.039(3) 0.023(2) 0.025(3) -0.005(2) -0.002(2) 0.0040(19) C(123) 0.058(4) 0.028(3) 0.031(3) -0.013(3) -0.002(2) 0.006(2) C(124) 0.068(4) 0.038(3) 0.025(3) -0.016(3) -0.015(3) 0.004(2) C(125) 0.061(4) 0.035(3) 0.044(4) -0.006(3) -0.024(3) 0.013(3) C(126) 0.041(3) 0.033(3) 0.038(3) -0.003(2) -0.009(2) 0.006(2) C(131) 0.042(3) 0.025(3) 0.032(3) -0.003(2) -0.014(2) 0.002(2) C(132) 0.061(4) 0.030(3) 0.031(3) -0.016(3) -0.012(3) 0.004(2) C(133) 0.085(5) 0.039(3) 0.040(4) -0.031(3) -0.022(3) 0.017(3) C(134) 0.071(5) 0.022(3) 0.071(5) -0.006(3) -0.038(4) 0.006(3) C(135) 0.063(4) 0.023(3) 0.059(4) -0.002(3) -0.023(3) 0.000(3) C(136) 0.046(3) 0.026(3) 0.042(3) -0.001(2) -0.013(2) -0.001(2) C(151) 0.036(3) 0.027(3) 0.025(3) -0.005(2) -0.008(2) 0.0064(19) C(152) 0.041(3) 0.036(3) 0.028(3) -0.001(2) -0.008(2) 0.002(2) C(153) 0.042(3) 0.039(3) 0.025(3) -0.007(2) -0.003(2) 0.002(2) C(154) 0.042(3) 0.040(3) 0.027(3) -0.018(2) -0.010(2) 0.011(2) C(155) 0.037(3) 0.042(3) 0.035(3) -0.007(2) -0.014(2) 0.010(2) C(156) 0.033(3) 0.038(3) 0.030(3) -0.006(2) -0.004(2) 0.006(2) C(161) 0.034(3) 0.026(3) 0.022(2) -0.003(2) -0.0061(19) 0.0041(19) C(162) 0.035(3) 0.034(3) 0.032(3) -0.006(2) -0.008(2) 0.004(2) C(163) 0.050(3) 0.037(3) 0.035(3) -0.019(3) -0.005(2) 0.004(2) C(164) 0.072(4) 0.026(3) 0.043(4) -0.009(3) -0.016(3) 0.008(2) C(165) 0.048(4) 0.029(3) 0.047(4) 0.006(3) -0.010(3) 0.004(2) C(166) 0.037(3) 0.029(3) 0.036(3) -0.003(2) -0.003(2) 0.003(2) C(221) 0.024(2) 0.029(3) 0.021(2) -0.0065(19) -0.0037(17) 0.0034(18) C(222) 0.028(2) 0.034(3) 0.026(3) -0.007(2) -0.0075(19) -0.001(2) C(223) 0.027(3) 0.044(3) 0.032(3) 0.000(2) -0.009(2) -0.001(2) C(224) 0.026(3) 0.058(4) 0.041(3) -0.004(3) -0.015(2) -0.002(3) C(225) 0.036(3) 0.054(4) 0.036(3) -0.023(3) -0.010(2) 0.004(3) C(226) 0.032(3) 0.038(3) 0.033(3) -0.015(2) -0.009(2) 0.003(2) C(231) 0.033(3) 0.031(3) 0.026(3) -0.011(2) -0.009(2) 0.007(2) C(232) 0.036(3) 0.036(3) 0.034(3) -0.014(2) -0.003(2) 0.001(2) C(233) 0.035(3) 0.055(4) 0.037(3) -0.015(3) 0.000(2) 0.000(3) C(234) 0.041(3) 0.068(4) 0.035(3) -0.029(3) -0.009(2) 0.017(3) C(235) 0.049(4) 0.045(4) 0.062(4) -0.023(3) -0.009(3) 0.019(3) C(236) 0.036(3) 0.040(3) 0.050(4) -0.014(3) 0.000(2) 0.009(3) C(251) 0.024(2) 0.040(3) 0.025(3) -0.005(2) -0.0068(19) -0.001(2) C(252) 0.045(3) 0.039(3) 0.043(3) -0.003(3) -0.020(3) -0.001(2) C(253) 0.047(4) 0.049(4) 0.054(4) 0.007(3) -0.028(3) -0.001(3) C(254) 0.036(3) 0.064(4) 0.043(4) 0.006(3) -0.016(3) -0.006(3) C(255) 0.031(3) 0.075(4) 0.025(3) -0.019(3) -0.008(2) 0.000(3) C(256) 0.033(3) 0.052(4) 0.030(3) -0.013(3) -0.010(2) 0.007(2) C(261) 0.025(2) 0.033(3) 0.033(3) -0.009(2) -0.009(2) 0.009(2) C(262) 0.036(3) 0.051(4) 0.046(4) -0.011(3) -0.004(2) 0.002(3) C(263) 0.036(4) 0.090(6) 0.048(4) -0.007(4) 0.005(3) 0.005(4) C(264) 0.038(4) 0.123(7) 0.044(4) -0.036(4) -0.016(3) 0.028(4) C(265) 0.059(4) 0.070(5) 0.051(4) -0.040(4) -0.032(3) 0.029(3) C(266) 0.040(3) 0.041(3) 0.038(3) -0.015(3) -0.013(2) 0.013(2) C(901) 0.078(7) 0.096(8) 0.136(10) -0.007(6) -0.046(7) -0.016(7) C(902) 0.079(6) 0.064(5) 0.094(7) -0.005(4) -0.042(5) -0.006(5) C(903) 0.073(6) 0.070(6) 0.099(7) -0.023(5) -0.037(5) -0.004(5) C(904) 0.094(7) 0.077(6) 0.084(7) -0.023(5) -0.036(5) 0.001(5) C(905) 0.072(6) 0.064(6) 0.154(11) -0.014(5) -0.031(6) 0.024(6) C(906) 0.088(7) 0.065(6) 0.167(12) -0.009(5) -0.080(8) -0.019(7) C(911) 0.103(8) 0.069(6) 0.085(7) -0.011(6) -0.020(6) -0.007(5) C(912) 0.072(7) 0.077(7) 0.221(15) -0.030(6) -0.005(8) -0.016(8) C(913) 0.085(8) 0.099(10) 0.197(15) -0.024(7) 0.050(9) -0.011(9) C(914) 0.178(15) 0.075(8) 0.119(10) -0.036(9) -0.007(10) -0.019(7) C(915) 0.168(15) 0.127(12) 0.181(15) -0.056(11) -0.110(13) 0.001(11) C(916) 0.077(7) 0.154(13) 0.123(10) 0.017(8) -0.038(7) -0.002(9) # 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) 1.825(3) ? Ta O(1) 1.865(3) ? Ta Br(2) 2.4679(5) ? Ta Br(3) 2.4995(6) ? Ta Br(1) 2.5037(6) ? O(1) C(11) 1.374(6) ? O(2) C(21) 1.394(5) ? C(11) C(12) 1.399(6) ? C(11) C(16) 1.407(7) ? C(12) C(13) 1.406(7) ? C(12) C(121) 1.500(7) ? C(13) C(14) 1.394(7) ? C(13) C(131) 1.493(7) ? C(14) C(15) 1.392(7) ? C(15) C(16) 1.399(7) ? C(15) C(151) 1.501(7) ? C(16) C(161) 1.491(7) ? C(21) C(26) 1.398(7) ? C(21) C(22) 1.400(6) ? C(22) C(23) 1.411(6) ? C(22) C(221) 1.485(6) ? C(23) C(24) 1.391(7) ? C(23) C(231) 1.490(6) ? C(24) C(25) 1.399(7) ? C(25) C(26) 1.413(6) ? C(25) C(251) 1.488(7) ? C(26) C(261) 1.488(6) ? C(121) C(126) 1.387(7) ? C(121) C(122) 1.396(7) ? C(122) C(123) 1.385(7) ? C(123) C(124) 1.380(8) ? C(124) C(125) 1.383(8) ? C(125) C(126) 1.390(7) ? C(131) C(132) 1.392(7) ? C(131) C(136) 1.400(7) ? C(132) C(133) 1.392(8) ? C(133) C(134) 1.367(9) ? C(134) C(135) 1.368(9) ? C(135) C(136) 1.386(7) ? C(151) C(156) 1.380(7) ? C(151) C(152) 1.399(7) ? C(152) C(153) 1.387(7) ? C(153) C(154) 1.382(8) ? C(154) C(155) 1.392(8) ? C(155) C(156) 1.385(7) ? C(161) C(162) 1.385(7) ? C(161) C(166) 1.389(7) ? C(162) C(163) 1.381(7) ? C(163) C(164) 1.378(8) ? C(164) C(165) 1.373(9) ? C(165) C(166) 1.387(7) ? C(221) C(226) 1.391(7) ? C(221) C(222) 1.395(7) ? C(222) C(223) 1.385(7) ? C(223) C(224) 1.385(8) ? C(224) C(225) 1.387(8) ? C(225) C(226) 1.381(7) ? C(231) C(232) 1.375(7) ? C(231) C(236) 1.389(7) ? C(232) C(233) 1.394(7) ? C(233) C(234) 1.372(8) ? C(234) C(235) 1.375(9) ? C(235) C(236) 1.389(8) ? C(251) C(256) 1.389(7) ? C(251) C(252) 1.406(8) ? C(252) C(253) 1.376(8) ? C(253) C(254) 1.369(9) ? C(254) C(255) 1.385(9) ? C(255) C(256) 1.393(7) ? C(261) C(262) 1.381(8) ? C(261) C(266) 1.382(7) ? C(262) C(263) 1.393(8) ? C(263) C(264) 1.371(11) ? C(264) C(265) 1.366(10) ? C(265) C(266) 1.396(8) ? C(901) C(902) 1.313(12) ? C(901) C(906) 1.342(15) ? C(902) C(903) 1.358(12) ? C(903) C(904) 1.342(12) ? C(904) C(905) 1.402(12) ? C(905) C(906) 1.405(14) ? C(911) C(912) 1.295(13) ? C(911) C(916) 1.341(15) ? C(912) C(913) 1.316(15) ? C(913) C(914) 1.326(18) ? C(914) C(915) 1.366(18) ? C(915) C(916) 1.415(17) ? 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) 104.30(14) ? O(2) Ta Br(2) 103.21(10) ? O(1) Ta Br(2) 90.45(10) ? O(2) Ta Br(3) 101.11(10) ? O(1) Ta Br(3) 154.38(10) ? Br(2) Ta Br(3) 86.97(2) ? O(2) Ta Br(1) 102.46(10) ? O(1) Ta Br(1) 85.61(10) ? Br(2) Ta Br(1) 154.21(2) ? Br(3) Ta Br(1) 85.73(2) ? C(11) O(1) Ta 152.9(3) ? C(21) O(2) Ta 162.2(3) ? O(1) C(11) C(12) 117.8(4) ? O(1) C(11) C(16) 118.4(4) ? C(12) C(11) C(16) 123.8(4) ? C(11) C(12) C(13) 117.8(4) ? C(11) C(12) C(121) 120.7(4) ? C(13) C(12) C(121) 121.4(4) ? C(14) C(13) C(12) 118.6(4) ? C(14) C(13) C(131) 117.8(4) ? C(12) C(13) C(131) 123.5(4) ? C(15) C(14) C(13) 123.0(4) ? C(14) C(15) C(16) 119.4(4) ? C(14) C(15) C(151) 118.8(4) ? C(16) C(15) C(151) 121.7(4) ? C(15) C(16) C(11) 117.2(4) ? C(15) C(16) C(161) 121.9(4) ? C(11) C(16) C(161) 120.8(4) ? O(2) C(21) C(26) 117.3(4) ? O(2) C(21) C(22) 118.0(4) ? C(26) C(21) C(22) 124.6(4) ? C(21) C(22) C(23) 117.1(4) ? C(21) C(22) C(221) 121.0(4) ? C(23) C(22) C(221) 121.8(4) ? C(24) C(23) C(22) 118.7(4) ? C(24) C(23) C(231) 118.9(4) ? C(22) C(23) C(231) 122.4(4) ? C(23) C(24) C(25) 123.8(5) ? C(24) C(25) C(26) 118.1(4) ? C(24) C(25) C(251) 119.2(4) ? C(26) C(25) C(251) 122.6(4) ? C(21) C(26) C(25) 117.5(4) ? C(21) C(26) C(261) 121.1(4) ? C(25) C(26) C(261) 121.4(4) ? C(126) C(121) C(122) 119.1(5) ? C(126) C(121) C(12) 119.6(4) ? C(122) C(121) C(12) 121.3(4) ? C(123) C(122) C(121) 119.8(5) ? C(124) C(123) C(122) 120.7(5) ? C(123) C(124) C(125) 119.9(5) ? C(126) C(125) C(124) 119.7(6) ? C(121) C(126) C(125) 120.8(5) ? C(132) C(131) C(136) 118.0(5) ? C(132) C(131) C(13) 122.5(5) ? C(136) C(131) C(13) 119.5(5) ? C(133) C(132) C(131) 120.1(6) ? C(134) C(133) C(132) 120.7(6) ? C(133) C(134) C(135) 120.3(6) ? C(134) C(135) C(136) 119.9(6) ? C(135) C(136) C(131) 121.1(6) ? C(156) C(151) C(152) 118.8(5) ? C(156) C(151) C(15) 122.4(5) ? C(152) C(151) C(15) 118.8(4) ? C(153) C(152) C(151) 120.4(5) ? C(154) C(153) C(152) 120.2(5) ? C(153) C(154) C(155) 119.6(5) ? C(156) C(155) C(154) 119.9(5) ? C(151) C(156) C(155) 121.0(5) ? C(162) C(161) C(166) 118.7(5) ? C(162) C(161) C(16) 120.2(4) ? C(166) C(161) C(16) 121.0(5) ? C(163) C(162) C(161) 120.3(5) ? C(164) C(163) C(162) 121.0(5) ? C(165) C(164) C(163) 118.9(5) ? C(164) C(165) C(166) 120.9(5) ? C(165) C(166) C(161) 120.1(5) ? C(226) C(221) C(222) 118.4(5) ? C(226) C(221) C(22) 121.5(4) ? C(222) C(221) C(22) 120.1(4) ? C(223) C(222) C(221) 121.3(5) ? C(222) C(223) C(224) 119.7(5) ? C(225) C(224) C(223) 119.3(5) ? C(226) C(225) C(224) 121.1(5) ? C(225) C(226) C(221) 120.2(5) ? C(232) C(231) C(236) 118.9(5) ? C(232) C(231) C(23) 122.7(5) ? C(236) C(231) C(23) 118.4(5) ? C(231) C(232) C(233) 120.2(5) ? C(234) C(233) C(232) 120.7(6) ? C(233) C(234) C(235) 119.4(5) ? C(234) C(235) C(236) 120.3(6) ? C(235) C(236) C(231) 120.5(6) ? C(256) C(251) C(252) 117.7(5) ? C(256) C(251) C(25) 123.2(5) ? C(252) C(251) C(25) 119.1(5) ? C(253) C(252) C(251) 120.9(6) ? C(254) C(253) C(252) 120.9(6) ? C(253) C(254) C(255) 119.5(6) ? C(254) C(255) C(256) 120.0(6) ? C(251) C(256) C(255) 121.0(6) ? C(262) C(261) C(266) 118.5(5) ? C(262) C(261) C(26) 121.0(5) ? C(266) C(261) C(26) 120.5(5) ? C(261) C(262) C(263) 120.5(6) ? C(264) C(263) C(262) 120.1(7) ? C(263) C(264) C(265) 120.5(6) ? C(264) C(265) C(266) 119.3(7) ? C(261) C(266) C(265) 121.2(6) ? C(902) C(901) C(906) 122.2(12) ? C(901) C(902) C(903) 119.5(10) ? C(904) C(903) C(902) 122.4(9) ? C(903) C(904) C(905) 118.4(10) ? C(904) C(905) C(906) 117.9(10) ? C(901) C(906) C(905) 119.5(10) ? C(912) C(911) C(916) 119.4(11) ? C(911) C(912) C(913) 123.3(12) ? C(912) C(913) C(914) 121.4(13) ? C(913) C(914) C(915) 118.3(12) ? C(914) C(915) C(916) 118.8(12) ? C(911) C(916) C(915) 118.8(11) ? #===END #============================================================================== data_SS2127 _database_code_CSD 164009 _audit_creation_date 22-02-00 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.17 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C73 H55 Cl2 O2 Ta' _chemical_formula_structural ? _chemical_formula_weight 1216.11 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6577(4) _cell_length_b 14.7497(5) _cell_length_c 19.1650(7) _cell_angle_alpha 96.494(2) _cell_angle_beta 93.782(2) _cell_angle_gamma 106.265(2) _cell_volume 2858.5(4) _cell_measurement_reflns_used 23365 _cell_measurement_theta_min 4 _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 2.039 _cell_measurement_temperature 173 _exptl_crystal_F_000 1232 # 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 0.4625 _exptl_absorpt_correction_T_max 0.6999 _diffrn_reflns_number 23365 _reflns_number_total 12058 _reflns_number_gt 10829 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 18 _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 0.045 _refine_ls_wR_factor_ref 0.113 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 12055 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+2.8702P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.005 _refine_diff_density_max 1.75 _refine_diff_density_min -1.46 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.54E-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_(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 0.110348(17) 0.189633(13) 0.196389(9) 0.03071(6) Uani ? Cl(1) 0.08253(17) 0.30950(12) 0.27656(8) 0.0600(5) Uani ? Cl(2) -0.06345(13) 0.07643(10) 0.12545(7) 0.0485(4) Uani ? O(10) 0.1150(3) 0.2608(2) 0.11940(16) 0.0317(9) Uani ? O(20) 0.0870(3) 0.1016(2) 0.26194(17) 0.0359(10) Uani ? C(11) 0.0763(4) 0.2782(3) 0.0542(2) 0.0290(11) Uani ? C(12) -0.0258(4) 0.3195(3) 0.0470(2) 0.0304(11) Uani ? C(13) -0.0668(4) 0.3356(3) -0.0210(2) 0.0304(11) Uani ? C(14) 0.0023(4) 0.3157(3) -0.0771(2) 0.0335(11) Uani ? C(15) 0.1062(4) 0.2772(3) -0.0692(2) 0.0317(11) Uani ? C(16) 0.1431(4) 0.2555(3) -0.0033(2) 0.0293(11) Uani ? C(21) 0.0448(5) 0.0274(3) 0.2988(2) 0.0341(11) Uani ? C(22) 0.1085(4) -0.0449(3) 0.2956(2) 0.0323(11) Uani ? C(23) 0.0736(5) -0.1159(3) 0.3394(2) 0.0334(11) Uani ? C(24) -0.0262(5) -0.1157(3) 0.3823(2) 0.0350(11) Uani ? C(25) -0.0943(4) -0.0479(3) 0.3831(2) 0.0338(13) Uani ? C(26) -0.0578(5) 0.0268(3) 0.3422(2) 0.0337(11) Uani ? C(30) 0.3162(4) 0.1865(3) 0.1880(2) 0.0253(11) Uani ? C(31) 0.3728(5) 0.2773(4) 0.2355(3) 0.0483(17) Uani ? C(32) 0.4146(6) 0.2770(6) 0.3069(4) 0.070(3) Uani ? C(33) 0.4634(8) 0.3615(8) 0.3512(4) 0.091(4) Uani ? C(34) 0.4759(9) 0.4458(8) 0.3256(6) 0.098(4) Uani ? C(35) 0.4374(7) 0.4499(6) 0.2574(5) 0.077(3) Uani ? C(36) 0.3892(6) 0.3679(5) 0.2117(4) 0.063(2) Uani ? C(121) -0.0871(5) 0.3476(3) 0.1103(2) 0.0343(13) Uani ? C(122) -0.2127(5) 0.2964(4) 0.1224(3) 0.0476(17) Uani ? C(123) -0.2743(7) 0.3305(6) 0.1771(4) 0.066(2) Uani ? C(124) -0.2111(8) 0.4125(6) 0.2202(4) 0.072(3) Uani ? C(125) -0.0850(8) 0.4629(5) 0.2111(3) 0.062(2) Uani ? C(126) -0.0226(6) 0.4313(4) 0.1556(3) 0.0471(17) Uani ? C(131) -0.1796(4) 0.3740(3) -0.0368(2) 0.0315(11) Uani ? C(132) -0.1992(5) 0.4523(3) 0.0040(3) 0.0366(13) Uani ? C(133) -0.3034(5) 0.4868(4) -0.0147(3) 0.0431(17) Uani ? C(134) -0.3896(5) 0.4450(4) -0.0736(3) 0.0454(17) Uani ? C(135) -0.3714(5) 0.3671(4) -0.1148(3) 0.0464(17) Uani ? C(136) -0.2674(5) 0.3324(4) -0.0966(3) 0.0392(15) Uani ? C(151) 0.1810(4) 0.2671(3) -0.1326(2) 0.0337(13) Uani ? C(152) 0.2241(5) 0.3452(4) -0.1686(3) 0.0394(15) Uani ? C(153) 0.2893(6) 0.3382(4) -0.2281(3) 0.0497(17) Uani ? C(154) 0.3147(6) 0.2545(5) -0.2516(3) 0.0518(19) Uani ? C(155) 0.2735(6) 0.1773(4) -0.2164(3) 0.0468(17) Uani ? C(156) 0.2076(5) 0.1835(4) -0.1571(3) 0.0393(15) Uani ? C(161) 0.2541(5) 0.2133(3) 0.0067(2) 0.0328(11) Uani ? C(162) 0.3826(5) 0.2708(4) 0.0137(3) 0.0402(15) Uani ? C(163) 0.4864(5) 0.2319(5) 0.0176(3) 0.0537(19) Uani ? C(164) 0.4629(6) 0.1347(5) 0.0150(3) 0.0524(19) Uani ? C(165) 0.3361(6) 0.0766(4) 0.0069(3) 0.0510(19) Uani ? C(166) 0.2305(5) 0.1149(4) 0.0040(3) 0.0417(17) Uani ? C(221) 0.2115(5) -0.0452(3) 0.2465(2) 0.0335(11) Uani ? C(222) 0.1756(5) -0.0720(3) 0.1746(3) 0.0418(15) Uani ? C(223) 0.2696(7) -0.0816(4) 0.1297(3) 0.0560(19) Uani ? C(224) 0.3994(7) -0.0616(5) 0.1561(4) 0.060(2) Uani ? C(225) 0.4352(6) -0.0330(5) 0.2271(4) 0.060(2) Uani ? C(226) 0.3421(5) -0.0251(4) 0.2724(3) 0.0466(17) Uani ? C(231) 0.1406(5) -0.1925(3) 0.3414(3) 0.0363(13) Uani ? C(232) 0.1433(7) -0.2538(4) 0.2822(3) 0.0550(19) Uani ? C(233) 0.2037(8) -0.3252(4) 0.2865(4) 0.065(2) Uani ? C(234) 0.2630(7) -0.3355(5) 0.3500(4) 0.069(3) Uani ? C(235) 0.2605(7) -0.2744(5) 0.4089(4) 0.067(3) Uani ? C(236) 0.1993(6) -0.2041(4) 0.4051(3) 0.0470(17) Uani ? C(251) -0.2058(5) -0.0600(3) 0.4278(3) 0.0385(15) Uani ? C(252) -0.1890(5) -0.0768(4) 0.4973(3) 0.0428(17) Uani ? C(253) -0.2941(6) -0.0965(4) 0.5381(3) 0.054(2) Uani ? C(254) -0.4181(6) -0.1012(5) 0.5095(3) 0.061(2) Uani ? C(255) -0.4364(6) -0.0838(5) 0.4412(4) 0.063(2) Uani ? C(256) -0.3320(5) -0.0636(4) 0.4003(3) 0.0486(19) Uani ? C(261) -0.1202(5) 0.1061(4) 0.3469(3) 0.0432(17) Uani ? C(262) -0.0875(9) 0.1745(5) 0.4065(3) 0.071(3) Uani ? C(263) -0.1460(11) 0.2473(6) 0.4131(4) 0.094(4) Uani ? C(264) -0.2418(10) 0.2511(7) 0.3611(5) 0.097(4) Uani ? C(265) -0.2730(7) 0.1836(6) 0.3019(5) 0.079(3) Uani ? C(266) -0.2115(5) 0.1106(5) 0.2933(4) 0.056(2) Uani ? C(901) 0.2666(16) 0.3683(10) 0.5056(9) 0.168(8) Uani ? C(902) 0.2300(12) 0.3455(8) 0.5690(7) 0.116(5) Uani ? C(903) 0.1530(11) 0.3925(9) 0.6046(6) 0.109(4) Uani ? C(904) 0.1252(13) 0.4682(8) 0.5775(6) 0.119(5) Uani ? C(905) 0.1710(15) 0.4918(9) 0.5148(7) 0.140(6) Uani ? C(906) 0.2381(15) 0.4388(10) 0.4772(8) 0.149(7) Uani ? H(14) -0.0221 0.3288 -0.1215 0.0440 Uiso calc H(24) -0.0484 -0.1627 0.4116 0.0450 Uiso calc H(32) 0.4090 0.2195 0.3239 0.0910 Uiso calc H(33) 0.4881 0.3612 0.3986 0.1180 Uiso calc H(34) 0.5120 0.5025 0.3560 0.1270 Uiso calc H(35) 0.4439 0.5085 0.2420 0.1010 Uiso calc H(36) 0.3665 0.3707 0.1645 0.0820 Uiso calc H(122) -0.2557 0.2393 0.0939 0.0620 Uiso calc H(123) -0.3593 0.2968 0.1842 0.0860 Uiso calc H(124) -0.2536 0.4348 0.2563 0.0930 Uiso calc H(125) -0.0414 0.5178 0.2418 0.0810 Uiso calc H(126) 0.0621 0.4659 0.1488 0.0610 Uiso calc H(132) -0.1419 0.4817 0.0440 0.0470 Uiso calc H(133) -0.3150 0.5391 0.0132 0.0560 Uiso calc H(134) -0.4591 0.4686 -0.0856 0.0590 Uiso calc H(135) -0.4292 0.3381 -0.1547 0.0600 Uiso calc H(136) -0.2560 0.2803 -0.1248 0.0510 Uiso calc H(152) 0.2088 0.4026 -0.1524 0.0510 Uiso calc H(153) 0.3160 0.3905 -0.2523 0.0650 Uiso calc H(154) 0.3596 0.2501 -0.2913 0.0670 Uiso calc H(155) 0.2900 0.1202 -0.2325 0.0610 Uiso calc H(156) 0.1808 0.1307 -0.1335 0.0510 Uiso calc H(162) 0.3995 0.3365 0.0157 0.0520 Uiso calc H(163) 0.5723 0.2714 0.0220 0.0700 Uiso calc H(164) 0.5327 0.1087 0.0187 0.0680 Uiso calc H(165) 0.3203 0.0109 0.0034 0.0660 Uiso calc H(166) 0.1449 0.0751 0.0003 0.0540 Uiso calc H(222) 0.0886 -0.0834 0.1565 0.0540 Uiso calc H(223) 0.2450 -0.1016 0.0817 0.0730 Uiso calc H(224) 0.4624 -0.0675 0.1259 0.0780 Uiso calc H(225) 0.5229 -0.0188 0.2448 0.0790 Uiso calc H(226) 0.3672 -0.0062 0.3204 0.0610 Uiso calc H(232) 0.1044 -0.2473 0.2389 0.0720 Uiso calc H(233) 0.2040 -0.3666 0.2462 0.0840 Uiso calc H(234) 0.3042 -0.3831 0.3527 0.0890 Uiso calc H(235) 0.3006 -0.2805 0.4521 0.0870 Uiso calc H(236) 0.1973 -0.1639 0.4458 0.0620 Uiso calc H(252) -0.1059 -0.0749 0.5169 0.0560 Uiso calc H(253) -0.2807 -0.1065 0.5847 0.0700 Uiso calc H(254) -0.4889 -0.1161 0.5362 0.0790 Uiso calc H(255) -0.5198 -0.0856 0.4222 0.0820 Uiso calc H(256) -0.3461 -0.0523 0.3541 0.0630 Uiso calc H(262) -0.0258 0.1713 0.4421 0.0920 Uiso calc H(263) -0.1214 0.2940 0.4524 0.1220 Uiso calc H(264) -0.2840 0.2984 0.3664 0.1260 Uiso calc H(265) -0.3359 0.1863 0.2668 0.1030 Uiso calc H(266) -0.2317 0.0664 0.2526 0.0730 Uiso calc H(30A) 0.3348 0.1326 0.2065 0.0330 Uiso calc H(30B) 0.3415 0.1897 0.1404 0.0330 Uiso calc H(901) 0.3136 0.3331 0.4810 0.2180 Uiso calc H(902) 0.2567 0.2983 0.5886 0.1500 Uiso calc H(903) 0.1205 0.3733 0.6461 0.1410 Uiso calc H(904) 0.0763 0.5027 0.6014 0.1550 Uiso calc H(905) 0.1565 0.5447 0.4974 0.1820 Uiso calc H(906) 0.2628 0.4522 0.4330 0.1940 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 0.03284(12) 0.03517(12) 0.02935(11) 0.01552(8) 0.00524(7) 0.01043(8) Cl(1) 0.0734(10) 0.0664(9) 0.0533(8) 0.0370(8) 0.0174(7) 0.0136(7) Cl(2) 0.0465(7) 0.0442(7) 0.0501(7) 0.0062(6) -0.0032(6) 0.0090(6) O(10) 0.0340(16) 0.0352(16) 0.0309(15) 0.0158(13) 0.0063(13) 0.0086(13) O(20) 0.0395(17) 0.0412(18) 0.0346(16) 0.0202(15) 0.0082(14) 0.0129(14) C(11) 0.029(2) 0.031(2) 0.030(2) 0.0108(18) 0.0036(17) 0.0107(18) C(12) 0.028(2) 0.035(2) 0.032(2) 0.0127(18) 0.0059(17) 0.0098(18) C(13) 0.029(2) 0.032(2) 0.035(2) 0.0147(18) 0.0032(18) 0.0095(18) C(14) 0.034(2) 0.041(2) 0.030(2) 0.016(2) 0.0013(18) 0.011(2) C(15) 0.032(2) 0.037(2) 0.031(2) 0.0146(19) 0.0078(18) 0.0103(19) C(16) 0.027(2) 0.030(2) 0.035(2) 0.0127(17) 0.0075(18) 0.0078(18) C(21) 0.038(2) 0.039(2) 0.032(2) 0.018(2) 0.0036(19) 0.0146(19) C(22) 0.035(2) 0.041(2) 0.027(2) 0.020(2) 0.0026(18) 0.0076(19) C(23) 0.037(2) 0.037(2) 0.030(2) 0.015(2) 0.0048(19) 0.0083(19) C(24) 0.041(2) 0.037(2) 0.032(2) 0.017(2) 0.0023(19) 0.0118(19) C(25) 0.034(2) 0.043(3) 0.030(2) 0.017(2) 0.0065(19) 0.011(2) C(26) 0.037(2) 0.042(2) 0.029(2) 0.021(2) 0.0043(18) 0.0085(19) C(30) 0.0201(18) 0.032(2) 0.028(2) 0.0101(16) 0.0060(16) 0.0127(17) C(31) 0.035(3) 0.060(3) 0.054(3) 0.019(3) 0.008(2) 0.010(3) C(32) 0.053(4) 0.108(6) 0.055(4) 0.029(4) 0.011(3) 0.016(4) C(33) 0.086(6) 0.135(8) 0.058(4) 0.059(6) -0.008(4) -0.020(5) C(34) 0.077(6) 0.095(7) 0.109(8) 0.019(5) 0.015(5) -0.025(6) C(35) 0.064(4) 0.063(4) 0.096(6) 0.011(4) 0.005(4) -0.007(4) C(36) 0.051(3) 0.058(4) 0.084(5) 0.016(3) 0.019(3) 0.017(4) C(121) 0.038(2) 0.045(3) 0.033(2) 0.028(2) 0.0109(19) 0.015(2) C(122) 0.043(3) 0.060(3) 0.054(3) 0.028(3) 0.017(2) 0.026(3) C(123) 0.059(4) 0.094(5) 0.074(4) 0.049(4) 0.038(3) 0.045(4) C(124) 0.106(6) 0.103(6) 0.049(4) 0.082(5) 0.036(4) 0.037(4) C(125) 0.093(5) 0.071(4) 0.041(3) 0.054(4) 0.011(3) 0.004(3) C(126) 0.062(3) 0.053(3) 0.039(3) 0.034(3) 0.011(2) 0.011(2) C(131) 0.028(2) 0.034(2) 0.038(2) 0.0129(18) 0.0082(18) 0.0147(19) C(132) 0.040(2) 0.035(2) 0.041(3) 0.016(2) 0.006(2) 0.017(2) C(133) 0.045(3) 0.040(3) 0.054(3) 0.024(2) 0.010(2) 0.014(2) C(134) 0.038(3) 0.051(3) 0.060(3) 0.027(2) 0.006(2) 0.024(3) C(135) 0.039(3) 0.059(3) 0.046(3) 0.019(2) -0.002(2) 0.018(3) C(136) 0.037(2) 0.046(3) 0.040(3) 0.021(2) 0.002(2) 0.007(2) C(151) 0.031(2) 0.044(3) 0.030(2) 0.016(2) 0.0041(18) 0.008(2) C(152) 0.044(3) 0.042(3) 0.038(2) 0.018(2) 0.011(2) 0.012(2) C(153) 0.057(3) 0.056(3) 0.041(3) 0.018(3) 0.016(3) 0.017(3) C(154) 0.050(3) 0.073(4) 0.038(3) 0.025(3) 0.016(2) 0.006(3) C(155) 0.054(3) 0.053(3) 0.040(3) 0.027(3) 0.009(2) 0.002(2) C(156) 0.044(3) 0.041(3) 0.036(2) 0.016(2) 0.008(2) 0.007(2) C(161) 0.036(2) 0.038(2) 0.031(2) 0.018(2) 0.0105(19) 0.0098(19) C(162) 0.036(2) 0.047(3) 0.045(3) 0.019(2) 0.009(2) 0.016(2) C(163) 0.038(3) 0.080(4) 0.059(3) 0.031(3) 0.018(3) 0.033(3) C(164) 0.055(3) 0.074(4) 0.052(3) 0.048(3) 0.021(3) 0.024(3) C(165) 0.073(4) 0.049(3) 0.047(3) 0.039(3) 0.014(3) 0.014(2) C(166) 0.045(3) 0.040(3) 0.046(3) 0.020(2) 0.006(2) 0.010(2) C(221) 0.037(2) 0.034(2) 0.037(2) 0.018(2) 0.0095(19) 0.0133(19) C(222) 0.053(3) 0.038(3) 0.036(2) 0.014(2) 0.007(2) 0.008(2) C(223) 0.077(4) 0.049(3) 0.047(3) 0.021(3) 0.028(3) 0.008(3) C(224) 0.065(4) 0.060(4) 0.070(4) 0.030(3) 0.042(3) 0.019(3) C(225) 0.048(3) 0.081(4) 0.071(4) 0.039(3) 0.024(3) 0.026(4) C(226) 0.046(3) 0.062(3) 0.042(3) 0.028(3) 0.010(2) 0.015(3) C(231) 0.043(3) 0.039(2) 0.035(2) 0.019(2) 0.012(2) 0.016(2) C(232) 0.083(4) 0.049(3) 0.043(3) 0.033(3) 0.011(3) 0.010(3) C(233) 0.101(5) 0.052(3) 0.062(4) 0.046(4) 0.033(4) 0.016(3) C(234) 0.088(5) 0.069(4) 0.077(5) 0.055(4) 0.029(4) 0.031(4) C(235) 0.081(5) 0.083(5) 0.061(4) 0.055(4) 0.011(3) 0.029(4) C(236) 0.057(3) 0.055(3) 0.040(3) 0.030(3) 0.006(2) 0.016(2) C(251) 0.045(3) 0.038(2) 0.040(3) 0.019(2) 0.015(2) 0.013(2) C(252) 0.045(3) 0.048(3) 0.039(3) 0.017(2) 0.005(2) 0.012(2) C(253) 0.065(4) 0.061(4) 0.040(3) 0.021(3) 0.018(3) 0.015(3) C(254) 0.057(4) 0.080(4) 0.057(4) 0.025(3) 0.030(3) 0.023(3) C(255) 0.044(3) 0.083(5) 0.075(4) 0.031(3) 0.021(3) 0.026(4) C(256) 0.047(3) 0.067(4) 0.043(3) 0.029(3) 0.011(2) 0.019(3) C(261) 0.055(3) 0.050(3) 0.039(3) 0.031(3) 0.017(2) 0.019(2) C(262) 0.133(7) 0.072(4) 0.041(3) 0.073(5) 0.027(4) 0.020(3) C(263) 0.176(9) 0.092(6) 0.061(4) 0.095(6) 0.054(5) 0.035(4) C(264) 0.127(7) 0.109(7) 0.113(7) 0.097(6) 0.075(6) 0.062(6) C(265) 0.063(4) 0.098(6) 0.105(6) 0.050(4) 0.021(4) 0.062(5) C(266) 0.044(3) 0.067(4) 0.074(4) 0.031(3) 0.012(3) 0.036(3) C(901) 0.219(16) 0.118(10) 0.207(16) 0.072(11) 0.138(14) 0.065(11) C(902) 0.119(8) 0.088(7) 0.135(10) 0.015(6) 0.023(8) 0.029(7) C(903) 0.117(8) 0.119(8) 0.086(7) 0.025(7) 0.018(6) 0.018(6) C(904) 0.150(10) 0.104(8) 0.102(8) 0.043(8) 0.008(7) -0.003(7) C(905) 0.206(15) 0.099(8) 0.125(10) 0.048(9) 0.043(10) 0.030(7) C(906) 0.189(14) 0.119(10) 0.149(12) 0.046(10) 0.086(11) 0.013(9) # 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(20) 1.885(3) ? Ta O(10) 1.900(3) ? Ta C(30) 2.223(4) ? Ta Cl(1) 2.3051(15) ? Ta Cl(2) 2.3429(13) ? O(10) C(11) 1.364(5) ? O(20) C(21) 1.358(5) ? C(11) C(12) 1.395(6) ? C(11) C(16) 1.411(6) ? C(12) C(13) 1.414(6) ? C(12) C(121) 1.489(6) ? C(13) C(14) 1.392(6) ? C(13) C(131) 1.494(6) ? C(14) C(15) 1.386(6) ? C(15) C(16) 1.396(6) ? C(15) C(151) 1.512(6) ? C(16) C(161) 1.494(6) ? C(21) C(22) 1.414(6) ? C(21) C(26) 1.415(6) ? C(22) C(23) 1.401(6) ? C(22) C(221) 1.493(6) ? C(23) C(24) 1.388(6) ? C(23) C(231) 1.498(6) ? C(24) C(25) 1.390(6) ? C(25) C(26) 1.406(6) ? C(25) C(251) 1.492(6) ? C(26) C(261) 1.495(6) ? C(30) C(31) 1.479(7) ? C(31) C(32) 1.411(9) ? C(31) C(36) 1.429(9) ? C(32) C(33) 1.373(11) ? C(33) C(34) 1.363(13) ? C(34) C(35) 1.358(13) ? C(35) C(36) 1.359(10) ? C(121) C(122) 1.389(7) ? C(121) C(126) 1.397(8) ? C(122) C(123) 1.392(8) ? C(123) C(124) 1.358(11) ? C(124) C(125) 1.375(11) ? C(125) C(126) 1.394(8) ? C(131) C(132) 1.392(7) ? C(131) C(136) 1.394(7) ? C(132) C(133) 1.387(6) ? C(133) C(134) 1.373(8) ? C(134) C(135) 1.385(8) ? C(135) C(136) 1.385(7) ? C(151) C(156) 1.380(7) ? C(151) C(152) 1.392(7) ? C(152) C(153) 1.384(7) ? C(153) C(154) 1.371(8) ? C(154) C(155) 1.370(8) ? C(155) C(156) 1.382(7) ? C(161) C(162) 1.383(7) ? C(161) C(166) 1.397(7) ? C(162) C(163) 1.383(7) ? C(163) C(164) 1.379(9) ? C(164) C(165) 1.370(9) ? C(165) C(166) 1.393(7) ? C(221) C(226) 1.383(7) ? C(221) C(222) 1.386(7) ? C(222) C(223) 1.390(8) ? C(223) C(224) 1.379(9) ? C(224) C(225) 1.374(9) ? C(225) C(226) 1.381(8) ? C(231) C(232) 1.375(7) ? C(231) C(236) 1.385(7) ? C(232) C(233) 1.386(8) ? C(233) C(234) 1.377(10) ? C(234) C(235) 1.370(10) ? C(235) C(236) 1.377(8) ? C(251) C(252) 1.392(7) ? C(251) C(256) 1.396(7) ? C(252) C(253) 1.391(8) ? C(253) C(254) 1.376(9) ? C(254) C(255) 1.374(9) ? C(255) C(256) 1.387(8) ? C(261) C(266) 1.388(8) ? C(261) C(262) 1.389(8) ? C(262) C(263) 1.384(9) ? C(263) C(264) 1.396(13) ? C(264) C(265) 1.378(13) ? C(265) C(266) 1.409(9) ? C(901) C(906) 1.324(18) ? C(901) C(902) 1.349(16) ? C(902) C(903) 1.380(15) ? C(903) C(904) 1.379(14) ? C(904) C(905) 1.371(16) ? C(905) C(906) 1.378(16) ? 