Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #============================================================================== _journal_coden_Cambridge 186 _audit_creation_date 1-12-99 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 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 ? _publ_requested_coeditor_name ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; 23349 Schweiger, Scott W 23353 Tillison, Dana L loop_ _publ_author_name _publ_author_address 'Rothwell, Ian' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; 'Thorn, Matt G.' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; 'Fanwick, P.' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; 'Schweiger, Scott W.' ; ? ; 'Tillison, Dana L.' ; ? ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _database_code_CSD 'MTTA1Q' _publ_section_experimental ; ? ; _publ_section_references ; P. T. Beurskens, G. Admirall, G. Beurskens, W. P. Bosman S. Garcia-Granda, R. O. Gould, J. M. M. Smits, '& C. Smykalla (1992). The DIRDIF92 Program System, 'Technical Report. Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. 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). 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_MTTA1 _database_code_CSD 159025 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C6 H20 Cl4 N3 Ta' _chemical_formula_structural ? _chemical_formula_weight 457.01 _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 8.6567(3) _cell_length_b 17.9638(7) _cell_length_c 10.2052(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.121(2) _cell_angle_gamma 90.00 _cell_volume 1516.65(17) _cell_measurement_reflns_used 11510 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 2.00 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 7.852 _cell_measurement_temperature 173 _exptl_crystal_F_000 872 # 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 0.0594 _exptl_absorpt_correction_T_max 0.1154 _diffrn_reflns_number 11510 _reflns_number_total 3617 _reflns_number_gt 3302 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.85 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_max 12 # 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 0.041 _refine_ls_wR_factor_ref 0.107 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 3500 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+0.6264P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.78 _refine_diff_density_min -3.53 _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 0.26617(2) 0.122735(11) 0.217905(19) 0.02485(9) Uani ? Cl(1) 0.17610(19) 0.01042(8) 0.31701(15) 0.0405(4) Uani ? Cl(2) 0.52560(17) 0.10360(8) 0.40574(14) 0.0329(4) Uani ? Cl(3) 0.3697(2) 0.03699(9) 0.08361(15) 0.0443(5) Uani ? Cl(4) 0.18472(19) 0.19538(8) 0.38356(16) 0.0400(4) Uani ? N(1) 0.3684(6) 0.2043(3) 0.1478(5) 0.0352(13) Uani ? N(2) 0.0548(6) 0.1350(3) 0.0845(6) 0.0374(16) Uani ? N(9) 0.3797(6) 0.0618(3) 0.6555(5) 0.0392(13) Uani ? C(11) 0.2871(9) 0.2738(4) 0.0945(7) 0.049(2) Uani ? C(12) 0.5356(8) 0.2067(4) 0.1449(8) 0.053(2) Uani ? C(21) 0.0346(9) 0.1472(4) -0.0623(7) 0.049(2) Uani ? C(22) -0.1006(9) 0.1269(4) 0.1098(10) 0.056(3) Uani ? C(91) 0.2196(8) 0.0437(4) 0.6700(7) 0.050(2) Uani ? C(92) 0.4538(11) 0.1267(3) 0.7362(8) 0.053(3) Uani ? H(9A) 0.4455 0.0223 0.6820 0.0510 Uiso calc H(9B) 0.3697 0.0705 0.5665 0.0510 Uiso calc H(11A) 0.3322 0.3136 0.1568 0.0640 Uiso calc H(11B) 0.1738 0.2694 0.0850 0.0640 Uiso calc H(11C) 0.3018 0.2843 0.0067 0.0640 Uiso calc H(12A) 0.5380 0.2135 0.0522 0.0690 Uiso calc H(12B) 0.5884 0.1608 0.1802 0.0690 Uiso calc H(12C) 0.5907 0.2473 0.2004 0.0690 Uiso calc H(21A) -0.0025 0.1021 -0.1120 0.0640 Uiso calc H(21B) 0.1363 0.1615 -0.0746 0.0640 Uiso calc H(21C) -0.0432 0.1860 -0.0960 0.0640 Uiso calc H(22A) -0.1644 0.1707 0.0790 0.0720 Uiso calc H(22B) -0.0845 0.1203 0.2063 0.0720 Uiso calc H(22C) -0.1557 0.0843 0.0611 0.0720 Uiso calc H(91A) 0.2303 0.0317 0.7639 0.0650 Uiso calc H(91B) 0.1751 0.0018 0.6129 0.0650 Uiso calc H(91C) 0.1491 0.0858 0.6427 0.0650 Uiso calc H(92A) 0.3885 0.1699 0.7037 0.0680 Uiso calc H(92B) 0.5599 0.1344 0.7271 0.0680 Uiso calc H(92C) 0.4618 0.1185 0.8309 0.0680 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 0.02777(16) 0.02709(16) 0.02106(16) 0.00596(7) 0.00932(10) 0.00041(7) Cl(1) 0.0482(8) 0.0325(7) 0.0382(7) -0.0085(6) 0.0087(6) 0.0036(6) Cl(2) 0.0307(7) 0.0357(6) 0.0289(6) 0.0006(5) 0.0037(5) -0.0001(5) Cl(3) 0.0510(9) 0.0525(9) 0.0289(7) 0.0237(7) 0.0108(6) -0.0065(6) Cl(4) 0.0531(9) 0.0362(7) 0.0380(7) 0.0057(6) 0.0247(7) -0.0063(6) N(1) 0.035(2) 0.042(3) 0.032(2) 0.004(2) 0.015(2) 0.013(2) N(2) 0.032(3) 0.041(3) 0.039(3) 0.009(2) 0.010(2) -0.003(2) N(9) 0.057(3) 0.031(2) 0.032(2) 0.005(2) 0.017(2) 0.001(2) C(11) 0.066(4) 0.034(3) 0.046(4) 0.002(3) 0.013(3) 0.011(3) C(12) 0.047(4) 0.064(4) 0.054(4) -0.001(3) 0.025(3) 0.022(3) C(21) 0.050(4) 0.060(4) 0.030(3) 0.017(3) -0.001(3) -0.004(3) C(22) 0.035(4) 0.063(5) 0.066(5) 0.006(3) 0.010(4) 0.013(4) C(91) 0.058(4) 0.055(4) 0.042(4) 0.001(3) 0.024(3) -0.003(3) C(92) 0.076(6) 0.041(4) 0.040(4) -0.010(3) 0.016(4) -0.003(3) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ta N(2) 1.945(5) ? Ta N(1) 1.954(5) ? Ta Cl(4) 2.4000(14) ? Ta Cl(3) 2.4038(14) ? Ta Cl(1) 2.4831(14) ? Ta Cl(2) 2.5103(14) ? N(1) C(12) 1.457(8) ? N(1) C(11) 1.457(8) ? N(2) C(22) 1.450(9) ? N(2) C(21) 1.473(9) ? N(9) C(92) 1.463(8) ? N(9) C(91) 1.473(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 N(2) Ta N(1) 95.3(2) ? N(2) Ta Cl(4) 91.17(16) ? N(1) Ta Cl(4) 96.24(15) ? N(2) Ta Cl(3) 96.06(16) ? N(1) Ta Cl(3) 89.24(16) ? Cl(4) Ta Cl(3) 170.50(5) ? N(2) Ta Cl(1) 91.95(17) ? N(1) Ta Cl(1) 171.58(15) ? Cl(4) Ta Cl(1) 87.84(5) ? Cl(3) Ta Cl(1) 85.76(6) ? N(2) Ta Cl(2) 174.73(17) ? N(1) Ta Cl(2) 88.99(14) ? Cl(4) Ta Cl(2) 85.35(5) ? Cl(3) Ta Cl(2) 87.00(5) ? Cl(1) Ta Cl(2) 83.99(5) ? C(12) N(1) C(11) 110.0(5) ? C(12) N(1) Ta 126.1(4) ? C(11) N(1) Ta 123.9(4) ? C(22) N(2) C(21) 110.9(6) ? C(22) N(2) Ta 126.5(5) ? C(21) N(2) Ta 122.3(4) ? C(92) N(9) C(91) 112.9(6) ? #===END #============================================================================== data_MT23I _database_code_CSD 159026 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C14 H22 Cl6 N4 O Ta2' _chemical_formula_structural ? _chemical_formula_weight 836.97 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.9310(6) _cell_length_b 14.3050(4) _cell_length_c 14.3949(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2456.8(3) _cell_measurement_reflns_used 14852 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 2.26 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 9.472 _cell_measurement_temperature 173 _exptl_crystal_F_000 1560 # 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 0.1883 _exptl_absorpt_correction_T_max 0.4914 _diffrn_reflns_number 14852 _reflns_number_total 5573 _reflns_number_gt 5011 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.094 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 17 _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 0.045 _refine_ls_wR_factor_ref 0.107 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 4901 _refine_ls_d_res_high 0.80 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.38 _refine_diff_density_min -2.34 _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, 2424' _refine_ls_abs_structure_Flack -0.012(17) # 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(1) 