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(20) Ta O(10) 170.25(13) ? O(20) Ta C(30) 91.32(14) ? O(10) Ta C(30) 91.62(14) ? O(20) Ta Cl(1) 93.31(11) ? O(10) Ta Cl(1) 93.74(10) ? C(30) Ta Cl(1) 116.11(12) ? O(20) Ta Cl(2) 86.11(11) ? O(10) Ta Cl(2) 84.37(10) ? C(30) Ta Cl(2) 120.27(12) ? Cl(1) Ta Cl(2) 123.62(6) ? C(11) O(10) Ta 155.8(3) ? C(21) O(20) Ta 166.7(3) ? O(10) C(11) C(12) 119.1(4) ? O(10) C(11) C(16) 118.6(4) ? C(12) C(11) C(16) 122.3(4) ? C(11) C(12) C(13) 118.6(4) ? C(11) C(12) C(121) 120.0(4) ? C(13) C(12) C(121) 121.4(4) ? C(14) C(13) C(12) 118.6(4) ? C(14) C(13) C(131) 117.3(4) ? C(12) C(13) C(131) 124.1(4) ? C(15) C(14) C(13) 122.5(4) ? C(14) C(15) C(16) 119.8(4) ? C(14) C(15) C(151) 117.3(4) ? C(16) C(15) C(151) 122.7(4) ? C(15) C(16) C(11) 118.1(4) ? C(15) C(16) C(161) 121.0(4) ? C(11) C(16) C(161) 120.8(4) ? O(20) C(21) C(22) 119.2(4) ? O(20) C(21) C(26) 119.0(4) ? C(22) C(21) C(26) 121.8(4) ? C(23) C(22) C(21) 118.8(4) ? C(23) C(22) C(221) 120.7(4) ? C(21) C(22) C(221) 120.5(4) ? C(24) C(23) C(22) 119.1(4) ? C(24) C(23) C(231) 118.8(4) ? C(22) C(23) C(231) 122.1(4) ? C(23) C(24) C(25) 122.5(4) ? C(24) C(25) C(26) 119.8(4) ? C(24) C(25) C(251) 116.9(4) ? C(26) C(25) C(251) 123.3(4) ? C(25) C(26) C(21) 117.9(4) ? C(25) C(26) C(261) 121.3(4) ? C(21) C(26) C(261) 120.8(4) ? C(31) C(30) Ta 93.6(3) ? C(32) C(31) C(36) 117.4(7) ? C(32) C(31) C(30) 120.4(6) ? C(36) C(31) C(30) 122.2(5) ? C(33) C(32) C(31) 120.0(8) ? C(34) C(33) C(32) 120.0(8) ? C(35) C(34) C(33) 122.3(9) ? C(34) C(35) C(36) 119.5(9) ? C(35) C(36) C(31) 120.7(7) ? C(122) C(121) C(126) 118.8(5) ? C(122) C(121) C(12) 121.1(5) ? C(126) C(121) C(12) 119.8(4) ? C(121) C(122) C(123) 120.1(6) ? C(124) C(123) C(122) 120.4(6) ? C(123) C(124) C(125) 120.7(6) ? C(124) C(125) C(126) 119.8(7) ? C(125) C(126) C(121) 120.1(6) ? C(132) C(131) C(136) 117.8(4) ? C(132) C(131) C(13) 123.1(4) ? C(136) C(131) C(13) 119.0(4) ? C(133) C(132) C(131) 120.6(5) ? C(134) C(133) C(132) 121.1(5) ? C(133) C(134) C(135) 119.1(5) ? C(134) C(135) C(136) 120.2(5) ? C(135) C(136) C(131) 121.3(5) ? C(156) C(151) C(152) 118.2(4) ? C(156) C(151) C(15) 123.0(4) ? C(152) C(151) C(15) 118.8(4) ? C(153) C(152) C(151) 120.7(5) ? C(154) C(153) C(152) 120.2(5) ? C(155) C(154) C(153) 119.6(5) ? C(154) C(155) C(156) 120.5(5) ? C(151) C(156) C(155) 120.8(5) ? C(162) C(161) C(166) 118.9(4) ? C(162) C(161) C(16) 120.2(4) ? C(166) C(161) C(16) 120.8(4) ? C(161) C(162) C(163) 120.8(5) ? C(164) C(163) C(162) 120.2(5) ? C(165) C(164) C(163) 119.6(5) ? C(164) C(165) C(166) 120.8(5) ? C(165) C(166) C(161) 119.6(5) ? C(226) C(221) C(222) 119.4(5) ? C(226) C(221) C(22) 120.6(4) ? C(222) C(221) C(22) 119.9(4) ? C(221) C(222) C(223) 120.0(5) ? C(224) C(223) C(222) 120.2(6) ? C(225) C(224) C(223) 119.7(5) ? C(224) C(225) C(226) 120.5(6) ? C(225) C(226) C(221) 120.2(5) ? C(232) C(231) C(236) 118.4(5) ? C(232) C(231) C(23) 122.3(4) ? C(236) C(231) C(23) 119.3(4) ? C(231) C(232) C(233) 120.6(6) ? C(234) C(233) C(232) 120.6(6) ? C(235) C(234) C(233) 118.9(6) ? C(234) C(235) C(236) 120.7(6) ? C(235) C(236) C(231) 120.8(5) ? C(252) C(251) C(256) 117.7(5) ? C(252) C(251) C(25) 120.1(4) ? C(256) C(251) C(25) 121.9(4) ? C(253) C(252) C(251) 121.2(5) ? C(254) C(253) C(252) 120.1(5) ? C(255) C(254) C(253) 119.6(5) ? C(254) C(255) C(256) 120.7(6) ? C(255) C(256) C(251) 120.7(5) ? C(266) C(261) C(262) 120.2(5) ? C(266) C(261) C(26) 120.7(5) ? C(262) C(261) C(26) 119.1(5) ? C(263) C(262) C(261) 120.4(7) ? C(262) C(263) C(264) 120.3(8) ? C(265) C(264) C(263) 119.0(6) ? C(264) C(265) C(266) 121.4(7) ? C(261) C(266) C(265) 118.6(7) ? C(906) C(901) C(902) 122.6(13) ? C(901) C(902) C(903) 119.9(12) ? C(904) C(903) C(902) 118.8(11) ? C(905) C(904) C(903) 118.7(12) ? C(904) C(905) C(906) 121.4(13) ? C(901) C(906) C(905) 118.2(14) ? #===END #============================================================================== data_SS213B _database_code_CSD 164010 _audit_creation_date 30-10-00 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.34 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C40 H37 Cl2 O2 Si1 Ta1' _chemical_formula_structural ? _chemical_formula_weight 829.68 _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 15.3362(3) _cell_length_b 12.7656(2) _cell_length_c 18.5286(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.3177(11) _cell_angle_gamma 90.00 _cell_volume 3611.84(19) _cell_measurement_reflns_used 34144 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.53 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.221 _cell_measurement_temperature 150 _exptl_crystal_F_000 1656 # 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 0.0664 _exptl_absorpt_correction_T_max 0.3372 _diffrn_reflns_number 34144 _reflns_number_total 8132 _reflns_number_gt 7228 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 23 # 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 0.031 _refine_ls_wR_factor_ref 0.073 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 8132 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0441P)^2^+1.5360P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.98 _refine_diff_density_min -1.60 _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 0.249387(8) 0.228032(10) 0.215427(6) 0.01763(4) Uani ? Cl(1) 0.22213(6) 0.16605(7) 0.32743(4) 0.0313(2) Uani ? Cl(2) 0.36310(5) 0.21822(6) 0.13872(5) 0.0269(2) Uani ? Si(1) 0.05593(6) 0.36857(8) 0.22739(6) 0.0296(3) Uani ? O(1) 0.21328(14) 0.09851(17) 0.17126(11) 0.0220(6) Uani ? O(2) 0.30505(14) 0.34840(16) 0.25499(11) 0.0195(6) Uani ? C(1) 0.1411(2) 0.3133(3) 0.17091(17) 0.0233(8) Uani ? C(2) -0.0110(3) 0.4602(3) 0.1664(2) 0.0433(12) Uani ? C(3) 0.1066(3) 0.4404(3) 0.3080(2) 0.0435(12) Uani ? C(4) -0.0137(3) 0.2597(4) 0.2566(3) 0.0548(16) Uani ? C(11) 0.2345(2) 0.0245(3) 0.12201(17) 0.0229(8) Uani ? C(12) 0.2882(2) -0.0593(3) 0.14560(18) 0.0247(9) Uani ? C(13) 0.3177(2) -0.1262(3) 0.09326(19) 0.0309(10) Uani ? C(14) 0.2934(3) -0.1100(3) 0.0202(2) 0.0391(12) Uani ? C(15) 0.2366(3) -0.0296(3) -0.00155(19) 0.0364(10) Uani ? C(16) 0.2054(2) 0.0388(3) 0.04860(18) 0.0280(9) Uani ? C(21) 0.34959(19) 0.4307(2) 0.28694(16) 0.0184(7) Uani ? C(22) 0.3366(2) 0.5319(3) 0.25733(17) 0.0213(8) Uani ? C(23) 0.3738(2) 0.6173(3) 0.29633(18) 0.0256(9) Uani ? C(24) 0.4245(2) 0.6032(3) 0.36180(18) 0.0266(9) Uani ? C(25) 0.4408(2) 0.5024(3) 0.38806(17) 0.0239(8) Uani ? C(26) 0.4039(2) 0.4145(2) 0.35123(16) 0.0193(8) Uani ? C(121) 0.3117(2) -0.0787(2) 0.22426(18) 0.0233(8) Uani ? C(122) 0.2467(2) -0.0922(3) 0.2711(2) 0.0323(10) Uani ? C(123) 0.2676(3) -0.1158(3) 0.3435(2) 0.0363(10) Uani ? C(124) 0.3538(3) -0.1249(3) 0.3708(2) 0.0351(9) Uani ? C(125) 0.4191(3) -0.1117(3) 0.3252(2) 0.0325(10) Uani ? C(126) 0.3983(2) -0.0882(3) 0.25255(19) 0.0276(9) Uani ? C(161) 0.1425(2) 0.1241(3) 0.02648(17) 0.0292(9) Uani ? C(162) 0.1695(3) 0.2148(3) -0.0072(2) 0.0329(10) Uani ? C(163) 0.1105(3) 0.2954(3) -0.0251(2) 0.0396(12) Uani ? C(164) 0.0241(3) 0.2854(4) -0.0114(2) 0.0434(12) Uani ? C(165) -0.0041(3) 0.1953(4) 0.0198(3) 0.0488(14) Uani ? C(166) 0.0550(3) 0.1154(3) 0.0398(2) 0.0382(10) Uani ? C(221) 0.2878(2) 0.5512(3) 0.18562(17) 0.0235(8) Uani ? C(222) 0.3076(2) 0.4956(3) 0.12431(17) 0.0255(9) Uani ? C(223) 0.2661(2) 0.5198(3) 0.05651(19) 0.0325(10) Uani ? C(224) 0.2047(3) 0.5994(3) 0.04904(19) 0.0375(12) Uani ? C(225) 0.1847(3) 0.6552(3) 0.1095(2) 0.0378(10) Uani ? C(226) 0.2261(2) 0.6317(3) 0.17689(19) 0.0296(9) Uani ? C(261) 0.4279(2) 0.3089(3) 0.37840(16) 0.0213(8) Uani ? C(262) 0.4247(2) 0.2829(3) 0.4512(2) 0.0289(10) Uani ? C(263) 0.4531(3) 0.1855(3) 0.47725(19) 0.0357(10) Uani ? C(264) 0.4866(3) 0.1138(3) 0.4312(2) 0.0388(12) Uani ? C(265) 0.4897(2) 0.1381(3) 0.35854(19) 0.0289(9) Uani ? C(266) 0.4606(2) 0.2344(3) 0.33250(18) 0.0214(8) Uani ? H(13) 0.3541 -0.1821 0.1077 0.0400 Uiso calc H(14) 0.3154 -0.1533 -0.0142 0.0510 Uiso calc H(15) 0.2189 -0.0210 -0.0506 0.0470 Uiso calc H(1A) 0.1639 0.3718 0.1451 0.0300 Uiso calc H(1B) 0.1103 0.2686 0.1346 0.0300 Uiso calc H(23) 0.3644 0.6846 0.2781 0.0330 Uiso calc H(24) 0.4473 0.6608 0.3878 0.0350 Uiso calc H(25) 0.4768 0.4930 0.4308 0.0310 Uiso calc H(2A) -0.0545 0.4931 0.1929 0.0570 Uiso calc H(2B) -0.0394 0.4219 0.1263 0.0570 Uiso calc H(2C) 0.0263 0.5128 0.1486 0.0570 Uiso calc H(3A) 0.1453 0.4934 0.2927 0.0570 Uiso calc H(3B) 0.1391 0.3923 0.3399 0.0570 Uiso calc H(3C) 0.0615 0.4727 0.3330 0.0570 Uiso calc H(4A) -0.0614 0.2881 0.2804 0.0710 Uiso calc H(4B) 0.0209 0.2148 0.2895 0.0710 Uiso calc H(4C) -0.0363 0.2201 0.2150 0.0710 Uiso calc H(122) 0.1883 -0.0852 0.2534 0.0420 Uiso calc H(123) 0.2233 -0.1254 0.3739 0.0470 Uiso calc H(124) 0.3680 -0.1400 0.4196 0.0460 Uiso calc H(125) 0.4775 -0.1185 0.3432 0.0420 Uiso calc H(126) 0.4429 -0.0788 0.2224 0.0360 Uiso calc H(162) 0.2274 0.2214 -0.0177 0.0430 Uiso calc H(163) 0.1294 0.3563 -0.0464 0.0520 Uiso calc H(164) -0.0152 0.3395 -0.0233 0.0560 Uiso calc H(165) -0.0628 0.1877 0.0276 0.0640 Uiso calc H(166) 0.0358 0.0556 0.0622 0.0500 Uiso calc H(222) 0.3488 0.4421 0.1289 0.0330 Uiso calc H(223) 0.2797 0.4823 0.0160 0.0420 Uiso calc H(224) 0.1769 0.6153 0.0036 0.0490 Uiso calc H(225) 0.1434 0.7087 0.1047 0.0490 Uiso calc H(226) 0.2127 0.6700 0.2171 0.0380 Uiso calc H(262) 0.4033 0.3313 0.4826 0.0380 Uiso calc H(263) 0.4495 0.1685 0.5257 0.0460 Uiso calc H(264) 0.5070 0.0493 0.4489 0.0500 Uiso calc H(265) 0.5114 0.0895 0.3274 0.0380 Uiso calc H(266) 0.4627 0.2501 0.2837 0.0280 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 0.01693(8) 0.01889(8) 0.01685(8) -0.00110(5) 0.00044(5) -0.00141(5) Cl(1) 0.0423(5) 0.0322(5) 0.0201(4) -0.0079(4) 0.0068(3) -0.0006(3) Cl(2) 0.0225(4) 0.0325(5) 0.0269(4) -0.0023(3) 0.0082(3) -0.0045(3) Si(1) 0.0233(5) 0.0283(5) 0.0380(5) 0.0025(4) 0.0078(4) 0.0033(4) O(1) 0.0218(11) 0.0227(11) 0.0214(11) -0.0001(9) 0.0014(9) -0.0006(9) O(2) 0.0184(11) 0.0190(11) 0.0203(11) 0.0009(9) -0.0019(8) 0.0010(8) C(1) 0.0184(15) 0.0247(16) 0.0258(16) -0.0011(13) -0.0035(12) -0.0018(14) C(2) 0.029(2) 0.042(2) 0.060(3) 0.0115(18) 0.0093(19) 0.008(2) C(3) 0.052(3) 0.042(2) 0.038(2) 0.012(2) 0.0127(19) -0.0053(18) C(4) 0.035(2) 0.049(3) 0.083(4) -0.002(2) 0.019(2) 0.022(2) C(11) 0.0272(17) 0.0194(16) 0.0228(16) -0.0045(13) 0.0064(13) -0.0062(12) C(12) 0.0288(18) 0.0196(16) 0.0264(17) -0.0014(14) 0.0068(14) -0.0022(13) C(13) 0.038(2) 0.0234(18) 0.0324(19) 0.0052(15) 0.0086(16) -0.0022(14) C(14) 0.055(3) 0.035(2) 0.029(2) 0.0068(19) 0.0136(18) -0.0069(16) C(15) 0.049(2) 0.038(2) 0.0216(18) 0.0006(18) 0.0008(16) -0.0040(15) C(16) 0.0308(18) 0.0281(18) 0.0249(17) -0.0014(15) 0.0009(14) -0.0039(14) C(21) 0.0173(15) 0.0204(15) 0.0176(14) -0.0014(12) 0.0019(11) -0.0013(12) C(22) 0.0194(15) 0.0234(16) 0.0213(15) -0.0019(13) 0.0032(12) 0.0007(12) C(23) 0.0278(18) 0.0196(16) 0.0294(17) -0.0022(13) 0.0026(14) -0.0015(13) C(24) 0.0262(18) 0.0255(17) 0.0278(17) -0.0061(14) 0.0012(14) -0.0055(14) C(25) 0.0220(16) 0.0294(18) 0.0196(15) -0.0036(14) -0.0025(12) -0.0040(13) C(26) 0.0184(15) 0.0223(16) 0.0173(14) -0.0020(12) 0.0014(12) -0.0002(12) C(121) 0.0266(17) 0.0167(15) 0.0271(17) 0.0000(13) 0.0051(13) -0.0013(13) C(122) 0.0294(19) 0.035(2) 0.0325(19) 0.0032(15) 0.0028(15) 0.0030(16) C(123) 0.040(2) 0.041(2) 0.0296(19) 0.0052(18) 0.0118(16) 0.0064(16) C(124) 0.053(2) 0.0239(18) 0.0275(18) 0.0064(17) -0.0008(17) 0.0028(14) C(125) 0.032(2) 0.0279(19) 0.036(2) 0.0035(15) -0.0047(15) -0.0010(15) C(126) 0.0270(18) 0.0236(17) 0.0325(18) 0.0012(14) 0.0051(14) 0.0011(14) C(161) 0.0311(19) 0.037(2) 0.0185(16) 0.0002(15) -0.0032(13) -0.0059(14) C(162) 0.033(2) 0.039(2) 0.0272(19) 0.0069(16) 0.0049(16) 0.0021(15) C(163) 0.051(3) 0.043(2) 0.0245(19) 0.0110(19) 0.0012(17) 0.0066(16) C(164) 0.036(2) 0.059(3) 0.033(2) 0.015(2) -0.0088(17) -0.0028(19) C(165) 0.026(2) 0.064(3) 0.054(3) -0.003(2) -0.0084(19) -0.007(2) C(166) 0.034(2) 0.042(2) 0.037(2) -0.0077(18) -0.0057(17) -0.0036(17) C(221) 0.0212(16) 0.0230(17) 0.0257(17) -0.0038(13) -0.0003(13) 0.0046(13) C(222) 0.0264(17) 0.0290(18) 0.0213(16) -0.0009(14) 0.0036(13) 0.0035(13) C(223) 0.034(2) 0.042(2) 0.0218(17) -0.0064(17) 0.0036(15) 0.0021(15) C(224) 0.032(2) 0.057(3) 0.0223(18) 0.0018(18) -0.0046(15) 0.0098(17) C(225) 0.033(2) 0.041(2) 0.038(2) 0.0104(17) -0.0034(16) 0.0084(17) C(226) 0.0294(19) 0.0291(19) 0.0296(18) 0.0008(15) -0.0004(15) 0.0003(15) C(261) 0.0199(15) 0.0251(16) 0.0182(15) -0.0002(13) -0.0013(12) -0.0002(13) C(262) 0.0294(19) 0.033(2) 0.0241(18) 0.0039(15) 0.0018(14) -0.0027(14) C(263) 0.046(2) 0.038(2) 0.0232(18) 0.0080(19) 0.0041(16) 0.0100(16) C(264) 0.056(3) 0.031(2) 0.0291(19) 0.0121(18) 0.0029(18) 0.0098(16) C(265) 0.0329(19) 0.0274(18) 0.0267(17) 0.0067(15) 0.0051(14) 0.0019(14) C(266) 0.0215(16) 0.0243(17) 0.0180(16) -0.0009(13) -0.0003(12) 0.0029(12) # 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) 1.874(2) ? Ta O(1) 1.904(2) ? Ta C(1) 2.090(3) ? Ta Cl(1) 2.2952(8) ? Ta Cl(2) 2.3529(8) ? Si(1) C(3) 1.860(4) ? Si(1) C(4) 1.863(4) ? Si(1) C(2) 1.867(4) ? Si(1) C(1) 1.885(3) ? O(1) C(11) 1.373(4) ? O(2) C(21) 1.359(4) ? C(11) C(12) 1.395(5) ? C(11) C(16) 1.403(5) ? C(12) C(13) 1.399(4) ? C(12) C(121) 1.489(5) ? C(13) C(14) 1.385(5) ? C(14) C(15) 1.383(6) ? C(15) C(16) 1.391(5) ? C(16) C(161) 1.488(5) ? C(21) C(26) 1.404(4) ? C(21) C(22) 1.410(4) ? C(22) C(23) 1.399(5) ? C(22) C(221) 1.484(4) ? C(23) C(24) 1.390(5) ? C(24) C(25) 1.390(5) ? C(25) C(26) 1.405(4) ? C(26) C(261) 1.474(5) ? C(121) C(126) 1.387(5) ? C(121) C(122) 1.391(5) ? C(122) C(123) 1.384(5) ? C(123) C(124) 1.376(6) ? C(124) C(125) 1.379(5) ? C(125) C(126) 1.387(5) ? C(161) C(166) 1.391(5) ? C(161) C(162) 1.396(5) ? C(162) C(163) 1.390(5) ? C(163) C(164) 1.379(6) ? C(164) C(165) 1.375(7) ? C(165) C(166) 1.391(6) ? C(221) C(222) 1.396(5) ? C(221) C(226) 1.397(5) ? C(222) C(223) 1.389(5) ? C(223) C(224) 1.384(6) ? C(224) C(225) 1.386(5) ? C(225) C(226) 1.380(5) ? C(261) C(262) 1.394(5) ? C(261) C(266) 1.398(5) ? C(262) C(263) 1.389(5) ? C(263) C(264) 1.382(5) ? C(264) C(265) 1.386(5) ? C(265) C(266) 1.380(5) ? 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) 169.71(9) ? O(2) Ta C(1) 92.52(11) ? O(1) Ta C(1) 95.38(11) ? O(2) Ta Cl(1) 92.49(7) ? O(1) Ta Cl(1) 91.10(7) ? C(1) Ta Cl(1) 109.37(9) ? O(2) Ta Cl(2) 86.77(7) ? O(1) Ta Cl(2) 84.06(7) ? C(1) Ta Cl(2) 113.30(9) ? Cl(1) Ta Cl(2) 137.31(3) ? C(3) Si(1) C(4) 110.0(2) ? C(3) Si(1) C(2) 110.0(2) ? C(4) Si(1) C(2) 110.2(2) ? C(3) Si(1) C(1) 111.78(17) ? C(4) Si(1) C(1) 109.1(2) ? C(2) Si(1) C(1) 105.61(16) ? C(11) O(1) Ta 143.7(2) ? C(21) O(2) Ta 175.6(2) ? Si(1) C(1) Ta 122.83(16) ? O(1) C(11) C(12) 119.2(3) ? O(1) C(11) C(16) 118.8(3) ? C(12) C(11) C(16) 121.9(3) ? C(11) C(12) C(13) 118.1(3) ? C(11) C(12) C(121) 121.1(3) ? C(13) C(12) C(121) 120.8(3) ? C(14) C(13) C(12) 120.7(3) ? C(15) C(14) C(13) 120.1(3) ? C(14) C(15) C(16) 121.1(3) ? C(15) C(16) C(11) 117.9(3) ? C(15) C(16) C(161) 122.0(3) ? C(11) C(16) C(161) 120.1(3) ? O(2) C(21) C(26) 119.3(3) ? O(2) C(21) C(22) 119.5(3) ? C(26) C(21) C(22) 121.1(3) ? C(23) C(22) C(21) 118.4(3) ? C(23) C(22) C(221) 118.8(3) ? C(21) C(22) C(221) 122.8(3) ? C(24) C(23) C(22) 121.2(3) ? C(25) C(24) C(23) 119.5(3) ? C(24) C(25) C(26) 121.2(3) ? C(21) C(26) C(25) 118.4(3) ? C(21) C(26) C(261) 122.3(3) ? C(25) C(26) C(261) 119.2(3) ? C(126) C(121) C(122) 118.0(3) ? C(126) C(121) C(12) 121.4(3) ? C(122) C(121) C(12) 120.6(3) ? C(123) C(122) C(121) 121.1(3) ? C(124) C(123) C(122) 120.2(3) ? C(123) C(124) C(125) 119.5(3) ? C(124) C(125) C(126) 120.4(3) ? C(125) C(126) C(121) 120.8(3) ? C(166) C(161) C(162) 118.5(4) ? C(166) C(161) C(16) 120.3(3) ? C(162) C(161) C(16) 121.2(3) ? C(163) C(162) C(161) 120.4(4) ? C(164) C(163) C(162) 120.2(4) ? C(163) C(164) C(165) 120.0(4) ? C(164) C(165) C(166) 120.2(4) ? C(161) C(166) C(165) 120.6(4) ? C(222) C(221) C(226) 118.4(3) ? C(222) C(221) C(22) 121.0(3) ? C(226) C(221) C(22) 120.4(3) ? C(223) C(222) C(221) 120.5(3) ? C(224) C(223) C(222) 120.2(3) ? C(223) C(224) C(225) 119.7(3) ? C(226) C(225) C(224) 120.1(4) ? C(225) C(226) C(221) 121.0(3) ? C(262) C(261) C(266) 118.3(3) ? C(262) C(261) C(26) 121.2(3) ? C(266) C(261) C(26) 120.4(3) ? C(263) C(262) C(261) 120.8(3) ? C(264) C(263) C(262) 120.0(3) ? C(263) C(264) C(265) 120.0(3) ? C(266) C(265) C(264) 120.0(3) ? C(265) C(266) C(261) 121.0(3) ? #===END #============================================================================== data_SS28G _database_code_CSD 164011 _audit_creation_date 2-06-99 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C64 H53 Cl2 Nb O2 Si' _chemical_formula_structural ? _chemical_formula_weight 1046.03 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9783(4) _cell_length_b 12.5003(6) _cell_length_c 22.6124(13) _cell_angle_alpha 97.143(3) _cell_angle_beta 91.442(3) _cell_angle_gamma 108.890(3) _cell_volume 2641.4(5) _cell_measurement_reflns_used 24738 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.32 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.384 _cell_measurement_temperature 193 _exptl_crystal_F_000 1084 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.6505 _exptl_absorpt_correction_T_max 0.9716 _diffrn_reflns_number 24738 _reflns_number_total 9225 _reflns_number_gt 6411 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.137 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 26 # 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 0.066 _refine_ls_wR_factor_ref 0.116 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 9225 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.33 _refine_diff_density_min -0.60 _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 Nb 0.22609(4) 0.33587(3) 0.241307(17) 0.02204(12) Uani ? Cl(1) 0.41080(11) 0.34410(10) 0.17716(5) 0.0352(4) Uani ? Cl(2) 0.06669(12) 0.19228(9) 0.28371(5) 0.0356(4) Uani ? Si(31) 0.02281(14) 0.49738(12) 0.30254(6) 0.0369(5) Uani ? O(4) 0.3638(3) 0.3599(2) 0.30427(12) 0.0225(9) Uani ? O(5) 0.1105(3) 0.3103(2) 0.16986(12) 0.0253(9) Uani ? C(30) 0.1911(4) 0.4885(3) 0.2675(2) 0.0269(13) Uani ? C(32) -0.1388(5) 0.3811(5) 0.2696(3) 0.062(2) Uani ? C(33) 0.0081(6) 0.6358(5) 0.2856(3) 0.059(2) Uani ? C(34) 0.0483(6) 0.4984(6) 0.3845(2) 0.065(3) Uani ? C(41) 0.4751(4) 0.3719(4) 0.34380(18) 0.0239(14) Uani ? C(42) 0.5011(4) 0.2741(3) 0.35836(18) 0.0236(12) Uani ? C(43) 0.6047(4) 0.2872(4) 0.40405(19) 0.0272(14) Uani ? C(44) 0.6730(4) 0.3959(4) 0.4354(2) 0.0289(15) Uani ? C(45) 0.6512(4) 0.4934(3) 0.42008(19) 0.0241(12) Uani ? C(46) 0.5529(4) 0.4827(3) 0.37228(18) 0.0221(12) Uani ? C(51) 0.0693(4) 0.2881(4) 0.11029(18) 0.0216(12) Uani ? C(52) -0.0317(4) 0.1817(3) 0.08850(18) 0.0213(12) Uani ? C(53) -0.0797(4) 0.1590(4) 0.02831(18) 0.0239(12) Uani ? C(54) -0.0149(4) 0.2387(4) -0.00924(19) 0.0249(14) Uani ? C(55) 0.0899(4) 0.3427(4) 0.01144(18) 0.0223(12) Uani ? C(56) 0.1287(4) 0.3711(3) 0.07332(18) 0.0222(12) Uani ? C(421) 0.4148(5) 0.1593(4) 0.3272(2) 0.0290(15) Uani ? C(422) 0.3267(5) 0.0781(4) 0.3583(2) 0.0354(17) Uani ? C(423) 0.2462(6) -0.0284(4) 0.3301(3) 0.048(2) Uani ? C(424) 0.2499(5) -0.0562(4) 0.2698(2) 0.0461(19) Uani ? C(425) 0.3364(6) 0.0221(4) 0.2377(2) 0.047(2) Uani ? C(426) 0.4185(5) 0.1295(4) 0.2664(2) 0.0348(17) Uani ? C(431) 0.6456(5) 0.1896(4) 0.4199(2) 0.0301(15) Uani ? C(432) 0.6913(5) 0.1213(4) 0.3781(2) 0.0455(18) Uani ? C(433) 0.7306(5) 0.0313(4) 0.3935(3) 0.056(2) Uani ? C(434) 0.7215(6) 0.0065(5) 0.4508(3) 0.062(3) Uani ? C(435) 0.6774(6) 0.0747(5) 0.4928(3) 0.064(2) Uani ? C(436) 0.6391(6) 0.1655(5) 0.4780(2) 0.052(2) Uani ? C(451) 0.7338(4) 0.6059(3) 0.45563(19) 0.0243(14) Uani ? C(452) 0.8228(5) 0.6947(4) 0.4293(2) 0.0354(17) Uani ? C(453) 0.9068(5) 0.7945(4) 0.4640(3) 0.0454(19) Uani ? C(454) 0.9007(5) 0.8075(4) 0.5252(3) 0.0482(19) Uani ? C(455) 0.8114(5) 0.7224(4) 0.5515(2) 0.0474(18) Uani ? C(456) 0.7284(5) 0.6222(4) 0.5173(2) 0.0368(17) Uani ? C(461) 0.5308(4) 0.5831(3) 0.34990(19) 0.0230(13) Uani ? C(462) 0.4795(5) 0.6591(4) 0.3857(2) 0.0325(17) Uani ? C(463) 0.4584(5) 0.7509(4) 0.3633(2) 0.0398(17) Uani ? C(464) 0.4892(5) 0.7693(4) 0.3054(2) 0.0411(17) Uani ? C(465) 0.5398(5) 0.6946(4) 0.2699(2) 0.0359(17) Uani ? C(466) 0.5612(4) 0.6031(4) 0.29152(19) 0.0272(15) Uani ? C(521) -0.0877(4) 0.0969(4) 0.13069(18) 0.0268(12) Uani ? C(522) -0.0142(5) 0.0237(4) 0.1427(2) 0.0399(17) Uani ? C(523) -0.0680(7) -0.0590(4) 0.1799(2) 0.057(2) Uani ? C(524) -0.1923(8) -0.0662(5) 0.2059(3) 0.071(3) Uani ? C(525) -0.2672(6) 0.0058(6) 0.1953(2) 0.061(2) Uani ? C(526) -0.2145(5) 0.0871(4) 0.1571(2) 0.0410(17) Uani ? C(531) -0.1980(4) 0.0555(4) 0.00087(18) 0.0252(14) Uani ? C(532) -0.3055(4) 0.0712(4) -0.03440(19) 0.0333(17) Uani ? C(533) -0.4152(5) -0.0215(5) -0.0628(2) 0.0421(18) Uani ? C(534) -0.4210(5) -0.1313(5) -0.0573(2) 0.0462(18) Uani ? C(535) -0.3153(5) -0.1484(4) -0.0222(2) 0.0479(19) Uani ? C(536) -0.2051(5) -0.0560(4) 0.0073(2) 0.0329(17) Uani ? C(551) 0.1524(4) 0.4181(4) -0.03396(18) 0.0263(14) Uani ? C(552) 0.1689(4) 0.5346(4) -0.0279(2) 0.0301(15) Uani ? C(553) 0.2228(5) 0.5998(4) -0.0723(2) 0.0382(17) Uani ? C(554) 0.2620(5) 0.5497(5) -0.1240(2) 0.045(2) Uani ? C(555) 0.2462(5) 0.4362(5) -0.1313(2) 0.049(2) Uani ? C(556) 0.1916(5) 0.3697(4) -0.0872(2) 0.0361(17) Uani ? C(561) 0.2200(4) 0.4898(4) 0.09799(19) 0.0253(12) Uani ? C(562) 0.3633(5) 0.5319(4) 0.0866(2) 0.0356(17) Uani ? C(563) 0.4395(5) 0.6493(5) 0.1020(2) 0.0489(19) Uani ? C(564) 0.3742(6) 0.7212(4) 0.1290(2) 0.049(2) Uani ? C(565) 0.2343(6) 0.6803(4) 0.1413(2) 0.042(2) Uani ? C(566) 0.1578(5) 0.5649(4) 0.12572(19) 0.0302(17) Uani ? H(44) 0.7358 0.4032 0.4680 0.0370 Uiso calc H(54) -0.0428 0.2216 -0.0498 0.0320 Uiso calc H(30A) 0.2698 0.5341 0.2956 0.0350 Uiso calc H(30B) 0.1995 0.5272 0.2325 0.0350 Uiso calc H(32A) -0.2212 0.3961 0.2843 0.0810 Uiso calc H(32B) -0.1365 0.3099 0.2805 0.0810 Uiso calc H(32C) -0.1425 0.3769 0.2269 0.0810 Uiso calc H(33A) 0.0047 0.6360 0.2432 0.0770 Uiso calc H(33B) 0.0890 0.6976 0.3041 0.0770 Uiso calc H(33C) -0.0770 0.6450 0.3009 0.0770 Uiso calc H(34A) -0.0323 0.5087 0.4036 0.0840 Uiso calc H(34B) 0.1325 0.5598 0.4002 0.0840 Uiso calc H(34C) 0.0578 0.4271 0.3919 0.0840 Uiso calc H(422) 0.3220 0.0961 0.3992 0.0460 Uiso calc H(423) 0.1891 -0.0816 0.3520 0.0630 Uiso calc H(424) 0.1942 -0.1276 0.2506 0.0600 Uiso calc H(425) 0.3401 0.0033 0.1969 0.0610 Uiso calc H(426) 0.4767 0.1820 0.2443 0.0450 Uiso calc H(432) 0.6958 0.1361 0.3388 0.0590 Uiso calc H(433) 0.7633 -0.0125 0.3648 0.0730 Uiso calc H(434) 0.7447 -0.0554 0.4611 0.0800 Uiso calc H(435) 0.6732 0.0596 0.5320 0.0840 Uiso calc H(436) 0.6090 0.2103 0.5071 0.0680 Uiso calc H(452) 0.8261 0.6871 0.3880 0.0460 Uiso calc H(453) 0.9675 0.8528 0.4460 0.0590 Uiso calc H(454) 0.9575 0.8744 0.5484 0.0620 Uiso calc H(455) 0.8062 0.7317 0.5927 0.0610 Uiso calc H(456) 0.6680 0.5647 0.5359 0.0480 Uiso calc H(462) 0.4595 0.6477 0.4248 0.0420 Uiso calc H(463) 0.4234 0.8004 0.3872 0.0520 Uiso calc H(464) 0.4760 0.8315 0.2904 0.0530 Uiso calc H(465) 0.5596 0.7065 0.2308 0.0470 Uiso calc H(466) 0.5961 0.5541 0.2671 0.0350 Uiso calc H(522) 0.0715 0.0299 0.1258 0.0520 Uiso calc H(523) -0.0196 -0.1090 0.1871 0.0740 Uiso calc H(524) -0.2271 -0.1207 0.2311 0.0920 Uiso calc H(525) -0.3514 0.0003 0.2134 0.0800 Uiso calc H(526) -0.2650 0.1351 0.1492 0.0530 Uiso calc H(532) -0.3032 0.1448 -0.0388 0.0430 Uiso calc H(533) -0.4860 -0.0096 -0.0860 0.0550 Uiso calc H(534) -0.4947 -0.1933 -0.0767 0.0600 Uiso calc H(535) -0.3182 -0.2223 -0.0184 0.0620 Uiso calc H(536) -0.1361 -0.0684 0.0314 0.0430 Uiso calc H(552) 0.1429 0.5688 0.0068 0.0390 Uiso calc H(553) 0.2328 0.6770 -0.0674 0.0500 Uiso calc H(554) 0.2991 0.5934 -0.1538 0.0590 Uiso calc H(555) 0.2723 0.4030 -0.1663 0.0630 Uiso calc H(556) 0.1810 0.2924 -0.0930 0.0470 Uiso calc H(562) 0.4082 0.4827 0.0689 0.0460 Uiso calc H(563) 0.5344 0.6778 0.0938 0.0630 Uiso calc H(564) 0.4251 0.7985 0.1391 0.0630 Uiso calc H(565) 0.1907 0.7296 0.1600 0.0540 Uiso calc H(566) 0.0629 0.5378 0.1341 0.0400 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 Nb 0.0238(2) 0.0216(2) 0.0183(2) 0.00453(17) -0.00289(16) 0.00274(16) Cl(1) 0.0327(6) 0.0466(7) 0.0301(7) 0.0162(6) 0.0064(5) 0.0096(6) Cl(2) 0.0391(6) 0.0313(7) 0.0292(7) 0.0004(5) -0.0022(5) 0.0088(5) Si(31) 0.0355(7) 0.0433(9) 0.0383(8) 0.0190(7) 0.0078(6) 0.0123(7) O(4) 0.0254(15) 0.0212(15) 0.0205(16) 0.0088(13) -0.0060(12) 0.0002(12) O(5) 0.0260(15) 0.0248(16) 0.0216(16) 0.0037(13) -0.0033(13) 0.0035(13) C(30) 0.026(2) 0.021(2) 0.031(3) 0.0057(19) -0.0034(19) 0.0007(19) C(32) 0.041(3) 0.067(4) 0.080(5) 0.015(3) -0.002(3) 0.022(3) C(33) 0.071(4) 0.064(4) 0.063(4) 0.047(3) 0.017(3) 0.018(3) C(34) 0.068(4) 0.097(5) 0.044(4) 0.043(4) 0.016(3) 0.018(3) C(41) 0.025(2) 0.029(3) 0.017(2) 0.008(2) 0.0005(18) 0.0036(19) C(42) 0.030(2) 0.019(2) 0.020(2) 0.0061(19) -0.0030(19) 0.0028(18) C(43) 0.028(2) 0.026(2) 0.026(3) 0.009(2) -0.0037(19) -0.001(2) C(44) 0.031(2) 0.031(3) 0.027(3) 0.014(2) -0.005(2) 0.004(2) C(45) 0.026(2) 0.023(2) 0.024(2) 0.0096(19) -0.0001(19) 0.0023(19) C(46) 0.022(2) 0.023(2) 0.022(2) 0.0075(19) 0.0033(18) 0.0056(19) C(51) 0.021(2) 0.028(2) 0.016(2) 0.0083(19) 0.0003(17) 0.0039(19) C(52) 0.021(2) 0.024(2) 0.019(2) 0.0077(19) -0.0001(18) 0.0031(18) C(53) 0.026(2) 0.025(2) 0.023(2) 0.0130(19) -0.0034(19) -0.0001(19) C(54) 0.029(2) 0.032(3) 0.017(2) 0.016(2) -0.0025(18) 0.0004(19) C(55) 0.024(2) 0.026(2) 0.020(2) 0.0120(19) 0.0006(18) 0.0052(19) C(56) 0.019(2) 0.024(2) 0.025(2) 0.0085(19) -0.0007(18) 0.0047(19) C(421) 0.034(3) 0.024(2) 0.030(3) 0.012(2) -0.006(2) 0.003(2) C(422) 0.047(3) 0.024(3) 0.034(3) 0.011(2) -0.002(2) 0.003(2) C(423) 0.061(4) 0.025(3) 0.056(4) 0.009(3) -0.009(3) 0.010(3) C(424) 0.054(3) 0.023(3) 0.053(4) 0.007(2) -0.018(3) -0.006(3) C(425) 0.069(4) 0.042(3) 0.031(3) 0.029(3) -0.012(3) -0.012(3) C(426) 0.048(3) 0.029(3) 0.029(3) 0.018(2) -0.003(2) -0.003(2) C(431) 0.032(3) 0.024(2) 0.036(3) 0.012(2) -0.006(2) 0.005(2) C(432) 0.045(3) 0.042(3) 0.049(3) 0.018(3) -0.013(3) -0.002(3) C(433) 0.049(3) 0.038(3) 0.087(5) 0.028(3) -0.015(3) -0.004(3) C(434) 0.054(4) 0.033(3) 0.102(6) 0.015(3) -0.023(4) 0.025(4) C(435) 0.081(4) 0.059(4) 0.068(4) 0.038(4) -0.007(4) 0.028(4) C(436) 0.079(4) 0.047(3) 0.043(3) 0.036(3) -0.004(3) 0.012(3) C(451) 0.025(2) 0.024(2) 0.025(3) 0.010(2) -0.0030(19) 0.003(2) C(452) 0.033(3) 0.035(3) 0.035(3) 0.009(2) 0.001(2) -0.001(2) C(453) 0.034(3) 0.031(3) 0.064(4) 0.003(2) 0.005(3) 0.001(3) C(454) 0.042(3) 0.035(3) 0.058(4) 0.009(3) -0.020(3) -0.015(3) C(455) 0.051(3) 0.049(3) 0.036(3) 0.014(3) -0.013(3) -0.007(3) C(456) 0.042(3) 0.036(3) 0.028(3) 0.009(2) -0.008(2) 0.001(2) C(461) 0.019(2) 0.022(2) 0.025(3) 0.0033(19) -0.0021(18) 0.0020(19) C(462) 0.041(3) 0.033(3) 0.026(3) 0.016(2) -0.004(2) 0.004(2) C(463) 0.051(3) 0.029(3) 0.042(3) 0.018(2) 0.000(3) 0.002(2) C(464) 0.053(3) 0.020(3) 0.052(3) 0.011(2) -0.007(3) 0.016(2) C(465) 0.032(3) 0.034(3) 0.038(3) 0.003(2) -0.004(2) 0.014(2) C(466) 0.025(2) 0.026(3) 0.027(3) 0.003(2) -0.0019(19) 0.006(2) C(521) 0.032(2) 0.025(2) 0.017(2) 0.002(2) -0.0047(19) 0.0008(19) C(522) 0.048(3) 0.032(3) 0.033(3) 0.005(2) -0.006(2) 0.004(2) C(523) 0.084(4) 0.029(3) 0.050(4) 0.007(3) -0.013(3) 0.009(3) C(524) 0.080(5) 0.052(4) 0.048(4) -0.027(4) -0.012(4) 0.024(3) C(525) 0.042(3) 0.073(5) 0.042(4) -0.021(3) 0.003(3) 0.016(3) C(526) 0.031(3) 0.046(3) 0.035(3) -0.002(2) -0.002(2) 0.006(2) C(531) 0.027(2) 0.028(3) 0.018(2) 0.007(2) 0.0012(19) -0.0011(19) C(532) 0.037(3) 0.034(3) 0.027(3) 0.010(2) -0.006(2) 0.004(2) C(533) 0.035(3) 0.051(3) 0.032(3) 0.007(3) -0.008(2) -0.004(3) C(534) 0.037(3) 0.045(3) 0.039(3) -0.003(3) -0.001(2) -0.014(3) C(535) 0.044(3) 0.035(3) 0.053(4) 0.003(3) 0.008(3) -0.011(3) C(536) 0.035(3) 0.029(3) 0.033(3) 0.010(2) 0.001(2) 0.000(2) C(551) 0.023(2) 0.038(3) 0.019(2) 0.010(2) -0.0031(18) 0.009(2) C(552) 0.024(2) 0.038(3) 0.027(3) 0.007(2) -0.0019(19) 0.009(2) C(553) 0.029(3) 0.042(3) 0.047(3) 0.010(2) -0.001(2) 0.024(3) C(554) 0.032(3) 0.061(4) 0.051(4) 0.015(3) 0.011(2) 0.037(3) C(555) 0.043(3) 0.080(4) 0.037(3) 0.033(3) 0.017(2) 0.024(3) C(556) 0.035(3) 0.046(3) 0.034(3) 0.020(2) 0.007(2) 0.012(2) C(561) 0.026(2) 0.025(2) 0.025(2) 0.007(2) -0.0055(19) 0.009(2) C(562) 0.029(3) 0.034(3) 0.044(3) 0.008(2) -0.006(2) 0.014(2) C(563) 0.036(3) 0.044(3) 0.059(4) -0.005(3) -0.013(3) 0.031(3) C(564) 0.060(4) 0.030(3) 0.050(4) 0.007(3) -0.021(3) 0.011(3) C(565) 0.062(4) 0.026(3) 0.038(3) 0.016(3) -0.008(3) 0.005(2) C(566) 0.038(3) 0.026(3) 0.026(3) 0.009(2) -0.003(2) 0.007(2) # 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 Nb O(4) 1.880(3) ? Nb O(5) 1.892(3) ? Nb C(30) 2.068(4) ? Nb Cl(2) 2.3080(11) ? Nb Cl(1) 2.3580(12) ? Si(31) C(32) 1.849(5) ? Si(31) C(34) 1.862(5) ? Si(31) C(33) 1.868(5) ? Si(31) C(30) 1.903(4) ? O(4) C(41) 1.365(5) ? O(5) C(51) 1.366(4) ? C(41) C(42) 1.404(6) ? C(41) C(46) 1.411(5) ? C(42) C(43) 1.399(6) ? C(42) C(421) 1.488(6) ? C(43) C(44) 1.396(6) ? C(43) C(431) 1.485(6) ? C(44) C(45) 1.389(6) ? C(45) C(46) 1.404(6) ? C(45) C(451) 1.496(6) ? C(46) C(461) 1.487(6) ? C(51) C(52) 1.404(5) ? C(51) C(56) 1.404(5) ? C(52) C(53) 1.395(5) ? C(52) C(521) 1.497(6) ? C(53) C(54) 1.398(6) ? C(53) C(531) 1.492(5) ? C(54) C(55) 1.395(5) ? C(55) C(56) 1.412(5) ? C(55) C(551) 1.491(6) ? C(56) C(561) 1.495(5) ? C(421) C(426) 1.384(6) ? C(421) C(422) 1.390(6) ? C(422) C(423) 1.376(6) ? C(423) C(424) 1.369(7) ? C(424) C(425) 1.374(7) ? C(425) C(426) 1.392(6) ? C(431) C(432) 1.378(7) ? C(431) C(436) 1.383(7) ? C(432) C(433) 1.386(7) ? C(433) C(434) 1.366(8) ? C(434) C(435) 1.372(8) ? C(435) C(436) 1.383(7) ? C(451) C(452) 1.388(6) ? C(451) C(456) 1.390(6) ? C(452) C(453) 1.387(6) ? C(453) C(454) 1.377(7) ? C(454) C(455) 1.360(7) ? C(455) C(456) 1.381(6) ? C(461) C(466) 1.396(6) ? C(461) C(462) 1.402(6) ? C(462) C(463) 1.384(6) ? C(463) C(464) 1.382(7) ? C(464) C(465) 1.382(7) ? C(465) C(466) 1.374(6) ? C(521) C(526) 1.389(6) ? C(521) C(522) 1.391(7) ? C(522) C(523) 1.395(7) ? C(523) C(524) 1.366(8) ? C(524) C(525) 1.380(9) ? C(525) C(526) 1.397(7) ? C(531) C(536) 1.398(6) ? C(531) C(532) 1.399(6) ? C(532) C(533) 1.383(6) ? C(533) C(534) 1.376(7) ? C(534) C(535) 1.390(7) ? C(535) C(536) 1.392(6) ? C(551) C(556) 1.402(6) ? C(551) C(552) 1.400(6) ? C(552) C(553) 1.382(6) ? C(553) C(554) 1.383(7) ? C(554) C(555) 1.363(7) ? C(555) C(556) 1.386(6) ? C(561) C(566) 1.382(6) ? C(561) C(562) 1.398(6) ? C(562) C(563) 1.411(6) ? C(563) C(564) 1.366(7) ? C(564) C(565) 1.372(7) ? C(565) C(566) 1.391(6) ? 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(4) Nb O(5) 170.89(12) ? O(4) Nb C(30) 93.60(14) ? O(5) Nb C(30) 91.15(15) ? O(4) Nb Cl(2) 91.35(9) ? O(5) Nb Cl(2) 94.40(8) ? C(30) Nb Cl(2) 109.37(12) ? O(4) Nb Cl(1) 86.20(9) ? O(5) Nb Cl(1) 84.73(9) ? C(30) Nb Cl(1) 116.02(12) ? Cl(2) Nb Cl(1) 134.60(5) ? C(32) Si(31) C(34) 111.6(3) ? C(32) Si(31) C(33) 108.3(3) ? C(34) Si(31) C(33) 111.2(3) ? C(32) Si(31) C(30) 113.0(2) ? C(34) Si(31) C(30) 107.8(2) ? C(33) Si(31) C(30) 104.7(2) ? C(41) O(4) Nb 171.6(3) ? C(51) O(5) Nb 159.9(3) ? Si(31) C(30) Nb 123.2(2) ? O(4) C(41) C(42) 119.4(4) ? O(4) C(41) C(46) 118.1(4) ? C(42) C(41) C(46) 122.3(4) ? C(43) C(42) C(41) 118.5(4) ? C(43) C(42) C(421) 121.5(4) ? C(41) C(42) C(421) 119.9(4) ? C(42) C(43) C(44) 118.9(4) ? C(42) C(43) C(431) 122.2(4) ? C(44) C(43) C(431) 118.9(4) ? C(45) C(44) C(43) 122.8(4) ? C(44) C(45) C(46) 119.0(4) ? C(44) C(45) C(451) 118.2(4) ? C(46) C(45) C(451) 122.8(4) ? C(45) C(46) C(41) 118.2(4) ? C(45) C(46) C(461) 122.6(4) ? C(41) C(46) C(461) 119.2(4) ? O(5) C(51) C(52) 118.0(3) ? O(5) C(51) C(56) 119.4(3) ? C(52) C(51) C(56) 122.6(4) ? C(53) C(52) C(51) 119.0(4) ? C(53) C(52) C(521) 121.7(3) ? C(51) C(52) C(521) 119.2(4) ? C(52) C(53) C(54) 118.4(4) ? C(52) C(53) C(531) 124.5(4) ? C(54) C(53) C(531) 117.1(4) ? C(55) C(54) C(53) 122.9(4) ? C(54) C(55) C(56) 118.8(4) ? C(54) C(55) C(551) 117.1(4) ? C(56) C(55) C(551) 124.1(3) ? C(51) C(56) C(55) 117.8(3) ? C(51) C(56) C(561) 122.1(4) ? C(55) C(56) C(561) 119.8(4) ? C(426) C(421) C(422) 117.6(4) ? C(426) C(421) C(42) 121.6(4) ? C(422) C(421) C(42) 120.9(4) ? C(423) C(422) C(421) 121.5(5) ? C(424) C(423) C(422) 120.3(5) ? C(425) C(424) C(423) 119.6(4) ? C(424) C(425) C(426) 120.2(5) ? C(421) C(426) C(425) 120.9(4) ? C(432) C(431) C(436) 118.2(5) ? C(432) C(431) C(43) 121.9(4) ? C(436) C(431) C(43) 119.9(4) ? C(431) C(432) C(433) 121.4(5) ? C(434) C(433) C(432) 120.2(6) ? C(433) C(434) C(435) 118.7(5) ? C(434) C(435) C(436) 121.5(6) ? C(431) C(436) C(435) 119.9(5) ? C(452) C(451) C(456) 117.9(4) ? C(452) C(451) C(45) 122.0(4) ? C(456) C(451) C(45) 120.1(4) ? C(451) C(452) C(453) 120.6(5) ? C(454) C(453) C(452) 120.2(5) ? C(455) C(454) C(453) 119.8(5) ? C(454) C(455) C(456) 120.4(5) ? C(455) C(456) C(451) 121.1(5) ? C(466) C(461) C(462) 118.4(4) ? C(466) C(461) C(46) 119.7(4) ? C(462) C(461) C(46) 121.9(4) ? C(463) C(462) C(461) 120.5(4) ? C(464) C(463) C(462) 120.2(5) ? C(463) C(464) C(465) 119.5(5) ? C(466) C(465) C(464) 120.9(5) ? C(465) C(466) C(461) 120.5(4) ? C(526) C(521) C(522) 118.8(4) ? C(526) C(521) C(52) 121.3(4) ? C(522) C(521) C(52) 119.9(4) ? C(521) C(522) C(523) 120.5(5) ? C(524) C(523) C(522) 119.6(6) ? C(523) C(524) C(525) 121.3(5) ? C(524) C(525) C(526) 119.0(6) ? C(521) C(526) C(525) 120.8(5) ? C(536) C(531) C(532) 118.5(4) ? C(536) C(531) C(53) 123.5(4) ? C(532) C(531) C(53) 118.0(4) ? C(533) C(532) C(531) 120.7(5) ? C(534) C(533) C(532) 120.9(5) ? C(533) C(534) C(535) 119.2(5) ? C(534) C(535) C(536) 120.7(5) ? C(535) C(536) C(531) 120.1(5) ? C(556) C(551) C(552) 117.4(4) ? C(556) C(551) C(55) 118.8(4) ? C(552) C(551) C(55) 123.8(4) ? C(553) C(552) C(551) 121.5(4) ? C(552) C(553) C(554) 119.7(5) ? C(555) C(554) C(553) 120.1(5) ? C(554) C(555) C(556) 120.8(5) ? C(555) C(556) C(551) 120.6(5) ? C(566) C(561) C(562) 118.5(4) ? C(566) C(561) C(56) 119.3(4) ? C(562) C(561) C(56) 121.5(4) ? C(561) C(562) C(563) 119.7(5) ? C(564) C(563) C(562) 120.2(5) ? C(563) C(564) C(565) 120.6(5) ? C(564) C(565) C(566) 119.7(5) ? C(561) C(566) C(565) 121.3(4) ? #===END #============================================================================== data_SS280 _database_code_CSD 164012 _audit_creation_date 13-09-99 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour pale yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C41 H35 Cl2 O2 Ta' _chemical_formula_structural ? _chemical_formula_weight 811.59 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9773(6) _cell_length_b 11.4412(6) _cell_length_c 16.3041(9) _cell_angle_alpha 101.983(3) _cell_angle_beta 94.502(3) _cell_angle_gamma 110.754(3) _cell_volume 1678.8(4) _cell_measurement_reflns_used 13777 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.430 _cell_measurement_temperature 193 _exptl_crystal_F_000 808 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.5164 _exptl_absorpt_correction_T_max 0.5978 _diffrn_reflns_number 13777 _reflns_number_total 7063 _reflns_number_gt 5893 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 20 # 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 0.043 _refine_ls_wR_factor_ref 0.097 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7063 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.16 _refine_diff_density_min -2.12 _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 0.17075(2) 0.46474(2) 0.220118(13) 0.02326(8) Uani ? Cl(1) 0.17663(17) 0.33989(14) 0.08658(9) 0.0382(5) Uani ? Cl(2) 0.39818(17) 0.46217(17) 0.26557(10) 0.0421(6) Uani ? O(1) 0.1791(4) 0.5372(3) 0.3377(2) 0.0258(12) Uani ? O(2) -0.0307(4) 0.3956(3) 0.2015(2) 0.0280(12) Uani ? C(1) 0.2205(6) 0.6342(5) 0.1768(3) 0.0260(18) Uani ? C(2) 0.3635(6) 0.6699(6) 0.1370(4) 0.0365(19) Uani ? C(3) 0.3448(7) 0.7601(6) 0.0839(4) 0.044(2) Uani ? C(4) 0.1872(7) 0.6980(7) 0.0439(4) 0.046(2) Uani ? C(5) 0.1037(6) 0.6355(6) 0.1078(4) 0.036(2) Uani ? C(11) 0.2638(5) 0.5769(5) 0.4166(3) 0.0220(18) Uani ? C(12) 0.2444(6) 0.4927(5) 0.4692(3) 0.0258(18) Uani ? C(13) 0.3431(6) 0.5334(6) 0.5460(3) 0.0320(19) Uani ? C(14) 0.4528(6) 0.6538(6) 0.5696(4) 0.0343(19) Uani ? C(15) 0.4655(6) 0.7387(5) 0.5183(4) 0.0320(18) Uani ? C(16) 0.3720(6) 0.7020(5) 0.4421(3) 0.0284(18) Uani ? C(21) -0.1734(6) 0.3124(5) 0.1818(3) 0.0263(18) Uani ? C(22) -0.2792(6) 0.3654(5) 0.1762(4) 0.0302(19) Uani ? C(23) -0.4238(6) 0.2801(6) 0.1475(4) 0.038(2) Uani ? C(24) -0.4604(7) 0.1478(6) 0.1268(4) 0.040(2) Uani ? C(25) -0.3542(7) 0.0974(6) 0.1344(4) 0.0374(19) Uani ? C(26) -0.2085(6) 0.1784(5) 0.1620(3) 0.0286(18) Uani ? C(121) 0.1241(6) 0.3629(5) 0.4498(3) 0.0273(18) Uani ? C(122) -0.0201(6) 0.3476(6) 0.4263(4) 0.0319(19) Uani ? C(123) -0.1321(6) 0.2287(6) 0.4140(4) 0.0367(19) Uani ? C(124) -0.1004(7) 0.1225(6) 0.4238(4) 0.041(2) Uani ? C(125) 0.0415(7) 0.1370(6) 0.4459(4) 0.038(2) Uani ? C(126) 0.1517(7) 0.2562(6) 0.4588(4) 0.0334(19) Uani ? C(161) 0.3835(6) 0.7990(5) 0.3910(3) 0.0294(19) Uani ? C(162) 0.2711(7) 0.8433(6) 0.3808(4) 0.035(2) Uani ? C(163) 0.2838(8) 0.9380(6) 0.3386(4) 0.040(2) Uani ? C(164) 0.4088(8) 0.9897(6) 0.3056(4) 0.043(2) Uani ? C(165) 0.5210(8) 0.9479(6) 0.3154(4) 0.045(2) Uani ? C(166) 0.5082(7) 0.8528(6) 0.3584(4) 0.0380(19) Uani ? C(221) -0.2416(6) 0.5077(5) 0.1965(4) 0.0293(18) Uani ? C(222) -0.1599(6) 0.5881(6) 0.2741(4) 0.0339(19) Uani ? C(223) -0.1307(7) 0.7196(6) 0.2938(4) 0.043(2) Uani ? C(224) -0.1815(8) 0.7727(7) 0.2346(5) 0.049(3) Uani ? C(225) -0.2608(7) 0.6951(7) 0.1577(5) 0.043(2) Uani ? C(226) -0.2928(6) 0.5621(6) 0.1388(4) 0.039(2) Uani ? C(261) -0.0965(6) 0.1214(5) 0.1633(3) 0.0284(18) Uani ? C(262) -0.1061(7) 0.0173(5) 0.0975(4) 0.0339(19) Uani ? C(263) -0.0033(7) -0.0375(6) 0.0972(4) 0.040(2) Uani ? C(264) 0.1153(7) 0.0122(6) 0.1621(4) 0.037(2) Uani ? C(265) 0.1272(7) 0.1139(6) 0.2283(4) 0.036(2) Uani ? C(266) 0.0217(6) 0.1681(5) 0.2305(3) 0.0308(19) Uani ? H(1) 0.2352 0.7055 0.2262 0.0340 Uiso calc H(13) 0.3337 0.4776 0.5813 0.0420 Uiso calc H(14) 0.5182 0.6783 0.6197 0.0440 Uiso calc H(15) 0.5376 0.8212 0.5354 0.0420 Uiso calc H(23) -0.4963 0.3127 0.1423 0.0490 Uiso calc H(24) -0.5569 0.0924 0.1076 0.0520 Uiso calc H(25) -0.3803 0.0083 0.1210 0.0490 Uiso calc H(2A) 0.4490 0.7134 0.1808 0.0480 Uiso calc H(2B) 0.3708 0.5937 0.1017 0.0480 Uiso calc H(3A) 0.3672 0.8461 0.1195 0.0570 Uiso calc H(3B) 0.4071 0.7659 0.0409 0.0570 Uiso calc H(4A) 0.1740 0.6334 -0.0084 0.0590 Uiso calc H(4B) 0.1527 0.7624 0.0307 0.0590 Uiso calc H(5A) 0.0363 0.5482 0.0803 0.0470 Uiso calc H(5B) 0.0494 0.6849 0.1332 0.0470 Uiso calc H(122) -0.0409 0.4181 0.4188 0.0410 Uiso calc H(123) -0.2279 0.2196 0.3993 0.0480 Uiso calc H(124) -0.1751 0.0421 0.4153 0.0540 Uiso calc H(125) 0.0630 0.0662 0.4521 0.0490 Uiso calc H(126) 0.2472 0.2648 0.4741 0.0430 Uiso calc H(162) 0.1867 0.8084 0.4029 0.0450 Uiso calc H(163) 0.2087 0.9673 0.3324 0.0520 Uiso calc H(164) 0.4170 1.0531 0.2765 0.0560 Uiso calc H(165) 0.6050 0.9833 0.2932 0.0590 Uiso calc H(166) 0.5845 0.8250 0.3653 0.0490 Uiso calc H(222) -0.1244 0.5531 0.3133 0.0440 Uiso calc H(223) -0.0774 0.7721 0.3463 0.0560 Uiso calc H(224) -0.1614 0.8610 0.2473 0.0650 Uiso calc H(225) -0.2936 0.7307 0.1179 0.0570 Uiso calc H(226) -0.3490 0.5096 0.0870 0.0510 Uiso calc H(262) -0.1838 -0.0158 0.0527 0.0440 Uiso calc H(263) -0.0136 -0.1081 0.0533 0.0520 Uiso calc H(264) 0.1864 -0.0230 0.1610 0.0490 Uiso calc H(265) 0.2064 0.1469 0.2722 0.0470 Uiso calc H(266) 0.0296 0.2352 0.2764 0.0400 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 0.02402(13) 0.02337(12) 0.02034(12) 0.00801(9) 0.00259(8) 0.00339(9) Cl(1) 0.0464(9) 0.0326(7) 0.0265(7) 0.0093(7) 0.0093(6) -0.0027(6) Cl(2) 0.0367(8) 0.0633(10) 0.0351(8) 0.0313(8) 0.0052(6) 0.0095(7) O(1) 0.0204(18) 0.0245(19) 0.027(2) 0.0029(16) 0.0024(15) 0.0057(16) O(2) 0.030(2) 0.0219(18) 0.027(2) 0.0059(17) 0.0018(16) 0.0036(16) C(1) 0.028(3) 0.024(3) 0.022(3) 0.007(2) 0.001(2) 0.004(2) C(2) 0.026(3) 0.038(3) 0.039(3) 0.003(3) 0.007(3) 0.012(3) C(3) 0.047(4) 0.043(4) 0.041(4) 0.009(3) 0.015(3) 0.017(3) C(4) 0.050(4) 0.054(4) 0.031(3) 0.013(3) 0.012(3) 0.017(3) C(5) 0.027(3) 0.042(3) 0.041(4) 0.010(3) 0.006(3) 0.019(3) C(11) 0.020(3) 0.027(3) 0.021(3) 0.011(2) 0.003(2) 0.007(2) C(12) 0.024(3) 0.031(3) 0.024(3) 0.012(2) 0.006(2) 0.007(2) C(13) 0.037(3) 0.041(3) 0.020(3) 0.017(3) -0.001(2) 0.010(2) C(14) 0.031(3) 0.041(3) 0.025(3) 0.011(3) -0.002(2) 0.003(3) C(15) 0.023(3) 0.027(3) 0.035(3) 0.002(2) -0.001(2) 0.000(2) C(16) 0.030(3) 0.024(3) 0.027(3) 0.008(2) 0.003(2) 0.002(2) C(21) 0.022(3) 0.026(3) 0.024(3) 0.002(2) 0.003(2) 0.005(2) C(22) 0.026(3) 0.033(3) 0.030(3) 0.008(3) 0.011(2) 0.008(2) C(23) 0.025(3) 0.046(4) 0.042(4) 0.010(3) 0.009(3) 0.013(3) C(24) 0.025(3) 0.038(3) 0.046(4) -0.001(3) 0.006(3) 0.008(3) C(25) 0.036(3) 0.029(3) 0.039(3) 0.000(3) 0.015(3) 0.010(3) C(26) 0.031(3) 0.027(3) 0.026(3) 0.006(2) 0.005(2) 0.012(2) C(121) 0.024(3) 0.031(3) 0.021(3) 0.005(2) 0.006(2) 0.003(2) C(122) 0.035(3) 0.037(3) 0.028(3) 0.020(3) 0.008(2) 0.005(3) C(123) 0.025(3) 0.038(3) 0.038(3) 0.007(3) 0.003(3) 0.000(3) C(124) 0.043(4) 0.037(3) 0.032(3) 0.001(3) 0.014(3) 0.006(3) C(125) 0.041(4) 0.033(3) 0.042(4) 0.012(3) 0.015(3) 0.017(3) C(126) 0.035(3) 0.035(3) 0.031(3) 0.013(3) 0.005(3) 0.011(3) C(161) 0.036(3) 0.024(3) 0.024(3) 0.007(3) 0.000(2) 0.007(2) C(162) 0.045(4) 0.033(3) 0.029(3) 0.016(3) 0.006(3) 0.008(3) C(163) 0.056(4) 0.033(3) 0.034(3) 0.025(3) 0.000(3) 0.004(3) C(164) 0.063(5) 0.028(3) 0.032(3) 0.013(3) -0.005(3) 0.007(3) C(165) 0.046(4) 0.035(3) 0.035(4) -0.008(3) 0.002(3) 0.011(3) C(166) 0.036(3) 0.035(3) 0.034(3) 0.005(3) 0.000(3) 0.007(3) C(221) 0.028(3) 0.028(3) 0.033(3) 0.009(2) 0.013(2) 0.010(2) C(222) 0.037(3) 0.035(3) 0.033(3) 0.016(3) 0.013(3) 0.009(3) C(223) 0.043(4) 0.043(4) 0.042(4) 0.020(3) 0.008(3) 0.001(3) C(224) 0.045(4) 0.035(3) 0.076(5) 0.018(3) 0.027(4) 0.019(4) C(225) 0.039(4) 0.047(4) 0.058(4) 0.023(3) 0.016(3) 0.028(4) C(226) 0.028(3) 0.044(4) 0.047(4) 0.012(3) 0.006(3) 0.017(3) C(261) 0.035(3) 0.019(3) 0.025(3) 0.001(2) 0.007(2) 0.008(2) C(262) 0.039(3) 0.027(3) 0.030(3) 0.007(3) 0.003(3) 0.006(2) C(263) 0.050(4) 0.028(3) 0.034(3) 0.010(3) 0.009(3) -0.001(3) C(264) 0.049(4) 0.032(3) 0.036(3) 0.021(3) 0.009(3) 0.010(3) C(265) 0.045(4) 0.032(3) 0.032(3) 0.017(3) 0.002(3) 0.009(3) C(266) 0.046(3) 0.023(3) 0.025(3) 0.014(3) 0.006(3) 0.008(2) # 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) 1.854(4) ? Ta O(1) 1.907(4) ? Ta C(1) 2.108(5) ? Ta Cl(2) 2.3434(14) ? Ta Cl(1) 2.3605(14) ? O(1) C(11) 1.374(6) ? O(2) C(21) 1.370(6) ? C(1) C(5) 1.561(7) ? C(1) C(2) 1.569(8) ? C(2) C(3) 1.527(8) ? C(3) C(4) 1.503(9) ? C(4) C(5) 1.521(8) ? C(11) C(12) 1.392(7) ? C(11) C(16) 1.405(7) ? C(12) C(13) 1.412(7) ? C(12) C(121) 1.493(8) ? C(13) C(14) 1.375(8) ? C(14) C(15) 1.387(8) ? C(15) C(16) 1.383(7) ? C(16) C(161) 1.500(7) ? C(21) C(22) 1.398(7) ? C(21) C(26) 1.405(7) ? C(22) C(23) 1.400(8) ? C(22) C(221) 1.492(8) ? C(23) C(24) 1.384(9) ? C(24) C(25) 1.383(8) ? C(25) C(26) 1.394(8) ? C(26) C(261) 1.481(8) ? C(121) C(126) 1.377(8) ? C(121) C(122) 1.398(7) ? C(122) C(123) 1.384(8) ? C(123) C(124) 1.396(8) ? C(124) C(125) 1.375(9) ? C(125) C(126) 1.377(8) ? C(161) C(166) 1.382(8) ? C(161) C(162) 1.397(8) ? C(162) C(163) 1.374(8) ? C(163) C(164) 1.382(9) ? C(164) C(165) 1.374(10) ? C(165) C(166) 1.387(8) ? C(221) C(226) 1.388(8) ? C(221) C(222) 1.390(8) ? C(222) C(223) 1.388(8) ? C(223) C(224) 1.395(9) ? C(224) C(225) 1.367(10) ? C(225) C(226) 1.399(9) ? C(261) C(262) 1.397(8) ? C(261) C(266) 1.408(8) ? C(262) C(263) 1.380(8) ? C(263) C(264) 1.386(8) ? C(264) C(265) 1.376(8) ? C(265) C(266) 1.398(8) ? 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) 91.97(15) ? O(2) Ta C(1) 103.18(18) ? O(1) Ta C(1) 99.01(18) ? O(2) Ta Cl(2) 152.62(12) ? O(1) Ta Cl(2) 84.11(11) ? C(1) Ta Cl(2) 104.20(15) ? O(2) Ta Cl(1) 91.53(12) ? O(1) Ta Cl(1) 166.66(11) ? C(1) Ta Cl(1) 92.71(15) ? Cl(2) Ta Cl(1) 86.87(6) ? C(11) O(1) Ta 143.7(3) ? C(21) O(2) Ta 163.7(3) ? C(5) C(1) C(2) 104.2(4) ? C(5) C(1) Ta 116.7(4) ? C(2) C(1) Ta 113.8(3) ? C(3) C(2) C(1) 102.6(5) ? C(4) C(3) C(2) 103.8(5) ? C(3) C(4) C(5) 107.1(5) ? C(4) C(5) C(1) 105.9(5) ? O(1) C(11) C(12) 120.1(5) ? O(1) C(11) C(16) 119.0(4) ? C(12) C(11) C(16) 120.8(5) ? C(11) C(12) C(13) 118.0(5) ? C(11) C(12) C(121) 123.8(5) ? C(13) C(12) C(121) 118.1(5) ? C(14) C(13) C(12) 121.2(5) ? C(13) C(14) C(15) 119.8(5) ? C(16) C(15) C(14) 120.7(5) ? C(15) C(16) C(11) 119.3(5) ? C(15) C(16) C(161) 119.1(5) ? C(11) C(16) C(161) 121.5(5) ? O(2) C(21) C(22) 117.7(5) ? O(2) C(21) C(26) 119.9(5) ? C(22) C(21) C(26) 122.2(5) ? C(21) C(22) C(23) 117.7(5) ? C(21) C(22) C(221) 122.1(5) ? C(23) C(22) C(221) 120.1(5) ? C(24) C(23) C(22) 120.9(6) ? C(25) C(24) C(23) 120.4(6) ? C(24) C(25) C(26) 120.9(6) ? C(25) C(26) C(21) 117.9(5) ? C(25) C(26) C(261) 119.4(5) ? C(21) C(26) C(261) 122.6(5) ? C(126) C(121) C(122) 118.3(5) ? C(126) C(121) C(12) 120.7(5) ? C(122) C(121) C(12) 121.0(5) ? C(123) C(122) C(121) 120.7(5) ? C(122) C(123) C(124) 119.5(6) ? C(125) C(124) C(123) 119.8(6) ? C(124) C(125) C(126) 120.0(6) ? C(121) C(126) C(125) 121.7(6) ? C(166) C(161) C(162) 118.7(5) ? C(166) C(161) C(16) 121.1(5) ? C(162) C(161) C(16) 120.0(5) ? C(163) C(162) C(161) 120.7(6) ? C(162) C(163) C(164) 119.8(6) ? C(165) C(164) C(163) 120.4(5) ? C(164) C(165) C(166) 119.7(6) ? C(161) C(166) C(165) 120.7(6) ? C(226) C(221) C(222) 118.5(5) ? C(226) C(221) C(22) 120.1(5) ? C(222) C(221) C(22) 121.3(5) ? C(223) C(222) C(221) 120.9(5) ? C(222) C(223) C(224) 119.7(6) ? C(225) C(224) C(223) 120.0(6) ? C(224) C(225) C(226) 120.1(6) ? C(221) C(226) C(225) 120.7(6) ? C(262) C(261) C(266) 117.6(5) ? C(262) C(261) C(26) 120.5(5) ? C(266) C(261) C(26) 121.9(5) ? C(263) C(262) C(261) 121.6(6) ? C(262) C(263) C(264) 120.3(6) ? C(265) C(264) C(263) 119.5(6) ? C(264) C(265) C(266) 120.8(6) ? C(265) C(266) C(261) 120.2(5) ? #===END #============================================================================== data_SS166 _database_code_CSD 164013 _audit_creation_date 6-08-99 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C42 H37 Cl2 O2 Ta' _chemical_formula_structural ? _chemical_formula_weight 825.62 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1243(5) _cell_length_b 12.5130(6) _cell_length_c 14.9163(5) _cell_angle_alpha 99.192(3) _cell_angle_beta 104.620(3) _cell_angle_gamma 114.392(2) _cell_volume 1745.7(3) _cell_measurement_reflns_used 13498 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.300 _cell_measurement_temperature 193 _exptl_crystal_F_000 824 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.3558 _exptl_absorpt_correction_T_max 0.4759 _diffrn_reflns_number 13498 _reflns_number_total 7340 _reflns_number_gt 6513 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 18 # 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 0.034 _refine_ls_wR_factor_ref 0.081 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7340 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+1.8697P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.94 _refine_diff_density_min -1.29 _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 0.064999(17) 0.290080(14) 0.204326(11) 0.01992(7) Uani ? Cl(4) -0.03511(13) 0.42020(11) 0.23047(10) 0.0408(5) Uani ? Cl(5) -0.16663(11) 0.13691(10) 0.11116(8) 0.0319(4) Uani ? O(2) 0.1189(3) 0.1781(2) 0.2424(2) 0.0218(10) Uani ? O(3) 0.2365(3) 0.4282(3) 0.2933(2) 0.0221(11) Uani ? C(1) 0.1212(5) 0.2983(4) 0.0777(3) 0.0258(15) Uani ? C(2) 0.1044(6) 0.1754(5) 0.0213(3) 0.036(2) Uani ? C(3) 0.1565(7) 0.1904(6) -0.0634(4) 0.049(2) Uani ? C(4) 0.0825(6) 0.2407(5) -0.1306(4) 0.046(2) Uani ? C(5) 0.0947(7) 0.3602(5) -0.0766(4) 0.047(2) Uani ? C(6) 0.0431(6) 0.3470(5) 0.0094(4) 0.039(2) Uani ? C(21) 0.1398(4) 0.0985(4) 0.2909(3) 0.0204(14) Uani ? C(22) 0.2493(4) 0.0723(4) 0.2875(3) 0.0241(15) Uani ? C(23) 0.2681(5) -0.0085(4) 0.3369(3) 0.0317(17) Uani ? C(24) 0.1822(5) -0.0604(5) 0.3884(4) 0.037(2) Uani ? C(25) 0.0732(5) -0.0348(4) 0.3879(3) 0.0306(17) Uani ? C(26) 0.0477(4) 0.0432(4) 0.3384(3) 0.0242(15) Uani ? C(31) 0.2963(4) 0.5458(4) 0.3527(3) 0.0219(14) Uani ? C(32) 0.3475(4) 0.6452(4) 0.3152(3) 0.0243(15) Uani ? C(33) 0.3951(5) 0.7634(4) 0.3738(3) 0.0261(15) Uani ? C(34) 0.3958(5) 0.7844(4) 0.4681(3) 0.0290(15) Uani ? C(35) 0.3535(5) 0.6872(4) 0.5060(3) 0.0263(15) Uani ? C(36) 0.3046(4) 0.5663(4) 0.4497(3) 0.0219(14) Uani ? C(221) 0.3440(4) 0.1247(4) 0.2331(3) 0.0258(15) Uani ? C(222) 0.3559(5) 0.0436(5) 0.1637(4) 0.037(2) Uani ? C(223) 0.4520(6) 0.0883(6) 0.1178(4) 0.047(2) Uani ? C(224) 0.5369(6) 0.2133(6) 0.1405(4) 0.046(2) Uani ? C(225) 0.5215(6) 0.2947(5) 0.2061(4) 0.040(2) Uani ? C(226) 0.4243(5) 0.2499(4) 0.2515(3) 0.0309(17) Uani ? C(261) -0.0751(4) 0.0654(4) 0.3340(3) 0.0227(15) Uani ? C(262) -0.2118(5) -0.0317(4) 0.2865(3) 0.0292(15) Uani ? C(263) -0.3278(5) -0.0129(5) 0.2802(3) 0.0336(17) Uani ? C(264) -0.3069(5) 0.1031(5) 0.3233(3) 0.0361(19) Uani ? C(265) -0.1719(5) 0.1997(5) 0.3705(4) 0.038(2) Uani ? C(266) -0.0575(5) 0.1798(4) 0.3752(3) 0.0314(17) Uani ? C(321) 0.3647(4) 0.6321(4) 0.2190(3) 0.0243(15) Uani ? C(322) 0.3122(5) 0.6837(4) 0.1526(3) 0.0320(19) Uani ? C(323) 0.3494(6) 0.6903(5) 0.0712(4) 0.044(2) Uani ? C(324) 0.4373(6) 0.6441(5) 0.0545(4) 0.043(2) Uani ? C(325) 0.4872(5) 0.5906(5) 0.1172(4) 0.038(2) Uani ? C(326) 0.4492(5) 0.5825(4) 0.1993(3) 0.0289(15) Uani ? C(361) 0.2709(4) 0.4678(4) 0.4978(3) 0.0254(15) Uani ? C(362) 0.3250(5) 0.3857(4) 0.4884(3) 0.0309(17) Uani ? C(363) 0.3057(5) 0.3013(5) 0.5402(4) 0.0418(19) Uani ? C(364) 0.2331(6) 0.2986(5) 0.6029(4) 0.053(2) Uani ? C(365) 0.1765(6) 0.3769(5) 0.6128(4) 0.051(2) Uani ? C(366) 0.1963(5) 0.4622(4) 0.5604(4) 0.0381(19) Uani ? H(1) 0.2218 0.3576 0.1003 0.0330 Uiso calc H(23) 0.3397 -0.0282 0.3354 0.0420 Uiso calc H(24) 0.1984 -0.1119 0.4227 0.0480 Uiso calc H(25) 0.0152 -0.0705 0.4216 0.0400 Uiso calc H(2A) 0.1578 0.1476 0.0646 0.0470 Uiso calc H(2B) 0.0058 0.1136 -0.0030 0.0470 Uiso calc H(33) 0.4271 0.8294 0.3492 0.0340 Uiso calc H(34) 0.4245 0.8635 0.5054 0.0370 Uiso calc H(35) 0.3574 0.7020 0.5701 0.0340 Uiso calc H(3A) 0.2573 0.2458 -0.0384 0.0630 Uiso calc H(3B) 0.1405 0.1113 -0.0998 0.0630 Uiso calc H(4A) -0.0164 0.1805 -0.1622 0.0600 Uiso calc H(4B) 0.1235 0.2544 -0.1806 0.0600 Uiso calc H(5A) 0.0393 0.3856 -0.1209 0.0610 Uiso calc H(5B) 0.1925 0.4238 -0.0528 0.0610 Uiso calc H(6A) 0.0588 0.4263 0.0451 0.0510 Uiso calc H(6B) -0.0574 0.2909 -0.0148 0.0510 Uiso calc H(222) 0.2990 -0.0408 0.1484 0.0480 Uiso calc H(223) 0.4592 0.0339 0.0718 0.0610 Uiso calc H(224) 0.6043 0.2431 0.1119 0.0610 Uiso calc H(225) 0.5762 0.3791 0.2196 0.0520 Uiso calc H(226) 0.4132 0.3045 0.2946 0.0400 Uiso calc H(262) -0.2253 -0.1097 0.2588 0.0380 Uiso calc H(263) -0.4188 -0.0775 0.2474 0.0440 Uiso calc H(264) -0.3842 0.1159 0.3203 0.0460 Uiso calc H(265) -0.1581 0.2775 0.3990 0.0500 Uiso calc H(266) 0.0333 0.2451 0.4070 0.0410 Uiso calc H(322) 0.2517 0.7137 0.1634 0.0420 Uiso calc H(323) 0.3152 0.7258 0.0280 0.0570 Uiso calc H(324) 0.4630 0.6494 0.0001 0.0570 Uiso calc H(325) 0.5463 0.5596 0.1050 0.0500 Uiso calc H(326) 0.4807 0.5438 0.2406 0.0380 Uiso calc H(362) 0.3749 0.3877 0.4467 0.0400 Uiso calc H(363) 0.3417 0.2466 0.5326 0.0540 Uiso calc H(364) 0.2223 0.2432 0.6388 0.0680 Uiso calc H(365) 0.1254 0.3732 0.6540 0.0660 Uiso calc H(366) 0.1589 0.5159 0.5676 0.0490 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 0.01934(10) 0.01846(9) 0.02184(10) 0.00983(7) 0.00529(6) 0.00652(7) Cl(4) 0.0361(6) 0.0355(6) 0.0566(8) 0.0254(5) 0.0129(6) 0.0101(6) Cl(5) 0.0200(5) 0.0321(6) 0.0326(6) 0.0064(4) 0.0034(4) 0.0080(5) O(2) 0.0203(14) 0.0199(14) 0.0249(15) 0.0090(12) 0.0074(11) 0.0082(12) O(3) 0.0256(15) 0.0203(14) 0.0214(15) 0.0119(12) 0.0083(11) 0.0062(12) C(1) 0.026(2) 0.024(2) 0.019(2) 0.0044(18) 0.0086(16) 0.0054(17) C(2) 0.051(3) 0.036(3) 0.029(3) 0.026(2) 0.015(2) 0.013(2) C(3) 0.066(4) 0.055(3) 0.036(3) 0.034(3) 0.026(3) 0.012(3) C(4) 0.053(3) 0.043(3) 0.029(3) 0.013(3) 0.013(2) 0.010(2) C(5) 0.064(4) 0.043(3) 0.036(3) 0.023(3) 0.016(3) 0.023(3) C(6) 0.060(3) 0.035(3) 0.033(3) 0.029(3) 0.018(2) 0.016(2) C(21) 0.0185(19) 0.0182(18) 0.021(2) 0.0082(16) 0.0018(15) 0.0070(16) C(22) 0.021(2) 0.021(2) 0.028(2) 0.0101(17) 0.0055(16) 0.0061(17) C(23) 0.025(2) 0.030(2) 0.043(3) 0.017(2) 0.0089(19) 0.012(2) C(24) 0.036(3) 0.037(3) 0.048(3) 0.023(2) 0.014(2) 0.025(2) C(25) 0.029(2) 0.029(2) 0.035(3) 0.012(2) 0.0125(19) 0.016(2) C(26) 0.021(2) 0.023(2) 0.026(2) 0.0093(17) 0.0048(16) 0.0097(17) C(31) 0.020(2) 0.0159(18) 0.026(2) 0.0076(16) 0.0048(16) 0.0046(16) C(32) 0.023(2) 0.025(2) 0.026(2) 0.0130(18) 0.0075(16) 0.0079(17) C(33) 0.028(2) 0.0175(19) 0.034(2) 0.0109(18) 0.0103(18) 0.0112(18) C(34) 0.033(2) 0.021(2) 0.032(2) 0.0140(19) 0.0095(19) 0.0050(18) C(35) 0.030(2) 0.026(2) 0.023(2) 0.0146(19) 0.0090(17) 0.0042(18) C(36) 0.021(2) 0.0207(19) 0.023(2) 0.0097(17) 0.0071(16) 0.0057(17) C(221) 0.020(2) 0.032(2) 0.025(2) 0.0138(18) 0.0047(16) 0.0084(18) C(222) 0.033(3) 0.041(3) 0.036(3) 0.023(2) 0.007(2) 0.001(2) C(223) 0.050(3) 0.071(4) 0.035(3) 0.042(3) 0.018(2) 0.010(3) C(224) 0.042(3) 0.074(4) 0.040(3) 0.033(3) 0.024(2) 0.032(3) C(225) 0.037(3) 0.042(3) 0.046(3) 0.018(2) 0.020(2) 0.022(2) C(226) 0.030(2) 0.036(2) 0.033(3) 0.018(2) 0.0142(19) 0.015(2) C(261) 0.020(2) 0.025(2) 0.024(2) 0.0090(17) 0.0090(16) 0.0123(18) C(262) 0.026(2) 0.024(2) 0.031(2) 0.0049(18) 0.0110(18) 0.0094(19) C(263) 0.024(2) 0.036(3) 0.028(2) 0.004(2) 0.0088(18) 0.007(2) C(264) 0.024(2) 0.052(3) 0.032(3) 0.019(2) 0.0120(19) 0.006(2) C(265) 0.030(3) 0.033(3) 0.046(3) 0.016(2) 0.010(2) 0.001(2) C(266) 0.024(2) 0.029(2) 0.032(3) 0.0095(19) 0.0054(18) 0.0019(19) C(321) 0.023(2) 0.020(2) 0.026(2) 0.0064(17) 0.0088(17) 0.0072(17) C(322) 0.036(3) 0.034(2) 0.032(3) 0.020(2) 0.011(2) 0.017(2) C(323) 0.054(3) 0.050(3) 0.036(3) 0.026(3) 0.019(2) 0.025(3) C(324) 0.048(3) 0.050(3) 0.033(3) 0.018(3) 0.022(2) 0.017(3) C(325) 0.038(3) 0.044(3) 0.034(3) 0.018(2) 0.020(2) 0.010(2) C(326) 0.030(2) 0.028(2) 0.028(2) 0.0128(19) 0.0096(18) 0.0106(19) C(361) 0.025(2) 0.021(2) 0.020(2) 0.0054(17) 0.0024(16) 0.0052(17) C(362) 0.022(2) 0.026(2) 0.034(3) 0.0065(18) 0.0015(18) 0.0094(19) C(363) 0.030(3) 0.029(2) 0.048(3) 0.005(2) -0.003(2) 0.018(2) C(364) 0.044(3) 0.040(3) 0.045(3) -0.002(3) -0.001(2) 0.027(3) C(365) 0.056(4) 0.044(3) 0.028(3) 0.000(3) 0.018(2) 0.010(2) C(366) 0.043(3) 0.028(2) 0.033(3) 0.007(2) 0.017(2) 0.005(2) # 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) 1.850(3) ? Ta O(3) 1.911(3) ? Ta C(1) 2.139(4) ? Ta Cl(5) 2.3466(10) ? Ta Cl(4) 2.3575(11) ? O(2) C(21) 1.380(5) ? O(3) C(31) 1.367(5) ? C(1) C(6) 1.533(6) ? C(1) C(2) 1.542(6) ? C(2) C(3) 1.524(7) ? C(3) C(4) 1.513(8) ? C(4) C(5) 1.516(8) ? C(5) C(6) 1.537(7) ? C(21) C(22) 1.396(6) ? C(21) C(26) 1.403(6) ? C(22) C(23) 1.395(6) ? C(22) C(221) 1.493(6) ? C(23) C(24) 1.393(7) ? C(24) C(25) 1.375(7) ? C(25) C(26) 1.390(6) ? C(26) C(261) 1.490(6) ? C(31) C(36) 1.401(6) ? C(31) C(32) 1.408(6) ? C(32) C(33) 1.392(6) ? C(32) C(321) 1.487(6) ? C(33) C(34) 1.387(6) ? C(34) C(35) 1.380(6) ? C(35) C(36) 1.405(6) ? C(36) C(361) 1.486(6) ? C(221) C(226) 1.382(6) ? C(221) C(222) 1.401(6) ? C(222) C(223) 1.386(7) ? C(223) C(224) 1.380(8) ? C(224) C(225) 1.391(8) ? C(225) C(226) 1.391(6) ? C(261) C(266) 1.376(6) ? C(261) C(262) 1.395(6) ? C(262) C(263) 1.388(7) ? C(263) C(264) 1.386(7) ? C(264) C(265) 1.381(7) ? C(265) C(266) 1.381(6) ? C(321) C(326) 1.385(6) ? C(321) C(322) 1.401(6) ? C(322) C(323) 1.382(7) ? C(323) C(324) 1.377(8) ? C(324) C(325) 1.370(7) ? C(325) C(326) 1.398(6) ? C(361) C(366) 1.389(6) ? C(361) C(362) 1.395(6) ? C(362) C(363) 1.383(6) ? C(363) C(364) 1.377(8) ? C(364) C(365) 1.375(9) ? C(365) C(366) 1.399(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 O(2) Ta O(3) 92.93(12) ? O(2) Ta C(1) 100.82(15) ? O(3) Ta C(1) 96.53(14) ? O(2) Ta Cl(5) 92.94(9) ? O(3) Ta Cl(5) 168.88(9) ? C(1) Ta Cl(5) 91.64(12) ? O(2) Ta Cl(4) 148.91(9) ? O(3) Ta Cl(4) 84.26(9) ? C(1) Ta Cl(4) 110.26(12) ? Cl(5) Ta Cl(4) 85.83(4) ? C(21) O(2) Ta 162.6(3) ? C(31) O(3) Ta 145.2(3) ? C(6) C(1) C(2) 110.4(4) ? C(6) C(1) Ta 112.8(3) ? C(2) C(1) Ta 113.5(3) ? C(3) C(2) C(1) 110.6(4) ? C(4) C(3) C(2) 111.9(5) ? C(3) C(4) C(5) 111.8(4) ? C(4) C(5) C(6) 111.7(4) ? C(1) C(6) C(5) 110.9(4) ? O(2) C(21) C(22) 118.4(4) ? O(2) C(21) C(26) 119.3(3) ? C(22) C(21) C(26) 122.3(4) ? C(23) C(22) C(21) 117.3(4) ? C(23) C(22) C(221) 119.3(4) ? C(21) C(22) C(221) 123.4(4) ? C(24) C(23) C(22) 121.6(4) ? C(25) C(24) C(23) 119.4(4) ? C(24) C(25) C(26) 121.5(4) ? C(25) C(26) C(21) 117.8(4) ? C(25) C(26) C(261) 121.2(4) ? C(21) C(26) C(261) 121.0(4) ? O(3) C(31) C(36) 119.9(3) ? O(3) C(31) C(32) 119.5(4) ? C(36) C(31) C(32) 120.6(4) ? C(33) C(32) C(31) 118.7(4) ? C(33) C(32) C(321) 117.7(4) ? C(31) C(32) C(321) 123.4(4) ? C(34) C(33) C(32) 121.2(4) ? C(35) C(34) C(33) 119.5(4) ? C(34) C(35) C(36) 121.3(4) ? C(31) C(36) C(35) 118.4(4) ? C(31) C(36) C(361) 123.5(4) ? C(35) C(36) C(361) 118.0(4) ? C(226) C(221) C(222) 119.1(4) ? C(226) C(221) C(22) 