0.79137(4) 0.79746(4) 0.82674(3) 0.02400(14) Uani ? Ta(2) 0.65387(4) 0.70347(4) 0.60743(3) 0.02320(12) Uani ? Cl(11) 0.9703(3) 0.7602(2) 0.7655(3) 0.0366(9) Uani ? Cl(12) 0.8835(3) 0.8911(2) 0.9404(2) 0.0414(10) Uani ? Cl(13) 0.6149(3) 0.8607(2) 0.8760(2) 0.0353(9) Uani ? Cl(21) 0.8276(3) 0.6999(3) 0.5293(2) 0.0394(9) Uani ? Cl(22) 0.5817(3) 0.6085(2) 0.4854(3) 0.0421(10) Uani ? Cl(23) 0.4834(3) 0.6800(2) 0.6904(3) 0.0361(9) Uani ? O 0.7189(7) 0.7502(5) 0.7209(6) 0.026(2) Uani ? N(1) 0.7784(9) 0.6875(7) 0.9029(8) 0.034(3) Uani ? N(2) 0.6109(9) 0.8222(7) 0.5556(7) 0.029(3) Uani ? N(11) 0.8059(9) 0.9365(6) 0.7355(7) 0.025(3) Uani ? N(21) 0.7109(8) 0.5585(6) 0.6702(8) 0.027(3) Uani ? C(12) 0.7705(12) 1.0195(8) 0.7673(9) 0.033(4) Uani ? C(13) 0.7751(12) 1.1015(8) 0.7164(11) 0.039(4) Uani ? C(14) 0.8194(13) 1.0960(10) 0.6252(11) 0.044(4) Uani ? C(15) 0.8531(11) 1.0089(8) 0.5921(9) 0.033(4) Uani ? C(16) 0.8439(11) 0.9316(9) 0.6484(9) 0.032(3) Uani ? C(22) 0.6422(11) 0.4854(8) 0.6812(9) 0.028(3) Uani ? C(23) 0.6716(12) 0.4053(9) 0.7234(10) 0.038(4) Uani ? C(24) 0.7779(12) 0.3944(9) 0.7584(11) 0.042(4) Uani ? C(25) 0.8484(14) 0.4667(9) 0.7443(13) 0.051(5) Uani ? C(26) 0.8154(12) 0.5459(9) 0.7029(11) 0.037(4) Uani ? C(101) 0.8642(16) 0.6640(11) 0.9737(12) 0.062(6) Uani ? C(102) 0.6769(13) 0.6264(9) 0.9018(13) 0.052(5) Uani ? C(201) 0.5638(10) 0.9003(9) 0.6101(9) 0.030(4) Uani ? C(202) 0.6210(13) 0.8476(9) 0.4545(10) 0.040(4) Uani ? H(12) 0.7412 1.0222 0.8271 0.0430 Uiso calc H(13) 0.7502 1.1579 0.7410 0.0510 Uiso calc H(14) 0.8258 1.1491 0.5884 0.0580 Uiso calc H(15) 0.8816 1.0030 0.5322 0.0430 Uiso calc H(16) 0.8651 0.8736 0.6249 0.0410 Uiso calc H(22) 0.5696 0.4904 0.6581 0.0370 Uiso calc H(23) 0.6197 0.3571 0.7290 0.0500 Uiso calc H(24) 0.7999 0.3405 0.7898 0.0540 Uiso calc H(25) 0.9224 0.4614 0.7640 0.0670 Uiso calc H(26) 0.8670 0.5943 0.6964 0.0480 Uiso calc H(10A) 0.8378 0.6822 1.0341 0.0800 Uiso calc H(10B) 0.9325 0.6966 0.9600 0.0800 Uiso calc H(10C) 0.8778 0.5978 0.9730 0.0800 Uiso calc H(10D) 0.6988 0.5630 0.8894 0.0670 Uiso calc H(10E) 0.6264 0.6473 0.8542 0.0670 Uiso calc H(10F) 0.6401 0.6294 0.9611 0.0670 Uiso calc H(20A) 0.5884 0.9586 0.5840 0.0390 Uiso calc H(20B) 0.5889 0.8957 0.6733 0.0390 Uiso calc H(20C) 0.4834 0.8973 0.6083 0.0390 Uiso calc H(20D) 0.5491 0.8666 0.4314 0.0520 Uiso calc H(20E) 0.6470 0.7943 0.4201 0.0520 Uiso calc H(20F) 0.6734 0.8980 0.4477 0.0520 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(1) 0.0256(3) 0.0230(2) 0.0234(3) 0.0001(2) -0.0026(2) -0.0003(2) Ta(2) 0.0241(2) 0.0210(2) 0.0245(3) -0.0020(2) -0.0011(2) -0.0014(2) Cl(11) 0.0201(15) 0.0336(16) 0.056(2) 0.0000(12) 0.0001(15) -0.0023(15) Cl(12) 0.047(2) 0.0413(18) 0.036(2) 0.0009(16) -0.0157(16) -0.0095(16) Cl(13) 0.0331(17) 0.0370(17) 0.0358(19) 0.0063(14) 0.0071(15) -0.0043(14) Cl(21) 0.0369(17) 0.0412(17) 0.0401(18) -0.0010(17) 0.0157(14) -0.0047(17) Cl(22) 0.056(2) 0.0322(17) 0.038(2) -0.0036(16) -0.0168(18) -0.0080(15) Cl(23) 0.0242(15) 0.0351(18) 0.049(2) -0.0021(12) 0.0099(15) 0.0035(14) O 0.023(4) 0.020(4) 0.034(5) -0.006(3) 0.001(4) -0.001(3) N(1) 0.036(6) 0.032(6) 0.035(6) -0.001(5) 0.007(5) 0.004(5) N(2) 0.030(6) 0.036(6) 0.020(5) -0.005(4) -0.002(5) 0.006(4) N(11) 0.031(6) 0.022(5) 0.021(5) 0.000(4) -0.001(5) 0.001(4) N(21) 0.023(5) 0.020(5) 0.039(6) 0.000(4) -0.002(6) -0.004(4) C(12) 0.048(9) 0.026(6) 0.025(7) -0.001(6) 0.006(7) -0.004(5) C(13) 0.033(8) 0.017(6) 0.068(10) -0.006(6) -0.004(7) 0.007(6) C(14) 0.044(9) 0.047(9) 0.042(9) -0.003(7) 0.001(7) 0.010(7) C(15) 0.037(7) 0.029(7) 0.032(8) 0.006(6) 0.011(6) 0.008(5) C(16) 0.024(7) 0.039(7) 0.032(7) -0.001(6) 0.006(6) -0.015(6) C(22) 0.031(7) 0.026(6) 0.028(7) 0.004(5) -0.015(6) -0.003(5) C(23) 0.044(8) 0.035(7) 0.035(8) 0.006(6) -0.003(7) -0.003(6) C(24) 0.042(9) 0.027(7) 0.057(10) 0.009(7) -0.016(8) 0.001(7) C(25) 0.041(9) 0.023(7) 0.089(14) 0.007(7) -0.009(10) 0.008(7) C(26) 0.032(8) 0.030(7) 0.048(9) -0.001(6) -0.004(6) 0.001(6) C(101) 0.083(14) 0.047(9) 0.056(11) 0.015(9) -0.013(10) 0.022(8) C(102) 0.049(10) 0.032(8) 0.074(12) -0.012(7) 0.002(9) 0.012(8) C(201) 0.019(6) 0.036(7) 0.036(8) 0.001(5) -0.007(6) 0.001(6) C(202) 0.048(9) 0.038(7) 0.033(8) -0.002(7) -0.003(7) 0.011(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(1) O 1.877(9) ? Ta(1) N(1) 1.924(10) ? Ta(1) Cl(11) 2.370(3) ? Ta(1) Cl(12) 2.383(3) ? Ta(1) N(11) 2.389(9) ? Ta(1) Cl(13) 2.399(3) ? Ta(2) N(2) 1.924(10) ? Ta(2) O 1.929(9) ? Ta(2) Cl(21) 2.358(3) ? Ta(2) N(21) 2.363(10) ? Ta(2) Cl(23) 2.382(3) ? Ta(2) Cl(22) 2.382(3) ? N(1) C(101) 1.483(19) ? N(1) C(102) 1.495(17) ? N(2) C(201) 1.477(16) ? N(2) C(202) 1.504(16) ? N(11) C(16) 1.336(16) ? N(11) C(12) 1.341(15) ? N(21) C(22) 1.337(15) ? N(21) C(26) 1.345(17) ? C(12) C(13) 1.384(17) ? C(13) C(14) 1.42(2) ? C(14) C(15) 1.393(19) ? C(15) C(16) 1.376(18) ? C(22) C(23) 1.345(17) ? C(23) C(24) 1.374(19) ? C(24) C(25) 1.349(19) ? C(25) C(26) 1.340(18) ? 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 Ta(1) N(1) 97.6(4) ? O Ta(1) Cl(11) 91.8(3) ? N(1) Ta(1) Cl(11) 95.8(3) ? O Ta(1) Cl(12) 166.4(2) ? N(1) Ta(1) Cl(12) 96.0(3) ? Cl(11) Ta(1) Cl(12) 88.08(13) ? O Ta(1) N(11) 83.5(3) ? N(1) Ta(1) N(11) 178.5(4) ? Cl(11) Ta(1) N(11) 85.3(3) ? Cl(12) Ta(1) N(11) 82.9(3) ? O Ta(1) Cl(13) 88.4(3) ? N(1) Ta(1) Cl(13) 94.0(3) ? Cl(11) Ta(1) Cl(13) 170.16(12) ? Cl(12) Ta(1) Cl(13) 89.42(13) ? N(11) Ta(1) Cl(13) 85.0(3) ? N(2) Ta(2) O 97.5(4) ? N(2) Ta(2) Cl(21) 93.9(3) ? O Ta(2) Cl(21) 93.3(3) ? N(2) Ta(2) N(21) 178.7(4) ? O Ta(2) N(21) 82.2(3) ? Cl(21) Ta(2) N(21) 84.9(3) ? N(2) Ta(2) Cl(23) 95.2(3) ? O Ta(2) Cl(23) 88.1(3) ? Cl(21) Ta(2) Cl(23) 170.46(12) ? N(21) Ta(2) Cl(23) 86.0(3) ? N(2) Ta(2) Cl(22) 96.9(3) ? O Ta(2) Cl(22) 165.5(2) ? Cl(21) Ta(2) Cl(22) 87.33(13) ? N(21) Ta(2) Cl(22) 83.4(3) ? Cl(23) Ta(2) Cl(22) 88.90(13) ? Ta(1) O Ta(2) 176.0(5) ? C(101) N(1) C(102) 115.7(12) ? C(101) N(1) Ta(1) 121.5(9) ? C(102) N(1) Ta(1) 122.5(9) ? C(201) N(2) C(202) 111.2(10) ? C(201) N(2) Ta(2) 124.3(8) ? C(202) N(2) Ta(2) 124.6(8) ? C(16) N(11) C(12) 118.3(11) ? C(16) N(11) Ta(1) 119.8(8) ? C(12) N(11) Ta(1) 121.8(8) ? C(22) N(21) C(26) 115.1(10) ? C(22) N(21) Ta(2) 123.7(8) ? C(26) N(21) Ta(2) 121.2(8) ? N(11) C(12) C(13) 123.9(13) ? C(12) C(13) C(14) 117.2(13) ? C(15) C(14) C(13) 118.3(13) ? C(16) C(15) C(14) 119.6(12) ? N(11) C(16) C(15) 122.6(12) ? N(21) C(22) C(23) 124.0(12) ? C(22) C(23) C(24) 120.3(14) ? C(25) C(24) C(23) 115.7(13) ? C(26) C(25) C(24) 122.2(15) ? C(25) C(26) N(21) 122.7(13) ? #===END #============================================================================== data_MT26I _database_code_CSD 159027 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C15 H21 Cl3 N3 Ta' _chemical_formula_structural ? _chemical_formula_weight 530.66 _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 19.1788(7) _cell_length_b 7.2144(4) _cell_length_c 14.3129(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.191(3) _cell_angle_gamma 90.00 _cell_volume 1919.9(3) _cell_measurement_reflns_used 14249 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.84 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 6.080 _cell_measurement_temperature 173 _exptl_crystal_F_000 1024 # 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 0.3723 _exptl_absorpt_correction_T_max 0.6338 _diffrn_reflns_number 14249 _reflns_number_total 4625 _reflns_number_gt 3872 