122.4(4) ? C(222) C(221) C(22) 118.5(4) ? C(223) C(222) C(221) 120.4(5) ? C(224) C(223) C(222) 120.1(5) ? C(223) C(224) C(225) 119.9(5) ? C(226) C(225) C(224) 120.0(5) ? C(221) C(226) C(225) 120.4(5) ? C(266) C(261) C(262) 118.7(4) ? C(266) C(261) C(26) 121.7(4) ? C(262) C(261) C(26) 119.5(4) ? C(263) C(262) C(261) 120.6(4) ? C(264) C(263) C(262) 119.4(4) ? C(265) C(264) C(263) 120.4(4) ? C(264) C(265) C(266) 119.5(5) ? C(261) C(266) C(265) 121.4(4) ? C(326) C(321) C(322) 118.8(4) ? C(326) C(321) C(32) 119.7(4) ? C(322) C(321) C(32) 121.0(4) ? C(323) C(322) C(321) 120.7(5) ? C(324) C(323) C(322) 119.6(5) ? C(325) C(324) C(323) 120.8(5) ? C(324) C(325) C(326) 120.0(5) ? C(321) C(326) C(325) 120.0(4) ? C(366) C(361) C(362) 118.1(4) ? C(366) C(361) C(36) 121.0(4) ? C(362) C(361) C(36) 120.6(4) ? C(363) C(362) C(361) 121.2(5) ? C(364) C(363) C(362) 119.7(5) ? C(363) C(364) C(365) 120.7(5) ? C(364) C(365) C(366) 119.4(5) ? C(361) C(366) C(365) 120.9(5) ? #===END #============================================================================== data_ROT1 _database_code_CSD 164014 _audit_creation_date 5-09-00 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour 'pale yellow ' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C44 H48 Cl1 O2 Si2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 881.45 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.0085(2) _cell_length_b 10.8522(2) _cell_length_c 11.2929(2) _cell_angle_alpha 63.9019(8) _cell_angle_beta 87.6411(7) _cell_angle_gamma 68.9612(8) _cell_volume 1018.06(4) _cell_measurement_reflns_used 11150 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 1 _exptl_crystal_density_diffrn 1.44 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.825 _cell_measurement_temperature 150 _exptl_crystal_F_000 446 # 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 0.2607 _exptl_absorpt_correction_T_max 0.5684 _diffrn_reflns_number 11150 _reflns_number_total 7777 _reflns_Friedl_coverage 0.7728 _reflns_number_gt 7776 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 14 # 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 0.042 _refine_ls_wR_factor_ref 0.108 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7769 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+6.2442P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.049 _refine_diff_density_max 1.12 _refine_diff_density_min -2.32 _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 0.403(13) # 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 0.00586(8) 0.00188(8) 0.00053(7) 0.02068(8) Uani ? Cl -0.0057(2) 0.2523(2) -0.1004(2) 0.0319(6) Uani ? Si(3) 0.1719(5) -0.1148(5) -0.2299(4) 0.0409(14) Uani ? Si(4) -0.1560(4) 0.0642(5) 0.2537(4) 0.0384(17) Uani ? O(1) -0.1770(12) 0.0727(11) -0.1001(10) 0.023(2) Uiso ? O(2) 0.1894(12) -0.0560(11) 0.0992(10) 0.024(2) Uani ? C(11) -0.270(2) 0.088(2) -0.1945(16) 0.027(6) Uani ? C(12) -0.317(2) -0.016(2) -0.1799(16) 0.038(6) Uani ? C(13) -0.392(3) -0.001(3) -0.2959(18) 0.052(9) Uani ? C(14) -0.435(2) 0.130(2) -0.4124(16) 0.046(7) Uani ? C(15) -0.3921(18) 0.2403(17) -0.4201(16) 0.030(5) Uani ? C(16) -0.3191(18) 0.2295(16) -0.3157(15) 0.028(4) Uani ? C(21) 0.2819(18) -0.0852(18) 0.2008(15) 0.022(5) Uani ? C(22) 0.3259(18) 0.0334(17) 0.1881(14) 0.024(4) Uani ? C(23) 0.412(2) 0.011(2) 0.2917(18) 0.040(7) Uani ? C(24) 0.448(2) -0.117(3) 0.4116(19) 0.052(9) Uani ? C(25) 0.413(2) -0.233(2) 0.4248(15) 0.049(8) Uani ? C(26) 0.3229(17) -0.2157(18) 0.3171(13) 0.027(5) Uani ? C(31) 0.0945(9) -0.1580(8) -0.0684(7) 0.026(3) Uani ? C(32) 0.0666(15) -0.1535(13) -0.3350(10) 0.053(5) Uani ? C(33) 0.1617(12) 0.0800(10) -0.3235(8) 0.043(3) Uani ? C(34) 0.3636(13) -0.2454(14) -0.1856(14) 0.053(5) Uani ? C(41) -0.0755(8) -0.0708(8) 0.1813(7) 0.025(3) Uani ? C(42) -0.0206(12) 0.1289(11) 0.2867(10) 0.040(4) Uani ? C(43) -0.2100(12) -0.0505(13) 0.4162(10) 0.045(4) Uani ? C(44) -0.3151(14) 0.2236(14) 0.1423(13) 0.050(5) Uani ? C(121) -0.285(2) -0.1611(19) -0.0530(16) 0.034(6) Uani ? C(122) -0.221(3) -0.296(2) -0.0561(16) 0.047(7) Uani ? C(123) -0.192(3) -0.429(2) 0.0641(19) 0.061(8) Uani ? C(124) -0.247(2) -0.418(2) 0.1794(16) 0.049(7) Uani ? C(125) -0.310(2) -0.284(2) 0.1744(16) 0.044(7) Uani ? C(126) -0.332(2) -0.149(2) 0.0592(15) 0.038(6) Uani ? C(161) -0.2872(19) 0.355(2) -0.3251(16) 0.028(5) Uani ? C(162) -0.206(2) 0.4205(18) -0.4252(17) 0.037(5) Uani ? C(163) -0.185(3) 0.543(2) -0.439(2) 0.052(8) Uani ? C(164) -0.242(2) 0.6077(19) -0.357(2) 0.048(6) Uani ? C(165) -0.303(3) 0.541(2) -0.253(2) 0.048(7) Uani ? C(166) -0.330(2) 0.4165(19) -0.2404(18) 0.040(7) Uani ? C(221) 0.297(2) 0.168(2) 0.0619(16) 0.037(6) Uani ? C(222) 0.231(3) 0.308(2) 0.056(2) 0.057(10) Uani ? C(223) 0.222(3) 0.437(3) -0.054(2) 0.067(9) Uani ? C(224) 0.261(3) 0.432(2) -0.1675(19) 0.070(9) Uani ? C(225) 0.325(2) 0.295(3) -0.1753(17) 0.051(8) Uani ? C(226) 0.3405(18) 0.169(2) -0.0605(17) 0.032(5) Uani ? C(261) 0.292(2) -0.3468(18) 0.3331(16) 0.029(5) Uani ? C(262) 0.227(2) -0.4143(19) 0.4357(17) 0.034(6) Uani ? C(263) 0.197(2) -0.537(2) 0.446(2) 0.043(7) Uani ? C(264) 0.237(3) -0.587(2) 0.351(2) 0.054(7) Uani ? C(265) 0.327(2) -0.527(2) 0.256(2) 0.045(6) Uani ? C(266) 0.3481(18) -0.4078(18) 0.2430(16) 0.033(6) Uani ? H(13) -0.4106 -0.0809 -0.2918 0.0670 Uiso calc H(14) -0.4916 0.1441 -0.4838 0.0600 Uiso calc H(15) -0.4143 0.3258 -0.5007 0.0390 Uiso calc H(23) 0.4469 0.0834 0.2819 0.0510 Uiso calc H(24) 0.4958 -0.1240 0.4844 0.0670 Uiso calc H(25) 0.4480 -0.3231 0.5022 0.0640 Uiso calc H(122) -0.1966 -0.2994 -0.1354 0.0610 Uiso calc H(123) -0.1388 -0.5211 0.0676 0.0780 Uiso calc H(124) -0.2388 -0.5028 0.2569 0.0640 Uiso calc H(125) -0.3419 -0.2792 0.2514 0.0570 Uiso calc H(126) -0.3742 -0.0571 0.0594 0.0490 Uiso calc H(162) -0.1670 0.3782 -0.4810 0.0490 Uiso calc H(163) -0.1328 0.5842 -0.5046 0.0680 Uiso calc H(164) -0.2371 0.6980 -0.3736 0.0620 Uiso calc H(165) -0.3272 0.5762 -0.1905 0.0620 Uiso calc H(166) -0.3782 0.3748 -0.1714 0.0520 Uiso calc H(222) 0.1912 0.3150 0.1293 0.0750 Uiso calc H(223) 0.1900 0.5262 -0.0494 0.0860 Uiso calc H(224) 0.2454 0.5204 -0.2437 0.0930 Uiso calc H(225) 0.3548 0.2914 -0.2534 0.0660 Uiso calc H(226) 0.3823 0.0787 -0.0621 0.0410 Uiso calc H(262) 0.2014 -0.3806 0.4994 0.0440 Uiso calc H(263) 0.1503 -0.5828 0.5149 0.0560 Uiso calc H(264) 0.2074 -0.6581 0.3490 0.0700 Uiso calc H(265) 0.3706 -0.5732 0.2039 0.0580 Uiso calc H(266) 0.3983 -0.3644 0.1766 0.0430 Uiso calc H(31A) 0.1706 -0.2413 0.0008 0.0330 Uiso calc H(31B) 0.0195 -0.1930 -0.0741 0.0330 Uiso calc H(32A) 0.1081 -0.1421 -0.4156 0.0680 Uiso calc H(32B) -0.0322 -0.0850 -0.3567 0.0680 Uiso calc H(32C) 0.0703 -0.2531 -0.2864 0.0680 Uiso calc H(33A) 0.2201 0.0980 -0.2724 0.0550 Uiso calc H(33B) 0.0632 0.1474 -0.3390 0.0550 Uiso calc H(33C) 0.1965 0.0948 -0.4072 0.0550 Uiso calc H(34A) 0.4145 -0.2259 -0.1298 0.0690 Uiso calc H(34B) 0.4074 -0.2324 -0.2652 0.0690 Uiso calc H(34C) 0.3682 -0.3454 -0.1387 0.0690 Uiso calc H(41A) -0.1494 -0.1048 0.1705 0.0320 Uiso calc H(41B) 0.0022 -0.1564 0.2470 0.0320 Uiso calc H(42A) -0.0621 0.1914 0.3287 0.0510 Uiso calc H(42B) 0.0084 0.1840 0.2043 0.0510 Uiso calc H(42C) 0.0623 0.0450 0.3444 0.0510 Uiso calc H(43A) -0.1269 -0.1368 0.4704 0.0590 Uiso calc H(43B) -0.2828 -0.0804 0.3979 0.0590 Uiso calc H(43C) -0.2475 0.0079 0.4626 0.0590 Uiso calc H(44A) -0.3805 0.1887 0.1189 0.0660 Uiso calc H(44B) -0.2850 0.2837 0.0632 0.0660 Uiso calc H(44C) -0.3630 0.2817 0.1869 0.0660 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 0.01655(11) 0.02350(12) 0.01909(10) -0.00503(8) -0.00228(7) -0.00889(8) Cl 0.0268(9) 0.0196(8) 0.0391(9) -0.0093(7) -0.0087(7) -0.0034(7) Si(3) 0.0373(17) 0.057(2) 0.0283(15) -0.0116(17) 0.0074(11) -0.0245(16) Si(4) 0.0243(14) 0.063(3) 0.0346(17) -0.0131(17) 0.0061(11) -0.0309(18) O(2) 0.020(3) 0.023(3) 0.023(3) -0.006(2) -0.0081(19) -0.006(2) C(11) 0.027(9) 0.032(9) 0.025(7) -0.009(7) 0.000(6) -0.016(6) C(12) 0.042(9) 0.052(9) 0.022(5) -0.016(7) -0.001(5) -0.020(6) C(13) 0.082(15) 0.058(12) 0.030(8) -0.051(11) -0.011(8) -0.010(7) C(14) 0.051(12) 0.052(10) 0.021(7) -0.023(9) -0.018(7) -0.001(6) C(15) 0.021(7) 0.029(7) 0.032(7) -0.010(6) -0.006(5) -0.007(5) C(16) 0.020(6) 0.015(5) 0.029(6) 0.002(4) 0.004(5) 0.000(4) C(21) 0.016(8) 0.024(7) 0.019(6) -0.009(6) -0.004(5) -0.003(5) C(22) 0.029(7) 0.023(5) 0.025(6) -0.019(5) -0.001(4) -0.007(4) C(23) 0.039(9) 0.054(10) 0.034(8) -0.029(8) 0.003(6) -0.017(7) C(24) 0.057(13) 0.082(14) 0.035(9) -0.049(11) -0.005(8) -0.024(8) C(25) 0.049(12) 0.062(12) 0.015(6) -0.017(9) -0.014(6) -0.002(6) C(26) 0.019(6) 0.042(8) 0.022(6) -0.013(5) -0.006(4) -0.015(5) C(31) 0.033(4) 0.021(3) 0.033(3) -0.009(3) 0.007(3) -0.022(3) C(32) 0.081(9) 0.045(6) 0.028(5) -0.024(6) -0.004(5) -0.012(4) C(33) 0.051(6) 0.037(5) 0.021(3) -0.014(4) 0.009(3) 0.000(3) C(34) 0.039(6) 0.039(6) 0.063(8) -0.012(5) 0.012(5) -0.010(5) C(41) 0.023(4) 0.027(4) 0.017(3) -0.009(3) 0.006(2) -0.005(2) C(42) 0.049(6) 0.040(5) 0.038(5) -0.020(4) 0.006(4) -0.022(4) C(43) 0.045(6) 0.058(6) 0.038(5) -0.026(5) 0.015(4) -0.022(4) C(44) 0.047(7) 0.042(6) 0.054(7) -0.010(5) 0.007(5) -0.021(5) C(121) 0.055(11) 0.032(8) 0.028(6) -0.031(8) 0.011(6) -0.013(5) C(122) 0.076(14) 0.031(8) 0.029(7) -0.023(8) -0.007(7) -0.006(6) C(123) 0.126(19) 0.025(7) 0.040(7) -0.045(10) 0.004(8) -0.009(5) C(124) 0.057(9) 0.066(11) 0.025(6) -0.035(8) 0.005(5) -0.012(6) C(125) 0.071(13) 0.043(9) 0.029(7) -0.039(9) 0.000(7) -0.012(6) C(126) 0.046(10) 0.047(9) 0.019(6) -0.024(7) 0.002(5) -0.009(5) C(161) 0.017(6) 0.029(7) 0.024(6) -0.006(5) 0.001(5) -0.003(5) C(162) 0.033(9) 0.025(7) 0.032(6) 0.002(6) 0.003(5) -0.005(5) C(163) 0.051(14) 0.033(10) 0.045(10) -0.016(9) 0.006(9) 0.005(8) C(164) 0.062(11) 0.015(6) 0.054(9) -0.016(6) 0.000(7) -0.003(5) C(165) 0.065(12) 0.032(8) 0.045(8) -0.022(8) 0.000(7) -0.013(6) C(166) 0.051(12) 0.030(9) 0.038(9) -0.017(8) 0.006(8) -0.013(7) C(221) 0.036(9) 0.047(10) 0.027(6) -0.019(8) -0.010(6) -0.013(6) C(222) 0.101(18) 0.048(11) 0.054(11) -0.051(11) 0.033(11) -0.033(8) C(223) 0.085(14) 0.062(13) 0.061(10) -0.041(11) 0.010(9) -0.024(9) C(224) 0.13(2) 0.026(7) 0.047(9) -0.047(10) -0.004(10) 0.003(6) C(225) 0.035(9) 0.075(14) 0.031(8) -0.028(9) 0.011(7) -0.009(8) C(226) 0.021(7) 0.031(6) 0.043(7) -0.013(5) -0.001(5) -0.014(5) C(261) 0.025(7) 0.022(7) 0.029(6) -0.002(5) -0.004(5) -0.008(5) C(262) 0.035(9) 0.035(8) 0.029(6) -0.019(7) 0.001(5) -0.007(5) C(263) 0.047(12) 0.033(9) 0.041(9) -0.021(9) 0.004(8) -0.006(7) C(264) 0.054(10) 0.032(8) 0.058(10) -0.008(7) -0.009(7) -0.011(7) C(265) 0.045(9) 0.033(8) 0.048(8) -0.002(7) 0.005(7) -0.020(6) C(266) 0.023(8) 0.028(8) 0.034(8) 0.001(6) -0.001(6) -0.010(6) # 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) 1.903(12) ? Ta O(2) 1.933(11) ? Ta C(41) 2.088(6) ? Ta C(31) 2.104(6) ? Ta Cl 2.3996(18) ? Si(3) C(34) 1.856(13) ? Si(3) C(33) 1.867(10) ? Si(3) C(31) 1.881(8) ? Si(3) C(32) 1.885(12) ? Si(4) C(44) 1.839(13) ? Si(4) C(42) 1.851(11) ? Si(4) C(43) 1.897(10) ? Si(4) C(41) 1.901(8) ? O(1) C(11) 1.36(2) ? O(2) C(21) 1.353(19) ? C(11) C(12) 1.33(3) ? C(11) C(16) 1.46(2) ? C(12) C(13) 1.45(2) ? C(12) C(121) 1.52(2) ? C(13) C(14) 1.38(3) ? C(14) C(15) 1.38(3) ? C(15) C(16) 1.35(2) ? C(16) C(161) 1.47(3) ? C(21) C(26) 1.37(2) ? C(21) C(22) 1.45(2) ? C(22) C(23) 1.36(2) ? C(22) C(221) 1.47(2) ? C(23) C(24) 1.39(3) ? C(24) C(25) 1.37(3) ? C(25) C(26) 1.45(2) ? C(26) C(261) 1.50(2) ? C(121) C(126) 1.38(2) ? C(121) C(122) 1.39(3) ? C(122) C(123) 1.42(2) ? C(123) C(124) 1.43(3) ? C(124) C(125) 1.34(3) ? C(125) C(126) 1.42(2) ? C(161) C(166) 1.36(3) ? C(161) C(162) 1.44(2) ? C(162) C(163) 1.36(3) ? C(163) C(164) 1.39(3) ? C(164) C(165) 1.33(3) ? C(165) C(166) 1.42(3) ? C(221) C(222) 1.39(3) ? C(221) C(226) 1.43(3) ? C(222) C(223) 1.37(3) ? C(223) C(224) 1.34(3) ? C(224) C(225) 1.44(3) ? C(225) C(226) 1.37(2) ? C(261) C(262) 1.36(2) ? C(261) C(266) 1.44(2) ? C(262) C(263) 1.42(3) ? C(263) C(264) 1.38(3) ? C(264) C(265) 1.46(3) ? C(265) C(266) 1.33(3) ? 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) 176.0(6) ? O(1) Ta C(41) 92.5(4) ? O(2) Ta C(41) 88.5(4) ? O(1) Ta C(31) 91.0(4) ? O(2) Ta C(31) 92.1(4) ? C(41) Ta C(31) 115.3(3) ? O(1) Ta Cl 88.4(3) ? O(2) Ta Cl 87.7(3) ? C(41) Ta Cl 117.0(2) ? C(31) Ta Cl 127.7(2) ? C(34) Si(3) C(33) 109.8(6) ? C(34) Si(3) C(31) 105.8(5) ? C(33) Si(3) C(31) 114.7(4) ? C(34) Si(3) C(32) 110.8(7) ? C(33) Si(3) C(32) 109.4(5) ? C(31) Si(3) C(32) 106.2(5) ? C(44) Si(4) C(42) 110.1(6) ? C(44) Si(4) C(43) 110.7(6) ? C(42) Si(4) C(43) 110.1(5) ? C(44) Si(4) C(41) 111.0(5) ? C(42) Si(4) C(41) 111.3(5) ? C(43) Si(4) C(41) 103.6(4) ? C(11) O(1) Ta 155.7(11) ? C(21) O(2) Ta 157.6(11) ? C(12) C(11) O(1) 123.2(16) ? C(12) C(11) C(16) 120.1(17) ? O(1) C(11) C(16) 116.7(16) ? C(11) C(12) C(13) 118.4(16) ? C(11) C(12) C(121) 124.6(16) ? C(13) C(12) C(121) 116.6(16) ? C(14) C(13) C(12) 120.5(18) ? C(15) C(14) C(13) 118.3(16) ? C(16) C(15) C(14) 122.9(14) ? C(15) C(16) C(11) 118.2(15) ? C(15) C(16) C(161) 120.9(14) ? C(11) C(16) C(161) 120.9(16) ? O(2) C(21) C(26) 122.2(14) ? O(2) C(21) C(22) 117.1(13) ? C(26) C(21) C(22) 120.4(15) ? C(23) C(22) C(21) 118.9(15) ? C(23) C(22) C(221) 118.5(14) ? C(21) C(22) C(221) 122.1(14) ? C(22) C(23) C(24) 121.0(18) ? C(25) C(24) C(23) 121.2(17) ? C(24) C(25) C(26) 119.4(16) ? C(21) C(26) C(25) 118.6(15) ? C(21) C(26) C(261) 123.2(14) ? C(25) C(26) C(261) 117.9(15) ? Si(3) C(31) Ta 122.1(4) ? Si(4) C(41) Ta 118.7(4) ? C(126) C(121) C(122) 123.4(16) ? C(126) C(121) C(12) 116.3(17) ? C(122) C(121) C(12) 120.2(16) ? C(121) C(122) C(123) 118.8(18) ? C(122) C(123) C(124) 118.2(19) ? C(125) C(124) C(123) 119.2(16) ? C(124) C(125) C(126) 124.2(17) ? C(121) C(126) C(125) 115.7(18) ? C(166) C(161) C(162) 115.7(18) ? C(166) C(161) C(16) 123.1(15) ? C(162) C(161) C(16) 121.1(16) ? C(163) C(162) C(161) 120.8(18) ? C(162) C(163) C(164) 120.5(18) ? C(165) C(164) C(163) 120.4(19) ? C(164) C(165) C(166) 119(2) ? C(161) C(166) C(165) 122.6(18) ? C(222) C(221) C(226) 114.4(16) ? C(222) C(221) C(22) 121.2(17) ? C(226) C(221) C(22) 124.3(18) ? C(223) C(222) C(221) 123(2) ? C(224) C(223) C(222) 119(2) ? C(223) C(224) C(225) 122.3(17) ? C(226) C(225) C(224) 115.6(17) ? C(225) C(226) C(221) 124.5(19) ? C(262) C(261) C(266) 121.2(17) ? C(262) C(261) C(26) 121.7(16) ? C(266) C(261) C(26) 116.8(15) ? C(261) C(262) C(263) 119.9(18) ? C(264) C(263) C(262) 119.1(19) ? C(263) C(264) C(265) 119(2) ? C(266) C(265) C(264) 120.6(18) ? C(265) C(266) C(261) 119.0(16) ? #===END #============================================================================== data_MMS221 _database_code_CSD 164015 _audit_creation_date 24-08-98 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description palte _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C92 H74 Cl1 Nb1 O2' _chemical_formula_structural ? _chemical_formula_weight 1339.97 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3332(4) _cell_length_b 15.3768(5) _cell_length_c 19.2026(5) _cell_angle_alpha 109.4762(15) _cell_angle_beta 97.3407(17) _cell_angle_gamma 102.6676(13) _cell_volume 3533.9(4) _cell_measurement_reflns_used 37974 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.249 _cell_measurement_temperature 203 _exptl_crystal_F_000 1400 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.5769 _exptl_absorpt_correction_T_max 0.9755 _diffrn_reflns_number 37974 _reflns_number_total 14354 _reflns_number_gt 9824 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.077 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_max 23 # 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 0.059 _refine_ls_wR_factor_ref 0.131 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 14354 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.6529P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 0.55 _refine_diff_density_min -0.72 _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 Direct_methods_(SIR97,_Altomare_et_al.,_1997) _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 Nb 0.20291(2) 0.16123(2) 0.255400(16) 0.02660(10) Uani ? Cl 0.19672(7) 0.02960(7) 0.14618(5) 0.0434(3) Uani ? O(1) 0.11178(15) 0.07408(16) 0.28667(11) 0.0281(8) Uani ? O(2) 0.29612(16) 0.24237(16) 0.22088(12) 0.0292(8) Uani ? C(3) 0.0830(2) 0.2387(2) 0.24811(17) 0.0256(11) Uani ? C(4) 0.3210(2) 0.2013(3) 0.35741(17) 0.0327(12) Uani ? C(11) 0.0469(2) 0.0051(2) 0.30303(16) 0.0248(10) Uani ? C(12) -0.0628(2) -0.0212(2) 0.27457(17) 0.0264(11) Uani ? C(13) -0.1287(2) -0.0862(2) 0.29733(18) 0.0307(11) Uani ? C(14) -0.0843(2) -0.1203(3) 0.34914(18) 0.0323(12) Uani ? C(15) 0.0228(2) -0.0977(2) 0.37557(18) 0.0289(11) Uani ? C(16) 0.0911(2) -0.0357(2) 0.35104(17) 0.0273(11) Uani ? C(21) 0.3615(2) 0.2970(2) 0.19242(17) 0.0279(11) Uani ? C(22) 0.4713(3) 0.3228(2) 0.22014(18) 0.0315(12) Uani ? C(23) 0.5361(3) 0.3903(3) 0.1986(2) 0.0380(12) Uani ? C(24) 0.4913(3) 0.4252(3) 0.1480(2) 0.0415(13) Uani ? C(25) 0.3832(3) 0.3947(3) 0.11533(19) 0.0346(12) Uani ? C(26) 0.3167(2) 0.3299(2) 0.13901(18) 0.0300(11) Uani ? C(31) 0.0875(3) 0.3306(3) 0.30303(19) 0.0379(13) Uani ? C(32) 0.1559(3) 0.4167(3) 0.3096(2) 0.0496(13) Uani ? C(33) 0.1520(4) 0.5035(3) 0.3599(2) 0.0575(17) Uani ? C(34) 0.0809(4) 0.5065(3) 0.4056(2) 0.0631(17) Uani ? C(35) 0.0140(4) 0.4232(3) 0.4014(2) 0.0641(19) Uani ? C(36) 0.0177(3) 0.3359(3) 0.3513(2) 0.0490(15) Uani ? C(41) 0.2939(3) 0.2815(3) 0.41204(19) 0.0352(12) Uani ? C(42) 0.3401(3) 0.3758(3) 0.4233(2) 0.0545(17) Uani ? C(43) 0.3190(4) 0.4498(4) 0.4773(3) 0.0720(19) Uani ? C(44) 0.2481(4) 0.4316(4) 0.5205(3) 0.076(2) Uani ? C(45) 0.1985(3) 0.3380(4) 0.5091(3) 0.0682(19) Uani ? C(46) 0.2211(3) 0.2637(3) 0.4555(2) 0.0471(13) Uani ? C(121) -0.1087(2) 0.0205(2) 0.22295(18) 0.0302(11) Uani ? C(122) -0.0909(3) -0.0001(3) 0.15029(19) 0.0367(12) Uani ? C(123) -0.1380(3) 0.0362(3) 0.1019(2) 0.0490(15) Uani ? C(124) -0.2011(3) 0.0956(4) 0.1259(2) 0.0568(18) Uani ? C(125) -0.2186(3) 0.1172(3) 0.1988(2) 0.0500(17) Uani ? C(126) -0.1745(3) 0.0789(3) 0.2460(2) 0.0384(12) Uani ? C(131) -0.2446(3) -0.1212(3) 0.26845(19) 0.0335(12) Uani ? C(132) -0.3126(3) -0.1148(3) 0.3180(2) 0.0458(15) Uani ? C(133) -0.4200(3) -0.1555(4) 0.2914(2) 0.0568(18) Uani ? C(134) -0.4621(3) -0.2014(4) 0.2160(3) 0.066(2) Uani ? C(135) -0.3967(3) -0.2080(4) 0.1660(3) 0.077(2) Uani ? C(136) -0.2882(3) -0.1682(3) 0.1922(2) 0.0569(15) Uani ? C(151) 0.0615(2) -0.1403(2) 0.42938(19) 0.0305(11) Uani ? C(152) 0.0236(3) -0.1268(2) 0.49546(18) 0.0321(12) Uani ? C(153) 0.0552(3) -0.1665(3) 0.54621(19) 0.0367(12) Uani ? C(154) 0.1257(3) -0.2201(3) 0.5330(2) 0.0418(13) Uani ? C(155) 0.1647(3) -0.2332(3) 0.4678(2) 0.0463(15) Uani ? C(156) 0.1328(3) -0.1943(3) 0.4166(2) 0.0415(13) Uani ? C(161) 0.2074(2) -0.0159(2) 0.37365(18) 0.0306(12) Uani ? C(162) 0.2649(3) -0.0451(3) 0.3188(2) 0.0367(12) Uani ? C(163) 0.3723(3) -0.0294(3) 0.3392(3) 0.0485(17) Uani ? C(164) 0.4235(3) 0.0157(3) 0.4143(3) 0.0559(18) Uani ? C(165) 0.3677(3) 0.0449(3) 0.4689(2) 0.0512(17) Uani ? C(166) 0.2604(3) 0.0287(3) 0.4492(2) 0.0380(12) Uani ? C(221) 0.5173(2) 0.2770(3) 0.26851(19) 0.0327(12) Uani ? C(222) 0.5042(3) 0.1781(3) 0.2393(2) 0.0374(12) Uani ? C(223) 0.5504(3) 0.1345(3) 0.2822(2) 0.0447(15) Uani ? C(224) 0.6098(3) 0.1893(3) 0.3549(2) 0.0503(17) Uani ? C(225) 0.6235(3) 0.2865(3) 0.3832(2) 0.0492(15) Uani ? C(226) 0.5786(3) 0.3306(3) 0.3408(2) 0.0391(12) Uani ? C(231) 0.6533(3) 0.4263(3) 0.2260(2) 0.0514(18) Uani ? C(232) 0.7160(3) 0.3641(4) 0.2167(3) 0.075(2) Uani ? C(233) 0.8261(4) 0.4009(6) 0.2380(4) 0.108(4) Uani ? C(234) 0.8703(4) 0.4973(8) 0.2690(5) 0.126(5) Uani ? C(235) 0.8108(5) 0.5583(6) 0.2798(4) 0.104(3) Uani ? C(236) 0.7014(4) 0.5249(4) 0.2589(3) 0.073(2) Uani ? C(251) 0.3464(3) 0.4318(3) 0.05745(19) 0.0372(13) Uani ? C(252) 0.3834(3) 0.5297(3) 0.0718(2) 0.0494(15) Uani ? C(253) 0.3544(4) 0.5667(4) 0.0180(3) 0.0602(19) Uani ? C(254) 0.2891(4) 0.5077(4) -0.0499(3) 0.066(2) Uani ? C(255) 0.2525(4) 0.4112(4) -0.0648(3) 0.079(2) Uani ? C(256) 0.2807(4) 0.3726(3) -0.0118(2) 0.0587(17) Uani ? C(261) 0.2012(3) 0.2959(3) 0.10617(18) 0.0343(12) Uani ? C(262) 0.1393(3) 0.3593(3) 0.1179(2) 0.0488(17) Uani ? C(263) 0.0322(3) 0.3260(4) 0.0870(3) 0.072(2) Uani ? C(264) -0.0136(4) 0.2292(4) 0.0436(3) 0.070(2) Uani ? C(265) 0.0467(3) 0.1667(4) 0.0305(2) 0.0567(15) Uani ? C(266) 0.1541(3) 0.1996(3) 0.06209(19) 0.0406(13) Uani ? C(901) 0.5345(4) 0.2877(4) 0.5641(3) 0.074(2) Uani ? C(902) 0.5197(4) 0.3745(4) 0.6066(4) 0.080(3) Uani ? C(903) 0.5706(5) 0.4205(4) 0.6811(4) 0.079(2) Uani ? C(904) 0.6357(4) 0.3804(4) 0.7137(3) 0.068(2) Uani ? C(905) 0.6506(3) 0.2947(4) 0.6718(3) 0.067(2) Uani ? C(906) 0.5990(4) 0.2492(4) 0.5970(3) 0.068(2) Uani ? C(911) 0.9105(9) 0.2503(6) 0.8699(4) 0.164(6) Uani ? C(912) 0.9631(5) 0.2508(5) 0.8180(4) 0.099(3) Uani ? C(913) 0.9702(6) 0.3273(6) 0.7935(5) 0.129(4) Uani ? C(914) 0.9310(8) 0.4000(6) 0.8241(5) 0.157(5) Uani ? C(915) 0.8799(7) 0.3996(6) 0.8844(5) 0.140(5) Uani ? C(916) 0.8592(7) 0.3256(7) 0.9033(4) 0.140(5) Uani ? C(921) 0.4446(6) 0.1013(6) 0.9764(4) 0.136(4) Uani ? C(922) 0.5045(9) 0.1826(6) 1.0261(4) 0.121(4) Uani ? C(923) 0.6111(9) 0.2147(5) 1.0215(4) 0.131(4) Uani ? C(924) 0.6457(5) 0.1560(6) 0.9608(5) 0.105(3) Uani ? C(925) 0.5809(5) 0.0759(5) 0.9129(4) 0.102(3) Uani ? C(926) 0.4805(5) 0.0459(6) 0.9200(4) 0.138(4) Uani ? H(14) -0.1290 -0.1598 0.3666 0.0420 Uiso calc H(24) 0.5350 0.4709 0.1352 0.0540 Uiso calc H(32) 0.2053 0.4158 0.2795 0.0640 Uiso calc H(33) 0.1979 0.5603 0.3628 0.0750 Uiso calc H(34) 0.0783 0.5652 0.4393 0.0820 Uiso calc H(35) -0.0344 0.4250 0.4323 0.0840 Uiso calc H(36) -0.0275 0.2795 0.3499 0.0640 Uiso calc H(3A) 0.0786 0.2462 0.1997 0.0330 Uiso calc H(3B) 0.0162 0.1953 0.2450 0.0330 Uiso calc H(42) 0.3866 0.3896 0.3937 0.0710 Uiso calc H(43) 0.3529 0.5130 0.4849 0.0940 Uiso calc H(44) 0.2339 0.4822 0.5569 0.0990 Uiso calc H(45) 0.1499 0.3249 0.5375 0.0880 Uiso calc H(46) 0.1873 0.2006 0.4481 0.0620 Uiso calc H(4A) 0.3167 0.1483 0.3746 0.0430 Uiso calc H(4B) 0.3913 0.2220 0.3495 0.0430 Uiso calc H(122) -0.0471 -0.0386 0.1340 0.0480 Uiso calc H(123) -0.1270 0.0205 0.0529 0.0640 Uiso calc H(124) -0.2316 0.1209 0.0936 0.0740 Uiso calc H(125) -0.2602 0.1578 0.2157 0.0650 Uiso calc H(126) -0.1887 0.0920 0.2940 0.0500 Uiso calc H(132) -0.2854 -0.0827 0.3698 0.0600 Uiso calc H(133) -0.4640 -0.1513 0.3256 0.0740 Uiso calc H(134) -0.5345 -0.2282 0.1985 0.0850 Uiso calc H(135) -0.4250 -0.2392 0.1143 0.1000 Uiso calc H(136) -0.2447 -0.1734 0.1577 0.0740 Uiso calc H(152) -0.0239 -0.0905 0.5055 0.0420 Uiso calc H(153) 0.0286 -0.1568 0.5898 0.0470 Uiso calc H(154) 0.1469 -0.2470 0.5671 0.0540 Uiso calc H(155) 0.2131 -0.2688 0.4585 0.0600 Uiso calc H(156) 0.1593 -0.2045 0.3729 0.0540 Uiso calc H(162) 0.2307 -0.0753 0.2681 0.0480 Uiso calc H(163) 0.4101 -0.0493 0.3023 0.0630 Uiso calc H(164) 0.4959 0.0264 0.4280 0.0720 Uiso calc H(165) 0.4026 0.0758 0.5195 0.0660 Uiso calc H(166) 0.2230 0.0476 0.4866 0.0500 Uiso calc H(222) 0.4642 0.1411 0.1907 0.0490 Uiso calc H(223) 0.5415 0.0686 0.2623 0.0590 Uiso calc H(224) 0.6402 0.1603 0.3841 0.0660 Uiso calc H(225) 0.6637 0.3234 0.4318 0.0640 Uiso calc H(226) 0.5894 0.3968 0.3609 0.0510 Uiso calc H(232) 0.6851 0.2980 0.1963 0.0970 Uiso calc H(233) 0.8685 0.3593 0.2309 0.1400 Uiso calc H(234) 0.9433 0.5215 0.2831 0.1630 Uiso calc H(235) 0.8431 0.6241 0.3016 0.1350 Uiso calc H(236) 0.6609 0.5680 0.2669 0.0940 Uiso calc H(252) 0.4281 0.5706 0.1180 0.0640 Uiso calc H(253) 0.3796 0.6321 0.0284 0.0780 Uiso calc H(254) 0.2696 0.5326 -0.0859 0.0860 Uiso calc H(255) 0.2080 0.3709 -0.1112 0.1030 Uiso calc H(256) 0.2555 0.3070 -0.0229 0.0760 Uiso calc H(262) 0.1700 0.4243 0.1465 0.0630 Uiso calc H(263) -0.0091 0.3685 0.0954 0.0940 Uiso calc H(264) -0.0858 0.2068 0.0234 0.0910 Uiso calc H(265) 0.0160 0.1022 0.0003 0.0730 Uiso calc H(266) 0.1948 0.1566 0.0536 0.0530 Uiso calc H(901) 0.5004 0.2562 0.5134 0.0960 Uiso calc H(902) 0.4753 0.4016 0.5845 0.1040 Uiso calc H(903) 0.5609 0.4789 0.7096 0.1030 Uiso calc H(904) 0.6698 0.4115 0.7645 0.0890 Uiso calc H(905) 0.6951 0.2674 0.6937 0.0880 Uiso calc H(906) 0.6087 0.1908 0.5685 0.0890 Uiso calc H(911) 0.9045 0.2000 0.8872 0.2140 Uiso calc H(912) 0.9948 0.2025 0.7980 0.1290 Uiso calc H(913) 1.0039 0.3274 0.7540 0.1670 Uiso calc H(914) 0.9370 0.4499 0.8064 0.2040 Uiso calc H(915) 0.8608 0.4539 0.9110 0.1830 Uiso calc H(916) 0.8146 0.3200 0.9360 0.1820 Uiso calc H(921) 0.3751 0.0806 0.9798 0.1770 Uiso calc H(922) 0.4780 0.2197 1.0643 0.1570 Uiso calc H(923) 0.6563 0.2719 1.0570 0.1710 Uiso calc H(924) 0.7145 0.1748 0.9553 0.1370 Uiso calc H(925) 0.6039 0.0381 0.8728 0.1330 Uiso calc H(926) 0.4364 -0.0128 0.8859 0.1790 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 Nb 0.02566(16) 0.02658(17) 0.03118(17) 0.00608(12) 0.00897(11) 0.01509(13) Cl 0.0516(5) 0.0361(5) 0.0421(5) 0.0127(4) 0.0158(4) 0.0117(4) O(1) 0.0246(11) 0.0272(13) 0.0335(12) 0.0040(9) 0.0063(9) 0.0148(10) O(2) 0.0277(11) 0.0294(13) 0.0333(12) 0.0053(10) 0.0079(9) 0.0165(10) C(3) 0.0199(15) 0.0287(18) 0.0348(17) 0.0057(13) 0.0050(13) 0.0211(14) C(4) 0.0293(17) 0.037(2) 0.0320(18) 0.0037(15) 0.0043(14) 0.0176(16) C(11) 0.0253(15) 0.0247(17) 0.0265(16) 0.0049(13) 0.0110(13) 0.0115(13) C(12) 0.0261(16) 0.0269(18) 0.0285(16) 0.0083(14) 0.0083(13) 0.0119(14) C(13) 0.0269(16) 0.0309(19) 0.0352(18) 0.0067(14) 0.0103(14) 0.0131(15) C(14) 0.0277(17) 0.035(2) 0.0405(19) 0.0062(15) 0.0147(15) 0.0208(16) C(15) 0.0304(17) 0.0268(18) 0.0341(17) 0.0085(14) 0.0126(14) 0.0148(15) C(16) 0.0287(16) 0.0260(18) 0.0302(17) 0.0089(14) 0.0094(13) 0.0125(14) C(21) 0.0289(16) 0.0265(18) 0.0314(17) 0.0055(14) 0.0107(14) 0.0145(14) C(22) 0.0332(18) 0.0309(19) 0.0351(18) 0.0077(15) 0.0122(15) 0.0173(15) C(23) 0.0301(18) 0.045(2) 0.051(2) 0.0107(16) 0.0162(16) 0.0302(19) C(24) 0.042(2) 0.043(2) 0.053(2) 0.0098(18) 0.0202(18) 0.0324(19) C(25) 0.042(2) 0.034(2) 0.0374(19) 0.0144(16) 0.0160(16) 0.0203(16) C(26) 0.0333(17) 0.0289(19) 0.0324(17) 0.0086(15) 0.0107(14) 0.0158(15) C(31) 0.0351(19) 0.046(2) 0.040(2) 0.0126(17) 0.0095(15) 0.0242(18) C(32) 0.052(2) 0.043(2) 0.052(2) 0.0059(19) 0.0206(19) 0.017(2) C(33) 0.078(3) 0.035(2) 0.056(3) 0.006(2) 0.023(2) 0.016(2) C(34) 0.093(3) 0.045(3) 0.051(2) 0.016(3) 0.031(2) 0.014(2) C(35) 0.086(3) 0.055(3) 0.054(3) 0.017(3) 0.041(2) 0.016(2) C(36) 0.062(3) 0.043(2) 0.046(2) 0.008(2) 0.024(2) 0.0215(19) C(41) 0.0286(17) 0.038(2) 0.0356(18) 0.0028(15) 0.0014(14) 0.0158(16) C(42) 0.053(2) 0.043(3) 0.060(3) 0.004(2) 0.012(2) 0.016(2) C(43) 0.075(3) 0.041(3) 0.081(3) 0.006(2) 0.008(3) 0.009(3) C(44) 0.065(3) 0.055(3) 0.082(3) 0.016(3) 0.016(3) -0.006(3) C(45) 0.051(3) 0.068(3) 0.065(3) 0.005(2) 0.022(2) 0.003(3) C(46) 0.037(2) 0.046(2) 0.050(2) 0.0035(18) 0.0120(18) 0.0119(19) C(121) 0.0241(16) 0.0316(19) 0.0333(18) 0.0029(14) 0.0040(13) 0.0139(15) C(122) 0.0324(18) 0.039(2) 0.0361(19) 0.0050(16) 0.0048(15) 0.0148(16) C(123) 0.043(2) 0.059(3) 0.041(2) 0.002(2) 0.0024(17) 0.024(2) C(124) 0.042(2) 0.075(3) 0.064(3) 0.013(2) -0.001(2) 0.046(3) C(125) 0.037(2) 0.058(3) 0.069(3) 0.020(2) 0.0110(19) 0.037(2) C(126) 0.0303(18) 0.044(2) 0.048(2) 0.0141(16) 0.0100(16) 0.0233(18) C(131) 0.0298(17) 0.032(2) 0.0381(19) 0.0031(15) 0.0065(15) 0.0163(16) C(132) 0.0322(19) 0.065(3) 0.043(2) 0.0120(19) 0.0131(16) 0.023(2) C(133) 0.033(2) 0.082(3) 0.064(3) 0.013(2) 0.019(2) 0.037(3) C(134) 0.031(2) 0.081(4) 0.076(3) -0.006(2) 0.001(2) 0.035(3) C(135) 0.040(2) 0.099(4) 0.053(3) -0.022(2) -0.006(2) 0.013(3) C(136) 0.040(2) 0.068(3) 0.046(2) -0.007(2) 0.0103(18) 0.014(2) C(151) 0.0275(16) 0.0264(18) 0.0437(19) 0.0070(14) 0.0120(14) 0.0194(15) C(152) 0.0338(18) 0.0314(19) 0.0373(18) 0.0118(15) 0.0123(15) 0.0171(15) C(153) 0.0397(19) 0.040(2) 0.0373(19) 0.0113(17) 0.0144(16) 0.0209(17) C(154) 0.041(2) 0.047(2) 0.051(2) 0.0145(18) 0.0156(17) 0.0317(19) C(155) 0.052(2) 0.048(2) 0.064(3) 0.028(2) 0.030(2) 0.037(2) C(156) 0.048(2) 0.044(2) 0.054(2) 0.0237(18) 0.0304(18) 0.0313(19) C(161) 0.0282(17) 0.0304(19) 0.0403(19) 0.0066(14) 0.0086(14) 0.0225(16) C(162) 0.0331(18) 0.036(2) 0.048(2) 0.0121(16) 0.0133(16) 0.0214(17) C(163) 0.036(2) 0.051(3) 0.077(3) 0.0191(19) 0.022(2) 0.039(2) C(164) 0.0270(19) 0.061(3) 0.093(3) 0.0087(19) 0.001(2) 0.052(3) C(165) 0.037(2) 0.061(3) 0.061(3) 0.006(2) -0.0044(19) 0.040(2) C(166) 0.0361(19) 0.041(2) 0.041(2) 0.0046(16) 0.0039(16) 0.0262(17) C(221) 0.0243(16) 0.038(2) 0.0423(19) 0.0058(15) 0.0124(15) 0.0232(17) C(222) 0.0320(18) 0.044(2) 0.045(2) 0.0150(16) 0.0155(16) 0.0222(18) C(223) 0.042(2) 0.046(2) 0.063(3) 0.0198(19) 0.0218(19) 0.033(2) C(224) 0.037(2) 0.066(3) 0.065(3) 0.017(2) 0.0119(19) 0.044(2) C(225) 0.036(2) 0.060(3) 0.052(2) 0.0042(19) -0.0005(17) 0.031(2) C(226) 0.0323(18) 0.041(2) 0.045(2) 0.0059(16) 0.0064(16) 0.0208(18) C(231) 0.036(2) 0.075(3) 0.065(3) 0.013(2) 0.0167(19) 0.053(3) C(232) 0.040(2) 0.108(4) 0.119(4) 0.025(3) 0.030(3) 0.088(4) C(233) 0.044(3) 0.171(7) 0.171(6) 0.035(4) 0.031(4) 0.136(6) C(234) 0.034(3) 0.206(10) 0.169(7) -0.006(4) 0.009(4) 0.139(7) C(235) 0.053(3) 0.131(6) 0.114(5) -0.025(4) 0.004(3) 0.067(5) C(236) 0.051(3) 0.083(4) 0.075(3) -0.016(3) 0.012(2) 0.041(3) C(251) 0.045(2) 0.038(2) 0.039(2) 0.0111(17) 0.0152(16) 0.0255(17) C(252) 0.057(2) 0.048(3) 0.051(2) 0.010(2) 0.0125(19) 0.031(2) C(253) 0.068(3) 0.058(3) 0.075(3) 0.016(2) 0.019(2) 0.050(3) C(254) 0.067(3) 0.088(4) 0.065(3) 0.015(3) 0.011(2) 0.060(3) C(255) 0.097(4) 0.085(4) 0.048(3) -0.002(3) -0.001(2) 0.040(3) C(256) 0.079(3) 0.052(3) 0.041(2) 0.002(2) 0.004(2) 0.026(2) C(261) 0.0343(18) 0.038(2) 0.0328(18) 0.0031(16) 0.0045(15) 0.0213(16) C(262) 0.042(2) 0.048(3) 0.070(3) 0.0155(19) 0.013(2) 0.037(2) C(263) 0.045(3) 0.084(4) 0.107(4) 0.026(3) 0.008(3) 0.059(3) C(264) 0.042(2) 0.088(4) 0.083(3) 0.005(3) -0.006(2) 0.051(3) C(265) 0.050(2) 0.064(3) 0.045(2) -0.007(2) 0.0000(19) 0.025(2) C(266) 0.044(2) 0.043(2) 0.0327(19) 0.0054(18) 0.0065(16) 0.0166(17) C(901) 0.073(3) 0.072(4) 0.062(3) -0.005(3) 0.018(3) 0.021(3) C(902) 0.073(3) 0.076(4) 0.108(5) 0.023(3) 0.027(3) 0.052(4) C(903) 0.084(4) 0.052(3) 0.096(4) 0.018(3) 0.044(3) 0.014(3) C(904) 0.064(3) 0.072(4) 0.061(3) 0.002(3) 0.028(2) 0.020(3) C(905) 0.042(2) 0.062(3) 0.106(4) 0.007(2) 0.029(3) 0.043(3) C(906) 0.057(3) 0.042(3) 0.095(4) 0.002(2) 0.038(3) 0.013(3) C(911) 0.342(14) 0.100(6) 0.086(5) 0.091(8) 0.056(7) 0.057(5) C(912) 0.123(5) 0.065(4) 0.077(4) 0.015(4) 0.009(4) -0.001(3) C(913) 0.125(6) 0.111(6) 0.176(8) 0.035(5) 0.095(6) 0.062(6) C(914) 0.269(11) 0.107(6) 0.196(8) 0.107(7) 0.162(9) 0.107(6) C(915) 0.207(9) 0.132(7) 0.178(8) 0.120(7) 0.108(7) 0.108(6) C(916) 0.223(9) 0.150(8) 0.144(7) 0.102(7) 0.115(7) 0.117(6) C(921) 0.100(5) 0.141(7) 0.120(6) 0.035(5) 0.023(5) -0.012(6) C(922) 0.217(9) 0.068(5) 0.078(5) 0.059(6) 0.029(6) 0.015(4) C(923) 0.215(10) 0.052(4) 0.084(5) -0.012(5) -0.044(6) 0.031(4) C(924) 0.089(4) 0.090(5) 0.133(6) 0.008(4) -0.011(4) 0.061(5) C(925) 0.068(4) 0.085(5) 0.123(5) 0.025(3) 0.012(4) 0.002(4) C(926) 0.084(5) 0.125(6) 0.135(6) 0.016(4) 0.032(4) -0.033(5) # 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 Nb O(2) 1.903(2) ? Nb O(1) 1.908(2) ? Nb C(4) 2.162(3) ? Nb C(3) 2.210(3) ? Nb Cl 2.3567(9) ? O(1) C(11) 1.365(3) ? O(2) C(21) 1.368(4) ? C(4) C(41) 1.477(5) ? C(3) C(31) 1.437(5) ? C(11) C(12) 1.410(4) ? C(11) C(16) 1.413(4) ? C(12) C(13) 1.403(4) ? C(12) C(121) 1.487(4) ? C(13) C(14) 1.395(5) ? C(13) C(131) 1.485(4) ? C(14) C(15) 1.377(4) ? C(15) C(16) 1.411(4) ? C(15) C(151) 1.492(5) ? C(16) C(161) 1.490(4) ? C(21) C(26) 1.409(4) ? C(21) C(22) 1.412(4) ? C(22) C(23) 1.407(5) ? C(22) C(221) 1.488(5) ? C(23) C(24) 1.389(5) ? C(23) C(231) 1.497(5) ? C(24) C(25) 1.403(5) ? C(25) C(26) 1.416(4) ? C(25) C(251) 1.486(5) ? C(26) C(261) 1.490(4) ? C(31) C(32) 1.389(5) ? C(31) C(36) 1.392(5) ? C(32) C(33) 1.379(6) ? C(33) C(34) 1.369(6) ? C(34) C(35) 1.363(6) ? C(35) C(36) 1.381(6) ? C(41) C(42) 1.376(5) ? C(41) C(46) 1.399(5) ? C(42) C(43) 1.370(6) ? C(43) C(44) 1.377(7) ? C(44) C(45) 1.377(7) ? C(45) C(46) 1.379(6) ? C(121) C(122) 1.388(4) ? C(121) C(126) 1.397(5) ? C(122) C(123) 1.386(5) ? C(123) C(124) 1.382(6) ? C(124) C(125) 1.391(6) ? C(125) C(126) 1.373(5) ? C(131) C(136) 1.377(5) ? C(131) C(132) 1.391(4) ? C(132) C(133) 1.381(5) ? C(133) C(134) 1.360(6) ? C(134) C(135) 1.370(6) ? C(135) C(136) 1.393(5) ? C(152) C(153) 1.379(5) ? C(152) C(151) 1.394(4) ? C(153) C(154) 1.375(5) ? C(154) C(155) 1.386(5) ? C(155) C(156) 1.380(5) ? C(156) C(151) 1.387(5) ? C(161) C(166) 1.391(5) ? C(161) C(162) 1.393(4) ? C(162) C(163) 1.379(5) ? C(163) C(164) 1.379(6) ? C(164) C(165) 1.373(6) ? C(165) C(166) 1.377(5) ? C(221) C(226) 1.388(5) ? C(221) C(222) 1.394(5) ? C(222) C(223) 1.389(5) ? C(223) C(224) 1.387(6) ? C(224) C(225) 1.370(6) ? C(225) C(226) 1.379(5) ? C(231) C(232) 1.386(6) ? C(231) C(236) 1.393(7) ? C(232) C(233) 1.404(7) ? C(233) C(234) 1.357(10) ? C(234) C(235) 1.338(10) ? C(235) C(236) 1.391(7) ? C(251) C(256) 1.381(5) ? C(251) C(252) 1.395(5) ? C(252) C(253) 1.388(5) ? C(253) C(254) 1.362(6) ? C(254) C(255) 1.374(7) ? C(255) C(256) 1.391(6) ? C(261) C(266) 1.387(5) ? C(261) C(262) 1.392(5) ? C(262) C(263) 1.383(6) ? C(263) C(264) 1.388(7) ? C(264) C(265) 1.366(7) ? C(265) C(266) 1.389(5) ? C(901) C(906) 1.350(7) ? C(901) C(902) 1.385(7) ? C(902) C(903) 1.368(7) ? C(903) C(904) 1.372(8) ? C(904) C(905) 1.368(7) ? C(905) C(906) 1.376(7) ? C(911) C(912) 1.291(10) ? C(911) C(916) 1.477(11) ? C(912) C(913) 1.395(10) ? C(913) C(914) 1.328(9) ? C(914) C(915) 1.418(9) ? C(915) C(916) 1.290(9) ? C(921) C(922) 1.297(10) ? C(921) C(926) 1.352(8) ? C(922) C(923) 1.423(11) ? C(923) C(924) 1.416(10) ? C(924) C(925) 1.298(9) ? C(925) C(926) 1.356(8) ? 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) Nb O(1) 176.87(9) ? O(2) Nb C(4) 90.39(11) ? O(1) Nb C(4) 90.01(11) ? O(2) Nb C(3) 91.18(10) ? O(1) Nb C(3) 91.22(10) ? C(4) Nb C(3) 122.57(12) ? O(2) Nb Cl 88.88(7) ? O(1) Nb Cl 88.24(7) ? C(4) Nb Cl 120.43(10) ? C(3) Nb Cl 117.00(8) ? C(11) O(1) Nb 174.6(2) ? C(21) O(2) Nb 177.0(2) ? C(41) C(4) Nb 103.2(2) ? C(31) C(3) Nb 124.1(2) ? O(1) C(11) C(12) 119.7(3) ? O(1) C(11) C(16) 118.9(3) ? C(12) C(11) C(16) 121.4(3) ? C(13) C(12) C(11) 118.7(3) ? C(13) C(12) C(121) 120.1(3) ? C(11) C(12) C(121) 121.1(3) ? C(14) C(13) C(12) 119.2(3) ? C(14) C(13) C(131) 118.0(3) ? C(12) C(13) C(131) 122.9(3) ? C(15) C(14) C(13) 122.8(3) ? C(14) C(15) C(16) 119.1(3) ? C(14) C(15) C(151) 118.2(3) ? C(16) C(15) C(151) 122.7(3) ? C(15) C(16) C(11) 118.7(3) ? C(15) C(16) C(161) 120.5(3) ? C(11) C(16) C(161) 120.8(3) ? O(2) C(21) C(26) 118.9(3) ? O(2) C(21) C(22) 119.1(3) ? C(26) C(21) C(22) 122.0(3) ? C(23) C(22) C(21) 118.1(3) ? C(23) C(22) C(221) 121.1(3) ? C(21) C(22) C(221) 120.7(3) ? C(24) C(23) C(22) 119.6(3) ? C(24) C(23) C(231) 116.8(3) ? C(22) C(23) C(231) 123.6(3) ? C(23) C(24) C(25) 123.0(3) ? C(24) C(25) C(26) 117.9(3) ? C(24) C(25) C(251) 117.7(3) ? C(26) C(25) C(251) 124.3(3) ? C(21) C(26) C(25) 119.1(3) ? C(21) C(26) C(261) 121.0(3) ? C(25) C(26) C(261) 119.9(3) ? C(32) C(31) C(36) 116.9(4) ? C(32) C(31) C(3) 123.8(3) ? C(36) C(31) C(3) 119.3(3) ? C(33) C(32) C(31) 121.4(4) ? C(34) C(33) C(32) 120.3(4) ? C(35) C(34) C(33) 119.7(4) ? C(34) C(35) C(36) 120.3(4) ? C(35) C(36) C(31) 121.4(4) ? C(42) C(41) C(46) 117.6(4) ? C(42) C(41) C(4) 121.8(3) ? C(46) C(41) C(4) 120.5(3) ? C(43) C(42) C(41) 121.3(4) ? C(42) C(43) C(44) 120.7(5) ? C(43) C(44) C(45) 119.4(4) ? C(44) C(45) C(46) 119.8(4) ? C(45) C(46) C(41) 121.2(4) ? C(122) C(121) C(126) 118.4(3) ? C(122) C(121) C(12) 121.3(3) ? C(126) C(121) C(12) 120.2(3) ? C(123) C(122) C(121) 120.5(3) ? C(124) C(123) C(122) 120.5(4) ? C(123) C(124) C(125) 119.3(4) ? C(126) C(125) C(124) 120.2(4) ? C(125) C(126) C(121) 121.0(3) ? C(136) C(131) C(132) 117.7(3) ? C(136) C(131) C(13) 121.2(3) ? C(132) C(131) C(13) 120.9(3) ? C(133) C(132) C(131) 120.9(4) ? C(134) C(133) C(132) 120.8(4) ? C(133) C(134) C(135) 119.3(4) ? C(134) C(135) C(136) 120.4(4) ? C(131) C(136) C(135) 120.8(4) ? C(153) C(152) C(151) 121.2(3) ? C(154) C(153) C(152) 120.6(3) ? C(153) C(154) C(155) 118.7(3) ? C(156) C(155) C(154) 120.9(3) ? C(155) C(156) C(151) 120.8(3) ? C(156) C(151) C(152) 117.8(3) ? C(156) C(151) C(15) 123.3(3) ? C(152) C(151) C(15) 119.0(3) ? C(166) C(161) C(162) 118.7(3) ? C(166) C(161) C(16) 121.4(3) ? C(162) C(161) C(16) 119.9(3) ? C(163) C(162) C(161) 120.5(3) ? C(162) C(163) C(164) 120.0(4) ? C(165) C(164) C(163) 120.1(3) ? C(164) C(165) C(166) 120.3(4) ? C(165) C(166) C(161) 120.5(4) ? C(226) C(221) C(222) 118.5(3) ? C(226) C(221) C(22) 121.8(3) ? C(222) C(221) C(22) 119.5(3) ? C(223) C(222) C(221) 120.5(4) ? C(224) C(223) C(222) 120.0(4) ? C(225) C(224) C(223) 119.5(4) ? C(224) C(225) C(226) 121.0(4) ? C(225) C(226) C(221) 120.5(4) ? C(232) C(231) C(236) 118.8(4) ? C(232) C(231) C(23) 121.6(4) ? C(236) C(231) C(23) 119.5(4) ? C(231) C(232) C(233) 119.9(6) ? C(234) C(233) C(232) 119.6(6) ? C(235) C(234) C(233) 121.1(6) ? C(234) C(235) C(236) 121.2(7) ? C(235) C(236) C(231) 119.3(6) ? C(256) C(251) C(252) 118.4(4) ? C(256) C(251) C(25) 122.7(3) ? C(252) C(251) C(25) 118.9(3) ? C(253) C(252) C(251) 120.8(4) ? C(254) C(253) C(252) 120.3(4) ? C(253) C(254) C(255) 119.5(4) ? C(254) C(255) C(256) 121.1(4) ? C(251) C(256) C(255) 120.0(4) ? C(266) C(261) C(262) 119.0(3) ? C(266) C(261) C(26) 119.8(3) ? C(262) C(261) C(26) 121.2(3) ? C(263) C(262) C(261) 120.2(4) ? C(262) C(263) C(264) 120.0(5) ? C(265) C(264) C(263) 120.3(4) ? C(264) C(265) C(266) 120.0(4) ? C(261) C(266) C(265) 120.6(4) ? C(906) C(901) C(902) 119.3(5) ? C(903) C(902) C(901) 120.0(6) ? C(902) C(903) C(904) 120.1(5) ? C(905) C(904) C(903) 120.1(5) ? C(904) C(905) C(906) 119.2(5) ? C(901) C(906) C(905) 121.4(5) ? C(912) C(911) C(916) 123.4(7) ? C(911) C(912) C(913) 116.7(7) ? C(914) C(913) C(912) 122.9(7) ? C(913) C(914) C(915) 118.4(7) ? C(916) C(915) C(914) 121.5(7) ? C(915) C(916) C(911) 116.2(7) ? C(922) C(921) C(926) 121.8(8) ? C(921) C(922) C(923) 119.5(7) ? C(924) C(923) C(922) 117.4(6) ? C(925) C(924) C(923) 119.6(7) ? C(924) C(925) C(926) 121.6(7) ? C(921) C(926) C(925) 120.1(7) ? #===END #============================================================================== data_SS2113 _database_code_CSD 164016 _audit_creation_date 18-01-00 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C92 H74 Cl O2 Ta' _chemical_formula_structural ? _chemical_formula_weight 1428.02 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3027(8) _cell_length_b 15.3219(9) _cell_length_c 19.1817(10) _cell_angle_alpha 109.364(3) _cell_angle_beta 97.258(4) _cell_angle_gamma 102.355(3) _cell_volume 3519.5(8) _cell_measurement_reflns_used 28890 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.35 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.629 _cell_measurement_temperature 173 _exptl_crystal_F_000 1464 # 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 0.6425 _exptl_absorpt_correction_T_max 0.8157 _diffrn_reflns_number 28890 _reflns_number_total 14779 _reflns_number_gt 12956 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.156 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_max 19 _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 0.057 _refine_ls_wR_factor_ref 0.108 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 11600 _refine_ls_d_res_high 0.84 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+3.8882P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.86 _refine_diff_density_min -1.41 _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 0.20249(2) 0.159820(18) 0.255070(15) 0.01821(8) Uani ? Cl 0.19864(13) 0.02837(11) 0.14652(9) 0.0316(5) Uani ? O(1) 0.1126(3) 0.0723(3) 0.2858(2) 0.0209(13) Uani ? O(2) 0.2946(3) 0.2405(3) 0.2201(2) 0.0223(13) Uani ? C(3) 0.3181(5) 0.2022(4) 0.3568(3) 0.0240(19) Uani ? C(4) 0.0834(4) 0.2393(4) 0.2511(3) 0.0125(19) Uani ? C(11) 0.0481(4) 0.0036(4) 0.3037(3) 0.0166(19) Uani ? C(12) -0.0618(4) -0.0232(4) 0.2751(3) 0.0204(19) Uani ? C(13) -0.1273(5) -0.0872(4) 0.2985(3) 0.0219(19) Uani ? C(14) -0.0829(5) -0.1218(4) 0.3501(3) 0.025(2) Uani ? C(15) 0.0254(5) -0.0981(4) 0.3767(3) 0.0203(19) Uani ? C(16) 0.0928(4) -0.0372(4) 0.3512(3) 0.0207(19) Uani ? C(21) 0.3604(5) 0.2954(4) 0.1910(3) 0.0221(19) Uani ? C(22) 0.4702(5) 0.3207(4) 0.2193(3) 0.024(2) Uani ? C(23) 0.5339(5) 0.3868(5) 0.1960(4) 0.030(2) Uani ? C(24) 0.4893(5) 0.4226(5) 0.1452(4) 0.032(2) Uani ? C(25) 0.3813(5) 0.3930(4) 0.1146(4) 0.026(2) Uani ? C(26) 0.3155(5) 0.3298(4) 0.1385(3) 0.0230(19) Uani ? C(31) 0.2919(5) 0.2828(5) 0.4139(3) 0.026(2) Uani ? C(32) 0.3404(6) 0.3780(5) 0.4254(4) 0.048(3) Uani ? C(33) 0.3216(7) 0.4536(6) 0.4805(5) 0.062(4) Uani ? C(34) 0.2492(7) 0.4348(6) 0.5240(5) 0.065(3) Uani ? C(35) 0.1979(6) 0.3399(6) 0.5103(5) 0.055(3) Uani ? C(36) 0.2194(5) 0.2650(5) 0.4575(4) 0.039(3) Uani ? C(41) 0.0879(5) 0.3320(5) 0.3057(4) 0.034(3) Uani ? C(42) 0.1567(6) 0.4161(5) 0.3109(4) 0.041(3) Uani ? C(43) 0.1526(7) 0.5037(5) 0.3601(4) 0.050(3) Uani ? C(44) 0.0781(7) 0.5080(6) 0.4046(4) 0.057(4) Uani ? C(45) 0.0095(7) 0.4252(6) 0.4013(5) 0.055(3) Uani ? C(46) 0.0158(6) 0.3390(5) 0.3525(4) 0.040(3) Uani ? C(121) -0.1084(4) 0.0193(4) 0.2225(4) 0.023(2) Uani ? C(122) -0.0902(5) -0.0024(5) 0.1499(4) 0.029(2) Uani ? C(123) -0.1376(5) 0.0325(5) 0.1002(4) 0.036(3) Uani ? C(124) -0.2015(6) 0.0922(6) 0.1247(4) 0.047(3) Uani ? C(125) -0.2202(5) 0.1148(5) 0.1976(4) 0.042(3) Uani ? C(126) -0.1740(5) 0.0772(5) 0.2464(4) 0.031(2) Uani ? C(131) -0.2439(5) -0.1245(4) 0.2686(4) 0.025(2) Uani ? C(132) -0.3119(5) -0.1182(5) 0.3173(4) 0.037(3) Uani ? C(133) -0.4191(5) -0.1567(6) 0.2918(4) 0.043(3) Uani ? C(134) -0.4596(6) -0.2052(6) 0.2141(5) 0.059(3) Uani ? C(135) -0.3947(6) -0.2120(7) 0.1638(5) 0.064(4) Uani ? C(136) -0.2852(6) -0.1708(5) 0.1917(4) 0.046(3) Uani ? C(151) 0.0642(5) -0.1403(4) 0.4311(4) 0.024(2) Uani ? C(152) 0.0236(5) -0.1277(4) 0.4964(3) 0.025(2) Uani ? C(153) 0.0549(5) -0.1674(5) 0.5481(4) 0.031(2) Uani ? C(154) 0.1276(5) -0.2194(5) 0.5358(4) 0.033(3) Uani ? C(155) 0.1676(5) -0.2325(5) 0.4710(4) 0.036(3) Uani ? C(156) 0.1367(5) -0.1926(5) 0.4195(4) 0.030(2) Uani ? C(161) 0.2096(5) -0.0158(4) 0.3742(3) 0.022(2) Uani ? C(162) 0.2659(5) -0.0463(4) 0.3191(4) 0.028(2) Uani ? C(163) 0.3743(5) -0.0296(5) 0.3396(4) 0.038(3) Uani ? C(164) 0.4246(6) 0.0153(5) 0.4141(5) 0.044(3) Uani ? C(165) 0.3693(6) 0.0459(5) 0.4690(4) 0.040(3) Uani ? C(166) 0.2620(5) 0.0305(4) 0.4502(4) 0.029(2) Uani ? C(221) 0.5165(5) 0.2748(4) 0.2669(4) 0.025(2) Uani ? C(222) 0.5035(5) 0.1759(5) 0.2394(4) 0.030(2) Uani ? C(223) 0.5484(5) 0.1322(5) 0.2817(4) 0.036(3) Uani ? C(224) 0.6089(6) 0.1874(6) 0.3543(4) 0.041(3) Uani ? C(225) 0.6219(5) 0.2861(5) 0.3831(4) 0.041(3) Uani ? C(226) 0.5774(5) 0.3288(5) 0.3402(4) 0.034(3) Uani ? C(231) 0.6519(5) 0.4220(6) 0.2229(4) 0.042(3) Uani ? C(232) 0.7142(6) 0.3609(7) 0.2143(5) 0.059(4) Uani ? C(233) 0.8235(7) 0.3945(9) 0.2344(6) 0.077(5) Uani ? C(234) 0.8695(8) 0.4920(11) 0.2667(8) 0.105(7) Uani ? C(235) 0.8097(8) 0.5558(9) 0.2761(6) 0.086(5) Uani ? C(236) 0.6984(6) 0.5178(6) 0.2531(5) 0.058(4) Uani ? C(251) 0.3440(5) 0.4329(5) 0.0580(4) 0.030(2) Uani ? C(252) 0.3824(6) 0.5293(5) 0.0715(4) 0.039(3) Uani ? C(253) 0.3527(6) 0.5673(6) 0.0192(5) 0.049(3) Uani ? C(254) 0.2836(7) 0.5100(6) -0.0485(5) 0.055(4) Uani ? C(255) 0.2455(7) 0.4123(7) -0.0631(5) 0.064(4) Uani ? C(256) 0.2748(6) 0.3735(6) -0.0110(4) 0.049(3) Uani ? C(261) 0.1977(5) 0.2945(5) 0.1068(4) 0.030(2) Uani ? C(262) 0.1357(6) 0.3589(5) 0.1204(4) 0.041(3) Uani ? C(263) 0.0291(6) 0.3273(6) 0.0914(5) 0.056(4) Uani ? C(264) -0.0158(6) 0.2314(7) 0.0478(5) 0.059(4) Uani ? C(265) 0.0446(6) 0.1676(6) 0.0321(4) 0.047(3) Uani ? C(266) 0.1515(5) 0.2004(5) 0.0624(3) 0.031(2) Uani ? C(901) 0.5349(7) 0.2898(6) 0.5650(5) 0.061(4) Uani ? C(902) 0.5198(7) 0.3775(7) 0.6072(6) 0.066(4) Uani ? C(903) 0.5694(7) 0.4217(6) 0.6816(5) 0.057(4) Uani ? C(904) 0.6358(7) 0.3830(6) 0.7150(5) 0.053(3) Uani ? C(905) 0.6519(6) 0.2965(6) 0.6741(5) 0.049(3) Uani ? C(906) 0.5993(7) 0.2499(6) 0.5999(6) 0.057(4) Uani ? C(911) 0.0371(8) 0.7460(6) 0.1848(5) 0.065(4) Uani ? C(912) 0.0349(8) 0.6763(7) 0.2120(7) 0.086(5) Uani ? C(913) 0.0823(10) 0.6048(8) 0.1819(7) 0.097(6) Uani ? C(914) 0.1182(9) 0.5986(8) 0.1167(6) 0.091(6) Uani ? C(915) 0.1242(12) 0.6720(9) 0.0928(7) 0.118(7) Uani ? C(916) 0.0789(11) 0.7455(8) 0.1268(6) 0.107(6) Uani ? C(921) 0.4822(9) 0.0486(9) 0.9168(8) 0.124(6) Uani ? C(922) 0.5796(8) 0.0753(7) 0.9065(7) 0.093(5) Uani ? C(923) 0.6471(9) 0.1572(9) 0.9575(7) 0.090(5) Uani ? C(924) 0.6155(16) 0.2128(8) 1.0183(7) 0.119(7) Uani ? C(925) 0.5131(16) 0.1808(11) 1.0263(8) 0.116(8) Uani ? C(926) 0.4471(10) 0.1003(10) 0.9770(7) 0.124(6) Uani ? H(14) -0.1272 -0.1621 0.3672 0.0320 Uiso calc H(24) 0.5327 0.4674 0.1315 0.0420 Uiso calc H(32) 0.3865 0.3909 0.3951 0.0610 Uiso calc H(33) 0.3568 0.5167 0.4887 0.0800 Uiso calc H(34) 0.2356 0.4849 0.5614 0.0850 Uiso calc H(35) 0.1477 0.3270 0.5378 0.0710 Uiso calc H(36) 0.1856 0.2020 0.4506 0.0500 Uiso calc H(3A) 0.3153 0.1488 0.3737 0.0310 Uiso calc H(3B) 0.3882 0.2234 0.3486 0.0310 Uiso calc H(42) 0.2065 0.4138 0.2808 0.0530 Uiso calc H(43) 0.1998 0.5601 0.3634 0.0650 Uiso calc H(44) 0.0745 0.5673 0.4369 0.0740 Uiso calc H(45) -0.0401 0.4276 0.4314 0.0720 Uiso calc H(46) -0.0300 0.2827 0.3506 0.0530 Uiso calc H(4A) 0.0771 0.2463 0.2024 0.0160 Uiso calc H(4B) 0.0171 0.1964 0.2493 0.0160 Uiso calc H(122) -0.0457 -0.0408 0.1344 0.0380 Uiso calc H(123) -0.1267 0.0161 0.0511 0.0460 Uiso calc H(124) -0.2321 0.1172 0.0921 0.0610 Uiso calc H(125) -0.2631 0.1547 0.2136 0.0540 Uiso calc H(126) -0.1872 0.0910 0.2948 0.0400 Uiso calc H(132) -0.2846 -0.0869 0.3690 0.0480 Uiso calc H(133) -0.4639 -0.1506 0.3257 0.0560 Uiso calc H(134) -0.5317 -0.2332 0.1964 0.0760 Uiso calc H(135) -0.4222 -0.2433 0.1121 0.0840 Uiso calc H(136) -0.2403 -0.1749 0.1581 0.0590 Uiso calc H(152) -0.0252 -0.0921 0.5055 0.0330 Uiso calc H(153) 0.0266 -0.1588 0.5911 0.0410 Uiso calc H(154) 0.1496 -0.2453 0.5706 0.0430 Uiso calc H(155) 0.2158 -0.2686 0.4619 0.0470 Uiso calc H(156) 0.1654 -0.2012 0.3767 0.0390 Uiso calc H(162) 0.2313 -0.0777 0.2686 0.0360 Uiso calc H(163) 0.4126 -0.0490 0.3028 0.0500 Uiso calc H(164) 0.4969 0.0253 0.4277 0.0570 Uiso calc H(165) 0.4047 0.0772 0.5193 0.0520 Uiso calc H(166) 0.2247 0.0506 0.4876 0.0380 Uiso calc H(222) 0.4633 0.1386 0.1911 0.0380 Uiso calc H(223) 0.5386 0.0660 0.2621 0.0470 Uiso calc H(224) 0.6403 0.1584 0.3833 0.0540 Uiso calc H(225) 0.6611 0.3231 0.4317 0.0530 Uiso calc H(226) 0.5875 0.3951 0.3599 0.0440 Uiso calc H(232) 0.6828 0.2949 0.1944 0.0760 Uiso calc H(233) 0.8647 0.3516 0.2261 0.1000 Uiso calc H(234) 0.9425 0.5149 0.2823 0.1360 Uiso calc H(235) 0.8408 0.6218 0.2970 0.1120 Uiso calc H(236) 0.6564 0.5600 0.2590 0.0760 Uiso calc H(252) 0.4293 0.5693 0.1168 0.0500 Uiso calc H(253) 0.3797 0.6326 0.0296 0.0640 Uiso calc H(254) 0.2629 0.5360 -0.0836 0.0720 Uiso calc H(255) 0.1995 0.3726 -0.1088 0.0820 Uiso calc H(256) 0.2487 0.3081 -0.0217 0.0640 Uiso calc H(262) 0.1669 0.4236 0.1493 0.0530 Uiso calc H(263) -0.0122 0.3700 0.1011 0.0730 Uiso calc H(264) -0.0881 0.2095 0.0286 0.0770 Uiso calc H(265) 0.0138 0.1034 0.0016 0.0620 Uiso calc H(266) 0.1926 0.1576 0.0524 0.0410 Uiso calc H(901) 0.5020 0.2585 0.5142 0.0790 Uiso calc H(902) 0.4765 0.4057 0.5850 0.0860 Uiso calc H(903) 0.5579 0.4794 0.7103 0.0750 Uiso calc H(904) 0.6701 0.4152 0.7655 0.0690 Uiso calc H(905) 0.6975 0.2702 0.6962 0.0630 Uiso calc H(906) 0.6073 0.1901 0.5725 0.0740 Uiso calc H(911) 0.0084 0.7958 0.2076 0.0840 Uiso calc H(912) 0.0011 0.6759 0.2515 0.1120 Uiso calc H(913) 0.0899 0.5616 0.2053 0.1260 Uiso calc H(914) 0.1379 0.5445 0.0898 0.1180 Uiso calc H(915) 0.1584 0.6742 0.0537 0.1540 Uiso calc H(916) 0.0785 0.7941 0.1080 0.1390 Uiso calc H(921) 0.4360 -0.0079 0.8814 0.1610 Uiso calc H(922) 0.6006 0.0382 0.8648 0.1210 Uiso calc H(923) 0.7156 0.1761 0.9515 0.1170 Uiso calc H(924) 0.6610 0.2700 1.0531 0.1550 Uiso calc H(925) 0.4906 0.2171 1.0675 0.1510 Uiso calc H(926) 0.3789 0.0795 0.9830 0.1610 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 0.01573(13) 0.01917(14) 0.02322(14) 0.00554(9) 0.00613(10) 0.01106(10) Cl 0.0349(9) 0.0248(8) 0.0338(9) 0.0095(7) 0.0109(8) 0.0071(7) O(1) 0.017(2) 0.018(2) 0.031(2) 0.0045(17) 0.0075(18) 0.0127(19) O(2) 0.020(2) 0.024(2) 0.029(2) 0.0060(18) 0.0089(19) 0.016(2) C(3) 0.024(3) 0.022(3) 0.026(3) 0.001(3) 0.009(3) 0.011(3) C(4) 0.005(3) 0.016(3) 0.026(3) 0.003(2) 0.005(2) 0.019(3) C(11) 0.021(3) 0.011(3) 0.021(3) 0.005(2) 0.012(3) 0.007(3) C(12) 0.019(3) 0.022(3) 0.017(3) 0.005(3) 0.005(3) 0.003(3) C(13) 0.023(3) 0.019(3) 0.026(3) 0.009(3) 0.009(3) 0.008(3) C(14) 0.022(3) 0.028(4) 0.029(4) 0.009(3) 0.011(3) 0.012(3) C(15) 0.025(3) 0.016(3) 0.020(3) 0.008(3) 0.006(3) 0.005(3) C(16) 0.019(3) 0.021(3) 0.026(3) 0.007(3) 0.009(3) 0.011(3) C(21) 0.023(3) 0.019(3) 0.026(3) 0.003(3) 0.009(3) 0.011(3) C(22) 0.027(4) 0.024(3) 0.026(3) 0.009(3) 0.014(3) 0.012(3) C(23) 0.027(4) 0.035(4) 0.042(4) 0.013(3) 0.017(3) 0.025(3) C(24) 0.033(4) 0.033(4) 0.040(4) 0.005(3) 0.022(3) 0.022(3) C(25) 0.030(4) 0.019(3) 0.029(4) 0.006(3) 0.010(3) 0.007(3) C(26) 0.024(3) 0.024(3) 0.025(3) 0.011(3) 0.006(3) 0.011(3) C(31) 0.020(3) 0.034(4) 0.027(4) 0.010(3) 0.004(3) 0.015(3) C(32) 0.048(5) 0.034(4) 0.057(5) 0.009(4) 0.015(4) 0.012(4) C(33) 0.053(6) 0.046(5) 0.076(6) 0.008(4) 0.017(5) 0.012(5) C(34) 0.047(5) 0.050(5) 0.068(6) 0.013(4) 0.003(5) -0.014(5) C(35) 0.029(4) 0.058(5) 0.060(5) 0.007(4) 0.015(4) 0.000(5) C(36) 0.031(4) 0.045(4) 0.038(4) 0.010(3) 0.012(3) 0.011(4) C(41) 0.029(4) 0.043(4) 0.034(4) 0.008(3) 0.006(3) 0.022(4) C(42) 0.045(5) 0.034(4) 0.046(5) 0.011(4) 0.019(4) 0.014(4) C(43) 0.061(5) 0.034(4) 0.052(5) 0.005(4) 0.010(4) 0.018(4) C(44) 0.092(7) 0.035(5) 0.043(5) 0.018(5) 0.027(5) 0.009(4) C(45) 0.067(6) 0.045(5) 0.059(5) 0.016(4) 0.042(5) 0.015(4) C(46) 0.053(5) 0.035(4) 0.036(4) 0.006(4) 0.024(4) 0.017(3) C(121) 0.010(3) 0.025(3) 0.038(4) 0.004(3) 0.007(3) 0.017(3) C(122) 0.021(3) 0.032(4) 0.035(4) 0.004(3) 0.004(3) 0.015(3) C(123) 0.026(4) 0.047(4) 0.032(4) -0.002(3) -0.002(3) 0.023(4) C(124) 0.029(4) 0.069(6) 0.053(5) 0.009(4) -0.002(4) 0.042(5) C(125) 0.027(4) 0.054(5) 0.058(5) 0.019(4) 0.007(4) 0.033(4) C(126) 0.021(3) 0.041(4) 0.036(4) 0.010(3) 0.006(3) 0.018(3) C(131) 0.020(3) 0.023(3) 0.029(4) 0.001(3) 0.005(3) 0.010(3) C(132) 0.027(4) 0.054(5) 0.034(4) 0.009(3) 0.010(3) 0.021(4) C(133) 0.023(4) 0.066(5) 0.059(5) 0.014(4) 0.020(4) 0.041(4) C(134) 0.028(4) 0.071(6) 0.069(6) -0.003(4) 0.003(4) 0.029(5) C(135) 0.035(5) 0.088(7) 0.045(5) -0.015(5) -0.001(4) 0.017(5) C(136) 0.034(4) 0.054(5) 0.034(4) -0.003(4) 0.010(3) 0.006(4) C(151) 0.019(3) 0.021(3) 0.034(4) 0.005(3) 0.007(3) 0.013(3) C(152) 0.026(3) 0.025(3) 0.032(4) 0.014(3) 0.012(3) 0.014(3) C(153) 0.038(4) 0.037(4) 0.030(4) 0.016(3) 0.017(3) 0.021(3) C(154) 0.030(4) 0.042(4) 0.040(4) 0.014(3) 0.011(3) 0.029(4) C(155) 0.036(4) 0.039(4) 0.054(5) 0.023(3) 0.024(4) 0.031(4) C(156) 0.029(4) 0.034(4) 0.042(4) 0.020(3) 0.021(3) 0.020(3) C(161) 0.019(3) 0.021(3) 0.036(4) 0.005(3) 0.008(3) 0.023(3) C(162) 0.031(4) 0.027(3) 0.035(4) 0.009(3) 0.011(3) 0.020(3) C(163) 0.027(4) 0.036(4) 0.067(5) 0.015(3) 0.018(4) 0.032(4) C(164) 0.019(4) 0.050(5) 0.074(6) 0.009(3) 0.000(4) 0.041(4) C(165) 0.032(4) 0.045(4) 0.043(4) 0.005(4) -0.007(4) 0.027(4) C(166) 0.028(4) 0.031(4) 0.034(4) 0.008(3) 0.002(3) 0.021(3) C(221) 0.020(3) 0.031(4) 0.036(4) 0.008(3) 0.015(3) 0.022(3) C(222) 0.020(3) 0.037(4) 0.043(4) 0.009(3) 0.017(3) 0.024(3) C(223) 0.037(4) 0.040(4) 0.050(5) 0.023(3) 0.020(4) 0.029(4) C(224) 0.036(4) 0.060(5) 0.050(5) 0.025(4) 0.016(4) 0.038(4) C(225) 0.025(4) 0.051(5) 0.046(5) 0.005(3) -0.001(3) 0.024(4) C(226) 0.021(4) 0.036(4) 0.044(4) 0.002(3) 0.004(3) 0.019(4) C(231) 0.026(4) 0.059(5) 0.057(5) 0.010(4) 0.014(4) 0.039(4) C(232) 0.027(4) 0.088(7) 0.098(7) 0.026(4) 0.028(4) 0.069(6) C(233) 0.028(5) 0.115(9) 0.118(9) 0.023(5) 0.026(5) 0.076(8) C(234) 0.041(6) 0.152(13) 0.153(12) 0.002(7) 0.017(7) 0.113(11) C(235) 0.059(7) 0.106(9) 0.091(8) -0.018(6) 0.005(6) 0.063(7) C(236) 0.034(5) 0.071(6) 0.066(6) -0.011(4) 0.007(4) 0.037(5) C(251) 0.033(4) 0.036(4) 0.027(4) 0.007(3) 0.013(3) 0.018(3) C(252) 0.046(5) 0.038(4) 0.040(4) 0.016(4) 0.015(4) 0.020(4) C(253) 0.056(5) 0.047(5) 0.060(5) 0.014(4) 0.012(4) 0.040(4) C(254) 0.059(6) 0.078(6) 0.053(5) 0.020(5) 0.015(4) 0.052(5) C(255) 0.075(6) 0.069(6) 0.039(5) -0.006(5) -0.004(4) 0.032(5) C(256) 0.069(6) 0.045(5) 0.039(4) 0.005(4) 0.006(4) 0.031(4) C(261) 0.026(4) 0.038(4) 0.033(4) 0.007(3) 0.009(3) 0.021(3) C(262) 0.046(5) 0.036(4) 0.053(5) 0.022(4) 0.007(4) 0.028(4) C(263) 0.036(5) 0.056(5) 0.085(7) 0.017(4) 0.006(4) 0.037(5) C(264) 0.034(5) 0.081(7) 0.065(6) 0.007(5) -0.004(4) 0.042(5) C(265) 0.037(5) 0.054(5) 0.046(5) -0.003(4) 0.007(4) 0.022(4) C(266) 0.036(4) 0.041(4) 0.021(3) 0.008(3) 0.008(3) 0.018(3) C(901) 0.064(6) 0.048(5) 0.062(6) -0.002(5) 0.020(5) 0.018(5) C(902) 0.069(6) 0.068(6) 0.094(8) 0.034(5) 0.035(6) 0.054(6) C(903) 0.058(6) 0.043(5) 0.064(6) 0.009(4) 0.028(5) 0.008(5) C(904) 0.048(5) 0.062(6) 0.040(5) -0.005(5) 0.024(4) 0.013(4) C(905) 0.034(4) 0.048(5) 0.065(6) 0.005(4) 0.015(4) 0.024(5) C(906) 0.060(6) 0.032(4) 0.087(7) 0.010(4) 0.052(5) 0.020(5) C(911) 0.089(7) 0.044(5) 0.052(6) 0.013(5) 0.005(5) 0.013(5) C(912) 0.078(8) 0.065(7) 0.125(10) 0.023(6) 0.058(7) 0.031(7) C(913) 0.131(10) 0.091(8) 0.125(10) 0.058(8) 0.074(9) 0.078(8) C(914) 0.145(11) 0.086(8) 0.107(9) 0.083(8) 0.086(8) 0.064(7) C(915) 0.211(15) 0.113(10) 0.111(9) 0.086(10) 0.106(10) 0.090(8) C(916) 0.212(15) 0.081(8) 0.067(7) 0.086(9) 0.048(9) 0.042(6) C(921) 0.056(7) 0.107(9) 0.145(12) 0.016(7) 0.028(8) -0.031(9) C(922) 0.052(6) 0.065(7) 0.123(10) 0.018(5) 0.002(7) -0.009(7) C(923) 0.086(8) 0.086(8) 0.099(9) 0.022(7) -0.003(7) 0.045(8) C(924) 0.210(17) 0.048(7) 0.059(8) -0.014(9) -0.038(10) 0.023(6) C(925) 0.201(17) 0.080(10) 0.083(10) 0.059(11) 0.044(11) 0.031(8) C(926) 0.085(9) 0.113(10) 0.105(10) 0.030(8) 0.013(8) -0.045(9) # 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) 1.894(4) ? Ta O(1) 1.894(4) ? Ta C(3) 2.137(6) ? Ta C(4) 2.203(5) ? Ta Cl 2.3542(15) ? O(1) C(11) 1.376(6) ? O(2) C(21) 1.380(7) ? C(3) C(31) 1.494(8) ? C(4) C(41) 1.443(8) ? C(11) C(16) 1.406(8) ? C(11) C(12) 1.414(8) ? C(12) C(13) 1.396(8) ? C(12) C(121) 1.509(8) ? C(13) C(14) 1.394(8) ? C(13) C(131) 1.496(8) ? C(14) C(15) 1.392(8) ? C(15) C(16) 1.404(8) ? C(15) C(151) 1.491(8) ? C(16) C(161) 1.493(8) ? C(21) C(26) 1.408(8) ? C(21) C(22) 1.413(8) ? C(22) C(23) 1.403(8) ? C(22) C(221) 1.477(9) ? C(23) C(24) 1.396(9) ? C(23) C(231) 1.506(9) ? C(24) C(25) 1.395(9) ? C(25) C(26) 1.396(8) ? C(25) C(251) 1.496(9) ? C(26) C(261) 1.516(8) ? C(31) C(36) 1.394(9) ? C(31) C(32) 1.394(9) ? C(32) C(33) 1.379(10) ? C(33) C(34) 1.395(12) ? C(34) C(35) 1.387(11) ? C(35) C(36) 1.368(10) ? C(41) C(42) 1.377(9) ? C(41) C(46) 1.391(9) ? C(42) C(43) 1.379(10) ? C(43) C(44) 1.386(11) ? C(44) C(45) 1.371(11) ? C(45) C(46) 1.370(10) ? C(121) C(126) 1.385(9) ? C(121) C(122) 1.385(9) ? C(122) C(123) 1.386(9) ? C(123) C(124) 1.389(10) ? C(124) C(125) 1.393(10) ? C(125) C(126) 1.397(9) ? C(131) C(132) 1.375(9) ? C(131) C(136) 1.383(9) ? C(132) C(133) 1.376(9) ? C(133) C(134) 1.398(10) ? C(134) C(135) 1.368(11) ? C(135) C(136) 1.412(10) ? C(151) C(156) 1.374(8) ? C(151) C(152) 1.399(8) ? C(152) C(153) 1.389(9) ? C(153) C(154) 1.374(9) ? C(154) C(155) 1.384(9) ? C(155) C(156) 1.388(9) ? C(161) C(162) 1.386(9) ? C(161) C(166) 1.399(8) ? C(162) C(163) 1.390(9) ? C(163) C(164) 1.368(10) ? C(164) C(165) 1.372(10) ? C(165) C(166) 1.376(9) ? C(221) C(222) 1.392(9) ? C(221) C(226) 1.404(9) ? C(222) C(223) 1.368(9) ? C(223) C(224) 1.396(9) ? C(224) C(225) 1.390(10) ? C(225) C(226) 1.362(9) ? C(231) C(236) 1.352(11) ? C(231) C(232) 1.363(10) ? C(232) C(233) 1.390(11) ? C(233) C(234) 1.375(15) ? C(234) C(235) 1.369(15) ? C(235) C(236) 1.422(12) ? C(251) C(252) 1.378(9) ? C(251) C(256) 1.401(9) ? C(252) C(253) 1.374(10) ? C(253) C(254) 1.377(10) ? C(254) C(255) 1.392(11) ? C(255) C(256) 1.378(10) ? C(261) C(266) 1.362(9) ? C(261) C(262) 1.397(9) ? C(262) C(263) 1.372(10) ? C(263) C(264) 1.377(11) ? C(264) C(265) 1.376(11) ? C(265) C(266) 1.379(9) ? C(901) C(906) 1.380(12) ? C(901) C(902) 1.392(12) ? C(902) C(903) 1.364(12) ? C(903) C(904) 1.370(12) ? C(904) C(905) 1.375(11) ? C(905) C(906) 1.372(11) ? C(911) C(916) 1.303(13) ? C(911) C(912) 1.332(13) ? C(912) C(913) 1.378(13) ? C(913) C(914) 1.376(13) ? C(914) C(915) 1.341(13) ? C(915) C(916) 1.400(14) ? C(921) C(922) 1.334(14) ? C(921) C(926) 1.366(14) ? C(922) C(923) 1.349(14) ? C(923) C(924) 1.370(17) ? C(924) C(925) 1.391(19) ? C(925) C(926) 1.318(17) ? 