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_max 22 # 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 0.037 _refine_ls_wR_factor_ref 0.085 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 4305 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.1492P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.80 _refine_diff_density_min -1.73 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.37E-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 0.170709(11) 0.17179(3) 0.234927(15) 0.02273(8) Uani ? Cl(1) 0.27064(8) 0.3117(2) 0.18789(12) 0.0360(5) Uani ? Cl(2) 0.18715(9) -0.0842(2) 0.13072(12) 0.0403(5) Uani ? Cl(3) 0.09115(8) -0.0186(2) 0.29651(12) 0.0380(4) Uani ? N(1) 0.2608(2) 0.0136(7) 0.3504(3) 0.0249(13) Uani ? N(2) 0.1796(3) 0.3653(7) 0.3324(4) 0.0325(14) Uani ? N(3) 0.0944(3) 0.2904(7) 0.1399(4) 0.0315(14) Uani ? C(2) 0.2554(3) -0.0153(9) 0.4415(4) 0.0273(16) Uani ? C(3) 0.3059(3) -0.1109(9) 0.5093(4) 0.0301(16) Uani ? C(4) 0.3670(3) -0.1798(7) 0.4856(4) 0.0248(16) Uani ? C(5) 0.3740(3) -0.1455(8) 0.3925(4) 0.0268(16) Uani ? C(6) 0.3203(3) -0.0521(8) 0.3284(4) 0.0296(18) Uani ? C(7) 0.4217(3) -0.2865(9) 0.5553(4) 0.0275(16) Uani ? C(8) 0.4004(4) -0.4159(10) 0.6153(5) 0.037(2) Uani ? C(9) 0.4520(5) -0.5135(12) 0.6817(5) 0.056(3) Uani ? C(10) 0.5234(4) -0.4886(12) 0.6887(5) 0.053(2) Uani ? C(11) 0.5455(4) -0.3646(11) 0.6299(6) 0.049(2) Uani ? C(12) 0.4944(3) -0.2669(9) 0.5625(5) 0.0361(18) Uani ? C(21) 0.2445(4) 0.4501(12) 0.3932(6) 0.055(2) Uani ? C(22) 0.1144(4) 0.4414(10) 0.3553(5) 0.046(2) Uani ? C(31) 0.0885(3) 0.4905(9) 0.1218(5) 0.043(2) Uani ? C(32) 0.0339(4) 0.1915(11) 0.0768(5) 0.045(2) Uani ? H(2) 0.2155 0.0320 0.4594 0.0350 Uiso calc H(3) 0.2991 -0.1294 0.5708 0.0400 Uiso calc H(5) 0.4146 -0.1855 0.3738 0.0350 Uiso calc H(6) 0.3255 -0.0334 0.2661 0.0380 Uiso calc H(8) 0.3518 -0.4365 0.6107 0.0480 Uiso calc H(9) 0.4376 -0.5978 0.7224 0.0730 Uiso calc H(10) 0.5571 -0.5560 0.7336 0.0690 Uiso calc H(11) 0.5943 -0.3458 0.6349 0.0640 Uiso calc H(12) 0.5096 -0.1860 0.5209 0.0470 Uiso calc H(21A) 0.2441 0.5808 0.3807 0.0710 Uiso calc H(21B) 0.2863 0.3952 0.3789 0.0710 Uiso calc H(21C) 0.2455 0.4297 0.4598 0.0710 Uiso calc H(22A) 0.1171 0.4239 0.4226 0.0590 Uiso calc H(22B) 0.0728 0.3786 0.3177 0.0590 Uiso calc H(22C) 0.1109 0.5714 0.3405 0.0590 Uiso calc H(31A) 0.0910 0.5150 0.0567 0.0560 Uiso calc H(31B) 0.1272 0.5531 0.1656 0.0560 Uiso calc H(31C) 0.0434 0.5344 0.1310 0.0560 Uiso calc H(32A) -0.0103 0.2315 0.0904 0.0590 Uiso calc H(32B) 0.0397 0.0605 0.0880 0.0590 Uiso calc H(32C) 0.0328 0.2178 0.0107 0.0590 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 0.02024(16) 0.02156(15) 0.02583(15) -0.00044(8) 0.00460(9) 0.00171(9) Cl(1) 0.0273(8) 0.0379(9) 0.0454(9) -0.0007(6) 0.0141(6) 0.0137(7) Cl(2) 0.0463(9) 0.0370(9) 0.0365(8) 0.0033(7) 0.0079(7) -0.0097(7) Cl(3) 0.0275(7) 0.0393(9) 0.0478(9) -0.0066(6) 0.0103(6) 0.0115(7) N(1) 0.024(2) 0.026(3) 0.025(2) 0.0043(19) 0.0068(18) 0.001(2) N(2) 0.022(2) 0.031(3) 0.044(3) -0.002(2) 0.007(2) -0.008(2) N(3) 0.021(2) 0.038(3) 0.034(3) -0.001(2) 0.004(2) 0.008(2) C(2) 0.023(3) 0.034(3) 0.027(3) 0.007(2) 0.010(2) -0.001(3) C(3) 0.033(3) 0.035(3) 0.023(3) 0.005(3) 0.008(2) -0.001(2) C(4) 0.025(3) 0.018(3) 0.030(3) 0.002(2) 0.004(2) -0.002(2) C(5) 0.020(3) 0.027(3) 0.036(3) 0.004(2) 0.012(2) 0.005(2) C(6) 0.028(3) 0.037(4) 0.026(3) 0.007(2) 0.011(2) 0.004(2) C(7) 0.026(3) 0.034(3) 0.021(3) 0.007(2) 0.003(2) -0.005(2) C(8) 0.039(4) 0.043(4) 0.033(3) 0.010(3) 0.016(3) 0.006(3) C(9) 0.078(6) 0.058(5) 0.034(4) 0.033(4) 0.020(4) 0.023(4) C(10) 0.055(5) 0.059(5) 0.037(4) 0.037(4) -0.005(3) -0.004(4) C(11) 0.026(3) 0.060(5) 0.054(5) 0.011(3) -0.006(3) -0.022(4) C(12) 0.031(3) 0.031(3) 0.044(4) 0.001(3) 0.005(3) -0.008(3) C(21) 0.032(4) 0.060(5) 0.069(5) -0.009(3) 0.006(3) -0.032(4) C(22) 0.042(4) 0.039(4) 0.058(5) 0.010(3) 0.017(3) -0.014(3) C(31) 0.032(3) 0.031(4) 0.059(4) 0.003(3) 0.000(3) 0.019(3) C(32) 0.032(4) 0.057(5) 0.038(4) 0.004(3) -0.006(3) -0.001(3) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ta N(3) 1.936(5) ? Ta N(2) 1.951(5) ? Ta N(1) 2.371(4) ? Ta Cl(3) 2.3771(14) ? Ta Cl(1) 2.4036(14) ? Ta Cl(2) 2.4423(16) ? N(1) C(6) 1.342(7) ? N(1) C(2) 1.349(7) ? N(2) C(21) 1.465(8) ? N(2) C(22) 1.475(8) ? N(3) C(31) 1.466(8) ? N(3) C(32) 1.470(8) ? C(2) C(3) 1.376(8) ? C(3) C(4) 1.391(8) ? C(4) C(5) 1.393(8) ? C(4) C(7) 1.475(8) ? C(5) C(6) 1.376(8) ? C(7) C(12) 1.379(8) ? C(7) C(8) 1.397(9) ? C(8) C(9) 1.385(9) ? C(9) C(10) 1.359(11) ? C(10) C(11) 1.366(12) ? C(11) C(12) 1.387(10) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N(3) Ta N(2) 96.0(2) ? N(3) Ta N(1) 177.30(19) ? N(2) Ta N(1) 85.67(19) ? N(3) Ta Cl(3) 94.16(15) ? N(2) Ta Cl(3) 95.73(16) ? N(1) Ta Cl(3) 83.56(11) ? N(3) Ta Cl(1) 97.75(15) ? N(2) Ta Cl(1) 87.92(15) ? N(1) Ta Cl(1) 84.39(11) ? Cl(3) Ta Cl(1) 167.11(5) ? N(3) Ta Cl(2) 95.38(17) ? N(2) Ta Cl(2) 167.36(15) ? N(1) Ta Cl(2) 83.15(12) ? Cl(3) Ta Cl(2) 88.87(6) ? Cl(1) Ta Cl(2) 85.14(6) ? C(6) N(1) C(2) 116.4(5) ? C(6) N(1) Ta 121.5(4) ? C(2) N(1) Ta 122.2(3) ? C(21) N(2) C(22) 110.8(5) ? C(21) N(2) Ta 129.5(4) ? C(22) N(2) Ta 119.7(4) ? C(31) N(3) C(32) 110.7(5) ? C(31) N(3) Ta 124.9(4) ? C(32) N(3) Ta 124.4(4) ? N(1) C(2) C(3) 123.5(5) ? C(2) C(3) C(4) 119.7(5) ? C(3) C(4) C(5) 117.0(5) ? C(3) C(4) C(7) 121.6(5) ? C(5) C(4) C(7) 121.3(5) ? C(6) C(5) C(4) 119.6(5) ? N(1) C(6) C(5) 123.8(5) ? C(12) C(7) C(8) 117.8(6) ? C(12) C(7) C(4) 122.4(6) ? C(8) C(7) C(4) 119.8(5) ? C(9) C(8) C(7) 119.6(6) ? C(10) C(9) C(8) 121.4(7) ? C(9) C(10) C(11) 120.1(7) ? C(10) C(11) C(12) 119.2(7) ? C(7) C(12) C(11) 121.9(7) ? #===END data_DTP22 _database_code_CSD 159028 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C97 H83 Cl2 N2 Nb1 O2' _chemical_formula_structural ? _chemical_formula_weight 1472.57 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 30.4539(2) _cell_length_b 22.0854(4) _cell_length_c 11.4593(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7707.4(5) _cell_measurement_reflns_used 37476 _cell_measurement_theta_min 5 _cell_measurement_theta_max 24 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.27 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.268 _cell_measurement_temperature 150 _exptl_crystal_F_000 3080 # 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 0.6883 _exptl_absorpt_correction_T_max 0.9735 _diffrn_reflns_number 37476 _reflns_number_total 12717 _reflns_Friedl_coverage 0.9202 _reflns_number_gt 10602 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.127 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 24.73 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_max 13 # 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 0.058 _refine_ls_wR_factor_ref 0.095 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 12716 _refine_ls_number_parameters 940 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.30 _refine_diff_density_min -0.41 _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 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) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(4) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Nb 0.018322(14) 0.219880(16) 0.01443(4) 0.01958(10) Uani ? Cl(1) -0.02664(5) 0.21897(5) -0.15698(10) 0.0292(4) Uani ? Cl(2) 0.05359(5) 0.22733(5) 0.20004(10) 0.0273(4) Uani ? O(1) 0.03971(11) 0.29917(12) -0.0267(2) 0.0205(9) Uani ? O(2) -0.01237(11) 