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) 176.32(17) ? O(2) Ta C(3) 90.4(2) ? O(1) Ta C(3) 90.5(2) ? O(2) Ta C(4) 91.45(18) ? O(1) Ta C(4) 91.26(18) ? C(3) Ta C(4) 119.8(2) ? O(2) Ta Cl 88.60(12) ? O(1) Ta Cl 87.91(12) ? C(3) Ta Cl 121.25(17) ? C(4) Ta Cl 118.93(14) ? C(11) O(1) Ta 176.0(4) ? C(21) O(2) Ta 177.0(4) ? C(31) C(3) Ta 106.1(4) ? C(41) C(4) Ta 125.5(4) ? O(1) C(11) C(16) 119.2(5) ? O(1) C(11) C(12) 119.3(5) ? C(16) C(11) C(12) 121.5(5) ? C(13) C(12) C(11) 118.8(5) ? C(13) C(12) C(121) 120.3(5) ? C(11) C(12) C(121) 120.9(5) ? C(14) C(13) C(12) 119.3(6) ? C(14) C(13) C(131) 117.5(6) ? C(12) C(13) C(131) 123.2(6) ? C(15) C(14) C(13) 122.2(6) ? C(14) C(15) C(16) 119.3(6) ? C(14) C(15) C(151) 117.6(5) ? C(16) C(15) C(151) 123.1(5) ? C(15) C(16) C(11) 118.6(5) ? C(15) C(16) C(161) 120.8(5) ? C(11) C(16) C(161) 120.6(5) ? O(2) C(21) C(26) 118.9(5) ? O(2) C(21) C(22) 118.5(5) ? C(26) C(21) C(22) 122.4(6) ? C(23) C(22) C(21) 117.1(6) ? C(23) C(22) C(221) 121.3(6) ? C(21) C(22) C(221) 121.4(5) ? C(24) C(23) C(22) 120.5(6) ? C(24) C(23) C(231) 116.6(6) ? C(22) C(23) C(231) 122.9(6) ? C(25) C(24) C(23) 121.8(6) ? C(24) C(25) C(26) 119.0(6) ? C(24) C(25) C(251) 116.7(6) ? C(26) C(25) C(251) 124.4(6) ? C(25) C(26) C(21) 119.0(6) ? C(25) C(26) C(261) 121.3(5) ? C(21) C(26) C(261) 119.6(5) ? C(36) C(31) C(32) 118.4(6) ? C(36) C(31) C(3) 121.1(6) ? C(32) C(31) C(3) 120.5(6) ? C(33) C(32) C(31) 121.5(8) ? C(32) C(33) C(34) 119.5(8) ? C(35) C(34) C(33) 118.9(8) ? C(36) C(35) C(34) 121.6(8) ? C(35) C(36) C(31) 120.1(7) ? C(42) C(41) C(46) 117.6(7) ? C(42) C(41) C(4) 122.9(6) ? C(46) C(41) C(4) 119.4(6) ? C(41) C(42) C(43) 120.7(7) ? C(42) C(43) C(44) 120.0(7) ? C(45) C(44) C(43) 120.4(7) ? C(46) C(45) C(44) 118.5(7) ? C(45) C(46) C(41) 122.7(7) ? C(126) C(121) C(122) 120.0(6) ? C(126) C(121) C(12) 119.1(6) ? C(122) C(121) C(12) 120.8(6) ? C(121) C(122) C(123) 120.8(6) ? C(122) C(123) C(124) 119.2(7) ? C(123) C(124) C(125) 120.5(7) ? C(124) C(125) C(126) 119.7(7) ? C(121) C(126) C(125) 119.7(7) ? C(132) C(131) C(136) 118.6(6) ? C(132) C(131) C(13) 120.5(6) ? C(136) C(131) C(13) 120.7(6) ? C(131) C(132) C(133) 122.0(7) ? C(132) C(133) C(134) 118.7(7) ? C(135) C(134) C(133) 121.0(7) ? C(134) C(135) C(136) 118.8(7) ? C(131) C(136) C(135) 120.8(7) ? C(156) C(151) C(152) 118.2(6) ? C(156) C(151) C(15) 123.2(6) ? C(152) C(151) C(15) 118.6(5) ? C(153) C(152) C(151) 121.1(6) ? C(154) C(153) C(152) 120.0(6) ? C(153) C(154) C(155) 119.1(6) ? C(154) C(155) C(156) 121.0(6) ? C(151) C(156) C(155) 120.6(6) ? C(162) C(161) C(166) 119.9(6) ? C(162) C(161) C(16) 118.7(6) ? C(166) C(161) C(16) 121.3(6) ? C(161) C(162) C(163) 119.6(6) ? C(164) C(163) C(162) 120.0(7) ? C(163) C(164) C(165) 120.7(7) ? C(164) C(165) C(166) 120.6(7) ? C(165) C(166) C(161) 119.3(7) ? C(222) C(221) C(226) 117.7(6) ? C(222) C(221) C(22) 120.7(6) ? C(226) C(221) C(22) 121.6(6) ? C(223) C(222) C(221) 121.7(6) ? C(222) C(223) C(224) 119.7(7) ? C(225) C(224) C(223) 119.5(7) ? C(226) C(225) C(224) 120.3(7) ? C(225) C(226) C(221) 121.2(7) ? C(236) C(231) C(232) 118.6(7) ? C(236) C(231) C(23) 119.1(7) ? C(232) C(231) C(23) 122.3(7) ? C(231) C(232) C(233) 121.7(9) ? C(234) C(233) C(232) 119.0(10) ? C(235) C(234) C(233) 121.0(10) ? C(234) C(235) C(236) 117.8(10) ? C(231) C(236) C(235) 121.8(10) ? C(252) C(251) C(256) 118.7(6) ? C(252) C(251) C(25) 119.8(6) ? C(256) C(251) C(25) 121.4(6) ? C(253) C(252) C(251) 121.1(7) ? C(252) C(253) C(254) 120.9(7) ? C(253) C(254) C(255) 118.4(7) ? C(256) C(255) C(254) 121.1(8) ? C(255) C(256) C(251) 119.8(7) ? C(266) C(261) C(262) 119.2(6) ? C(266) C(261) C(26) 120.5(6) ? C(262) C(261) C(26) 120.3(6) ? C(263) C(262) C(261) 120.5(7) ? C(262) C(263) C(264) 119.1(8) ? C(265) C(264) C(263) 121.1(8) ? C(264) C(265) C(266) 119.0(7) ? C(261) C(266) C(265) 121.1(7) ? C(906) C(901) C(902) 118.9(9) ? C(903) C(902) C(901) 119.1(9) ? C(902) C(903) C(904) 121.5(8) ? C(903) C(904) C(905) 120.1(8) ? C(906) C(905) C(904) 118.7(8) ? C(905) C(906) C(901) 121.6(8) ? C(916) C(911) C(912) 121.0(10) ? C(911) C(912) C(913) 120.4(11) ? C(914) C(913) C(912) 118.9(10) ? C(915) C(914) C(913) 118.6(10) ? C(914) C(915) C(916) 119.7(10) ? C(911) C(916) C(915) 120.3(10) ? C(922) C(921) C(926) 123.1(12) ? C(921) C(922) C(923) 118.8(12) ? C(922) C(923) C(924) 120.6(13) ? C(923) C(924) C(925) 117.9(12) ? C(926) C(925) C(924) 121.9(14) ? C(925) C(926) C(921) 117.7(13) ? #===END #============================================================================== data_SS_1_4 _database_code_CSD 164017 _audit_creation_date 20-01-99 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C75 H78 Nb O2 Si3' _chemical_formula_structural ? _chemical_formula_weight 1188.62 _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 12.7620(3) _cell_length_b 18.0027(4) _cell_length_c 28.8284(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.5229(14) _cell_angle_gamma 90.00 _cell_volume 6592.6(5) _cell_measurement_reflns_used 40016 _cell_measurement_theta_min 4 _cell_measurement_theta_max 26 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.269 _cell_measurement_temperature 203 _exptl_crystal_F_000 2508 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.6519 _exptl_absorpt_correction_T_max 0.9604 _diffrn_reflns_number 40016 _reflns_number_total 13250 _reflns_number_gt 9196 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 26.38 _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 22 _diffrn_reflns_limit_l_max 35 # 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 0.049 _refine_ls_wR_factor_ref 0.110 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 13250 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details ' ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.43 _refine_diff_density_min -0.98 _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 Nb 0.207824(19) 0.130077(13) 0.306552(8) 0.02464(7) Uani ? Si(1) 0.48025(7) 0.16260(5) 0.27957(3) 0.0383(3) Uani ? Si(2) 0.01520(7) 0.03462(5) 0.37334(3) 0.0413(3) Uani ? Si(3) 0.17067(7) 0.32202(4) 0.27174(3) 0.0351(2) Uani ? O(4) 0.27384(15) 0.13197(9) 0.36950(6) 0.0275(5) Uani ? O(5) 0.13630(14) 0.11459(9) 0.24516(6) 0.0278(5) Uani ? C(11) 0.3580(2) 0.10634(16) 0.28286(10) 0.0328(8) Uani ? C(12) 0.4646(3) 0.2267(2) 0.22861(13) 0.0610(12) Uani ? C(13) 0.5895(3) 0.0965(2) 0.26940(14) 0.0559(12) Uani ? C(14) 0.5191(3) 0.2164(2) 0.33369(13) 0.0597(10) Uani ? C(21) 0.1155(2) 0.03571(15) 0.32893(9) 0.0295(7) Uani ? C(22) 0.0554(3) -0.0312(3) 0.42197(14) 0.0787(17) Uani ? C(23) -0.0031(3) 0.1272(2) 0.40035(13) 0.0601(12) Uani ? C(24) -0.1158(3) -0.0010(2) 0.34766(13) 0.0574(10) Uani ? C(31) 0.1486(2) 0.24096(14) 0.31003(10) 0.0323(8) Uani ? C(32) 0.2983(3) 0.36965(19) 0.28904(14) 0.0584(12) Uani ? C(33) 0.0665(3) 0.39300(18) 0.27818(13) 0.0535(10) Uani ? C(34) 0.1702(3) 0.29238(19) 0.20982(11) 0.0510(10) Uani ? C(41) 0.2860(2) 0.11532(14) 0.41572(9) 0.0258(7) Uani ? C(42) 0.3209(2) 0.04404(14) 0.43028(9) 0.0262(7) Uani ? C(43) 0.3120(2) 0.02320(15) 0.47705(9) 0.0297(8) Uani ? C(44) 0.2760(2) 0.07534(15) 0.50744(10) 0.0331(8) Uani ? C(45) 0.2538(2) 0.14815(15) 0.49420(10) 0.0313(8) Uani ? C(46) 0.2597(2) 0.16960(15) 0.44784(9) 0.0288(7) Uani ? C(51) 0.0817(2) 0.09159(15) 0.20514(9) 0.0265(7) Uani ? C(52) -0.0192(2) 0.12215(14) 0.19178(9) 0.0283(7) Uani ? C(53) -0.0711(2) 0.10283(16) 0.14827(9) 0.0304(7) Uani ? C(54) -0.0247(2) 0.05368(16) 0.11969(9) 0.0330(8) Uani ? C(55) 0.0723(2) 0.02056(15) 0.13322(9) 0.0293(8) Uani ? C(56) 0.1267(2) 0.03988(14) 0.17605(9) 0.0259(7) Uani ? C(421) 0.3758(2) -0.00616(15) 0.39922(9) 0.0307(8) Uani ? C(422) 0.3364(3) -0.07551(16) 0.38475(10) 0.0420(9) Uani ? C(423) 0.3985(4) -0.12413(18) 0.36159(12) 0.0570(12) Uani ? C(424) 0.4985(4) -0.1048(2) 0.35321(13) 0.0626(14) Uani ? C(425) 0.5386(3) -0.0362(2) 0.36689(12) 0.0536(10) Uani ? C(426) 0.4772(2) 0.01304(17) 0.38918(10) 0.0383(9) Uani ? C(431) 0.3381(2) -0.05285(15) 0.49611(9) 0.0311(8) Uani ? C(432) 0.4324(2) -0.08879(15) 0.49076(9) 0.0326(8) Uani ? C(433) 0.4538(3) -0.15831(17) 0.51105(10) 0.0399(9) Uani ? C(434) 0.3810(3) -0.19200(17) 0.53670(11) 0.0454(9) Uani ? C(435) 0.2884(3) -0.15669(18) 0.54240(12) 0.0513(10) Uani ? C(436) 0.2664(3) -0.08738(17) 0.52241(11) 0.0429(9) Uani ? C(451) 0.2264(3) 0.20155(16) 0.53099(10) 0.0388(9) Uani ? C(452) 0.2907(4) 0.2601(2) 0.54477(15) 0.0805(15) Uani ? C(453) 0.2658(5) 0.3079(3) 0.57944(18) 0.106(2) Uani ? C(454) 0.1761(5) 0.2984(2) 0.60017(15) 0.0852(19) Uani ? C(455) 0.1114(4) 0.2424(3) 0.58683(16) 0.0885(19) Uani ? C(456) 0.1360(4) 0.1927(2) 0.55203(14) 0.0710(15) Uani ? C(461) 0.2466(2) 0.24958(15) 0.43419(10) 0.0325(8) Uani ? C(462) 0.1546(3) 0.28861(17) 0.43917(11) 0.0430(9) Uani ? C(463) 0.1499(3) 0.36489(18) 0.43064(13) 0.0553(10) Uani ? C(464) 0.2373(4) 0.4018(2) 0.41795(15) 0.0661(13) Uani ? C(465) 0.3281(3) 0.36311(19) 0.41253(14) 0.0614(14) Uani ? C(466) 0.3325(3) 0.28732(17) 0.42045(11) 0.0420(9) Uani ? C(521) -0.0727(2) 0.17363(15) 0.22244(10) 0.0306(8) Uani ? C(522) -0.0973(2) 0.15059(18) 0.26595(10) 0.0385(9) Uani ? C(523) -0.1587(2) 0.19523(19) 0.29204(12) 0.0459(10) Uani ? C(524) -0.1945(3) 0.26290(19) 0.27489(12) 0.0485(10) Uani ? C(525) -0.1688(3) 0.28641(18) 0.23239(12) 0.0475(10) Uani ? C(526) -0.1078(2) 0.24277(16) 0.20605(11) 0.0383(9) Uani ? C(531) -0.1788(3) 0.13143(17) 0.13176(10) 0.0401(9) Uani ? C(532) -0.2660(3) 0.1126(2) 0.15448(13) 0.0524(10) Uani ? C(533) -0.3648(3) 0.1399(3) 0.13834(16) 0.0698(14) Uani ? C(534) -0.3765(4) 0.1864(3) 0.10103(17) 0.0868(17) Uani ? C(535) -0.2909(4) 0.2051(3) 0.07772(14) 0.0821(16) Uani ? C(536) -0.1914(3) 0.1773(2) 0.09297(12) 0.0591(12) Uani ? C(551) 0.1102(2) -0.03671(16) 0.10131(10) 0.0329(8) Uani ? C(552) 0.1166(3) -0.02112(18) 0.05450(10) 0.0443(9) Uani ? C(553) 0.1440(3) -0.0760(2) 0.02426(12) 0.0648(13) Uani ? C(554) 0.1640(4) -0.1469(2) 0.04035(14) 0.0730(16) Uani ? C(555) 0.1578(3) -0.1636(2) 0.08631(13) 0.0642(12) Uani ? C(556) 0.1313(3) -0.10865(17) 0.11667(11) 0.0447(9) Uani ? C(561) 0.2322(2) 0.00683(15) 0.18901(9) 0.0289(8) Uani ? C(562) 0.3141(2) 0.01845(17) 0.16095(11) 0.0413(9) Uani ? C(563) 0.4109(3) -0.0161(2) 0.17124(14) 0.0580(12) Uani ? C(564) 0.4267(3) -0.0627(2) 0.20883(15) 0.0582(12) Uani ? C(565) 0.3474(3) -0.07424(17) 0.23679(13) 0.0475(10) Uani ? C(566) 0.2499(2) -0.04000(15) 0.22698(10) 0.0345(8) Uani ? C(901) 0.4326(7) -0.0564(5) -0.0041(4) 0.186(5) Uani ? C(902) 0.4177(6) -0.0083(7) 0.0266(3) 0.179(4) Uani ? C(903) 0.4835(8) 0.0473(6) 0.0317(4) 0.208(5) Uani ? H(44) 0.2665 0.0608 0.5377 0.0430 Uiso calc H(54) -0.0590 0.0423 0.0906 0.0430 Uiso calc H(11A) 0.3821 0.0629 0.3007 0.0430 Uiso calc H(11B) 0.3411 0.0888 0.2512 0.0430 Uiso calc H(12A) 0.4150 0.2650 0.2342 0.0920 Uiso calc H(12B) 0.4396 0.1994 0.2012 0.0920 Uiso calc H(12C) 0.5314 0.2489 0.2242 0.0920 Uiso calc H(13A) 0.6504 0.1241 0.2623 0.0830 Uiso calc H(13B) 0.5674 0.0644 0.2437 0.0830 Uiso calc H(13C) 0.6068 0.0672 0.2969 0.0830 Uiso calc H(14A) 0.5819 0.2442 0.3299 0.0900 Uiso calc H(14B) 0.5320 0.1828 0.3595 0.0900 Uiso calc H(14C) 0.4634 0.2499 0.3396 0.0900 Uiso calc H(21A) 0.0785 0.0162 0.3005 0.0380 Uiso calc H(21B) 0.1670 -0.0017 0.3395 0.0380 Uiso calc H(22A) 0.1171 -0.0125 0.4399 0.1180 Uiso calc H(22B) 0.0706 -0.0789 0.4093 0.1180 Uiso calc H(22C) -0.0008 -0.0360 0.4417 0.1180 Uiso calc H(23A) -0.0611 0.1249 0.4192 0.0900 Uiso calc H(23B) -0.0176 0.1637 0.3763 0.0900 Uiso calc H(23C) 0.0598 0.1407 0.4194 0.0900 Uiso calc H(24A) -0.1062 -0.0472 0.3320 0.0860 Uiso calc H(24B) -0.1473 0.0347 0.3258 0.0860 Uiso calc H(24C) -0.1608 -0.0086 0.3721 0.0860 Uiso calc H(31A) 0.0728 0.2356 0.3086 0.0420 Uiso calc H(31B) 0.1710 0.2577 0.3414 0.0420 Uiso calc H(32A) 0.2947 0.3942 0.3184 0.0880 Uiso calc H(32B) 0.3117 0.4056 0.2658 0.0880 Uiso calc H(32C) 0.3540 0.3336 0.2919 0.0880 Uiso calc H(33A) 0.0681 0.4075 0.3103 0.0800 Uiso calc H(33B) -0.0012 0.3723 0.2680 0.0800 Uiso calc H(33C) 0.0791 0.4357 0.2595 0.0800 Uiso calc H(34A) 0.1826 0.3347 0.1908 0.0770 Uiso calc H(34B) 0.1031 0.2709 0.1995 0.0770 Uiso calc H(34C) 0.2246 0.2562 0.2072 0.0770 Uiso calc H(422) 0.2686 -0.0893 0.3906 0.0550 Uiso calc H(423) 0.3717 -0.1701 0.3518 0.0740 Uiso calc H(424) 0.5398 -0.1380 0.3382 0.0810 Uiso calc H(425) 0.6067 -0.0232 0.3611 0.0700 Uiso calc H(426) 0.5038 0.0597 0.3976 0.0500 Uiso calc H(432) 0.4817 -0.0664 0.4735 0.0420 Uiso calc H(433) 0.5172 -0.1820 0.5073 0.0520 Uiso calc H(434) 0.3950 -0.2384 0.5500 0.0590 Uiso calc H(435) 0.2395 -0.1792 0.5598 0.0670 Uiso calc H(436) 0.2031 -0.0639 0.5267 0.0560 Uiso calc H(452) 0.3521 0.2676 0.5305 0.1050 Uiso calc H(453) 0.3110 0.3468 0.5886 0.1380 Uiso calc H(454) 0.1595 0.3307 0.6236 0.1110 Uiso calc H(455) 0.0493 0.2363 0.6008 0.1150 Uiso calc H(456) 0.0906 0.1536 0.5433 0.0930 Uiso calc H(462) 0.0959 0.2639 0.4482 0.0560 Uiso calc H(463) 0.0878 0.3908 0.4335 0.0720 Uiso calc H(464) 0.2348 0.4529 0.4131 0.0860 Uiso calc H(465) 0.3867 0.3879 0.4035 0.0790 Uiso calc H(466) 0.3941 0.2615 0.4164 0.0550 Uiso calc H(522) -0.0727 0.1051 0.2778 0.0500 Uiso calc H(523) -0.1756 0.1793 0.3211 0.0600 Uiso calc H(524) -0.2360 0.2925 0.2922 0.0630 Uiso calc H(525) -0.1927 0.3324 0.2210 0.0620 Uiso calc H(526) -0.0903 0.2597 0.1773 0.0500 Uiso calc H(532) -0.2585 0.0817 0.1805 0.0680 Uiso calc H(533) -0.4234 0.1263 0.1532 0.0910 Uiso calc H(534) -0.4426 0.2056 0.0912 0.1130 Uiso calc H(535) -0.2994 0.2363 0.0519 0.1070 Uiso calc H(536) -0.1337 0.1896 0.0771 0.0770 Uiso calc H(552) 0.1023 0.0267 0.0434 0.0580 Uiso calc H(553) 0.1488 -0.0648 -0.0070 0.0840 Uiso calc H(554) 0.1819 -0.1838 0.0199 0.0950 Uiso calc H(555) 0.1712 -0.2117 0.0971 0.0830 Uiso calc H(556) 0.1277 -0.1202 0.1479 0.0580 Uiso calc H(562) 0.3037 0.0496 0.1352 0.0540 Uiso calc H(563) 0.4652 -0.0076 0.1526 0.0750 Uiso calc H(564) 0.4912 -0.0864 0.2153 0.0760 Uiso calc H(565) 0.3587 -0.1053 0.2626 0.0610 Uiso calc H(566) 0.1964 -0.0487 0.2461 0.0450 Uiso calc H(901) 0.3883 -0.0974 -0.0083 0.2420 Uiso calc H(902) 0.3619 -0.0124 0.0449 0.2330 Uiso calc H(903) 0.4743 0.0824 0.0546 0.2710 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 Nb 0.02824(14) 0.02455(13) 0.02115(13) -0.00075(11) 0.00254(9) 0.00025(10) Si(1) 0.0326(5) 0.0445(5) 0.0387(5) -0.0046(4) 0.0073(4) 0.0037(4) Si(2) 0.0377(5) 0.0492(5) 0.0380(5) -0.0118(4) 0.0095(4) 0.0034(4) Si(3) 0.0371(5) 0.0296(4) 0.0390(5) 0.0004(4) 0.0055(4) 0.0047(4) O(4) 0.0328(10) 0.0278(10) 0.0222(9) 0.0011(8) 0.0038(8) -0.0003(8) O(5) 0.0302(10) 0.0284(10) 0.0245(10) 0.0021(8) 0.0012(8) -0.0019(8) C(11) 0.0318(16) 0.0391(16) 0.0276(15) 0.0005(13) 0.0035(12) -0.0029(12) C(12) 0.067(3) 0.064(2) 0.056(2) 0.008(2) 0.027(2) 0.0164(19) C(13) 0.0352(19) 0.061(2) 0.073(3) -0.0020(17) 0.0134(18) 0.0052(19) C(14) 0.055(2) 0.067(2) 0.057(2) -0.0161(19) 0.0046(19) -0.0064(19) C(21) 0.0337(16) 0.0285(14) 0.0264(14) -0.0043(12) 0.0037(12) 0.0012(12) C(22) 0.055(3) 0.112(4) 0.070(3) -0.018(2) 0.010(2) 0.045(3) C(23) 0.047(2) 0.080(3) 0.056(2) -0.016(2) 0.0195(18) -0.024(2) C(24) 0.049(2) 0.060(2) 0.064(2) -0.0148(18) 0.0095(18) -0.0003(19) C(31) 0.0361(17) 0.0294(15) 0.0312(15) 0.0015(13) 0.0029(13) -0.0018(12) C(32) 0.055(2) 0.050(2) 0.071(3) -0.0117(18) 0.0104(19) -0.0009(19) C(33) 0.055(2) 0.0396(18) 0.066(2) 0.0094(16) 0.0070(19) 0.0098(17) C(34) 0.060(2) 0.050(2) 0.044(2) -0.0019(18) 0.0103(17) 0.0058(16) C(41) 0.0284(15) 0.0276(14) 0.0213(13) -0.0002(12) 0.0013(11) 0.0000(11) C(42) 0.0282(15) 0.0275(14) 0.0228(14) -0.0001(12) 0.0018(11) -0.0010(11) C(43) 0.0348(16) 0.0274(14) 0.0271(15) 0.0011(13) 0.0036(12) -0.0004(12) C(44) 0.0407(17) 0.0346(15) 0.0251(14) -0.0003(14) 0.0088(13) 0.0029(12) C(45) 0.0374(16) 0.0300(15) 0.0274(15) 0.0047(13) 0.0079(13) -0.0035(12) C(46) 0.0317(15) 0.0269(14) 0.0277(15) 0.0028(12) 0.0031(12) -0.0021(12) C(51) 0.0310(15) 0.0294(14) 0.0189(13) -0.0021(12) 0.0017(11) 0.0039(11) C(52) 0.0320(15) 0.0275(14) 0.0257(14) 0.0032(12) 0.0042(12) -0.0008(12) C(53) 0.0310(15) 0.0336(15) 0.0262(14) 0.0041(13) 0.0003(12) -0.0012(12) C(54) 0.0390(17) 0.0370(16) 0.0222(14) 0.0039(14) -0.0019(12) -0.0026(12) C(55) 0.0360(16) 0.0306(15) 0.0214(14) 0.0015(13) 0.0038(12) 0.0002(11) C(56) 0.0289(15) 0.0248(13) 0.0243(14) 0.0020(12) 0.0038(12) 0.0034(11) C(421) 0.0440(18) 0.0272(14) 0.0206(14) 0.0079(13) 0.0018(13) 0.0021(11) C(422) 0.059(2) 0.0307(16) 0.0343(17) 0.0048(15) -0.0054(15) -0.0028(13) C(423) 0.089(3) 0.0325(18) 0.046(2) 0.0127(19) -0.012(2) -0.0096(16) C(424) 0.079(3) 0.066(3) 0.043(2) 0.034(2) 0.007(2) -0.0132(18) C(425) 0.053(2) 0.068(2) 0.042(2) 0.0243(19) 0.0159(17) 0.0047(18) C(426) 0.0465(19) 0.0388(17) 0.0306(16) 0.0089(15) 0.0083(14) 0.0048(13) C(431) 0.0428(17) 0.0285(14) 0.0218(14) -0.0001(13) 0.0016(13) 0.0015(12) C(432) 0.0379(17) 0.0321(15) 0.0268(15) -0.0010(13) -0.0015(13) 0.0007(12) C(433) 0.0467(19) 0.0349(16) 0.0365(17) 0.0062(15) -0.0045(15) 0.0002(14) C(434) 0.063(2) 0.0285(16) 0.0430(19) -0.0010(16) -0.0032(17) 0.0088(14) C(435) 0.064(2) 0.0400(18) 0.052(2) -0.0033(18) 0.0168(18) 0.0136(16) C(436) 0.048(2) 0.0370(17) 0.0453(19) 0.0045(15) 0.0126(16) 0.0058(15) C(451) 0.058(2) 0.0336(16) 0.0264(15) 0.0110(15) 0.0116(15) 0.0002(13) C(452) 0.095(3) 0.079(3) 0.072(3) -0.016(3) 0.031(3) -0.044(2) C(453) 0.153(5) 0.081(3) 0.091(4) -0.019(3) 0.045(4) -0.053(3) C(454) 0.153(5) 0.052(3) 0.058(3) 0.021(3) 0.049(3) -0.010(2) C(455) 0.108(4) 0.092(4) 0.075(3) 0.015(3) 0.057(3) -0.010(3) C(456) 0.090(3) 0.065(3) 0.065(3) -0.004(2) 0.043(2) -0.015(2) C(461) 0.0416(17) 0.0288(15) 0.0264(15) 0.0053(13) 0.0002(13) -0.0011(12) C(462) 0.0460(19) 0.0348(16) 0.0476(19) 0.0062(15) 0.0009(16) -0.0028(15) C(463) 0.059(2) 0.0385(19) 0.067(2) 0.0200(18) -0.001(2) -0.0036(18) C(464) 0.087(3) 0.0314(18) 0.079(3) 0.010(2) 0.003(2) 0.0115(19) C(465) 0.071(3) 0.041(2) 0.073(3) -0.0086(19) 0.011(2) 0.0130(19) C(466) 0.048(2) 0.0353(17) 0.0432(18) 0.0033(15) 0.0069(15) 0.0024(14) C(521) 0.0254(15) 0.0347(16) 0.0313(15) 0.0007(12) 0.0007(12) -0.0066(12) C(522) 0.0346(17) 0.0459(18) 0.0352(17) 0.0054(14) 0.0049(14) -0.0048(14) C(523) 0.0380(18) 0.060(2) 0.0411(19) -0.0009(17) 0.0103(15) -0.0090(16) C(524) 0.0408(19) 0.050(2) 0.056(2) 0.0023(16) 0.0108(17) -0.0233(18) C(525) 0.046(2) 0.0360(17) 0.060(2) 0.0064(15) 0.0024(17) -0.0139(16) C(526) 0.0410(18) 0.0356(16) 0.0379(17) 0.0037(14) 0.0018(14) -0.0049(14) C(531) 0.0421(18) 0.0464(18) 0.0301(16) 0.0117(15) -0.0059(14) -0.0145(14) C(532) 0.040(2) 0.065(2) 0.051(2) 0.0040(17) -0.0024(17) -0.0134(18) C(533) 0.035(2) 0.099(3) 0.074(3) 0.011(2) -0.002(2) -0.027(3) C(534) 0.060(3) 0.125(4) 0.070(3) 0.048(3) -0.022(2) -0.031(3) C(535) 0.089(3) 0.106(4) 0.047(2) 0.050(3) -0.015(2) 0.002(2) C(536) 0.060(2) 0.080(3) 0.0356(19) 0.029(2) -0.0046(17) 0.0003(18) C(551) 0.0350(16) 0.0360(16) 0.0273(15) 0.0055(13) 0.0011(13) -0.0065(12) C(552) 0.055(2) 0.0485(19) 0.0295(17) 0.0114(17) 0.0041(15) -0.0006(14) C(553) 0.081(3) 0.084(3) 0.0296(18) 0.024(2) 0.0062(18) -0.0149(19) C(554) 0.104(4) 0.067(3) 0.047(2) 0.036(3) 0.002(2) -0.022(2) C(555) 0.095(3) 0.047(2) 0.049(2) 0.026(2) -0.001(2) -0.0129(17) C(556) 0.060(2) 0.0406(17) 0.0337(17) 0.0110(16) 0.0051(16) -0.0054(14) C(561) 0.0313(16) 0.0253(14) 0.0297(15) 0.0013(12) 0.0007(12) -0.0033(12) C(562) 0.0383(18) 0.0429(18) 0.0446(18) 0.0013(15) 0.0132(15) 0.0006(15) C(563) 0.036(2) 0.065(2) 0.076(3) 0.0026(18) 0.0207(19) -0.008(2) C(564) 0.036(2) 0.049(2) 0.088(3) 0.0109(16) -0.003(2) -0.003(2) C(565) 0.044(2) 0.0334(17) 0.062(2) 0.0039(15) -0.0103(17) 0.0061(16) C(566) 0.0357(17) 0.0294(15) 0.0373(17) 0.0021(13) -0.0020(13) 0.0007(13) C(901) 0.135(8) 0.204(9) 0.225(11) -0.050(7) 0.045(7) -0.093(8) C(902) 0.114(6) 0.252(10) 0.170(8) -0.048(7) 0.009(5) -0.119(8) C(903) 0.127(7) 0.239(11) 0.264(12) -0.037(7) 0.047(8) -0.147(9) # 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 Nb O(4) 1.9264(17) ? Nb O(5) 1.9321(17) ? Nb C(11) 2.139(3) ? Nb C(31) 2.140(3) ? Nb C(21) 2.199(3) ? Si(1) C(14) 1.863(4) ? Si(1) C(12) 1.864(3) ? Si(1) C(11) 1.870(3) ? Si(1) C(13) 1.878(4) ? Si(2) C(23) 1.863(4) ? Si(2) C(22) 1.869(4) ? Si(2) C(24) 1.875(4) ? Si(2) C(21) 1.895(3) ? Si(3) C(34) 1.863(3) ? Si(3) C(32) 1.865(4) ? Si(3) C(33) 1.866(3) ? Si(3) C(31) 1.867(3) ? O(4) C(41) 1.360(3) ? O(5) C(51) 1.354(3) ? C(41) C(46) 1.409(4) ? C(41) C(42) 1.409(4) ? C(42) C(43) 1.415(4) ? C(42) C(421) 1.493(4) ? C(43) C(44) 1.392(4) ? C(43) C(431) 1.501(4) ? C(44) C(45) 1.386(4) ? C(45) C(46) 1.400(4) ? C(45) C(451) 1.498(4) ? C(46) C(461) 1.497(4) ? C(51) C(56) 1.412(4) ? C(51) C(52) 1.419(4) ? C(52) C(53) 1.405(4) ? C(52) C(521) 1.491(4) ? C(53) C(54) 1.380(4) ? C(53) C(531) 1.502(4) ? C(54) C(55) 1.395(4) ? C(55) C(56) 1.402(4) ? C(55) C(551) 1.493(4) ? C(56) C(561) 1.486(4) ? C(421) C(422) 1.395(4) ? C(421) C(426) 1.396(4) ? C(422) C(423) 1.394(5) ? C(423) C(424) 1.367(6) ? C(424) C(425) 1.379(5) ? C(425) C(426) 1.382(4) ? C(431) C(432) 1.388(4) ? C(431) C(436) 1.390(4) ? C(432) C(433) 1.397(4) ? C(433) C(434) 1.381(5) ? C(434) C(435) 1.366(5) ? C(435) C(436) 1.391(4) ? C(451) C(456) 1.363(5) ? C(451) C(452) 1.370(5) ? C(452) C(453) 1.379(5) ? C(453) C(454) 1.353(7) ? C(454) C(455) 1.336(7) ? C(455) C(456) 1.402(5) ? C(461) C(466) 1.379(4) ? C(461) C(462) 1.388(4) ? C(462) C(463) 1.395(4) ? C(463) C(464) 1.378(5) ? C(464) C(465) 1.374(5) ? C(465) C(466) 1.383(4) ? C(521) C(522) 1.385(4) ? C(521) C(526) 1.390(4) ? C(522) C(523) 1.392(4) ? C(523) C(524) 1.376(5) ? C(524) C(525) 1.365(5) ? C(525) C(526) 1.383(4) ? C(531) C(536) 1.388(5) ? C(531) C(532) 1.387(5) ? C(532) C(533) 1.392(5) ? C(533) C(534) 1.359(6) ? C(534) C(535) 1.379(6) ? C(535) C(536) 1.396(5) ? C(551) C(556) 1.386(4) ? C(551) C(552) 1.388(4) ? C(552) C(553) 1.384(4) ? C(553) C(554) 1.375(5) ? C(554) C(555) 1.369(5) ? C(555) C(556) 1.384(4) ? C(561) C(566) 1.383(4) ? C(561) C(562) 1.397(4) ? C(562) C(563) 1.390(5) ? C(563) C(564) 1.369(5) ? C(564) C(565) 1.369(5) ? C(565) C(566) 1.393(4) ? C(902) C(901) 1.264(10) ? C(902) C(903) 1.305(11) ? C(901) C(903) 1.404(11) ? C(903) C(901) 1.404(11) ? 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(4) Nb O(5) 172.28(7) ? O(4) Nb C(11) 88.86(9) ? O(5) Nb C(11) 92.16(9) ? O(4) Nb C(31) 93.66(9) ? O(5) Nb C(31) 92.27(9) ? C(11) Nb C(31) 122.18(11) ? O(4) Nb C(21) 86.31(9) ? O(5) Nb C(21) 86.44(9) ? C(11) Nb C(21) 117.48(11) ? C(31) Nb C(21) 120.33(11) ? C(14) Si(1) C(12) 109.77(18) ? C(14) Si(1) C(11) 113.27(15) ? C(12) Si(1) C(11) 110.41(16) ? C(14) Si(1) C(13) 108.56(17) ? C(12) Si(1) C(13) 107.10(17) ? C(11) Si(1) C(13) 107.51(15) ? C(23) Si(2) C(22) 106.9(2) ? C(23) Si(2) C(24) 109.11(17) ? C(22) Si(2) C(24) 104.48(18) ? C(23) Si(2) C(21) 113.15(14) ? C(22) Si(2) C(21) 111.01(17) ? C(24) Si(2) C(21) 111.77(15) ? C(34) Si(3) C(32) 108.10(17) ? C(34) Si(3) C(33) 110.75(17) ? C(32) Si(3) C(33) 105.70(17) ? C(34) Si(3) C(31) 110.85(14) ? C(32) Si(3) C(31) 112.23(15) ? C(33) Si(3) C(31) 109.09(15) ? C(41) O(4) Nb 156.55(17) ? C(51) O(5) Nb 169.66(17) ? Si(1) C(11) Nb 133.29(15) ? Si(2) C(21) Nb 128.45(14) ? Si(3) C(31) Nb 128.85(15) ? O(4) C(41) C(46) 118.7(2) ? O(4) C(41) C(42) 119.7(2) ? C(46) C(41) C(42) 121.6(2) ? C(41) C(42) C(43) 118.2(2) ? C(41) C(42) C(421) 121.7(2) ? C(43) C(42) C(421) 119.8(2) ? C(44) C(43) C(42) 118.9(2) ? C(44) C(43) C(431) 117.4(2) ? C(42) C(43) C(431) 123.7(2) ? C(45) C(44) C(43) 122.3(3) ? C(44) C(45) C(46) 119.7(2) ? C(44) C(45) C(451) 117.8(3) ? C(46) C(45) C(451) 122.4(2) ? C(45) C(46) C(41) 118.3(2) ? C(45) C(46) C(461) 120.1(2) ? C(41) C(46) C(461) 121.4(2) ? O(5) C(51) C(56) 120.1(2) ? O(5) C(51) C(52) 119.5(2) ? C(56) C(51) C(52) 120.3(2) ? C(53) C(52) C(51) 119.0(2) ? C(53) C(52) C(521) 118.7(2) ? C(51) C(52) C(521) 122.4(2) ? C(54) C(53) C(52) 120.0(3) ? C(54) C(53) C(531) 117.5(2) ? C(52) C(53) C(531) 122.5(2) ? C(53) C(54) C(55) 121.8(3) ? C(54) C(55) C(56) 119.5(2) ? C(54) C(55) C(551) 117.0(2) ? C(56) C(55) C(551) 123.4(3) ? C(55) C(56) C(51) 119.4(2) ? C(55) C(56) C(561) 118.9(2) ? C(51) C(56) C(561) 121.7(2) ? C(422) C(421) C(426) 118.3(3) ? C(422) C(421) C(42) 123.0(3) ? C(426) C(421) C(42) 118.1(3) ? C(423) C(422) C(421) 120.0(3) ? C(424) C(423) C(422) 120.6(3) ? C(423) C(424) C(425) 120.3(3) ? C(424) C(425) C(426) 119.7(4) ? C(425) C(426) C(421) 121.0(3) ? C(432) C(431) C(436) 118.4(3) ? C(432) C(431) C(43) 123.3(3) ? C(436) C(431) C(43) 118.2(3) ? C(431) C(432) C(433) 120.5(3) ? C(434) C(433) C(432) 120.2(3) ? C(435) C(434) C(433) 119.6(3) ? C(434) C(435) C(436) 120.6(3) ? C(431) C(436) C(435) 120.6(3) ? C(456) C(451) C(452) 118.1(3) ? C(456) C(451) C(45) 120.3(3) ? C(452) C(451) C(45) 121.6(3) ? C(451) C(452) C(453) 121.1(4) ? C(454) C(453) C(452) 120.4(5) ? C(455) C(454) C(453) 119.6(4) ? C(454) C(455) C(456) 120.9(4) ? C(451) C(456) C(455) 120.0(4) ? C(466) C(461) C(462) 118.9(3) ? C(466) C(461) C(46) 118.5(3) ? C(462) C(461) C(46) 122.2(3) ? C(461) C(462) C(463) 120.2(3) ? C(464) C(463) C(462) 120.0(3) ? C(465) C(464) C(463) 119.9(3) ? C(464) C(465) C(466) 120.2(4) ? C(461) C(466) C(465) 120.8(3) ? C(522) C(521) C(526) 118.8(3) ? C(522) C(521) C(52) 120.5(3) ? C(526) C(521) C(52) 120.4(3) ? C(521) C(522) C(523) 120.3(3) ? C(524) C(523) C(522) 120.1(3) ? C(525) C(524) C(523) 119.8(3) ? C(524) C(525) C(526) 120.8(3) ? C(525) C(526) C(521) 120.1(3) ? C(536) C(531) C(532) 119.3(3) ? C(536) C(531) C(53) 119.5(3) ? C(532) C(531) C(53) 121.2(3) ? C(531) C(532) C(533) 119.9(4) ? C(534) C(533) C(532) 120.6(4) ? C(533) C(534) C(535) 120.3(4) ? C(534) C(535) C(536) 119.9(4) ? C(531) C(536) C(535) 120.0(4) ? C(556) C(551) C(552) 118.1(3) ? C(556) C(551) C(55) 120.8(3) ? C(552) C(551) C(55) 120.8(3) ? C(553) C(552) C(551) 120.7(3) ? C(554) C(553) C(552) 120.0(3) ? C(555) C(554) C(553) 120.3(3) ? C(554) C(555) C(556) 119.7(4) ? C(555) C(556) C(551) 121.1(3) ? C(566) C(561) C(562) 118.4(3) ? C(566) C(561) C(56) 121.2(3) ? C(562) C(561) C(56) 120.3(2) ? C(563) C(562) C(561) 120.6(3) ? C(564) C(563) C(562) 120.2(3) ? C(563) C(564) C(565) 119.8(3) ? C(564) C(565) C(566) 120.7(3) ? C(561) C(566) C(565) 120.3(3) ? C(901) C(902) C(903) 117.7(9) ? C(902) C(901) C(903) 119.3(9) ? C(902) C(903) C(901) 122.9(8) ? #===END #============================================================================== data_SS294 _database_code_CSD 164018 _audit_creation_date 12-11-99 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description cube _exptl_crystal_colour 'red-orange' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C77 H77 Nb O2 Si2' _chemical_formula_structural ? _chemical_formula_weight 1183.55 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 23.6191(5) _cell_length_b 10.9492(2) _cell_length_c 27.7450(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.9677(8) _cell_angle_gamma 90.00 _cell_volume 6504.6(4) _cell_measurement_reflns_used 42658 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.256 _cell_measurement_temperature 163 _exptl_crystal_F_000 2496 # 6. DATA COLLECTION _diffrn_ambient_temperature 163 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996) _exptl_absorpt_correction_T_min 0.7359 _exptl_absorpt_correction_T_max 0.9144 _diffrn_reflns_number 42658 _reflns_number_total 15330 _reflns_number_gt 12114 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 32 # 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 0.121 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding, U=1.3*Ueq of bonding atom ; _refine_ls_number_reflns 14574 _refine_ls_number_parameters 762 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+2.7014P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 0.79 _refine_diff_density_min -0.89 _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 Nb 0.207638(10) 0.258235(19) 0.424782(9) 0.02379(8) Uani ? Si(30) 0.36457(4) 0.33671(8) 0.49737(3) 0.0392(3) Uani ? Si(40) 0.23858(4) 0.13108(7) 0.32049(3) 0.0359(3) Uani ? O(1) 0.22687(8) 0.18319(15) 0.49234(7) 0.0273(6) Uani ? O(2) 0.14836(8) 0.34592(15) 0.36597(7) 0.0262(5) Uani ? C(11) 0.21742(11) 0.1610(2) 0.53665(9) 0.0241(8) Uani ? C(12) 0.24572(11) 0.0580(2) 0.56735(9) 0.0243(8) Uani ? C(13) 0.23410(11) 0.0325(2) 0.61226(10) 0.0257(8) Uani ? C(14) 0.19743(12) 0.1122(2) 0.62588(10) 0.0279(8) Uani ? C(15) 0.17109(11) 0.2172(2) 0.59661(10) 0.0261(8) Uani ? C(16) 0.18092(11) 0.2430(2) 0.55081(9) 0.0246(8) Uani ? C(21) 0.09221(11) 0.3800(2) 0.32773(9) 0.0237(8) Uani ? C(22) 0.08743(11) 0.4945(2) 0.30373(9) 0.0234(8) Uani ? C(23) 0.02965(11) 0.5299(2) 0.26317(9) 0.0233(8) Uani ? C(24) -0.02043(11) 0.4490(2) 0.24823(10) 0.0260(8) Uani ? C(25) -0.01600(11) 0.3349(2) 0.27213(9) 0.0244(8) Uani ? C(26) 0.04140(11) 0.2986(2) 0.31282(9) 0.0238(8) Uani ? C(30) 0.28613(13) 0.3737(3) 0.44426(12) 0.0348(10) Uani ? C(31) 0.38735(16) 0.1769(3) 0.49157(15) 0.0572(12) Uani ? C(32) 0.36563(17) 0.3547(4) 0.56480(14) 0.0647(14) Uani ? C(33) 0.42289(17) 0.4438(4) 0.4916(2) 0.0850(19) Uani ? C(40) 0.22758(15) 0.1120(3) 0.38286(11) 0.0316(9) Uani ? C(41) 0.30098(16) 0.2438(3) 0.32741(14) 0.0496(12) Uani ? C(42) 0.16433(15) 0.1795(3) 0.26425(12) 0.0480(11) Uani ? C(43) 0.2632(2) -0.0158(3) 0.30101(15) 0.0643(15) Uani ? C(121) 0.28975(12) -0.0201(2) 0.55496(10) 0.0272(8) Uani ? C(122) 0.27078(14) -0.0872(3) 0.50828(11) 0.0377(9) Uani ? C(123) 0.31228(16) -0.1677(3) 0.50111(13) 0.0515(12) Uani ? C(124) 0.37223(15) -0.1799(3) 0.53969(13) 0.0500(12) Uani ? C(125) 0.39214(14) -0.1120(3) 0.58530(12) 0.0420(10) Uani ? C(126) 0.35110(12) -0.0321(2) 0.59302(11) 0.0328(9) Uani ? C(131) 0.25876(11) -0.0792(2) 0.64549(10) 0.0282(8) Uani ? C(132) 0.28866(12) -0.0701(3) 0.70062(11) 0.0332(9) Uani ? C(133) 0.30841(13) -0.1741(3) 0.73176(12) 0.0391(10) Uani ? C(134) 0.29925(14) -0.2873(3) 0.70851(13) 0.0446(11) Uani ? C(135) 0.26981(15) -0.2977(3) 0.65388(13) 0.0440(11) Uani ? C(136) 0.24965(13) -0.1951(3) 0.62247(12) 0.0351(9) Uani ? C(151) 0.13442(12) 0.2989(2) 0.61553(10) 0.0279(8) Uani ? C(152) 0.14767(13) 0.4224(2) 0.62400(11) 0.0350(9) Uani ? C(153) 0.11380(16) 0.4962(3) 0.64253(12) 0.0459(11) Uani ? C(154) 0.06537(16) 0.4486(3) 0.65225(12) 0.0497(12) Uani ? C(155) 0.05208(14) 0.3255(3) 0.64465(12) 0.0435(10) Uani ? C(156) 0.08613(13) 0.2508(3) 0.62646(11) 0.0339(9) Uani ? C(161) 0.15290(12) 0.3525(2) 0.51716(10) 0.0283(8) Uani ? C(162) 0.08860(13) 0.3753(3) 0.49751(10) 0.0329(9) Uani ? C(163) 0.06267(15) 0.4780(3) 0.46653(12) 0.0428(11) Uani ? C(164) 0.09974(17) 0.5566(3) 0.45411(14) 0.0546(13) Uani ? C(165) 0.16347(16) 0.5370(3) 0.47389(14) 0.0506(12) Uani ? C(166) 0.18984(14) 0.4354(2) 0.50554(12) 0.0358(10) Uani ? C(221) 0.14416(11) 0.5742(2) 0.32370(10) 0.0257(8) Uani ? C(222) 0.14495(13) 0.6839(2) 0.34883(11) 0.0334(9) Uani ? C(223) 0.19768(15) 0.7566(3) 0.36774(13) 0.0439(11) Uani ? C(224) 0.25067(14) 0.7192(3) 0.36249(12) 0.0431(10) Uani ? C(225) 0.25062(13) 0.6101(3) 0.33774(12) 0.0399(10) Uani ? C(226) 0.19755(12) 0.5378(2) 0.31846(11) 0.0326(9) Uani ? C(231) 0.01917(11) 0.6508(2) 0.23532(10) 0.0261(8) Uani ? C(232) -0.03460(12) 0.7177(2) 0.22586(10) 0.0304(8) Uani ? C(233) -0.04661(13) 0.8279(3) 0.19909(12) 0.0376(10) Uani ? C(234) -0.00514(14) 0.8730(3) 0.18016(12) 0.0436(11) Uani ? C(235) 0.04844(14) 0.8073(3) 0.18852(13) 0.0435(11) Uani ? C(236) 0.06057(12) 0.6974(3) 0.21591(11) 0.0335(9) Uani ? C(251) -0.07366(11) 0.2596(2) 0.25569(10) 0.0253(8) Uani ? C(252) -0.11199(12) 0.2395(2) 0.20204(11) 0.0331(9) Uani ? C(253) -0.16777(13) 0.1776(3) 0.18702(12) 0.0418(10) Uani ? C(254) -0.18718(14) 0.1360(3) 0.22471(13) 0.0427(10) Uani ? C(255) -0.14934(13) 0.1550(3) 0.27802(12) 0.0396(10) Uani ? C(256) -0.09273(12) 0.2150(2) 0.29370(11) 0.0317(8) Uani ? C(261) 0.05176(11) 0.1773(2) 0.33883(10) 0.0244(8) Uani ? C(262) 0.04118(12) 0.0702(2) 0.30881(11) 0.0305(8) Uani ? C(263) 0.05305(14) -0.0428(2) 0.33358(12) 0.0384(10) Uani ? C(264) 0.07566(14) -0.0518(3) 0.38800(12) 0.0385(10) Uani ? C(265) 0.08617(12) 0.0527(2) 0.41844(11) 0.0323(9) Uani ? C(266) 0.07392(11) 0.1665(2) 0.39380(10) 0.0274(8) Uani ? C(901) 0.56851(17) 0.1103(4) 0.56776(16) 0.0659(16) Uani ? C(902) 0.54829(19) 0.0407(4) 0.59832(18) 0.0727(18) Uani ? C(903) 0.53486(19) 0.0936(5) 0.63705(17) 0.0740(18) Uani ? C(904) 0.54104(18) 0.2166(5) 0.64536(16) 0.0719(16) Uani ? C(905) 0.06207(19) 0.2126(4) 0.11472(17) 0.0712(16) Uani ? C(906) 0.57530(18) 0.2333(4) 0.57650(17) 0.0654(16) Uani ? C(911) 0.9199(2) 0.2291(4) 0.4400(2) 0.098(3) Uani ? C(912) 0.93713(19) 0.1009(4) 0.44592(17) 0.0724(16) Uani ? C(913) 0.9923(2) 0.0642(4) 0.4964(2) 0.0757(19) Uani ? H(14) 0.1902 0.0949 0.6556 0.0360 Uiso calc H(24) -0.0585 0.4720 0.2212 0.0340 Uiso calc H(122) 0.2304 -0.0784 0.4818 0.0490 Uiso calc H(123) 0.2993 -0.2135 0.4700 0.0670 Uiso calc H(124) 0.3994 -0.2346 0.5348 0.0650 Uiso calc H(125) 0.4330 -0.1194 0.6110 0.0550 Uiso calc H(126) 0.3647 0.0141 0.6240 0.0430 Uiso calc H(132) 0.2954 0.0064 0.7167 0.0430 Uiso calc H(133) 0.3280 -0.1671 0.7686 0.0510 Uiso calc H(134) 0.3129 -0.3568 0.7295 0.0580 Uiso calc H(135) 0.2635 -0.3746 0.6382 0.0570 Uiso calc H(136) 0.2298 -0.2031 0.5857 0.0460 Uiso calc H(152) 0.1797 0.4559 0.6171 0.0450 Uiso calc H(153) 0.1236 0.5787 0.6485 0.0590 Uiso calc H(154) 0.0420 0.4992 0.6638 0.0650 Uiso calc H(155) 0.0201 0.2926 0.6518 0.0570 Uiso calc H(156) 0.0769 0.1679 0.6214 0.0440 Uiso calc H(162) 0.0631 0.3213 0.5052 0.0430 Uiso calc H(163) 0.0201 0.4934 0.4542 0.0560 Uiso calc H(164) 0.0820 0.6235 0.4323 0.0710 Uiso calc H(165) 0.1886 0.5916 0.4661 0.0650 Uiso calc H(166) 0.2327 0.4228 0.5191 0.0470 Uiso calc H(222) 0.1097 0.7088 0.3530 0.0430 Uiso calc H(223) 0.1975 0.8308 0.3840 0.0570 Uiso calc H(224) 0.2863 0.7677 0.3757 0.0560 Uiso calc H(225) 0.2862 0.5850 0.3340 0.0520 Uiso calc H(226) 0.1977 0.4641 0.3018 0.0420 Uiso calc H(232) -0.0632 0.6875 0.2378 0.0400 Uiso calc H(233) -0.0825 0.8717 0.1938 0.0490 Uiso calc H(234) -0.0131 0.9469 0.1619 0.0570 Uiso calc H(235) 0.0763 0.8371 0.1757 0.0570 Uiso calc H(236) 0.0967 0.6542 0.2214 0.0440 Uiso calc H(252) -0.0999 0.2679 0.1762 0.0430 Uiso calc H(253) -0.1926 0.1637 0.1511 0.0540 Uiso calc H(254) -0.2252 0.0958 0.2143 0.0560 Uiso calc H(255) -0.1620 0.1271 0.3036 0.0510 Uiso calc H(256) -0.0673 0.2257 0.3297 0.0410 Uiso calc H(262) 0.0261 0.0749 0.2720 0.0400 Uiso calc H(263) 0.0457 -0.1134 0.3132 0.0500 Uiso calc H(264) 0.0838 -0.1281 0.4042 0.0500 Uiso calc H(265) 0.1014 0.0471 0.4552 0.0420 Uiso calc H(266) 0.0806 0.2366 0.4144 0.0360 Uiso calc H(30A) 0.2742(17) 0.459(4) 0.4496(15) 0.067(11) Uiso ? H(30B) 0.2882(16) 0.385(3) 0.4127(15) 0.055(10) Uiso ? H(31A) 0.3609 0.1216 0.4995 0.0740 Uiso calc H(31B) 0.4300 0.1639 0.5162 0.0740 Uiso calc H(31C) 0.3829 0.1625 0.4560 0.0740 Uiso calc H(32A) 0.3355 0.3005 0.5681 0.0840 Uiso calc H(32B) 0.3554 0.4375 0.5694 0.0840 Uiso calc H(32C) 0.4065 0.3354 0.5915 0.0840 Uiso calc H(33A) 0.4634 0.4270 0.5193 0.1100 Uiso calc H(33B) 0.4113 0.5264 0.4947 0.1100 Uiso calc H(33C) 0.4240 0.4329 0.4576 0.1100 Uiso calc H(40A) 0.2666(17) 0.079(3) 0.4092(14) 0.059(10) Uiso ? H(40B) 0.1966(15) 0.066(3) 0.3741(12) 0.037(9) Uiso ? H(41A) 0.3075 0.2439 0.2955 0.0650 Uiso calc H(41B) 0.3391 0.2215 0.3571 0.0650 Uiso calc H(41C) 0.2884 0.3238 0.3332 0.0650 Uiso calc H(42A) 0.1719 0.1956 0.2335 0.0620 Uiso calc H(42B) 0.1490 0.2522 0.2740 0.0620 Uiso calc H(42C) 0.1339 0.1155 0.2563 0.0620 Uiso calc H(43A) 0.3004 -0.0451 0.3299 0.0840 Uiso calc H(43B) 0.2714 -0.0029 0.2703 0.0840 Uiso calc H(43C) 0.2305 -0.0752 0.2928 0.0840 Uiso calc H(901) 0.5775 0.0744 0.5414 0.0860 Uiso calc H(902) 0.5436 -0.0431 0.5928 0.0940 Uiso calc H(903) 0.5215 0.0453 0.6578 0.0960 Uiso calc H(904) 0.5313 0.2527 0.6713 0.0940 Uiso calc H(905) 0.0671 0.1288 0.1203 0.0920 Uiso calc H(906) 0.5892 0.2810 0.5559 0.0850 Uiso calc H(91A) 0.9119 0.2549 0.4696 0.1280 Uiso calc H(91B) 0.8830 0.2407 0.4076 0.1280 Uiso calc H(91C) 0.9535 0.2767 0.4388 0.1280 Uiso calc H(91D) 0.9459 0.0773 0.4160 0.0930 Uiso calc H(91E) 0.9012 0.0539 0.4436 0.0930 Uiso calc H(91F) 1.0287 0.1080 0.4978 0.0980 Uiso calc H(91G) 0.9846 0.0916 0.5263 0.0980 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 Nb 0.02236(12) 0.02907(13) 0.01991(12) 0.00254(9) 0.00889(9) 0.00452(9) Si(30) 0.0236(4) 0.0495(5) 0.0380(5) -0.0031(3) 0.0066(3) 0.0105(4) Si(40) 0.0429(5) 0.0421(4) 0.0304(4) 0.0089(4) 0.0229(4) 0.0056(3) O(1) 0.0282(9) 0.0331(9) 0.0221(9) 0.0041(7) 0.0121(7) 0.0035(7) O(2) 0.0220(8) 0.0293(9) 0.0244(9) 0.0008(7) 0.0070(7) 0.0030(7) C(11) 0.0242(12) 0.0305(13) 0.0174(12) -0.0019(10) 0.0087(10) -0.0002(9) C(12) 0.0252(12) 0.0289(12) 0.0189(12) 0.0005(10) 0.0093(10) -0.0004(9) C(13) 0.0241(12) 0.0298(13) 0.0213(12) -0.0011(10) 0.0077(10) 0.0018(10) C(14) 0.0274(13) 0.0355(14) 0.0220(13) -0.0008(11) 0.0116(11) 0.0017(10) C(15) 0.0238(12) 0.0319(13) 0.0221(13) -0.0020(10) 0.0093(10) -0.0030(10) C(16) 0.0232(12) 0.0301(13) 0.0193(12) -0.0024(10) 0.0077(10) -0.0024(9) C(21) 0.0209(12) 0.0281(12) 0.0199(12) 0.0028(10) 0.0065(10) 0.0007(9) C(22) 0.0234(12) 0.0266(12) 0.0222(12) -0.0002(10) 0.0115(10) -0.0014(9) C(23) 0.0235(12) 0.0276(12) 0.0199(12) 0.0020(10) 0.0102(10) 0.0007(9) C(24) 0.0225(12) 0.0317(13) 0.0214(12) 0.0032(10) 0.0069(10) 0.0008(10) C(25) 0.0236(12) 0.0300(13) 0.0199(12) 0.0009(10) 0.0094(10) -0.0015(9) C(26) 0.0246(12) 0.0259(12) 0.0214(12) 0.0009(10) 0.0103(10) 0.0004(9) C(30) 0.0276(14) 0.0475(18) 0.0284(15) 0.0021(12) 0.0109(12) 0.0091(12) C(31) 0.0396(18) 0.067(2) 0.056(2) 0.0134(16) 0.0115(16) 0.0142(17) C(32) 0.044(2) 0.094(3) 0.040(2) -0.0016(19) 0.0020(16) 0.0029(19) C(33) 0.038(2) 0.090(3) 0.111(4) -0.012(2) 0.016(2) 0.042(3) C(40) 0.0348(15) 0.0354(15) 0.0288(15) 0.0032(13) 0.0174(13) 0.0010(11) C(41) 0.0470(18) 0.066(2) 0.048(2) 0.0065(16) 0.0318(16) 0.0135(15) C(42) 0.0490(19) 0.066(2) 0.0309(16) 0.0045(16) 0.0188(14) 0.0021(14) C(43) 0.108(3) 0.055(2) 0.056(2) 0.023(2) 0.060(2) 0.0113(17) C(121) 0.0281(13) 0.0324(13) 0.0234(13) 0.0034(11) 0.0132(11) 0.0046(10) C(122) 0.0350(15) 0.0475(17) 0.0267(14) 0.0070(13) 0.0091(12) -0.0018(12) C(123) 0.055(2) 0.062(2) 0.0353(17) 0.0164(16) 0.0170(16) -0.0100(15) C(124) 0.0510(19) 0.061(2) 0.0434(19) 0.0268(16) 0.0253(16) 0.0042(15) C(125) 0.0317(15) 0.0574(19) 0.0361(17) 0.0120(14) 0.0135(13) 0.0096(14) C(126) 0.0300(14) 0.0389(15) 0.0289(14) 0.0020(11) 0.0118(12) 0.0001(11) C(131) 0.0243(13) 0.0347(14) 0.0273(14) 0.0007(10) 0.0126(11) 0.0061(10) C(132) 0.0292(14) 0.0446(16) 0.0273(14) -0.0004(12) 0.0134(11) 0.0053(11) C(133) 0.0309(15) 0.0555(19) 0.0314(15) 0.0043(13) 0.0135(12) 0.0144(13) C(134) 0.0386(17) 0.0451(17) 0.052(2) 0.0070(14) 0.0211(15) 0.0243(15) C(135) 0.0452(18) 0.0329(15) 0.057(2) -0.0006(13) 0.0246(16) 0.0073(14) C(136) 0.0349(15) 0.0368(15) 0.0329(15) -0.0032(12) 0.0137(12) 0.0031(12) C(151) 0.0274(13) 0.0350(14) 0.0197(13) 0.0047(11) 0.0084(11) -0.0002(10) C(152) 0.0394(16) 0.0377(15) 0.0283(14) 0.0027(12) 0.0147(12) -0.0012(11) C(153) 0.062(2) 0.0419(17) 0.0346(17) 0.0139(15) 0.0211(15) -0.0017(13) C(154) 0.056(2) 0.064(2) 0.0320(17) 0.0270(17) 0.0214(15) 0.0003(14) C(155) 0.0333(15) 0.069(2) 0.0316(16) 0.0100(14) 0.0169(13) 0.0020(14) C(156) 0.0301(14) 0.0454(16) 0.0255(14) 0.0012(12) 0.0111(11) -0.0021(11) C(161) 0.0324(14) 0.0309(13) 0.0213(13) 0.0020(11) 0.0111(11) -0.0005(10) C(162) 0.0317(14) 0.0388(15) 0.0269(14) 0.0047(12) 0.0112(12) -0.0012(11) C(163) 0.0410(17) 0.0475(17) 0.0383(17) 0.0168(14) 0.0151(14) 0.0074(13) C(164) 0.062(2) 0.0472(19) 0.059(2) 0.0235(17) 0.0298(18) 0.0241(16) C(165) 0.058(2) 0.0387(17) 0.065(2) 0.0084(15) 0.0355(18) 0.0174(15) C(166) 0.0390(16) 0.0327(14) 0.0395(16) 0.0037(12) 0.0202(13) 0.0040(12) C(221) 0.0252(12) 0.0274(13) 0.0228(13) -0.0012(10) 0.0086(10) 0.0036(10) C(222) 0.0341(15) 0.0293(14) 0.0361(15) -0.0020(11) 0.0140(12) -0.0017(11) C(223) 0.0472(18) 0.0352(16) 0.0398(17) -0.0078(13) 0.0092(14) -0.0043(12) C(224) 0.0345(16) 0.0474(17) 0.0383(17) -0.0139(13) 0.0064(13) 0.0051(13) C(225) 0.0279(14) 0.0522(18) 0.0402(17) -0.0046(13) 0.0150(13) 0.0099(14) C(226) 0.0321(14) 0.0366(15) 0.0309(15) -0.0023(11) 0.0151(12) 0.0011(11) C(231) 0.0254(12) 0.0290(13) 0.0215(13) -0.0007(10) 0.0075(10) -0.0004(10) C(232) 0.0286(13) 0.0312(13) 0.0301(14) 0.0013(11) 0.0110(11) 0.0016(10) C(233) 0.0310(15) 0.0361(15) 0.0393(17) 0.0084(12) 0.0087(13) 0.0039(12) C(234) 0.0430(17) 0.0313(15) 0.0472(19) 0.0036(13) 0.0100(14) 0.0146(13) C(235) 0.0398(17) 0.0441(17) 0.0498(19) 0.0007(14) 0.0219(15) 0.0163(14) C(236) 0.0286(14) 0.0356(14) 0.0366(16) 0.0045(11) 0.0141(12) 0.0100(12) C(251) 0.0197(11) 0.0260(12) 0.0273(13) -0.0002(10) 0.0072(10) -0.0014(10) C(252) 0.0270(13) 0.0400(15) 0.0283(14) -0.0029(11) 0.0077(11) -0.0003(11) C(253) 0.0306(15) 0.0484(18) 0.0365(17) -0.0046(13) 0.0046(13) -0.0057(13) C(254) 0.0283(14) 0.0444(17) 0.0528(19) -0.0123(13) 0.0146(14) -0.0048(14) C(255) 0.0319(15) 0.0445(17) 0.0467(18) -0.0067(12) 0.0207(14) 0.0033(13) C(256) 0.0277(13) 0.0368(14) 0.0297(14) -0.0012(11) 0.0113(11) 0.0004(11) C(261) 0.0200(12) 0.0242(12) 0.0289(13) -0.0020(9) 0.0102(10) -0.0009(10) C(262) 0.0324(14) 0.0292(13) 0.0254(13) -0.0005(11) 0.0077(11) -0.0033(10) C(263) 0.0453(17) 0.0255(14) 0.0388(17) 0.0002(12) 0.0124(14) -0.0044(11) C(264) 0.0410(16) 0.0299(14) 0.0419(17) 0.0016(12) 0.0148(14) 0.0088(12) C(265) 0.0336(14) 0.0361(14) 0.0279(14) 0.0000(11) 0.0138(12) 0.0064(11) C(266) 0.0251(12) 0.0291(13) 0.0272(13) -0.0021(10) 0.0103(11) -0.0022(10) C(901) 0.054(2) 0.083(3) 0.068(3) 0.018(2) 0.033(2) 0.019(2) C(902) 0.064(3) 0.072(3) 0.089(3) 0.015(2) 0.039(2) 0.029(2) C(903) 0.056(2) 0.103(4) 0.062(3) -0.003(2) 0.024(2) 0.028(2) C(904) 0.050(2) 0.118(4) 0.041(2) -0.011(2) 0.0128(18) -0.005(2) C(905) 0.053(2) 0.080(3) 0.067(3) 0.009(2) 0.012(2) -0.002(2) C(906) 0.048(2) 0.083(3) 0.067(3) 0.0045(19) 0.026(2) 0.026(2) C(911) 0.067(3) 0.087(4) 0.121(5) -0.005(3) 0.020(3) 0.001(3) C(912) 0.059(2) 0.078(3) 0.068(3) -0.011(2) 0.015(2) 0.002(2) C(913) 0.068(3) 0.076(3) 0.095(3) -0.017(2) 0.046(3) -0.003(2) # 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 Nb O(2) 1.9016(16) ? Nb O(1) 1.9174(17) ? Nb C(30) 2.117(3) ? Nb C(40) 2.145(3) ? Si(30) C(31) 1.858(4) ? Si(30) C(30) 1.861(3) ? Si(30) C(33) 1.867(4) ? Si(30) C(32) 1.871(4) ? Si(40) C(42) 1.866(3) ? Si(40) C(43) 1.867(3) ? Si(40) C(40) 1.867(3) ? Si(40) C(41) 1.869(3) ? O(1) C(11) 1.361(3) ? O(2) C(21) 1.355(3) ? C(11) C(12) 1.401(3) ? C(11) C(16) 1.411(3) ? C(12) C(13) 1.412(3) ? C(12) C(121) 1.494(3) ? C(13) C(14) 1.390(3) ? C(13) C(131) 1.494(3) ? C(14) C(15) 1.393(4) ? C(15) C(16) 1.413(3) ? C(15) C(151) 1.487(3) ? C(16) C(161) 1.491(3) ? C(21) C(22) 1.402(3) ? C(21) C(26) 1.409(3) ? C(22) C(23) 1.408(3) ? C(22) C(221) 1.496(3) ? C(23) C(24) 1.393(3) ? C(23) C(231) 1.500(3) ? C(24) C(25) 1.398(3) ? C(25) C(26) 1.407(3) ? C(25) C(251) 1.489(3) ? C(26) C(261) 1.482(3) ? C(30) H(30B) 0.91(4) ? C(30) H(30A) 1.01(4) ? C(40) H(40B) 0.83(3) ? C(40) H(40A) 0.97(4) ? C(121) C(122) 1.388(4) ? C(121) C(126) 1.393(4) ? C(122) C(123) 1.394(4) ? C(123) C(124) 1.374(4) ? C(124) C(125) 1.369(4) ? C(125) C(126) 1.388(4) ? C(131) C(132) 1.391(4) ? C(131) C(136) 1.396(4) ? C(132) C(133) 1.386(4) ? C(133) C(134) 1.371(5) ? C(134) C(135) 1.380(5) ? C(135) C(136) 1.378(4) ? C(151) C(152) 1.386(4) ? C(151) C(156) 1.401(4) ? C(152) C(153) 1.380(4) ? C(153) C(154) 1.383(5) ? C(154) C(155) 1.380(5) ? C(155) C(156) 1.383(4) ? C(161) C(166) 1.388(4) ? C(161) C(162) 1.402(4) ? C(162) C(163) 1.391(4) ? C(163) C(164) 1.372(5) ? C(164) C(165) 1.384(5) ? C(165) C(166) 1.391(4) ? C(221) C(222) 1.384(4) ? C(221) C(226) 1.387(4) ? C(222) C(223) 1.382(4) ? C(223) C(224) 1.382(5) ? C(224) C(225) 1.378(4) ? C(225) C(226) 1.385(4) ? C(231) C(232) 1.392(4) ? C(231) C(236) 1.397(4) ? C(232) C(233) 1.382(4) ? C(233) C(234) 1.383(4) ? C(234) C(235) 1.388(4) ? C(235) C(236) 1.387(4) ? C(251) C(252) 1.395(4) ? C(251) C(256) 1.398(4) ? C(252) C(253) 1.380(4) ? C(253) C(254) 1.384(4) ? C(254) C(255) 1.383(4) ? C(255) C(256) 1.385(4) ? C(261) C(266) 1.393(4) ? C(261) C(262) 1.398(3) ? C(262) C(263) 1.385(4) ? C(263) C(264) 1.376(4) ? C(264) C(265) 1.381(4) ? C(265) C(266) 1.391(4) ? C(901) C(906) 1.366(6) ? C(901) C(902) 1.367(5) ? C(902) C(903) 1.370(6) ? C(903) C(904) 1.364(6) ? C(904) C(905) 1.388(6) ? C(905) C(906) 1.361(6) ? C(905) C(904) 1.388(6) ? C(906) C(905) 1.361(6) ? C(912) C(911) 1.452(6) ? C(912) C(913) 1.510(6) ? C(913) C(913) 1.445(8) ? 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) Nb O(1) 147.15(7) ? O(2) Nb C(30) 99.54(9) ? O(1) Nb C(30) 100.71(9) ? O(2) Nb C(40) 99.34(9) ? O(1) Nb C(40) 101.21(9) ? C(30) Nb C(40) 102.42(12) ? C(31) Si(30) C(30) 111.37(15) ? C(31) Si(30) C(33) 109.4(2) ? C(30) Si(30) C(33) 108.61(16) ? C(31) Si(30) C(32) 107.68(18) ? C(30) Si(30) C(32) 110.95(15) ? C(33) Si(30) C(32) 108.8(2) ? C(42) Si(40) C(43) 107.49(18) ? C(42) Si(40) C(40) 110.96(14) ? C(43) Si(40) C(40) 110.75(14) ? C(42) Si(40) C(41) 108.69(16) ? C(43) Si(40) C(41) 105.65(17) ? C(40) Si(40) C(41) 113.02(15) ? C(11) O(1) Nb 153.93(15) ? C(21) O(2) Nb 159.02(16) ? O(1) C(11) C(12) 118.3(2) ? O(1) C(11) C(16) 119.4(2) ? C(12) C(11) C(16) 122.3(2) ? C(11) C(12) C(13) 118.3(2) ? C(11) C(12) C(121) 121.4(2) ? C(13) C(12) C(121) 120.2(2) ? C(14) C(13) C(12) 119.4(2) ? C(14) C(13) C(131) 118.2(2) ? C(12) C(13) C(131) 122.4(2) ? C(13) C(14) C(15) 122.4(2) ? C(14) C(15) C(16) 119.1(2) ? C(14) C(15) C(151) 118.3(2) ? C(16) C(15) C(151) 122.6(2) ? C(11) C(16) C(15) 118.3(2) ? C(11) C(16) C(161) 119.9(2) ? C(15) C(16) C(161) 121.7(2) ? O(2) C(21) C(22) 118.3(2) ? O(2) C(21) C(26) 119.1(2) ? C(22) C(21) C(26) 122.6(2) ? C(21) C(22) C(23) 118.8(2) ? C(21) C(22) C(221) 117.8(2) ? C(23) C(22) C(221) 123.4(2) ? C(24) C(23) C(22) 118.6(2) ? C(24) C(23) C(231) 118.2(2) ? C(22) C(23) C(231) 123.2(2) ? C(23) C(24) C(25) 122.9(2) ? C(24) C(25) C(26) 119.2(2) ? C(24) C(25) C(251) 118.3(2) ? C(26) C(25) C(251) 122.4(2) ? C(25) C(26) C(21) 118.0(2) ? C(25) C(26) C(261) 123.3(2) ? C(21) C(26) C(261) 118.6(2) ? H(30B) C(30) H(30A) 98(3) ? H(30B) C(30) Si(30) 111(2) ? H(30A) C(30) Si(30) 109(2) ? H(30B) C(30) Nb 104(2) ? H(30A) C(30) Nb 109(2) ? Si(30) C(30) Nb 122.96(15) ? H(40B) C(40) H(40A) 116(3) ? H(40B) C(40) Si(40) 104(2) ? H(40A) C(40) Si(40) 106(2) ? H(40B) C(40) Nb 104(2) ? H(40A) C(40) Nb 103(2) ? Si(40) C(40) Nb 124.56(15) ? C(122) C(121) C(126) 118.7(2) ? C(122) C(121) C(12) 122.4(2) ? C(126) C(121) C(12) 118.8(2) ? C(121) C(122) C(123) 119.9(3) ? C(124) C(123) C(122) 120.4(3) ? C(125) C(124) C(123) 120.4(3) ? C(124) C(125) C(126) 119.7(3) ? C(125) C(126) C(121) 120.9(3) ? C(132) C(131) C(136) 118.5(2) ? C(132) C(131) C(13) 120.3(2) ? C(136) C(131) C(13) 121.1(2) ? C(133) C(132) C(131) 120.5(3) ? C(134) C(133) C(132) 120.3(3) ? C(133) C(134) C(135) 119.9(3) ? C(136) C(135) C(134) 120.4(3) ? C(135) C(136) C(131) 120.4(3) ? C(152) C(151) C(156) 118.4(2) ? C(152) C(151) C(15) 121.6(2) ? C(156) C(151) C(15) 119.9(2) ? C(153) C(152) C(151) 120.6(3) ? C(152) C(153) C(154) 120.6(3) ? C(155) C(154) C(153) 119.5(3) ? C(154) C(155) C(156) 120.2(3) ? C(155) C(156) C(151) 120.6(3) ? C(166) C(161) C(162) 118.5(2) ? C(166) C(161) C(16) 121.0(2) ? C(162) C(161) C(16) 120.5(2) ? C(163) C(162) C(161) 120.4(3) ? C(164) C(163) C(162) 120.1(3) ? C(163) C(164) C(165) 120.4(3) ? C(164) C(165) C(166) 119.8(3) ? C(161) C(166) C(165) 120.8(3) ? C(222) C(221) C(226) 118.9(2) ? C(222) C(221) C(22) 120.8(2) ? C(226) C(221) C(22) 120.3(2) ? C(223) C(222) C(221) 120.6(3) ? C(224) C(223) C(222) 120.1(3) ? C(225) C(224) C(223) 119.9(3) ? C(224) C(225) C(226) 119.9(3) ? C(225) C(226) C(221) 120.6(3) ? C(232) C(231) C(236) 117.8(2) ? C(232) C(231) C(23) 120.0(2) ? C(236) C(231) C(23) 122.1(2) ? C(233) C(232) C(231) 121.7(2) ? C(232) C(233) C(234) 119.9(3) ? C(233) C(234) C(235) 119.6(3) ? C(236) C(235) C(234) 120.3(3) ? C(235) C(236) C(231) 120.8(2) ? C(252) C(251) C(256) 118.6(2) ? C(252) C(251) C(25) 120.8(2) ? C(256) C(251) C(25) 120.4(2) ? C(253) C(252) C(251) 120.4(3) ? C(252) C(253) C(254) 120.8(3) ? C(255) C(254) C(253) 119.2(3) ? C(254) C(255) C(256) 120.6(3) ? C(255) C(256) C(251) 120.3(3) ? C(266) C(261) C(262) 118.1(2) ? C(266) C(261) C(26) 121.2(2) ? C(262) C(261) C(26) 120.7(2) ? C(263) C(262) C(261) 120.4(2) ? C(264) C(263) C(262) 120.8(3) ? C(263) C(264) C(265) 119.9(3) ? C(264) C(265) C(266) 119.7(2) ? C(265) C(266) C(261) 121.2(2) ? C(906) C(901) C(902) 119.0(4) ? C(901) C(902) C(903) 120.5(4) ? C(904) C(903) C(902) 120.4(4) ? C(903) C(904) C(905) 119.2(4) ? C(906) C(905) C(904) 119.6(4) ? C(905) C(906) C(901) 121.3(4) ? C(911) C(912) C(913) 116.9(4) ? C(913) C(913) C(912) 117.1(5) ? #===END #============================================================================== data_MMS172 _database_code_CSD 164019 _audit_creation_date 26-09-97 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ? # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C66 H86 Nb1 O2 P2' _chemical_formula_structural ? _chemical_formula_weight 1066.27 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4726(17) _cell_length_b 11.9803(19) _cell_length_c 12.491(3) _cell_angle_alpha 106.078(16) _cell_angle_beta 97.680(16) _cell_angle_gamma 111.580(13) _cell_volume 1479.8(13) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 19 _cell_formula_units_z 1 _exptl_crystal_density_diffrn 1.20 _exptl_crystal_density_meas ? _diffrn_radiation_type Mo-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.287 _cell_measurement_temperature 203 _exptl_crystal_F_000 569 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type none _diffrn_reflns_number 4869 _reflns_number_total 4629 _reflns_number_gt 3479 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 24.06 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_time 83 _diffrn_standards_decay_% 0.71 # 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 0.043 _refine_ls_wR_factor_ref 0.117 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding, U=1.3*Ueq of bonding atom ; _refine_ls_number_reflns 4629 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.3591P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.013 _refine_diff_density_max 0.43 _refine_diff_density_min -0.62 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C) ' # 8. COMPUTING DATA _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _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 Nb 1.0000 1.0000 1.0000 0.0310(2) Uani ? P 1.19135(11) 0.95885(11) 1.08656(13) 0.0596(5) Uani ? O(10) 0.8845(2) 0.8228(2) 0.95847(19) 0.0260(9) Uani ? C(2) 1.1463(5) 0.7960(4) 1.0779(4) 0.058(2) Uani ? C(11) 0.8203(3) 0.6959(3) 0.9410(3) 0.0216(12) Uani ? C(12) 0.7949(3) 0.6070(3) 0.8292(3) 0.0227(12) Uani ? C(13) 0.7346(3) 0.4766(3) 0.8153(3) 0.0239(12) Uani ? C(14) 0.7028(3) 0.4412(3) 0.9076(3) 0.0260(13) Uani ? C(15) 0.7263(3) 0.5293(3) 1.0166(3) 0.0221(12) Uani ? C(16) 0.7842(3) 0.6610(3) 1.0349(3) 0.0218(12) Uani ? C(1A) 1.252(3) 1.032(2) 1.252(2) 0.075(8) Uani ? C(1B) 1.299(3) 1.059(3) 1.216(3) 0.18(2) Uani ? C(3A) 1.3399(18) 1.0187(19) 1.0568(15) 0.086(9) Uani ? C(3B) 1.3108(17) 0.9539(19) 0.9893(18) 0.100(11) Uani ? C(121) 0.8342(3) 0.6575(3) 0.7341(3) 0.0263(13) Uani ? C(122) 0.9665(4) 0.6637(4) 0.7209(3) 0.0354(14) Uani ? C(123) 1.0107(4) 0.7269(4) 0.6338(4) 0.0442(18) Uani ? C(124) 0.9106(4) 0.6581(4) 0.5182(3) 0.0474(18) Uani ? C(125) 0.7814(4) 0.6583(4) 0.5314(3) 0.0438(18) Uani ? C(126) 0.7347(4) 0.5921(4) 0.6157(3) 0.0374(14) Uani ? C(131) 0.7017(3) 0.3674(3) 0.7045(3) 0.0284(13) Uani ? C(132) 0.7938(4) 0.3257(3) 0.6722(3) 0.0387(14) Uani ? C(133) 0.7609(5) 0.2222(4) 0.5718(4) 0.0510(18) Uani ? C(134) 0.6351(5) 0.1583(4) 0.5045(4) 0.060(2) Uani ? C(135) 0.5431(5) 0.1967(4) 0.5365(4) 0.060(2) Uani ? C(136) 0.5750(4) 0.3001(4) 0.6368(3) 0.0431(14) Uani ? C(151) 0.6869(3) 0.4738(3) 1.1069(3) 0.0242(12) Uani ? C(152) 0.5680(4) 0.4513(4) 1.1309(3) 0.0334(14) Uani ? C(153) 0.5311(4) 0.3922(4) 1.2094(4) 0.0428(17) Uani ? C(154) 0.6125(4) 0.3549(4) 1.2658(4) 0.044(2) Uani ? C(155) 0.7309(4) 0.3756(4) 1.2424(4) 0.046(2) Uani ? C(156) 0.7676(4) 0.4333(4) 1.1633(3) 0.0360(14) Uani ? C(161) 0.8060(3) 0.7670(3) 1.1461(3) 0.0256(13) Uani ? C(162) 0.8707(4) 0.7610(3) 1.2588(3) 0.0352(14) Uani ? C(163) 0.9033(4) 0.8853(4) 1.3579(3) 0.0404(14) Uani ? C(164) 0.7822(4) 0.9041(4) 1.3706(3) 0.0483(16) Uani ? C(165) 0.7088(4) 0.9026(4) 1.2596(4) 0.0478(18) Uani ? C(166) 0.6808(4) 0.7825(4) 1.1570(3) 0.0372(14) Uani ? H(1) 1.054(5) 0.967(5) 0.874(5) 0.101(18) Uiso ? H(14) 0.6637 0.3542 0.8963 0.0340 Uiso calc H(2A) 1.2180 0.7900 1.1213 0.0760 Uiso calc H(2B) 1.1239 0.7417 0.9986 0.0760 Uiso calc H(2C) 1.0730 0.7690 1.1090 0.0760 Uiso calc H(121) 0.8455 0.7468 0.7607 0.0340 Uiso calc H(12A) 0.9616 0.5775 0.6956 0.0460 Uiso calc H(12B) 1.0302 0.7120 0.7953 0.0460 Uiso calc H(12C) 1.0243 0.8159 0.6628 0.0580 Uiso calc H(12D) 1.0927 0.7252 0.6244 0.0580 Uiso calc H(12E) 0.9004 0.5704 0.4871 0.0620 Uiso calc H(12F) 0.9398 0.7004 0.4646 0.0620 Uiso calc H(12G) 0.7178 0.6138 