0.14973(13) 0.0686(2) 0.0204(9) Uani ? N(31) 0.06536(14) 0.17535(17) -0.0596(3) 0.0230(12) Uani ? N(41) -0.04038(15) 0.27499(17) 0.1039(3) 0.0233(12) Uani ? C(11) 0.05162(18) 0.35862(19) -0.0161(4) 0.0220(14) Uani ? C(12) 0.09395(16) 0.37138(18) 0.0299(4) 0.0193(14) Uani ? C(13) 0.10551(17) 0.4327(2) 0.0468(4) 0.0220(15) Uani ? C(14) 0.07596(16) 0.47769(19) 0.0190(5) 0.0260(12) Uani ? C(15) 0.03494(17) 0.4653(2) -0.0287(4) 0.0227(14) Uani ? C(16) 0.02222(19) 0.4050(2) -0.0469(4) 0.0213(14) Uani ? C(21) -0.04901(17) 0.11475(19) 0.0850(4) 0.0177(14) Uani ? C(22) -0.07198(16) 0.11765(19) 0.1915(4) 0.0190(12) Uani ? C(23) -0.11171(17) 0.0863(2) 0.2024(4) 0.0210(12) Uani ? C(24) -0.12757(18) 0.0529(2) 0.1086(4) 0.0237(15) Uani ? C(25) -0.10393(15) 0.04699(17) 0.0047(4) 0.0180(12) Uani ? C(26) -0.06415(17) 0.07751(18) -0.0094(3) 0.0183(14) Uani ? C(31) 0.08794(18) 0.1234(2) -0.0058(5) 0.0337(17) Uani ? C(32) 0.0834(2) 0.1895(2) -0.1756(4) 0.0353(17) Uani ? C(42) -0.03231(19) 0.3174(2) 0.1858(4) 0.0290(17) Uani ? C(43) -0.0644(2) 0.3499(2) 0.2428(5) 0.0350(19) Uani ? C(44) -0.1071(2) 0.3398(2) 0.2141(5) 0.0413(19) Uani ? C(45) -0.1172(2) 0.2973(2) 0.1285(5) 0.0357(18) Uani ? C(46) -0.08284(19) 0.2659(2) 0.0765(4) 0.0320(17) Uani ? C(121) 0.12616(17) 0.3225(2) 0.0622(4) 0.0223(15) Uani ? C(122) 0.14301(19) 0.2849(2) -0.0216(5) 0.0370(17) Uani ? C(123) 0.17506(18) 0.2422(2) 0.0085(8) 0.0453(19) Uani ? C(124) 0.1889(2) 0.2374(3) 0.1198(7) 0.052(2) Uani ? C(125) 0.1723(2) 0.2741(3) 0.2057(6) 0.049(2) Uani ? C(126) 0.14080(18) 0.3173(2) 0.1766(5) 0.0317(17) Uani ? C(131) 0.14988(19) 0.4507(2) 0.0906(4) 0.0253(16) Uani ? C(132) 0.18815(19) 0.4342(2) 0.0353(5) 0.0323(17) Uani ? C(133) 0.2291(2) 0.4537(2) 0.0734(5) 0.0440(18) Uani ? C(134) 0.2316(2) 0.4906(2) 0.1727(6) 0.0447(18) Uani ? C(135) 0.1935(2) 0.5066(2) 0.2298(5) 0.0407(18) Uani ? C(136) 0.15332(19) 0.4876(2) 0.1900(5) 0.0330(17) Uani ? C(151) 0.00687(17) 0.5187(2) -0.0589(4) 0.0243(15) Uani ? C(152) 0.00425(16) 0.56720(18) 0.0186(5) 0.0300(12) Uani ? C(153) -0.0194(2) 0.6188(2) -0.0092(4) 0.0400(18) Uani ? C(154) -0.04090(19) 0.6236(2) -0.1148(4) 0.0333(17) Uani ? C(155) -0.03837(19) 0.5763(2) -0.1924(4) 0.0327(17) Uani ? C(156) -0.01478(19) 0.5248(2) -0.1661(4) 0.0297(17) Uani ? C(161) -0.0216(2) 0.3897(2) -0.0990(4) 0.0253(17) Uani ? C(162) -0.06002(19) 0.4085(2) -0.0455(4) 0.0303(17) Uani ? C(163) -0.1002(2) 0.3984(2) -0.0985(5) 0.0410(18) Uani ? C(164) -0.1028(2) 0.3699(2) -0.2055(5) 0.042(2) Uani ? C(165) -0.0646(2) 0.3504(2) -0.2595(5) 0.040(2) Uani ? C(166) -0.0238(2) 0.3608(2) -0.2053(4) 0.0307(17) Uani ? C(221) -0.05316(17) 0.1511(2) 0.2923(4) 0.0193(14) Uani ? C(222) -0.07628(18) 0.1971(2) 0.3481(4) 0.0270(17) Uani ? C(223) -0.0600(2) 0.2240(2) 0.4484(4) 0.0340(17) Uani ? C(224) -0.0207(2) 0.2053(2) 0.4955(4) 0.0333(17) Uani ? C(225) 0.0026(2) 0.1605(2) 0.4398(4) 0.0303(17) Uani ? C(226) -0.01299(18) 0.1339(2) 0.3390(4) 0.0243(16) Uani ? C(231) -0.13864(19) 0.0858(2) 0.3125(4) 0.0247(17) Uani ? C(232) -0.1828(2) 0.0996(2) 0.3088(4) 0.0333(17) Uani ? C(233) -0.2085(2) 0.0955(2) 0.4089(5) 0.043(2) Uani ? C(234) -0.1896(2) 0.0772(2) 0.5123(6) 0.0490(19) Uani ? C(235) -0.1458(2) 0.0626(2) 0.5171(6) 0.0460(19) Uani ? C(236) -0.1205(2) 0.0674(2) 0.4188(4) 0.0303(17) Uani ? C(251) -0.12249(18) 0.0055(2) -0.0858(4) 0.0223(15) Uani ? C(252) -0.16420(19) 0.0148(2) -0.1303(4) 0.0287(17) Uani ? C(253) -0.1823(2) -0.0250(2) -0.2107(5) 0.0367(17) Uani ? C(254) -0.1586(2) -0.0744(2) -0.2473(4) 0.0363(19) Uani ? C(255) -0.1174(2) -0.0848(2) -0.2061(4) 0.0337(17) Uani ? C(256) -0.0988(2) -0.0448(2) -0.1249(4) 0.0310(17) Uani ? C(261) -0.03728(18) 0.06810(19) -0.1179(4) 0.0207(16) Uani ? C(262) 0.00477(19) 0.0454(2) -0.1113(4) 0.0247(17) Uani ? C(263) 0.02862(19) 0.0338(2) -0.2124(4) 0.0330(17) Uani ? C(264) 0.0101(2) 0.0451(2) -0.3203(4) 0.0347(17) Uani ? C(265) -0.03217(19) 0.0684(2) -0.3272(4) 0.0293(17) Uani ? C(266) -0.05594(19) 0.0789(2) -0.2271(4) 0.0250(17) Uani ? C(901) 0.7701(3) 0.3806(3) 0.9779(7) 0.071(3) Uani ? C(902) 0.7344(3) 0.4184(3) 0.9824(7) 0.074(3) Uani ? C(903) 0.7054(3) 0.4196(3) 0.8880(8) 0.074(3) Uani ? C(904) 0.7128(3) 0.3823(3) 0.7945(7) 0.070(3) Uani ? C(905) 0.7477(3) 0.3439(3) 0.7926(7) 0.069(3) Uani ? C(906) 0.7763(3) 0.3425(3) 0.8864(8) 0.076(3) Uani ? C(911) 0.3288(2) 0.1918(3) 0.5133(7) 0.061(2) Uani ? C(912) 0.3134(2) 0.1336(3) 0.5062(7) 0.065(2) Uani ? C(913) 0.2860(3) 0.1173(3) 0.4200(6) 0.065(3) Uani ? C(914) 0.2733(3) 0.1586(4) 0.3376(6) 0.070(3) Uani ? C(915) 0.2883(2) 0.2178(4) 0.3458(7) 0.069(2) Uani ? C(916) 0.3163(2) 0.2332(3) 0.4342(6) 0.055(2) Uani ? C(921) 0.2593(3) 0.3214(3) 0.8391(7) 0.059(2) Uani ? C(922) 0.2780(2) 0.3210(2) 0.9475(6) 0.047(2) Uani ? C(923) 0.3230(2) 0.3193(2) 0.9593(5) 0.045(2) Uani ? C(924) 0.3491(2) 0.3166(2) 0.8595(6) 0.045(2) Uani ? C(925) 0.3306(2) 0.3162(3) 0.7521(6) 0.052(2) Uani ? C(926) 0.2853(2) 0.3185(3) 0.7393(6) 0.055(2) Uani ? C(931) 0.1940(3) 0.2437(5) 0.5499(8) 0.100(4) Uani ? C(932) 0.1698(3) 0.1961(4) 0.5155(9) 0.095(3) Uani ? C(933) 0.1252(3) 0.2001(3) 0.5122(9) 0.082(3) Uani ? C(934) 0.1048(3) 0.2505(3) 0.5477(7) 0.079(3) Uani ? C(935) 0.1285(3) 0.2975(3) 0.5861(8) 0.082(3) Uani ? C(936) 0.1738(4) 0.2947(4) 0.5857(9) 0.107(4) Uani ? C(941) 0.1115(3) 0.4807(4) 0.6907(10) 0.084(4) Uani ? C(942) 0.1158(5) 0.4657(3) 0.5807(11) 0.098(4) Uani ? C(943) 0.1552(6) 0.4598(4) 0.5306(8) 0.106(5) Uani ? C(944) 0.1920(4) 0.4682(4) 0.5994(14) 0.117(5) Uani ? C(945) 0.1862(4) 0.4826(5) 0.7115(11) 0.123(5) Uani ? C(946) 0.1459(4) 0.4888(4) 0.7548(7) 0.093(4) Uani ? H(14) 0.0837 0.5178 0.0327 0.0340 Uiso calc H(24) -0.1547 0.0339 0.1152 0.0310 Uiso calc H(42) -0.0032 0.3251 0.2050 0.0380 Uiso calc H(43) -0.0570 0.3781 0.2997 0.0460 Uiso calc H(44) -0.1294 0.3611 0.2513 0.0540 Uiso calc H(45) -0.1461 0.2901 0.1067 0.0460 Uiso calc H(46) -0.0895 0.2372 0.0200 0.0420 Uiso calc H(122) 0.1332 0.2877 -0.0982 0.0480 Uiso calc H(123) 0.1869 0.2170 -0.0484 0.0590 Uiso calc H(124) 0.2100 0.2086 0.1387 0.0680 Uiso calc H(125) 0.1820 0.2702 0.2823 0.0640 Uiso calc H(126) 0.1295 0.3428 0.2338 0.0410 Uiso calc H(132) 0.1866 0.4091 -0.0297 0.0420 Uiso calc H(133) 0.2544 0.4424 0.0337 0.0570 Uiso calc H(134) 0.2586 0.5040 0.1998 0.0580 Uiso calc H(135) 0.1951 0.5307 0.2962 0.0530 Uiso calc H(136) 0.1280 0.4992 0.2294 0.0430 Uiso calc H(152) 0.0186 0.5649 0.0900 0.0390 Uiso calc H(153) -0.0208 0.6507 0.0437 0.0520 Uiso calc H(154) -0.0569 0.6582 -0.1331 0.0430 Uiso calc H(155) -0.0528 0.5791 -0.2636 0.0430 Uiso calc H(156) -0.0132 0.4935 -0.2203 0.0390 Uiso calc H(162) -0.0588 0.4279 0.0263 0.0390 Uiso calc H(163) -0.1258 0.4109 -0.0616 0.0530 Uiso calc H(164) -0.1299 0.3639 -0.2410 0.0550 Uiso calc H(165) -0.0658 0.3305 -0.3309 0.0520 Uiso calc H(166) 0.0018 0.3480 -0.2416 0.0400 Uiso calc H(222) -0.1030 0.2099 0.3178 0.0350 Uiso calc H(223) -0.0758 0.2548 0.4842 0.0440 Uiso calc H(224) -0.0100 0.2227 0.5637 0.0440 Uiso calc H(225) 0.0293 0.1478 0.4705 0.0400 Uiso calc H(226) 0.0036 0.1042 0.3020 0.0320 Uiso calc H(232) -0.1955 0.1117 0.2389 0.0430 Uiso calc H(233) -0.2382 0.1051 0.4060 0.0560 Uiso calc H(234) -0.2066 0.0748 0.5794 0.0640 Uiso calc H(235) -0.1334 0.0494 0.5867 0.0600 Uiso calc H(236) -0.0907 0.0583 0.4228 0.0390 Uiso calc H(252) -0.1803 0.0483 -0.1060 0.0370 Uiso calc H(253) -0.2104 -0.0182 -0.2397 0.0480 Uiso calc H(254) -0.1709 -0.1011 -0.3009 0.0470 Uiso calc H(255) -0.1016 -0.1183 -0.2317 0.0440 Uiso calc H(256) -0.0706 -0.0517 -0.0969 0.0410 Uiso calc H(262) 0.0173 0.0378 -0.0389 0.0320 Uiso calc H(263) 0.0570 0.0184 -0.2074 0.0430 Uiso calc H(264) 0.0259 0.0371 -0.3880 0.0450 Uiso calc H(265) -0.0444 0.0770 -0.3996 0.0380 Uiso calc H(266) -0.0846 0.0933 -0.2323 0.0320 Uiso calc H(31A) 0.0939 0.0933 -0.0642 0.0440 Uiso calc H(31B) 0.0696 0.1062 0.0537 0.0440 Uiso calc H(31C) 0.1151 0.1367 0.0282 0.0440 Uiso calc H(32A) 0.1147 0.1838 -0.1747 0.0460 Uiso calc H(32B) 0.0769 0.2308 -0.1950 0.0460 Uiso calc H(32C) 0.0706 0.1631 -0.2326 0.0460 Uiso calc H(901) 0.7904 0.3810 1.0384 0.0930 Uiso calc H(902) 0.7296 0.4429 1.0471 0.0970 Uiso calc H(903) 0.6813 0.4455 0.8886 0.0960 Uiso calc H(904) 0.6936 0.3832 0.7314 0.0910 Uiso calc H(905) 0.7523 0.3188 0.7287 0.0890 Uiso calc H(906) 0.7997 0.3154 0.8867 0.0990 Uiso calc H(911) 0.3480 0.2026 0.5728 0.0790 Uiso calc H(912) 0.3220 0.1051 0.5615 0.0850 Uiso calc H(913) 0.2757 0.0777 0.4162 0.0840 Uiso calc H(914) 0.2548 0.1471 0.2770 0.0920 Uiso calc H(915) 0.2794 0.2467 0.2918 0.0900 Uiso calc H(916) 0.3267 0.2727 0.4396 0.0720 Uiso calc H(921) 0.2289 0.3236 0.8319 0.0770 Uiso calc H(922) 0.2603 0.3219 1.0135 0.0610 Uiso calc H(923) 0.3358 0.3200 1.0329 0.0580 Uiso calc H(924) 0.3795 0.3150 0.8668 0.0590 Uiso calc H(925) 0.3484 0.3144 0.6864 0.0680 Uiso calc H(926) 0.2726 0.3182 0.6657 0.0710 Uiso calc H(931) 0.2245 0.2414 0.5491 0.1300 Uiso calc H(932) 0.1836 0.1602 0.4939 0.1230 Uiso calc H(933) 0.1087 0.1675 0.4851 0.1070 Uiso calc H(934) 0.0744 0.2529 0.5457 0.1020 Uiso calc H(935) 0.1144 0.3321 0.6132 0.1070 Uiso calc H(936) 0.1903 0.3279 0.6099 0.1390 Uiso calc H(941) 0.0837 0.4855 0.7227 0.1090 Uiso calc H(942) 0.0907 0.4590 0.5363 0.1270 Uiso calc H(943) 0.1578 0.4503 0.4519 0.1380 Uiso calc H(944) 0.2200 0.4640 0.5685 0.1520 Uiso calc H(945) 0.2104 0.4884 0.7595 0.1600 Uiso calc H(946) 0.1424 0.4991 0.8328 0.1210 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 0.0212(2) 0.01658(18) 0.02095(19) -0.0023(2) 0.0013(2) -0.0003(2) Cl(1) 0.0372(9) 0.0239(6) 0.0264(6) -0.0043(7) -0.0064(6) 0.0017(6) Cl(2) 0.0309(8) 0.0268(7) 0.0242(6) -0.0046(6) -0.0039(6) -0.0003(6) O(1) 0.025(2) 0.0147(16) 0.0219(16) -0.0026(14) 0.0009(14) -0.0016(12) O(2) 0.021(2) 0.0185(16) 0.0218(15) 0.0000(16) -0.0012(15) 0.0002(13) N(31) 0.022(3) 0.020(2) 0.027(2) -0.0025(19) 0.0016(19) -0.0019(18) N(41) 0.021(3) 0.022(2) 0.027(2) -0.003(2) 0.0026(18) 0.0016(19) C(11) 0.026(3) 0.015(2) 0.025(3) -0.007(2) 0.005(2) 0.0007(19) C(12) 0.020(3) 0.017(2) 0.021(3) 0.000(2) 0.004(2) 0.001(2) C(13) 0.020(3) 0.025(3) 0.021(3) -0.003(2) 0.001(2) -0.0017(19) C(14) 0.030(3) 0.019(2) 0.029(2) -0.002(2) 0.002(3) -0.004(3) C(15) 0.021(3) 0.022(3) 0.025(2) 0.002(2) -0.003(2) 0.002(2) C(16) 0.030(4) 0.017(2) 0.017(2) 0.003(2) 0.001(2) 0.0041(19) C(21) 0.017(3) 0.011(2) 0.025(3) -0.003(2) -0.001(2) 0.003(2) C(22) 0.023(3) 0.018(2) 0.016(2) 0.000(2) 0.001(2) -0.002(2) C(23) 0.026(3) 0.017(2) 0.020(2) 0.000(2) 0.000(2) -0.001(2) C(24) 0.019(3) 0.021(3) 0.031(3) -0.011(2) -0.001(2) 0.001(2) C(25) 0.015(3) 0.020(2) 0.019(2) -0.0009(19) 0.003(3) -0.001(2) C(26) 0.026(3) 0.015(2) 0.014(3) 0.002(2) 0.000(2) -0.0014(19) C(31) 0.026(3) 0.027(3) 0.048(4) 0.002(2) 0.001(3) -0.004(3) C(32) 0.040(4) 0.034(3) 0.032(3) -0.003(3) 0.010(3) -0.005(2) C(42) 0.031(4) 0.027(3) 0.029(3) 0.001(3) 0.007(3) -0.006(2) C(43) 0.039(5) 0.027(3) 0.039(3) -0.002(3) 0.002(3) -0.002(2) C(44) 0.047(5) 0.034(3) 0.043(3) 0.010(3) 0.016(3) -0.002(3) C(45) 0.025(4) 0.030(3) 0.052(4) 0.005(3) -0.001(3) -0.001(3) C(46) 0.031(4) 0.030(3) 0.035(3) 0.002(3) 0.006(3) 0.002(2) C(121) 0.013(3) 0.019(3) 0.035(3) -0.005(2) -0.001(2) 0.002(2) C(122) 0.025(3) 0.031(3) 0.055(4) -0.002(3) 0.001(3) -0.002(3) C(123) 0.021(3) 0.035(3) 0.080(5) 0.002(2) 0.005(4) -0.011(4) C(124) 0.029(4) 0.036(4) 0.092(5) -0.002(3) 0.001(4) 0.011(4) C(125) 0.035(4) 0.045(4) 0.066(4) -0.004(3) -0.010(3) 0.021(4) C(126) 0.021(4) 0.033(3) 0.041(3) -0.002(3) 0.003(3) 0.005(2) C(131) 0.029(4) 0.015(2) 0.032(3) 0.001(2) -0.003(3) 0.002(2) C(132) 0.031(4) 0.029(3) 0.037(3) -0.004(2) 0.000(3) -0.005(2) C(133) 0.025(4) 0.039(3) 0.068(4) 0.005(3) 0.001(3) 0.002(3) C(134) 0.031(4) 0.033(3) 0.070(4) -0.004(3) -0.011(4) -0.007(3) C(135) 0.036(4) 0.030(3) 0.056(4) -0.004(3) -0.014(3) -0.011(3) C(136) 0.030(4) 0.026(3) 0.043(3) -0.005(3) -0.003(3) -0.001(3) C(151) 0.019(3) 0.025(3) 0.029(3) -0.003(2) -0.004(2) 0.011(2) C(152) 0.037(3) 0.025(2) 0.028(2) 0.003(2) -0.006(3) -0.005(3) C(153) 0.053(4) 0.027(3) 0.040(4) 0.015(3) -0.004(3) -0.002(2) C(154) 0.036(4) 0.027(3) 0.037(3) 0.006(3) -0.003(3) 0.014(3) C(155) 0.037(4) 0.031(3) 0.030(3) 0.000(3) -0.011(3) 0.010(2) C(156) 0.035(4) 0.022(3) 0.032(3) -0.002(3) 0.000(3) 0.003(2) C(161) 0.030(4) 0.014(3) 0.032(3) -0.002(3) -0.002(3) 0.002(2) C(162) 0.033(4) 0.026(3) 0.032(3) 0.000(3) -0.001(3) 0.015(2) C(163) 0.031(4) 0.036(3) 0.056(4) -0.002(3) -0.003(3) 0.010(3) C(164) 0.035(5) 0.035(4) 0.056(4) -0.008(3) -0.023(3) 0.015(3) C(165) 0.047(5) 0.024(3) 0.049(4) -0.007(3) -0.020(3) -0.001(3) C(166) 0.031(4) 0.024(3) 0.037(3) -0.004(3) -0.004(3) 0.005(2) C(221) 0.027(4) 0.018(2) 0.013(2) -0.005(2) 0.002(2) 0.003(2) C(222) 0.031(4) 0.025(3) 0.025(3) 0.002(2) 0.002(2) -0.004(2) C(223) 0.046(4) 0.027(3) 0.029(3) 0.000(3) 0.002(3) -0.007(2) C(224) 0.045(4) 0.033(3) 0.022(3) -0.010(3) -0.004(3) -0.006(2) C(225) 0.032(4) 0.029(3) 0.030(3) -0.003(3) -0.009(2) -0.001(3) C(226) 0.032(4) 0.017(2) 0.024(3) -0.003(2) 0.003(3) 0.001(2) C(231) 0.027(4) 0.027(3) 0.020(3) -0.006(2) 0.008(2) -0.008(2) C(232) 0.036(4) 0.034(3) 0.030(3) -0.007(3) 0.009(3) -0.008(2) C(233) 0.031(4) 0.045(4) 0.052(4) -0.007(3) 0.017(3) -0.011(3) C(234) 0.060(5) 0.052(3) 0.035(3) -0.025(3) 0.027(4) -0.020(4) C(235) 0.056(5) 0.053(3) 0.029(3) -0.017(3) 0.007(4) -0.003(3) C(236) 0.030(4) 0.038(3) 0.023(3) -0.009(3) 0.002(3) -0.003(2) C(251) 0.023(3) 0.025(3) 0.019(3) -0.008(2) 0.003(2) -0.003(2) C(252) 0.030(4) 0.025(3) 0.031(3) -0.007(3) 0.005(3) -0.004(2) C(253) 0.031(4) 0.042(3) 0.037(3) -0.009(3) 0.002(3) -0.010(3) C(254) 0.042(5) 0.039(3) 0.028(3) -0.017(3) -0.005(3) -0.010(3) C(255) 0.040(4) 0.023(3) 0.038(3) -0.004(3) 0.003(3) -0.015(2) C(256) 0.037(4) 0.027(3) 0.029(3) -0.002(3) 0.003(3) -0.006(2) C(261) 0.027(4) 0.012(2) 0.023(3) -0.004(2) -0.001(2) -0.003(2) C(262) 0.031(4) 0.022(3) 0.021(3) -0.002(2) 0.005(2) -0.003(2) C(263) 0.032(4) 0.031(3) 0.036(3) 0.003(3) 0.007(3) -0.001(2) C(264) 0.038(4) 0.036(3) 0.030(3) -0.010(3) 0.016(3) -0.011(2) C(265) 0.038(4) 0.032(3) 0.018(3) -0.010(3) 0.001(2) -0.002(2) C(266) 0.024(4) 0.027(3) 0.024(3) -0.001(2) 0.001(2) -0.002(2) C(901) 0.080(7) 0.048(4) 0.086(6) -0.007(4) 0.019(5) 0.013(4) C(902) 0.101(8) 0.064(5) 0.058(6) -0.009(5) 0.030(5) -0.004(4) C(903) 0.083(7) 0.039(4) 0.099(6) 0.002(4) 0.044(6) 0.011(4) C(904) 0.078(7) 0.052(5) 0.080(5) -0.023(5) 0.012(5) 0.011(4) C(905) 0.092(8) 0.039(4) 0.075(5) -0.020(5) 0.037(5) -0.010(4) C(906) 0.084(7) 0.035(4) 0.109(7) -0.003(4) 0.053(6) 0.012(5) C(911) 0.053(5) 0.066(4) 0.064(4) -0.012(3) 0.001(5) 0.011(5) C(912) 0.083(6) 0.068(4) 0.045(4) 0.003(4) -0.004(5) 0.018(4) C(913) 0.085(7) 0.044(4) 0.065(5) -0.015(4) -0.001(4) 0.001(4) C(914) 0.057(6) 0.084(6) 0.070(5) -0.004(5) -0.021(4) -0.002(4) C(915) 0.048(5) 0.069(5) 0.090(5) 0.011(4) -0.001(4) 