0.4569 0.0570 Uiso calc H(12H) 0.7908 0.7459 0.5598 0.0570 Uiso calc H(12I) 0.7200 0.5029 0.5845 0.0490 Uiso calc H(12J) 0.6527 0.5942 0.6246 0.0490 Uiso calc H(132) 0.8787 0.3676 0.7185 0.0500 Uiso calc H(133) 0.8239 0.1962 0.5501 0.0660 Uiso calc H(134) 0.6127 0.0888 0.4371 0.0780 Uiso calc H(135) 0.4579 0.1530 0.4907 0.0780 Uiso calc H(136) 0.5109 0.3243 0.6585 0.0560 Uiso calc H(152) 0.5117 0.4763 1.0935 0.0430 Uiso calc H(153) 0.4504 0.3777 1.2240 0.0560 Uiso calc H(154) 0.5881 0.3161 1.3192 0.0570 Uiso calc H(155) 0.7868 0.3504 1.2802 0.0600 Uiso calc H(156) 0.8474 0.4453 1.1475 0.0470 Uiso calc H(161) 0.8653 0.8468 1.1399 0.0340 Uiso calc H(16A) 0.8124 0.6883 1.2741 0.0460 Uiso calc H(16B) 0.9495 0.7502 1.2519 0.0460 Uiso calc H(16C) 0.9451 0.8825 1.4293 0.0520 Uiso calc H(16D) 0.9635 0.9574 1.3431 0.0520 Uiso calc H(16E) 0.8060 0.9854 1.4316 0.0630 Uiso calc H(16F) 0.7260 0.8364 1.3930 0.0630 Uiso calc H(16G) 0.7595 0.9783 1.2439 0.0620 Uiso calc H(16H) 0.6274 0.9058 1.2690 0.0620 Uiso calc H(16I) 0.6415 0.7889 1.0865 0.0490 Uiso calc H(16J) 0.6196 0.7074 1.1672 0.0490 Uiso calc H(1A1) 1.3161 1.0056 1.2779 0.0970 Uiso calc H(1A2) 1.1801 1.0041 1.2847 0.0970 Uiso calc H(1A3) 1.2894 1.1243 1.2756 0.0970 Uiso calc H(1B1) 1.3623 1.0274 1.2332 0.2350 Uiso calc H(1B2) 1.2535 1.0628 1.2755 0.2350 Uiso calc H(1B3) 1.3417 1.1433 1.2136 0.2350 Uiso calc H(3A1) 1.3670 1.1081 1.0688 0.1120 Uiso calc H(3A2) 1.3324 0.9729 0.9780 0.1120 Uiso calc H(3A3) 1.4029 1.0083 1.1072 0.1120 Uiso calc H(3B1) 1.3652 1.0397 0.9957 0.1280 Uiso calc H(3B2) 1.2620 0.9045 0.9104 0.1280 Uiso calc H(3B3) 1.3640 0.9151 1.0141 0.1280 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 Nb 0.0325(3) 0.0195(3) 0.0340(3) 0.0071(2) 0.0004(2) 0.0085(2) P 0.0361(7) 0.0379(6) 0.0971(11) 0.0132(5) -0.0052(7) 0.0269(7) O(10) 0.0325(14) 0.0201(12) 0.0196(13) 0.0075(10) 0.0035(11) 0.0053(10) C(2) 0.067(3) 0.052(3) 0.068(3) 0.037(3) 0.010(3) 0.027(2) C(11) 0.0237(18) 0.0189(16) 0.0181(18) 0.0074(14) 0.0010(14) 0.0049(14) C(12) 0.0236(18) 0.0255(18) 0.0190(18) 0.0119(15) 0.0035(14) 0.0068(14) C(13) 0.0262(18) 0.0213(17) 0.0209(19) 0.0099(14) 0.0054(15) 0.0035(14) C(14) 0.0293(19) 0.0186(16) 0.026(2) 0.0087(15) 0.0033(16) 0.0058(15) C(15) 0.0241(18) 0.0241(17) 0.0176(18) 0.0113(14) 0.0040(14) 0.0060(14) C(16) 0.0216(17) 0.0233(17) 0.0166(18) 0.0089(14) 0.0014(14) 0.0039(14) C(1A) 0.081(15) 0.053(10) 0.059(8) 0.037(10) -0.035(8) -0.013(7) C(1B) 0.11(3) 0.090(18) 0.22(4) 0.046(18) -0.12(2) -0.04(2) C(3A) 0.051(8) 0.104(15) 0.103(15) 0.023(10) 0.005(9) 0.056(11) C(3B) 0.057(11) 0.122(17) 0.19(2) 0.058(12) 0.063(13) 0.114(16) C(121) 0.033(2) 0.0243(17) 0.0188(18) 0.0111(15) 0.0050(15) 0.0057(15) C(122) 0.035(2) 0.044(2) 0.029(2) 0.0148(18) 0.0087(17) 0.0181(18) C(123) 0.041(2) 0.059(3) 0.044(3) 0.020(2) 0.019(2) 0.033(2) C(124) 0.059(3) 0.061(3) 0.031(2) 0.027(2) 0.018(2) 0.024(2) C(125) 0.054(3) 0.058(3) 0.020(2) 0.023(2) 0.0044(19) 0.0181(19) C(126) 0.035(2) 0.049(2) 0.022(2) 0.0141(19) 0.0032(17) 0.0109(18) C(131) 0.040(2) 0.0189(17) 0.0212(19) 0.0084(16) 0.0119(17) 0.0036(15) C(132) 0.049(2) 0.029(2) 0.036(2) 0.0181(19) 0.0125(19) 0.0059(18) C(133) 0.069(3) 0.034(2) 0.053(3) 0.026(2) 0.033(3) 0.006(2) C(134) 0.084(4) 0.033(2) 0.037(3) 0.010(2) 0.027(3) -0.010(2) C(135) 0.055(3) 0.048(3) 0.037(3) 0.001(2) 0.007(2) -0.012(2) C(136) 0.041(2) 0.039(2) 0.030(2) 0.0087(19) 0.0074(19) -0.0035(18) C(151) 0.032(2) 0.0191(16) 0.0169(18) 0.0091(15) 0.0036(15) 0.0033(14) C(152) 0.032(2) 0.041(2) 0.028(2) 0.0156(17) 0.0066(17) 0.0137(17) C(153) 0.038(2) 0.056(3) 0.042(2) 0.020(2) 0.018(2) 0.025(2) C(154) 0.051(3) 0.051(3) 0.039(3) 0.020(2) 0.018(2) 0.030(2) C(155) 0.053(3) 0.060(3) 0.045(3) 0.034(2) 0.014(2) 0.032(2) C(156) 0.035(2) 0.042(2) 0.037(2) 0.0197(18) 0.0117(18) 0.0171(19) C(161) 0.034(2) 0.0200(17) 0.0162(18) 0.0080(15) 0.0050(15) 0.0023(14) C(162) 0.044(2) 0.032(2) 0.018(2) 0.0145(18) -0.0001(17) -0.0020(16) C(163) 0.049(2) 0.035(2) 0.019(2) 0.0135(19) -0.0049(18) -0.0043(17) C(164) 0.063(3) 0.040(2) 0.029(2) 0.021(2) 0.012(2) -0.0053(19) C(165) 0.056(3) 0.041(2) 0.043(3) 0.029(2) 0.012(2) -0.001(2) C(166) 0.042(2) 0.038(2) 0.026(2) 0.0209(19) 0.0028(18) 0.0006(17) # 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 Nb H(1) 1.77(5) ? Nb H(1) 1.77(5) ? Nb O(10) 1.916(2) ? Nb O(10) 1.916(2) ? Nb P 2.5862(12) ? Nb P 2.5863(12) ? P C(1B) 1.70(3) ? P C(3A) 1.72(2) ? P C(2) 1.792(4) ? P C(1A) 1.92(2) ? P C(3B) 1.955(19) ? O(10) C(11) 1.360(4) ? C(11) C(16) 1.412(5) ? C(11) C(12) 1.417(5) ? C(12) C(13) 1.405(4) ? C(12) C(121) 1.523(5) ? C(13) C(14) 1.383(5) ? C(13) C(131) 1.505(4) ? C(14) C(15) 1.392(5) ? C(15) C(16) 1.405(4) ? C(15) C(151) 1.500(5) ? C(16) C(161) 1.517(4) ? C(121) C(122) 1.526(5) ? C(121) C(126) 1.534(5) ? C(122) C(123) 1.529(5) ? C(123) C(124) 1.512(6) ? C(124) C(125) 1.513(6) ? C(125) C(126) 1.525(5) ? C(131) C(136) 1.382(5) ? C(131) C(132) 1.385(5) ? C(132) C(133) 1.386(5) ? C(133) C(134) 1.372(7) ? C(134) C(135) 1.362(7) ? C(135) C(136) 1.386(5) ? C(151) C(152) 1.381(5) ? C(151) C(156) 1.390(5) ? C(152) C(153) 1.386(5) ? C(153) C(154) 1.369(6) ? C(154) C(155) 1.375(6) ? C(155) C(156) 1.381(5) ? C(161) C(166) 1.533(5) ? C(161) C(162) 1.534(5) ? C(162) C(163) 1.529(5) ? C(163) C(164) 1.508(6) ? C(164) C(165) 1.515(6) ? C(165) C(166) 1.532(5) ? 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 H(1) Nb H(1) 180.00(3) ? H(1) Nb O(10) 91.5(17) ? H(1) Nb O(10) 88.5(17) ? H(1) Nb O(10) 88.5(17) ? H(1) Nb O(10) 91.5(17) ? O(10) Nb O(10) 180.0(17) ? H(1) Nb P 82.8(17) ? H(1) Nb P 97.2(17) ? O(10) Nb P 90.46(7) ? O(10) Nb P 89.54(7) ? H(1) Nb P 97.2(17) ? H(1) Nb P 82.8(17) ? O(10) Nb P 89.54(7) ? O(10) Nb P 90.46(7) ? P Nb P 180.00(7) ? C(1B) P C(3A) 74.6(12) ? C(1B) P C(2) 109.1(12) ? C(3A) P C(2) 110.0(7) ? C(1B) P C(1A) 23.9(15) ? C(3A) P C(1A) 97.7(9) ? C(2) P C(1A) 95.7(8) ? C(1B) P C(3B) 100.3(12) ? C(3A) P C(3B) 27.2(7) ? C(2) P C(3B) 93.4(6) ? C(1A) P C(3B) 121.8(10) ? C(1B) P Nb 122.1(12) ? C(3A) P Nb 121.3(7) ? C(2) P Nb 113.77(16) ? C(1A) P Nb 114.4(8) ? C(3B) P Nb 113.7(6) ? C(11) O(10) Nb 169.7(2) ? O(10) C(11) C(16) 118.3(3) ? O(10) C(11) C(12) 117.5(3) ? C(16) C(11) C(12) 124.2(3) ? C(13) C(12) C(11) 116.2(3) ? C(13) C(12) C(121) 124.8(3) ? C(11) C(12) C(121) 119.0(3) ? C(14) C(13) C(12) 120.1(3) ? C(14) C(13) C(131) 115.4(3) ? C(12) C(13) C(131) 124.5(3) ? C(13) C(14) C(15) 123.2(3) ? C(14) C(15) C(16) 119.1(3) ? C(14) C(15) C(151) 116.0(3) ? C(16) C(15) C(151) 124.9(3) ? C(15) C(16) C(11) 117.1(3) ? C(15) C(16) C(161) 124.7(3) ? C(11) C(16) C(161) 118.2(3) ? C(12) C(121) C(122) 112.2(3) ? C(12) C(121) C(126) 116.7(3) ? C(122) C(121) C(126) 110.2(3) ? C(121) C(122) C(123) 111.5(3) ? C(124) C(123) C(122) 110.9(3) ? C(123) C(124) C(125) 110.2(3) ? C(124) C(125) C(126) 110.0(3) ? C(125) C(126) C(121) 111.4(3) ? C(136) C(131) C(132) 118.4(3) ? C(136) C(131) C(13) 119.9(3) ? C(132) C(131) C(13) 121.5(3) ? C(131) C(132) C(133) 120.8(4) ? C(134) C(133) C(132) 119.8(4) ? C(135) C(134) C(133) 120.0(4) ? C(134) C(135) C(136) 120.7(4) ? C(131) C(136) C(135) 120.2(4) ? C(152) C(151) C(156) 117.6(3) ? C(152) C(151) C(15) 122.6(3) ? C(156) C(151) C(15) 119.6(3) ? C(151) C(152) C(153) 121.3(4) ? C(154) C(153) C(152) 120.5(4) ? C(153) C(154) C(155) 119.0(4) ? C(154) C(155) C(156) 120.7(4) ? C(155) C(156) C(151) 120.9(4) ? C(16) C(161) C(166) 111.7(3) ? C(16) C(161) C(162) 117.0(3) ? C(166) C(161) C(162) 109.7(3) ? C(163) C(162) C(161) 109.1(3) ? C(164) C(163) C(162) 110.9(3) ? C(163) C(164) C(165) 111.9(3) ? C(164) C(165) C(166) 111.8(3) ? C(165) C(166) C(161) 110.9(3) ? #===END data_MMS229 _database_code_CSD 164020 _audit_creation_date 22-10-98 _audit_creation_method 'from_MolEN_and_SHELXL' _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C70 H56 Cl3 Nb1 O2' _chemical_formula_structural ? _chemical_formula_weight 1128.49 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.3325(2) _cell_length_b 21.2903(3) _cell_length_c 23.9340(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.2926(9) _cell_angle_gamma 90.00 _cell_volume 5739.8(3) _cell_measurement_reflns_used 46609 _cell_measurement_theta_min 4 _cell_measurement_theta_max 30 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.384 _cell_measurement_temperature 203 _exptl_crystal_F_000 2336 # 6. DATA COLLECTION _diffrn_ambient_temperature 203 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7239 _exptl_absorpt_correction_T_max 0.9260 _diffrn_reflns_number 46609 _reflns_number_total 15178 _reflns_number_gt 10376 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.52 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_max 32 # 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 0.049 _refine_ls_wR_factor_ref 0.119 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 15178 _refine_ls_number_parameters 690 _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^)+(0.0685P)^2^+0.9643P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.052 _refine_diff_density_max 0.53 _refine_diff_density_min -0.83 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.44E-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 Direct_methods_(SIR97,_Altomare_et_al.,_1997) _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 Nb 0.969041(18) -0.048710(10) 0.738270(9) 0.02863(6) Uani ? Cl1 1.11344(8) 0.03043(4) 0.73855(5) 0.0726(3) Uani ? Cl2 1.09227(6) -0.09627(4) 0.81107(3) 0.0447(2) Uani ? Cl3 0.91171(8) -0.01761(3) 0.64533(3) 0.0557(2) Uani ? O10 0.85900(14) -0.01039(8) 0.77620(7) 0.0316(5) Uani ? O20 0.89853(13) -0.12479(7) 0.71540(6) 0.0271(4) Uani ? C11 0.7741(2) 0.01896(10) 0.80498(10) 0.0282(6) Uani ? C12 0.7034(2) 0.06479(11) 0.77663(10) 0.0292(6) Uani ? C13 0.6150(2) 0.09293(11) 0.80550(10) 0.0301(6) Uani ? C14 0.6093(2) 0.07673(12) 0.86148(10) 0.0337(6) Uani ? C15 0.6828(2) 0.03205(11) 0.88948(10) 0.0297(6) Uani ? C16 0.7646(2) -0.00040(11) 0.85995(10) 0.0285(6) Uani ? C21 0.86114(19) -0.16868(10) 0.67525(9) 0.0254(5) Uani ? C22 0.74688(19) -0.19346(10) 0.67701(9) 0.0249(5) Uani ? C23 0.70740(19) -0.23944(10) 0.63720(10) 0.0262(6) Uani ? C24 0.7818(2) -0.25661(11) 0.59732(10) 0.0287(6) Uani ? C25 0.89383(19) -0.23055(11) 0.59457(9) 0.0266(6) Uani ? C26 0.93670(19) -0.18568(10) 0.63487(9) 0.0253(5) Uani ? C121 0.7194(2) 0.08307(11) 0.71777(10) 0.0316(6) Uani ? C122 0.6328(2) 0.06885(13) 0.67397(11) 0.0399(7) Uani ? C123 0.6450(3) 0.08837(14) 0.61961(12) 0.0499(9) Uani ? C124 0.7426(3) 0.12331(14) 0.60770(12) 0.0526(9) Uani ? C125 0.8282(3) 0.13674(13) 0.65137(13) 0.0498(9) Uani ? C126 0.8187(2) 0.11661(11) 0.70594(11) 0.0377(7) Uani ? C127 0.7538(5) 0.1451(2) 0.54847(15) 0.0908(16) Uani ? C131 0.5273(2) 0.13868(11) 0.77770(10) 0.0326(6) Uani ? C132 0.4062(2) 0.12755(13) 0.77886(12) 0.0421(7) Uani ? C133 0.3218(3) 0.16810(14) 0.75243(14) 0.0497(9) Uani ? C134 0.3574(3) 0.21978(14) 0.72375(13) 0.0484(8) Uani ? C135 0.4773(3) 0.23203(13) 0.72293(12) 0.0452(8) Uani ? C136 0.5613(2) 0.19140(11) 0.74955(11) 0.0377(7) Uani ? C151 0.6767(2) 0.02144(11) 0.95091(10) 0.0328(6) Uani ? C152 0.7022(3) 0.07116(14) 0.98768(12) 0.0481(8) Uani ? C153 0.7056(3) 0.06302(17) 1.04536(13) 0.0600(11) Uani ? C154 0.6818(3) 0.00547(16) 1.06678(13) 0.0575(9) Uani ? C155 0.6516(3) -0.04382(14) 1.03101(13) 0.0548(9) Uani ? C156 0.6500(3) -0.03634(12) 0.97325(12) 0.0432(8) Uani ? C161 0.8364(2) -0.05392(11) 0.88603(10) 0.0297(6) Uani ? C162 0.9212(3) -0.04554(13) 0.93221(12) 0.0439(8) Uani ? C163 0.9789(3) -0.09701(16) 0.95792(12) 0.0533(9) Uani ? C164 0.9543(3) -0.15789(15) 0.93944(13) 0.0495(9) Uani ? C165 0.8715(2) -0.16559(13) 0.89268(12) 0.0410(7) Uani ? C166 0.8131(2) -0.11462(11) 0.86634(10) 0.0325(6) Uani ? C167 1.0165(4) -0.21343(19) 0.96813(17) 0.0823(15) Uani ? C221 0.67033(19) -0.17014(11) 0.71944(9) 0.0267(6) Uani ? C222 0.6375(2) -0.10736(11) 0.72056(10) 0.0288(6) Uani ? C223 0.5589(2) -0.08648(12) 0.75723(10) 0.0329(6) Uani ? C224 0.5116(2) -0.12784(13) 0.79397(10) 0.0353(7) Uani ? C225 0.5459(2) -0.19039(13) 0.79305(11) 0.0372(7) Uani ? C226 0.6242(2) -0.21148(11) 0.75654(10) 0.0317(6) Uani ? C227 0.4273(3) -0.10462(17) 0.83374(13) 0.0534(9) Uani ? C231 0.58948(19) -0.27058(11) 0.63509(10) 0.0287(6) Uani ? C232 0.5826(2) -0.33572(12) 0.63327(11) 0.0350(7) Uani ? C233 0.4732(2) -0.36613(14) 0.63082(12) 0.0458(8) Uani ? C234 0.3699(2) -0.33121(16) 0.62951(14) 0.0538(9) Uani ? C235 0.3755(2) -0.26634(16) 0.63071(15) 0.0558(9) Uani ? C236 0.4844(2) -0.23595(13) 0.63339(12) 0.0422(8) Uani ? C251 0.9612(2) -0.25090(11) 0.54732(10) 0.0290(6) Uani ? C252 1.0753(2) -0.27498(11) 0.55633(11) 0.0352(7) Uani ? C253 1.1338(2) -0.29402(13) 0.51101(12) 0.0429(8) Uani ? C254 1.0790(3) -0.28934(14) 0.45687(13) 0.0492(9) Uani ? C255 0.9650(3) -0.26570(15) 0.44755(12) 0.0511(9) Uani ? C256 0.9066(2) -0.24641(13) 0.49240(11) 0.0387(7) Uani ? C261 1.05247(19) -0.15275(10) 0.63280(10) 0.0264(6) Uani ? C262 1.0777(2) -0.12313(11) 0.58355(10) 0.0315(6) Uani ? C263 1.1799(2) -0.08776(12) 0.58264(12) 0.0375(7) Uani ? C264 1.2611(2) -0.08123(13) 0.63001(13) 0.0421(8) Uani ? C265 1.2374(2) -0.11190(13) 0.67855(12) 0.0417(7) Uani ? C266 1.1348(2) -0.14753(11) 0.68025(10) 0.0325(6) Uani ? C267 1.3706(3) -0.04091(17) 0.62881(18) 0.0700(12) Uani ? C901 0.6539(4) -0.12351(19) 0.4758(2) 0.0833(17) Uani ? C902 0.6752(4) -0.13467(19) 0.4215(2) 0.0792(14) Uani ? C903 0.7740(5) -0.1118(2) 0.40236(19) 0.0850(17) Uani ? C904 0.8539(4) -0.0759(2) 0.4378(2) 0.0873(16) Uani ? C905 0.8299(4) -0.06440(19) 0.4918(2) 0.0826(14) Uani ? C906 0.7333(5) -0.0884(2) 0.51081(19) 0.0836(17) Uani ? H14 0.5536 0.0968 0.8810 0.0440 Uiso calc H24 0.7554 -0.2871 0.5711 0.0370 Uiso calc H122 0.5661 0.0460 0.6811 0.0520 Uiso calc H123 0.5868 0.0779 0.5907 0.0650 Uiso calc H125 0.8944 0.1600 0.6442 0.0650 Uiso calc H126 0.8788 0.1256 0.7345 0.0490 Uiso calc H12A 0.7315 0.1886 0.5448 0.1180 Uiso calc H12B 0.7025 0.1205 0.5225 0.1180 Uiso calc H12C 0.8345 0.1403 0.5405 0.1180 Uiso calc H132 0.3816 0.0925 0.7976 0.0550 Uiso calc H133 0.2414 0.1605 0.7540 0.0650 Uiso calc H134 0.3010 0.2463 0.7050 0.0630 Uiso calc H135 0.5015 0.2675 0.7045 0.0590 Uiso calc H136 0.6416 0.1997 0.7485 0.0490 Uiso calc H152 0.7173 0.1106 0.9734 0.0620 Uiso calc H153 0.7240 0.0967 1.0694 0.0780 Uiso calc H154 0.6860 -0.0003 1.1055 0.0750 Uiso calc H155 0.6322 -0.0825 1.0456 0.0710 Uiso calc H156 0.6309 -0.0702 0.9494 0.0560 Uiso calc H162 0.9391 -0.0053 0.9458 0.0570 Uiso calc H163 1.0358 -0.0906 0.9885 0.0700 Uiso calc H165 0.8549 -0.2058 0.8787 0.0530 Uiso calc H166 0.7578 -0.1211 0.8352 0.0420 Uiso calc H16A 0.9875 -0.2514 0.9498 0.1070 Uiso calc H16B 1.0014 -0.2144 1.0068 0.1070 Uiso calc H16C 1.1004 -0.2100 0.9661 0.1070 Uiso calc H222 0.6685 -0.0789 0.6965 0.0370 Uiso calc H223 0.5375 -0.0443 0.7572 0.0430 Uiso calc H225 0.5158 -0.2187 0.8174 0.0480 Uiso calc H226 0.6461 -0.2536 0.7568 0.0410 Uiso calc H22A 0.3794 -0.1389 0.8443 0.0700 Uiso calc H22B 0.3769 -0.0727 0.8156 0.0700 Uiso calc H22C 0.4716 -0.0874 0.8667 0.0700 Uiso calc H232 0.6518 -0.3593 0.6337 0.0450 Uiso calc H233 0.4697 -0.4098 0.6301 0.0600 Uiso calc H234 0.2968 -0.3514 0.6278 0.0700 Uiso calc H235 0.3060 -0.2429 0.6297 0.0720 Uiso calc H236 0.4875 -0.1923 0.6341 0.0550 Uiso calc H252 1.1129 -0.2784 0.5927 0.0460 Uiso calc H253 1.2105 -0.3100 0.5173 0.0560 Uiso calc H254 1.1186 -0.3020 0.4267 0.0640 Uiso calc H255 0.9274 -0.2628 0.4111 0.0660 Uiso calc H256 0.8301 -0.2303 0.4858 0.0500 Uiso calc H262 1.0253 -0.1272 0.5510 0.0410 Uiso calc H263 1.1944 -0.0679 0.5495 0.0490 Uiso calc H265 1.2911 -0.1086 0.7107 0.0540 Uiso calc H266 1.1212 -0.1680 0.7133 0.0420 Uiso calc H26A 1.3672 -0.0063 0.6543 0.0910 Uiso calc H26B 1.3741 -0.0252 0.5914 0.0910 Uiso calc H26C 1.4401 -0.0656 0.6399 0.0910 Uiso calc H901 0.5860 -0.1396 0.4891 0.1080 Uiso calc H902 0.6214 -0.1581 0.3978 0.1030 Uiso calc H903 0.7890 -0.1198 0.3656 0.1100 Uiso calc H904 0.9225 -0.0601 0.4249 0.1140 Uiso calc H905 0.8815 -0.0397 0.5154 0.1070 Uiso calc H906 0.7193 -0.0815 0.5479 0.1090 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 Nb 0.02835(12) 0.02881(12) 0.02997(13) -0.00453(8) 0.00880(8) -0.00854(8) Cl1 0.0534(5) 0.0475(4) 0.1216(8) -0.0227(4) 0.0302(5) -0.0128(5) Cl2 0.0310(3) 0.0662(5) 0.0358(4) 0.0039(3) -0.0011(3) -0.0116(3) Cl3 0.0952(6) 0.0404(4) 0.0344(4) 0.0199(4) 0.0208(4) 0.0020(3) O10 0.0333(9) 0.0338(9) 0.0285(9) 0.0010(7) 0.0073(7) -0.0056(7) O20 0.0262(8) 0.0285(8) 0.0268(8) -0.0009(6) 0.0042(6) -0.0075(6) C11 0.0254(11) 0.0279(11) 0.0321(12) -0.0039(9) 0.0067(9) -0.0096(9) C12 0.0308(11) 0.0263(11) 0.0308(12) -0.0053(9) 0.0051(9) -0.0058(9) C13 0.0302(12) 0.0279(11) 0.0325(13) -0.0022(9) 0.0044(10) -0.0024(9) C14 0.0344(12) 0.0338(12) 0.0346(13) 0.0014(11) 0.0112(10) -0.0046(10) C15 0.0308(12) 0.0312(11) 0.0279(12) -0.0024(10) 0.0068(9) -0.0041(9) C16 0.0290(11) 0.0288(11) 0.0277(12) -0.0015(9) 0.0035(9) -0.0055(9) C21 0.0255(11) 0.0256(10) 0.0253(11) 0.0004(9) 0.0031(9) -0.0043(9) C22 0.0243(10) 0.0261(10) 0.0246(11) 0.0028(9) 0.0037(8) -0.0012(9) C23 0.0239(10) 0.0261(11) 0.0285(12) 0.0006(9) 0.0022(9) -0.0024(9) C24 0.0288(11) 0.0288(11) 0.0284(12) -0.0021(9) 0.0031(9) -0.0093(9) C25 0.0252(11) 0.0289(11) 0.0260(11) 0.0010(9) 0.0039(9) -0.0040(9) C26 0.0237(10) 0.0262(11) 0.0265(11) 0.0012(9) 0.0047(9) 0.0004(9) C121 0.0388(13) 0.0270(11) 0.0299(12) 0.0011(10) 0.0084(10) -0.0019(9) C122 0.0458(15) 0.0408(14) 0.0330(14) -0.0033(12) 0.0043(11) -0.0025(11) C123 0.066(2) 0.0506(17) 0.0327(15) 0.0013(15) 0.0037(13) -0.0027(12) C124 0.084(2) 0.0431(16) 0.0341(15) 0.0020(16) 0.0217(15) 0.0013(12) C125 0.0659(19) 0.0358(14) 0.0526(18) -0.0071(14) 0.0290(15) -0.0004(13) C126 0.0431(14) 0.0314(12) 0.0404(15) -0.0050(11) 0.0122(11) -0.0043(11) C127 0.140(4) 0.092(3) 0.045(2) -0.014(3) 0.031(2) 0.008(2) C131 0.0361(13) 0.0309(12) 0.0316(13) 0.0016(10) 0.0076(10) -0.0035(10) C132 0.0377(14) 0.0403(14) 0.0495(16) 0.0026(12) 0.0104(12) 0.0056(12) C133 0.0369(15) 0.0508(17) 0.061(2) 0.0071(13) 0.0029(14) -0.0004(15) C134 0.0533(17) 0.0430(15) 0.0470(17) 0.0138(13) -0.0036(14) 0.0013(13) C135 0.0588(18) 0.0329(13) 0.0446(16) 0.0033(13) 0.0083(14) 0.0016(12) C136 0.0390(13) 0.0310(12) 0.0439(15) -0.0010(11) 0.0080(11) -0.0021(11) C151 0.0348(12) 0.0342(12) 0.0311(13) 0.0051(10) 0.0117(10) -0.0021(10) C152 0.070(2) 0.0386(14) 0.0398(15) -0.0084(14) 0.0241(14) -0.0054(12) C153 0.088(3) 0.0612(19) 0.0344(16) -0.0108(18) 0.0223(16) -0.0150(14) C154 0.083(2) 0.064(2) 0.0290(15) 0.0149(18) 0.0215(15) -0.0003(14) C155 0.083(2) 0.0417(15) 0.0445(17) 0.0107(15) 0.0280(16) 0.0095(13) C156 0.0589(18) 0.0343(13) 0.0387(15) 0.0027(12) 0.0153(13) -0.0009(11) C161 0.0280(11) 0.0363(12) 0.0253(11) 0.0037(10) 0.0057(9) -0.0058(9) C162 0.0423(15) 0.0480(16) 0.0396(15) 0.0086(12) -0.0037(12) -0.0142(12) C163 0.0513(17) 0.066(2) 0.0385(16) 0.0172(15) -0.0141(13) -0.0091(14) C164 0.0494(17) 0.0554(18) 0.0433(16) 0.0217(14) 0.0031(13) 0.0048(14) C165 0.0428(15) 0.0345(13) 0.0467(16) 0.0052(11) 0.0094(12) 0.0010(12) C166 0.0311(12) 0.0354(13) 0.0312(13) 0.0041(10) 0.0046(10) -0.0032(10) C167 0.095(3) 0.077(3) 0.069(3) 0.036(2) -0.017(2) 0.008(2) C221 0.0226(10) 0.0314(11) 0.0262(12) 0.0013(9) 0.0026(9) -0.0041(9) C222 0.0268(11) 0.0320(12) 0.0282(12) -0.0002(9) 0.0053(9) -0.0017(9) C223 0.0280(11) 0.0335(12) 0.0376(14) 0.0059(10) 0.0056(10) -0.0071(10) C224 0.0255(11) 0.0508(15) 0.0303(13) 0.0030(11) 0.0061(10) -0.0074(11) C225 0.0355(13) 0.0461(14) 0.0314(13) -0.0040(11) 0.0094(10) 0.0027(11) C226 0.0308(12) 0.0305(12) 0.0347(13) 0.0003(10) 0.0073(10) -0.0007(10) C227 0.0420(16) 0.075(2) 0.0462(17) 0.0109(15) 0.0189(13) -0.0054(15) C231 0.0248(11) 0.0351(12) 0.0263(12) -0.0034(9) 0.0026(9) -0.0056(9) C232 0.0307(12) 0.0357(13) 0.0384(14) -0.0016(10) 0.0035(10) -0.0039(11) C233 0.0443(15) 0.0404(15) 0.0531(17) -0.0143(12) 0.0069(13) -0.0029(13) C234 0.0314(14) 0.063(2) 0.068(2) -0.0167(13) 0.0098(14) -0.0128(16) C235 0.0256(13) 0.063(2) 0.078(2) -0.0016(13) 0.0023(14) -0.0283(17) C236 0.0289(12) 0.0432(15) 0.0538(17) -0.0001(11) 0.0013(12) -0.0161(13) C251 0.0305(12) 0.0260(11) 0.0319(12) -0.0013(9) 0.0093(10) -0.0066(9) C252 0.0336(12) 0.0356(13) 0.0377(14) 0.0001(10) 0.0095(11) -0.0041(11) C253 0.0391(14) 0.0410(14) 0.0518(17) 0.0040(12) 0.0189(13) -0.0046(13) C254 0.0566(18) 0.0528(17) 0.0433(17) 0.0015(14) 0.0282(14) -0.0120(13) C255 0.0592(19) 0.0615(19) 0.0340(15) 0.0049(15) 0.0110(13) -0.0096(13) C256 0.0388(14) 0.0443(14) 0.0337(14) 0.0040(12) 0.0076(11) -0.0061(11) C261 0.0252(11) 0.0249(10) 0.0300(12) 0.0006(9) 0.0072(9) -0.0053(9) C262 0.0308(12) 0.0332(12) 0.0313(13) -0.0011(10) 0.0067(10) -0.0048(10) C263 0.0381(13) 0.0343(13) 0.0424(15) -0.0032(11) 0.0145(11) 0.0019(11) C264 0.0290(12) 0.0370(14) 0.0605(18) -0.0035(11) 0.0057(12) 0.0047(13) C265 0.0309(13) 0.0412(14) 0.0503(17) -0.0049(11) -0.0071(12) 0.0039(12) C266 0.0305(12) 0.0330(12) 0.0338(13) -0.0014(10) 0.0026(10) 0.0015(10) C267 0.0424(17) 0.068(2) 0.096(3) -0.0237(16) -0.0081(18) 0.030(2) C901 0.075(3) 0.067(3) 0.106(4) -0.002(2) 0.001(3) 0.003(2) C902 0.090(3) 0.063(2) 0.078(3) 0.005(2) -0.021(2) -0.003(2) C903 0.113(4) 0.070(3) 0.071(3) 0.015(3) 0.005(3) 0.009(2) C904 0.080(3) 0.058(2) 0.122(4) 0.002(2) 0.002(3) 0.030(3) C905 0.090(3) 0.054(2) 0.095(3) -0.001(2) -0.029(3) 0.005(2) C906 0.110(4) 0.066(3) 0.071(3) 0.014(3) -0.007(3) 0.001(2) # 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 Nb O(10) 1.8147(16) ? Nb O(20) 1.8617(15) ? Nb Cl(2) 2.3405(7) ? Nb Cl(3) 2.3434(8) ? Nb Cl(1) 2.3483(8) ? O(10) C(11) 1.391(3) ? O(20) C(21) 1.374(3) ? C(11) C(12) 1.391(3) ? C(11) C(16) 1.394(3) ? C(12) C(13) 1.411(3) ? C(12) C(121) 1.492(3) ? C(13) C(14) 1.392(3) ? C(13) C(131) 1.495(3) ? C(14) C(15) 1.387(4) ? C(15) C(16) 1.407(3) ? C(15) C(151) 1.497(3) ? C(16) C(161) 1.496(3) ? C(21) C(22) 1.403(3) ? C(21) C(26) 1.407(3) ? C(22) C(23) 1.405(3) ? C(22) C(221) 1.491(3) ? C(23) C(24) 1.390(3) ? C(23) C(231) 1.488(3) ? C(24) C(25) 1.393(3) ? C(25) C(26) 1.406(3) ? C(25) C(251) 1.496(3) ? C(26) C(261) 1.493(3) ? C(121) C(126) 1.388(3) ? C(121) C(122) 1.388(4) ? C(122) C(123) 1.387(4) ? C(123) C(124) 1.389(4) ? C(124) C(125) 1.376(5) ? C(124) C(127) 1.510(4) ? C(125) C(126) 1.390(4) ? C(131) C(136) 1.385(3) ? C(131) C(132) 1.397(4) ? C(132) C(133) 1.388(4) ? C(133) C(134) 1.380(4) ? C(134) C(135) 1.386(4) ? C(135) C(136) 1.388(4) ? C(151) C(152) 1.387(4) ? C(151) C(156) 1.388(3) ? C(152) C(153) 1.388(4) ? C(153) C(154) 1.366(5) ? C(154) C(155) 1.374(4) ? C(155) C(156) 1.390(4) ? C(161) C(166) 1.391(3) ? C(161) C(162) 1.395(3) ? C(162) C(163) 1.385(4) ? C(163) C(164) 1.388(4) ? C(164) C(165) 1.389(4) ? C(164) C(167) 1.503(4) ? C(165) C(166) 1.386(4) ? C(221) C(222) 1.388(3) ? C(221) C(226) 1.392(3) ? C(222) C(223) 1.391(3) ? C(223) C(224) 1.393(4) ? C(224) C(225) 1.388(4) ? C(224) C(227) 1.504(3) ? C(225) C(226) 1.387(3) ? C(231) C(232) 1.389(3) ? C(231) C(236) 1.397(3) ? C(232) C(233) 1.394(3) ? C(233) C(234) 1.385(4) ? C(234) C(235) 1.383(4) ? C(235) C(236) 1.389(4) ? C(251) C(252) 1.386(3) ? C(251) C(256) 1.393(3) ? C(252) C(253) 1.392(3) ? C(253) C(254) 1.378(4) ? C(254) C(255) 1.382(4) ? C(255) C(256) 1.383(4) ? C(261) C(266) 1.393(3) ? C(261) C(262) 1.394(3) ? C(262) C(263) 1.384(3) ? C(263) C(264) 1.387(4) ? C(264) C(265) 1.385(4) ? C(264) C(267) 1.512(4) ? C(265) C(266) 1.392(3) ? C(901) C(902) 1.368(6) ? C(901) C(906) 1.380(6) ? C(902) C(903) 1.347(6) ? C(903) C(904) 1.397(6) ? C(904) C(905) 1.373(7) ? C(905) C(906) 1.333(6) ? 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(10) Nb O(20) 104.00(7) ? O(10) Nb Cl(2) 102.05(6) ? O(20) Nb Cl(2) 92.54(5) ? O(10) Nb Cl(3) 102.33(6) ? O(20) Nb Cl(3) 84.34(5) ? Cl(2) Nb Cl(3) 155.45(3) ? O(10) Nb Cl(1) 101.12(6) ? O(20) Nb Cl(1) 154.37(5) ? Cl(2) Nb Cl(1) 87.11(3) ? Cl(3) Nb Cl(1) 85.45(4) ? C(11) O(10) Nb 179.64(16) ? C(21) O(20) Nb 152.50(15) ? O(10) C(11) C(12) 117.8(2) ? O(10) C(11) C(16) 117.6(2) ? C(12) C(11) C(16) 124.6(2) ? C(11) C(12) C(13) 117.4(2) ? C(11) C(12) C(121) 121.4(2) ? C(13) C(12) C(121) 121.2(2) ? C(14) C(13) C(12) 118.4(2) ? C(14) C(13) C(131) 119.4(2) ? C(12) C(13) C(131) 122.1(2) ? C(15) C(14) C(13) 123.1(2) ? C(14) C(15) C(16) 119.2(2) ? C(14) C(15) C(151) 119.2(2) ? C(16) C(15) C(151) 121.5(2) ? C(11) C(16) C(15) 116.9(2) ? C(11) C(16) C(161) 121.6(2) ? C(15) C(16) C(161) 121.5(2) ? O(20) C(21) C(22) 116.72(19) ? O(20) C(21) C(26) 119.42(19) ? C(22) C(21) C(26) 123.9(2) ? C(21) C(22) C(23) 117.91(19) ? C(21) C(22) C(221) 120.19(19) ? C(23) C(22) C(221) 121.88(19) ? C(24) C(23) C(22) 118.5(2) ? C(24) C(23) C(231) 118.0(2) ? C(22) C(23) C(231) 123.5(2) ? C(23) C(24) C(25) 123.5(2) ? C(24) C(25) C(26) 119.1(2) ? C(24) C(25) C(251) 117.60(19) ? C(26) C(25) C(251) 123.3(2) ? C(25) C(26) C(21) 117.10(19) ? C(25) C(26) C(261) 122.36(19) ? C(21) C(26) C(261) 120.34(19) ? C(126) C(121) C(122) 118.7(2) ? C(126) C(121) C(12) 120.8(2) ? C(122) C(121) C(12) 120.5(2) ? C(123) C(122) C(121) 120.6(3) ? C(122) C(123) C(124) 121.1(3) ? C(125) C(124) C(123) 117.8(3) ? C(125) C(124) C(127) 121.7(3) ? C(123) C(124) C(127) 120.5(3) ? C(124) C(125) C(126) 121.9(3) ? C(121) C(126) C(125) 119.9(3) ? C(136) C(131) C(132) 118.3(2) ? C(136) C(131) C(13) 122.5(2) ? C(132) C(131) C(13) 119.2(2) ? C(133) C(132) C(131) 121.0(3) ? C(134) C(133) C(132) 119.9(3) ? C(133) C(134) C(135) 119.8(3) ? C(134) C(135) C(136) 120.0(3) ? C(131) C(136) C(135) 121.0(3) ? C(152) C(151) C(156) 118.1(2) ? C(152) C(151) C(15) 118.6(2) ? C(156) C(151) C(15) 123.2(2) ? C(151) C(152) C(153) 121.1(3) ? C(154) C(153) C(152) 120.0(3) ? C(153) C(154) C(155) 119.8(3) ? C(154) C(155) C(156) 120.5(3) ? C(151) C(156) C(155) 120.3(3) ? C(166) C(161) C(162) 118.4(2) ? C(166) C(161) C(16) 119.5(2) ? C(162) C(161) C(16) 122.0(2) ? C(163) C(162) C(161) 120.1(3) ? C(162) C(163) C(164) 121.9(3) ? C(163) C(164) C(165) 117.5(3) ? C(163) C(164) C(167) 121.4(3) ? C(165) C(164) C(167) 121.1(3) ? C(166) C(165) C(164) 121.4(3) ? C(165) C(166) C(161) 120.7(2) ? C(222) C(221) C(226) 118.4(2) ? C(222) C(221) C(22) 120.7(2) ? C(226) C(221) C(22) 120.7(2) ? C(221) C(222) C(223) 120.7(2) ? C(222) C(223) C(224) 120.9(2) ? C(225) C(224) C(223) 118.0(2) ? C(225) C(224) C(227) 121.6(3) ? C(223) C(224) C(227) 120.4(3) ? C(226) C(225) C(224) 121.4(2) ? C(225) C(226) C(221) 120.5(2) ? C(232) C(231) C(236) 118.8(2) ? C(232) C(231) C(23) 119.5(2) ? C(236) C(231) C(23) 121.7(2) ? C(231) C(232) C(233) 120.7(2) ? C(234) C(233) C(232) 119.8(3) ? C(235) C(234) C(233) 119.9(2) ? C(234) C(235) C(236) 120.3(3) ? C(235) C(236) C(231) 120.4(3) ? C(252) C(251) C(256) 118.8(2) ? C(252) C(251) C(25) 122.3(2) ? C(256) C(251) C(25) 118.9(2) ? C(251) C(252) C(253) 120.2(3) ? C(254) C(253) C(252) 120.5(3) ? C(253) C(254) C(255) 119.7(3) ? C(254) C(255) C(256) 120.1(3) ? C(255) C(256) C(251) 120.8(3) ? C(266) C(261) C(262) 118.2(2) ? C(266) C(261) C(26) 121.5(2) ? C(262) C(261) C(26) 120.2(2) ? C(263) C(262) C(261) 120.6(2) ? C(262) C(263) C(264) 121.6(2) ? C(265) C(264) C(263) 117.8(2) ? C(265) C(264) C(267) 121.3(3) ? C(263) C(264) C(267) 120.9(3) ? C(264) C(265) C(266) 121.4(2) ? C(265) C(266) C(261) 120.4(2) ? C(902) C(901) C(906) 120.0(5) ? C(903) C(902) C(901) 119.9(4) ? C(902) C(903) C(904) 120.0(5) ? C(905) C(904) C(903) 119.1(4) ? C(906) C(905) C(904) 120.5(4) ? C(905) C(906) C(901) 120.4(5) ? #END==================================