0.027(5) C(916) 0.041(5) 0.053(4) 0.072(5) -0.008(3) 0.005(4) 0.004(4) C(921) 0.046(5) 0.054(4) 0.078(5) -0.006(4) -0.009(4) 0.015(4) C(922) 0.038(5) 0.033(3) 0.070(4) 0.000(3) 0.011(4) 0.001(3) C(923) 0.056(5) 0.031(3) 0.047(4) -0.003(3) -0.005(3) 0.000(3) C(924) 0.035(4) 0.039(4) 0.062(4) -0.002(3) -0.009(4) 0.015(3) C(925) 0.049(5) 0.049(4) 0.058(4) 0.003(3) 0.004(4) 0.007(3) C(926) 0.048(5) 0.059(4) 0.057(4) -0.011(4) -0.014(4) 0.013(3) C(931) 0.071(7) 0.101(7) 0.127(9) -0.001(6) -0.010(6) 0.016(6) C(932) 0.094(8) 0.101(6) 0.089(5) 0.001(6) 0.013(7) -0.030(6) C(933) 0.055(6) 0.088(6) 0.104(6) -0.006(4) 0.008(6) -0.036(6) C(934) 0.068(6) 0.061(5) 0.108(7) -0.010(5) -0.007(5) -0.005(5) C(935) 0.075(7) 0.054(5) 0.117(6) 0.001(5) -0.020(6) 0.005(4) C(936) 0.088(9) 0.071(6) 0.161(9) -0.020(6) -0.063(7) 0.011(6) C(941) 0.045(6) 0.096(7) 0.111(8) -0.001(5) 0.015(6) 0.014(6) C(942) 0.132(12) 0.058(5) 0.103(8) 0.003(6) -0.051(8) -0.017(6) C(943) 0.205(15) 0.064(5) 0.049(5) -0.004(7) 0.037(8) -0.006(5) C(944) 0.084(10) 0.113(8) 0.154(10) -0.017(7) 0.071(8) -0.040(8) C(945) 0.056(8) 0.169(11) 0.144(10) 0.002(7) -0.031(7) -0.062(9) C(946) 0.085(9) 0.140(8) 0.055(5) 0.030(7) -0.004(6) 0.021(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) 1.913(3) ? Nb O(1) 1.926(3) ? Nb N(31) 1.935(4) ? Nb Cl(2) 2.3914(12) ? Nb N(41) 2.395(4) ? Nb Cl(1) 2.3971(12) ? O(1) C(11) 1.367(5) ? O(2) C(21) 1.370(6) ? N(31) C(31) 1.473(6) ? N(31) C(32) 1.474(6) ? N(41) C(46) 1.347(7) ? N(41) C(42) 1.348(6) ? C(11) C(16) 1.405(7) ? C(11) C(12) 1.421(7) ? C(12) C(13) 1.411(6) ? C(12) C(121) 1.505(6) ? C(13) C(14) 1.379(6) ? C(13) C(131) 1.496(7) ? C(14) C(15) 1.392(7) ? C(15) C(16) 1.404(6) ? C(15) C(151) 1.497(6) ? C(16) C(161) 1.500(7) ? C(21) C(22) 1.410(6) ? C(21) C(26) 1.436(6) ? C(22) C(23) 1.400(6) ? C(22) C(221) 1.487(6) ? C(23) C(24) 1.391(6) ? C(23) C(231) 1.507(7) ? C(24) C(25) 1.399(7) ? C(25) C(26) 1.396(6) ? C(25) C(251) 1.497(6) ? C(26) C(261) 1.505(6) ? C(42) C(43) 1.378(7) ? C(43) C(44) 1.363(8) ? C(44) C(45) 1.392(7) ? C(45) C(46) 1.389(7) ? C(121) C(122) 1.370(7) ? C(121) C(126) 1.391(7) ? C(122) C(123) 1.401(7) ? C(123) C(124) 1.349(10) ? C(124) C(125) 1.373(8) ? C(125) C(126) 1.394(8) ? C(131) C(132) 1.377(7) ? C(131) C(136) 1.405(7) ? C(132) C(133) 1.391(8) ? C(133) C(134) 1.403(8) ? C(134) C(135) 1.379(8) ? C(135) C(136) 1.373(8) ? C(151) C(152) 1.393(7) ? C(151) C(156) 1.402(7) ? C(152) C(153) 1.386(6) ? C(153) C(154) 1.382(7) ? C(154) C(155) 1.373(7) ? C(155) C(156) 1.380(7) ? C(161) C(166) 1.378(7) ? C(161) C(162) 1.387(8) ? C(162) C(163) 1.385(8) ? C(163) C(164) 1.381(8) ? C(164) C(165) 1.389(8) ? C(165) C(166) 1.407(8) ? C(221) C(226) 1.389(7) ? C(221) C(222) 1.392(6) ? C(222) C(223) 1.387(7) ? C(223) C(224) 1.378(8) ? C(224) C(225) 1.376(7) ? C(225) C(226) 1.381(7) ? C(231) C(232) 1.380(7) ? C(231) C(236) 1.399(7) ? C(232) C(233) 1.392(7) ? C(233) C(234) 1.380(9) ? C(234) C(235) 1.374(8) ? C(235) C(236) 1.370(8) ? C(251) C(252) 1.385(7) ? C(251) C(256) 1.397(7) ? C(252) C(253) 1.388(7) ? C(253) C(254) 1.375(8) ? C(254) C(255) 1.360(8) ? C(255) C(256) 1.405(7) ? C(261) C(262) 1.378(7) ? C(261) C(266) 1.397(7) ? C(262) C(263) 1.393(7) ? C(263) C(264) 1.384(7) ? C(264) C(265) 1.389(8) ? C(265) C(266) 1.378(7) ? C(901) C(906) 1.358(10) ? C(901) C(902) 1.372(10) ? C(902) C(903) 1.399(11) ? C(903) C(904) 1.371(10) ? C(904) C(905) 1.360(11) ? C(905) C(906) 1.385(11) ? C(911) C(916) 1.343(9) ? C(911) C(912) 1.371(8) ? C(912) C(913) 1.343(9) ? C(913) C(914) 1.370(9) ? C(914) C(915) 1.387(9) ? C(915) C(916) 1.369(10) ? C(921) C(922) 1.369(9) ? C(921) C(926) 1.394(9) ? C(922) C(923) 1.377(9) ? C(923) C(924) 1.397(8) ? C(924) C(925) 1.355(8) ? C(925) C(926) 1.390(9) ? C(931) C(932) 1.343(11) ? C(931) C(936) 1.349(12) ? C(932) C(933) 1.365(11) ? C(933) C(934) 1.336(9) ? C(934) C(935) 1.338(10) ? C(935) C(936) 1.382(12) ? C(941) C(946) 1.292(12) ? C(941) C(942) 1.311(12) ? C(942) C(943) 1.338(15) ? C(943) C(944) 1.385(15) ? C(944) C(945) 1.336(14) ? C(945) C(946) 1.333(13) ? 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) 168.69(14) ? O(2) Nb N(31) 95.37(15) ? O(1) Nb N(31) 95.94(15) ? O(2) Nb Cl(2) 89.20(10) ? O(1) Nb Cl(2) 90.22(9) ? N(31) Nb Cl(2) 95.36(12) ? O(2) Nb N(41) 84.65(13) ? O(1) Nb N(41) 84.04(13) ? N(31) Nb N(41) 179.31(16) ? Cl(2) Nb N(41) 85.33(10) ? O(2) Nb Cl(1) 88.88(10) ? O(1) Nb Cl(1) 89.99(9) ? N(31) Nb Cl(1) 93.36(12) ? Cl(2) Nb Cl(1) 171.21(5) ? N(41) Nb Cl(1) 85.95(11) ? C(11) O(1) Nb 160.1(3) ? C(21) O(2) Nb 154.0(3) ? C(31) N(31) C(32) 111.7(4) ? C(31) N(31) Nb 123.9(3) ? C(32) N(31) Nb 124.5(3) ? C(46) N(41) C(42) 116.2(5) ? C(46) N(41) Nb 122.8(3) ? C(42) N(41) Nb 121.0(4) ? O(1) C(11) C(16) 120.5(5) ? O(1) C(11) C(12) 117.7(4) ? C(16) C(11) C(12) 121.8(4) ? C(13) C(12) C(11) 117.9(4) ? C(13) C(12) C(121) 119.4(4) ? C(11) C(12) C(121) 122.7(4) ? C(14) C(13) C(12) 119.8(5) ? C(14) C(13) C(131) 118.4(4) ? C(12) C(13) C(131) 121.8(4) ? C(13) C(14) C(15) 122.4(4) ? C(14) C(15) C(16) 119.5(4) ? C(14) C(15) C(151) 116.7(4) ? C(16) C(15) C(151) 123.8(5) ? C(15) C(16) C(11) 118.6(5) ? C(15) C(16) C(161) 121.2(4) ? C(11) C(16) C(161) 120.3(4) ? O(2) C(21) C(22) 119.9(4) ? O(2) C(21) C(26) 118.7(4) ? C(22) C(21) C(26) 121.3(4) ? C(23) C(22) C(21) 119.0(4) ? C(23) C(22) C(221) 120.6(4) ? C(21) C(22) C(221) 120.4(4) ? C(24) C(23) C(22) 119.6(4) ? C(24) C(23) C(231) 117.1(4) ? C(22) C(23) C(231) 123.3(4) ? C(23) C(24) C(25) 122.0(5) ? C(26) C(25) C(24) 120.1(4) ? C(26) C(25) C(251) 122.9(4) ? C(24) C(25) C(251) 117.0(4) ? C(25) C(26) C(21) 117.9(4) ? C(25) C(26) C(261) 120.1(4) ? C(21) C(26) C(261) 121.9(4) ? N(41) C(42) C(43) 124.3(5) ? C(44) C(43) C(42) 118.5(5) ? C(43) C(44) C(45) 119.4(6) ? C(46) C(45) C(44) 118.2(6) ? N(41) C(46) C(45) 123.3(5) ? C(122) C(121) C(126) 119.5(5) ? C(122) C(121) C(12) 120.4(4) ? C(126) C(121) C(12) 120.0(5) ? C(121) C(122) C(123) 119.7(5) ? C(124) C(123) C(122) 120.3(6) ? C(123) C(124) C(125) 121.3(6) ? C(124) C(125) C(126) 119.0(6) ? C(121) C(126) C(125) 120.2(5) ? C(132) C(131) C(136) 117.7(5) ? C(132) C(131) C(13) 122.7(5) ? C(136) C(131) C(13) 119.6(5) ? C(131) C(132) C(133) 122.2(5) ? C(132) C(133) C(134) 118.9(6) ? C(135) C(134) C(133) 119.3(6) ? C(136) C(135) C(134) 120.9(6) ? C(135) C(136) C(131) 120.9(6) ? C(152) C(151) C(156) 117.4(4) ? C(152) C(151) C(15) 119.3(4) ? C(156) C(151) C(15) 123.1(4) ? C(153) C(152) C(151) 121.0(5) ? C(154) C(153) C(152) 120.7(5) ? C(155) C(154) C(153) 119.0(5) ? C(154) C(155) C(156) 121.0(5) ? C(155) C(156) C(151) 121.0(5) ? C(166) C(161) C(162) 119.2(5) ? C(166) C(161) C(16) 120.1(5) ? C(162) C(161) C(16) 120.5(4) ? C(163) C(162) C(161) 120.3(5) ? C(164) C(163) C(162) 121.0(6) ? C(163) C(164) C(165) 119.2(6) ? C(164) C(165) C(166) 119.5(6) ? C(161) C(166) C(165) 120.8(6) ? C(226) C(221) C(222) 117.9(4) ? C(226) C(221) C(22) 120.3(4) ? C(222) C(221) C(22) 121.6(5) ? C(223) C(222) C(221) 120.9(5) ? C(224) C(223) C(222) 120.6(5) ? C(225) C(224) C(223) 118.8(5) ? C(224) C(225) C(226) 121.1(5) ? C(225) C(226) C(221) 120.7(5) ? C(232) C(231) C(236) 118.4(5) ? C(232) C(231) C(23) 120.2(4) ? C(236) C(231) C(23) 121.2(5) ? C(231) C(232) C(233) 120.5(5) ? C(234) C(233) C(232) 119.6(6) ? C(235) C(234) C(233) 120.6(6) ? C(236) C(235) C(234) 119.7(6) ? C(235) C(236) C(231) 121.2(6) ? C(252) C(251) C(256) 118.3(5) ? C(252) C(251) C(25) 120.7(4) ? C(256) C(251) C(25) 120.9(5) ? C(251) C(252) C(253) 121.1(5) ? C(254) C(253) C(252) 119.7(6) ? C(255) C(254) C(253) 120.9(5) ? C(254) C(255) C(256) 119.8(5) ? C(251) C(256) C(255) 120.3(6) ? C(262) C(261) C(266) 119.4(5) ? C(262) C(261) C(26) 120.7(4) ? C(266) C(261) C(26) 119.8(5) ? C(261) C(262) C(263) 120.4(5) ? C(264) C(263) C(262) 119.9(5) ? C(263) C(264) C(265) 119.8(5) ? C(266) C(265) C(264) 120.1(5) ? C(265) C(266) C(261) 120.4(5) ? C(906) C(901) C(902) 121.0(8) ? C(901) C(902) C(903) 118.9(7) ? C(904) C(903) C(902) 119.4(8) ? C(905) C(904) C(903) 121.0(8) ? C(904) C(905) C(906) 119.6(7) ? C(901) C(906) C(905) 120.0(8) ? C(916) C(911) C(912) 120.0(7) ? C(913) C(912) C(911) 120.5(7) ? C(912) C(913) C(914) 120.4(7) ? C(913) C(914) C(915) 119.2(7) ? C(916) C(915) C(914) 119.3(7) ? C(911) C(916) C(915) 120.6(7) ? C(922) C(921) C(926) 120.6(7) ? C(921) C(922) C(923) 120.3(6) ? C(922) C(923) C(924) 119.2(6) ? C(925) C(924) C(923) 120.6(6) ? C(924) C(925) C(926) 120.6(6) ? C(925) C(926) C(921) 118.7(6) ? C(932) C(931) C(936) 119.5(10) ? C(931) C(932) C(933) 120.3(8) ? C(934) C(933) C(932) 120.6(7) ? C(933) C(934) C(935) 119.7(8) ? C(934) C(935) C(936) 120.2(8) ? C(931) C(936) C(935) 119.6(9) ? C(946) C(941) C(942) 120.1(10) ? C(941) C(942) C(943) 121.9(11) ? C(942) C(943) C(944) 117.9(9) ? C(945) C(944) C(943) 118.3(10) ? C(946) C(945) C(944) 120.3(10) ? C(941) C(946) C(945) 121.5(10) ? #===END #============================================================================== data_DTP74 _database_code_CSD 159029 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C97 H83 Cl2 N2 O2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 1560.61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'p n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 30.47090(10) _cell_length_b 22.0751(2) _cell_length_c 11.4756(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7719.0(2) _cell_measurement_reflns_used 48885 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.526 _cell_measurement_temperature 150 _exptl_crystal_F_000 3208 # 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 0.5990 _exptl_absorpt_correction_T_max 0.8263 _diffrn_reflns_number 48885 _reflns_number_total 16606 _reflns_Friedl_coverage 0.9024 _reflns_number_gt 13281 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.092 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_max 27 _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 0.046 _refine_ls_wR_factor_ref 0.085 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 16602 _refine_ls_number_parameters 940 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.008 _refine_diff_density_max 1.83 _refine_diff_density_min -1.14 _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 0.547(6) # 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 0.018357(6) 0.219715(7) 0.01380(3) 0.01924(5) Uani ? Cl(1) -0.02641(5) 0.21909(6) -0.15504(13) 0.0283(4) Uani ? Cl(2) 0.05325(5) 0.22714(6) 0.19941(12) 0.0264(4) Uani ? O(1) 0.03907(12) 0.29958(15) -0.0258(3) 0.0205(10) Uani ? O(2) -0.01299(12) 0.14937(16) 0.0695(3) 0.0240(10) Uani ? N(31) 0.06578(15) 0.17562(19) -0.0583(4) 0.0250(14) Uani ? N(41) -0.04063(16) 0.2744(2) 0.1040(4) 0.0250(14) Uani ? C(11) 0.05241(17) 0.3584(2) -0.0148(4) 0.0183(16) Uani ? C(12) 0.09392(16) 0.3718(2) 0.0285(7) 0.0197(16) Uani ? C(13) 0.10561(18) 0.4323(2) 0.0465(4) 0.0227(17) Uani ? C(14) 0.07588(15) 0.47755(19) 0.0175(8) 0.0247(14) Uani ? C(15) 0.03516(18) 0.4658(2) -0.0282(5) 0.0220(15) Uani ? C(16) 0.02210(18) 0.4047(2) -0.0460(5) 0.0217(15) Uani ? C(21) -0.04937(18) 0.1146(2) 0.0845(5) 0.0193(15) Uani ? C(22) -0.07195(17) 0.1180(2) 0.1924(5) 0.0193(15) Uani ? C(23) -0.11177(18) 0.0866(2) 0.2032(5) 0.0223(15) Uani ? C(24) -0.1277(2) 0.0528(2) 0.1099(5) 0.0233(15) Uani ? C(25) -0.10420(15) 0.04671(18) 0.0066(8) 0.0210(14) Uani ? C(26) -0.06376(17) 0.0776(2) -0.0082(5) 0.0180(16) Uani ? C(31) 0.08812(18) 0.1234(2) -0.0048(8) 0.033(2) Uani ? C(32) 0.0823(2) 0.1888(3) -0.1754(5) 0.0360(18) Uani ? C(42) -0.0319(2) 0.3178(2) 0.1857(5) 0.0263(15) Uani ? C(43) -0.0641(2) 0.3494(3) 0.2423(7) 0.034(2) Uani ? C(44) -0.1071(2) 0.3392(3) 0.2136(6) 0.037(2) Uani ? C(45) -0.1166(2) 0.2963(3) 0.1300(6) 0.0337(18) Uani ? C(46) -0.08249(19) 0.2649(3) 0.0763(5) 0.0303(17) Uani ? C(121) 0.12593(18) 0.3230(3) 0.0624(5) 0.0237(15) Uani ? C(122) 0.14304(18) 0.2849(2) -0.0207(5) 0.0320(19) Uani ? C(123) 0.17432(17) 0.2416(2) 0.0111(12) 0.0443(19) Uani ? C(124) 0.1889(2) 0.2367(3) 0.1223(8) 0.052(3) Uani ? C(125) 0.1716(2) 0.2750(3) 0.2059(7) 0.044(2) Uani ? C(126) 0.14074(19) 0.3172(3) 0.1770(6) 0.0317(18) Uani ? C(131) 0.1499(2) 0.4509(2) 0.0908(5) 0.0250(17) Uani ? C(132) 0.18827(17) 0.4340(2) 0.0341(7) 0.0313(19) Uani ? C(133) 0.2287(2) 0.4538(3) 0.0731(6) 0.041(2) Uani ? C(134) 0.2315(2) 0.4903(3) 0.1717(7) 0.043(2) Uani ? C(135) 0.1934(2) 0.5066(3) 0.2310(6) 0.039(2) Uani ? C(136) 0.1526(2) 0.4879(3) 0.1899(6) 0.0323(18) Uani ? C(151) 0.00643(18) 0.5191(2) -0.0599(5) 0.0227(17) Uani ? C(152) 0.00415(17) 0.5673(2) 0.0175(9) 0.0307(14) Uani ? C(153) -0.0192(2) 0.6196(2) -0.0078(7) 0.038(2) Uani ? C(154) -0.0414(2) 0.6245(3) -0.1145(6) 0.034(2) Uani ? C(155) -0.03871(19) 0.5761(2) -0.1923(5) 0.0283(17) Uani ? C(156) -0.01463(18) 0.5242(3) -0.1652(5) 0.0273(15) Uani ? C(161) -0.0209(2) 0.3903(2) -0.0981(5) 0.0230(15) Uani ? C(162) -0.05990(18) 0.4089(3) -0.0433(6) 0.0283(15) Uani ? C(163) -0.1002(2) 0.3984(3) -0.0968(6) 0.038(2) Uani ? C(164) -0.1027(2) 0.3698(3) -0.2029(7) 0.042(2) Uani ? C(165) -0.0643(3) 0.3517(3) -0.2570(7) 0.042(3) Uani ? C(166) -0.0237(2) 0.3609(2) -0.2049(5) 0.0280(18) Uani ? C(221) -0.05319(18) 0.1509(2) 0.2934(5) 0.0210(15) Uani ? C(222) -0.0758(2) 0.1970(2) 0.3486(5) 0.0260(15) Uani ? C(223) -0.0594(2) 0.2238(3) 0.4487(5) 0.036(2) Uani ? C(224) -0.0204(2) 0.2055(3) 0.4966(8) 0.0350(19) Uani ? C(225) 0.0027(2) 0.1602(3) 0.4413(5) 0.0327(18) Uani ? C(226) -0.01294(19) 0.1330(3) 0.3404(5) 0.0287(17) Uani ? C(231) -0.1383(2) 0.0851(2) 0.3138(5) 0.0273(18) Uani ? C(232) -0.1830(2) 0.0998(3) 0.3097(6) 0.035(2) Uani ? C(233) -0.2082(2) 0.0956(3) 0.4107(7) 0.043(2) Uani ? C(234) -0.1898(2) 0.0775(2) 0.5127(10) 0.0463(18) Uani ? C(235) -0.1463(2) 0.0627(2) 0.5171(9) 0.0427(17) Uani ? C(236) -0.1202(2) 0.0668(3) 0.4189(5) 0.035(2) Uani ? C(251) -0.12261(18) 0.0053(2) -0.0849(5) 0.0230(15) Uani ? C(252) -0.1643(2) 0.0142(3) -0.1282(5) 0.0280(17) Uani ? C(253) -0.1823(2) -0.0247(3) -0.2106(6) 0.035(2) Uani ? C(254) -0.1583(2) -0.0743(3) -0.2470(6) 0.038(2) Uani ? C(255) -0.1168(2) -0.0849(3) -0.2036(5) 0.036(2) Uani ? C(256) -0.0993(2) -0.0446(2) -0.1226(5) 0.0273(18) Uani ? C(261) -0.03741(19) 0.0690(2) -0.1174(5) 0.0207(15) Uani ? C(262) 0.0048(2) 0.0462(3) -0.1113(5) 0.0277(18) Uani ? C(263) 0.0284(2) 0.0342(3) -0.2103(5) 0.0310(18) Uani ? C(264) 0.0098(2) 0.0453(3) -0.3203(5) 0.032(2) Uani ? C(265) -0.0320(2) 0.0676(3) -0.3258(6) 0.0340(18) Uani ? C(266) -0.0559(2) 0.0792(2) -0.2256(5) 0.0267(18) Uani ? C(901) 0.7696(3) 0.3802(4) 0.9796(7) 0.067(3) Uani ? C(902) 0.7341(3) 0.4177(4) 0.9821(8) 0.071(4) Uani ? C(903) 0.7052(3) 0.4194(3) 0.8902(9) 0.066(3) Uani ? C(904) 0.7124(3) 0.3821(4) 0.7943(8) 0.070(3) Uani ? C(905) 0.7475(3) 0.3436(4) 0.7937(9) 0.070(3) Uani ? C(906) 0.7760(3) 0.3427(4) 0.8851(10) 0.072(3) Uani ? C(911) 0.3295(2) 0.1916(3) 0.5113(12) 0.065(2) Uani ? C(912) 0.3141(3) 0.1325(3) 0.5036(11) 0.066(3) Uani ? C(913) 0.2858(3) 0.1170(4) 0.4196(8) 0.068(3) Uani ? C(914) 0.2733(3) 0.1581(4) 0.3372(9) 0.076(3) Uani ? C(915) 0.2891(3) 0.2166(4) 0.3447(9) 0.069(3) Uani ? C(916) 0.3165(3) 0.2331(4) 0.4345(8) 0.059(3) Uani ? C(921) 0.2589(2) 0.3206(3) 0.8394(8) 0.054(3) Uani ? C(922) 0.2781(3) 0.3210(3) 0.9486(7) 0.048(2) Uani ? C(923) 0.3225(3) 0.3193(3) 0.9590(7) 0.045(2) Uani ? C(924) 0.3489(2) 0.3171(3) 0.8623(7) 0.043(2) Uani ? C(925) 0.3295(3) 0.3173(3) 0.7532(7) 0.053(2) Uani ? C(926) 0.2848(3) 0.3182(3) 0.7427(7) 0.055(3) Uani ? C(931) 0.1948(4) 0.2435(6) 0.5492(9) 0.093(4) Uani ? C(932) 0.1705(3) 0.1955(4) 0.5160(13) 0.086(3) Uani ? C(933) 0.1259(3) 0.1986(4) 0.5130(13) 0.091(3) Uani ? C(934) 0.1059(3) 0.2498(4) 0.5484(8) 0.075(4) Uani ? C(935) 0.1287(4) 0.2979(4) 0.5865(10) 0.092(4) Uani ? C(936) 0.1744(4) 0.2935(5) 0.5838(11) 0.103(5) Uani ? C(941) 0.1118(3) 0.4800(4) 0.6916(11) 0.080(4) Uani ? C(942) 0.1157(4) 0.4657(4) 0.5802(12) 0.088(4) Uani ? C(943) 0.1568(6) 0.4597(4) 0.5322(10) 0.096(4) Uani ? C(944) 0.1919(4) 0.4702(5) 0.5986(14) 0.102(5) Uani ? C(945) 0.1867(4) 0.4834(6) 0.7102(13) 0.122(6) Uani ? C(946) 0.1470(4) 0.4898(5) 0.7563(9) 0.089(4) Uani ? H(14) 0.0840 0.5177 0.0296 0.0320 Uiso calc H(24) -0.1548 0.0338 0.1168 0.0300 Uiso calc H(42) -0.0028 0.3263 0.2037 0.0340 Uiso calc H(43) -0.0568 0.3775 0.2995 0.0450 Uiso calc H(44) -0.1294 0.3608 0.2500 0.0480 Uiso calc H(45) -0.1456 0.2884 0.1096 0.0440 Uiso calc H(46) -0.0892 0.2365 0.0192 0.0400 Uiso calc H(122) 0.1338 0.2879 -0.0977 0.0420 Uiso calc H(123) 0.1854 0.2156 -0.0455 0.0580 Uiso calc H(124) 0.2100 0.2080 0.1421 0.0670 Uiso calc H(125) 0.1812 0.2721 0.2826 0.0570 Uiso calc H(126) 0.1294 0.3425 0.2344 0.0410 Uiso calc H(132) 0.1867 0.4090 -0.0310 0.0410 Uiso calc H(133) 0.2541 0.4428 0.0334 0.0540 Uiso calc H(134) 0.2587 0.5037 0.1979 0.0560 Uiso calc H(135) 0.1953 0.5300 0.2982 0.0510 Uiso calc H(136) 0.1272 0.4999 0.2282 0.0420 Uiso calc H(152) 0.0187 0.5644 0.0884 0.0400 Uiso calc H(153) -0.0202 0.6512 0.0457 0.0490 Uiso calc H(154) -0.0575 0.6591 -0.1329 0.0450 Uiso calc H(155) -0.0532 0.5784 -0.2635 0.0370 Uiso calc H(156) -0.0128 0.4928 -0.2190 0.0360 Uiso calc H(162) -0.0588 0.4282 0.0286 0.0370 Uiso calc H(163) -0.1258 0.4109 -0.0601 0.0490 Uiso calc H(164) -0.1298 0.3628 -0.2378 0.0540 Uiso calc H(165) -0.0657 0.3330 -0.3295 0.0540 Uiso calc H(166) 0.0016 0.3473 -0.2417 0.0370 Uiso calc H(222) -0.1024 0.2102 0.3181 0.0330 Uiso calc H(223) -0.0751 0.2549 0.4841 0.0470 Uiso calc H(224) -0.0099 0.2231 0.5646 0.0450 Uiso calc H(225) 0.0294 0.1475 0.4723 0.0430 Uiso calc H(226) 0.0034 0.1028 0.3041 0.0370 Uiso calc H(232) -0.1958 0.1123 0.2401 0.0450 Uiso calc H(233) -0.2379 0.1054 0.4083 0.0560 Uiso calc H(234) -0.2069 0.0751 0.5797 0.0600 Uiso calc H(235) -0.1341 0.0497 0.5871 0.0560 Uiso calc H(236) -0.0905 0.0572 0.4233 0.0450 Uiso calc H(252) -0.1808 0.0468 -0.1017 0.0370 Uiso calc H(253) -0.2101 -0.0174 -0.2409 0.0450 Uiso calc H(254) -0.1703 -0.1008 -0.3013 0.0490 Uiso calc H(255) -0.1008 -0.1184 -0.2281 0.0460 Uiso calc H(256) -0.0712 -0.0515 -0.0932 0.0350 Uiso calc H(262) 0.0174 0.0390 -0.0388 0.0360 Uiso calc H(263) 0.0567 0.0187 -0.2047 0.0400 Uiso calc H(264) 0.0256 0.0376 -0.3880 0.0420 Uiso calc H(265) -0.0446 0.0751 -0.3981 0.0440 Uiso calc H(266) -0.0844 0.0940 -0.2311 0.0350 Uiso calc H(31A) 0.0929 0.0927 -0.0628 0.0430 Uiso calc H(31B) 0.0702 0.1073 0.0567 0.0430 Uiso calc H(31C) 0.1158 0.1362 0.0264 0.0430 Uiso calc H(32A) 0.1138 0.1876 -0.1749 0.0470 Uiso calc H(32B) 0.0727 0.2283 -0.1990 0.0470 Uiso calc H(32C) 0.0714 0.1591 -0.2291 0.0470 Uiso calc H(901) 0.7894 0.3799 1.0412 0.0870 Uiso calc H(902) 0.7294 0.4423 1.0466 0.0920 Uiso calc H(903) 0.6811 0.4453 0.8920 0.0860 Uiso calc H(904) 0.6934 0.3833 0.7310 0.0910 Uiso calc H(905) 0.7521 0.3180 0.7305 0.0900 Uiso calc H(906) 0.7999 0.3166 0.8839 0.0940 Uiso calc H(911) 0.3491 0.2022 0.5702 0.0840 Uiso calc H(912) 0.3234 0.1036 0.5572 0.0850 Uiso calc H(913) 0.2745 0.0779 0.4173 0.0890 Uiso calc H(914) 0.2545 0.1468 0.2771 0.0990 Uiso calc H(915) 0.2811 0.2450 0.2887 0.0900 Uiso calc H(916) 0.3258 0.2731 0.4415 0.0760 Uiso calc H(921) 0.2285 0.3220 0.8319 0.0710 Uiso calc H(922) 0.2605 0.3223 1.0149 0.0630 Uiso calc H(923) 0.3351 0.3197 1.0328 0.0590 Uiso calc H(924) 0.3792 0.3155 0.8698 0.0560 Uiso calc H(925) 0.3469 0.3168 0.6867 0.0690 Uiso calc H(926) 0.2720 0.3171 0.6691 0.0720 Uiso calc H(931) 0.2253 0.2417 0.5479 0.1210 Uiso calc H(932) 0.1844 0.1596 0.4949 0.1120 Uiso calc H(933) 0.1095 0.1659 0.4868 0.1180 Uiso calc H(934) 0.0754 0.2519 0.5464 0.0970 Uiso calc H(935) 0.1147 0.3326 0.6135 0.1190 Uiso calc H(936) 0.1911 0.3267 0.6069 0.1340 Uiso calc H(941) 0.0841 0.4833 0.7247 0.1040 Uiso calc H(942) 0.0908 0.4597 0.5347 0.1150 Uiso calc H(943) 0.1600 0.4485 0.4545 0.1260 Uiso calc H(944) 0.2199 0.4682 0.5665 0.1340 Uiso calc H(945) 0.2113 0.4883 0.7572 0.1580 Uiso calc H(946) 0.1440 0.5010 0.8339 0.1150 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 0.02268(10) 0.01560(9) 0.01943(10) -0.00193(9) 0.00076(18) -0.00033(17) Cl(1) 0.0412(9) 0.0218(7) 0.0220(8) -0.0042(7) -0.0057(6) 0.0019(6) Cl(2) 0.0334(8) 0.0237(7) 0.0222(8) -0.0031(6) -0.0041(7) 0.0000(6) O(1) 0.026(2) 0.0164(17) 0.019(2) 0.0012(15) 0.0027(15) -0.0020(13) O(2) 0.030(2) 0.021(2) 0.0209(19) -0.0007(17) 0.0006(18) -0.0018(15) N(31) 0.028(3) 0.021(2) 0.026(3) -0.009(2) 0.002(2) -0.003(2) N(41) 0.023(3) 0.021(2) 0.031(3) 0.002(2) 0.005(2) -0.001(2) C(11) 0.022(3) 0.011(2) 0.022(4) -0.007(2) 0.005(2) 0.0014(19) C(12) 0.026(3) 0.012(2) 0.021(4) 0.0008(19) -0.003(3) 0.000(3) C(13) 0.026(3) 0.021(3) 0.021(4) -0.002(2) 0.002(2) -0.002(2) C(14) 0.032(3) 0.019(2) 0.023(3) -0.007(2) 0.004(5) -0.008(4) C(15) 0.026(3) 0.019(3) 0.021(3) -0.001(2) -0.003(2) 0.002(2) C(16) 0.021(3) 0.024(3) 0.020(3) 0.004(2) 0.002(3) -0.001(2) C(21) 0.025(3) 0.013(3) 0.020(3) 0.000(2) -0.001(3) -0.002(2) C(22) 0.025(3) 0.013(3) 0.020(3) 0.005(2) 0.001(3) 0.000(2) C(23) 0.025(3) 0.022(3) 0.020(3) 0.002(2) 0.001(3) -0.001(2) C(24) 0.028(3) 0.020(3) 0.022(3) -0.004(3) 0.000(3) 0.001(2) C(25) 0.028(3) 0.014(2) 0.021(3) 0.0010(18) -0.001(4) -0.007(4) C(26) 0.029(3) 0.011(2) 0.014(4) 0.000(2) -0.002(2) -0.003(2) C(31) 0.027(3) 0.023(3) 0.049(6) 0.003(2) 0.002(4) 0.002(3) C(32) 0.048(4) 0.030(3) 0.030(4) -0.017(3) 0.010(3) -0.001(3) C(42) 0.034(3) 0.023(3) 0.022(3) -0.006(3) -0.001(3) -0.003(3) C(43) 0.034(4) 0.019(3) 0.050(5) 0.008(3) 0.006(4) -0.004(3) C(44) 0.038(4) 0.028(4) 0.044(5) 0.011(3) 0.016(3) 0.013(3) C(45) 0.036(4) 0.024(3) 0.041(4) 0.002(3) 0.004(3) -0.003(3) C(46) 0.026(3) 0.035(3) 0.030(4) -0.007(3) 0.000(3) -0.001(3) C(121) 0.020(3) 0.023(3) 0.028(3) -0.006(2) -0.001(2) -0.001(2) C(122) 0.024(3) 0.025(3) 0.047(5) -0.006(3) 0.003(3) -0.004(3) C(123) 0.026(3) 0.026(3) 0.081(5) 0.001(2) 0.002(6) -0.002(6) C(124) 0.033(4) 0.028(4) 0.094(7) -0.004(3) -0.010(4) 0.011(4) C(125) 0.042(4) 0.042(4) 0.048(5) -0.008(3) -0.011(4) 0.008(4) C(126) 0.032(4) 0.030(3) 0.033(4) 0.000(3) 0.002(3) 0.005(3) C(131) 0.033(3) 0.014(3) 0.028(4) -0.005(2) -0.002(3) 0.000(2) C(132) 0.026(3) 0.024(3) 0.044(5) -0.005(2) 0.003(3) -0.002(3) C(133) 0.029(4) 0.033(4) 0.062(5) 0.002(3) 0.003(3) -0.006(3) C(134) 0.035(4) 0.031(4) 0.064(5) -0.008(3) -0.017(4) -0.006(3) C(135) 0.046(5) 0.029(3) 0.042(5) -0.008(3) -0.014(4) -0.008(3) C(136) 0.036(4) 0.029(3) 0.032(4) 0.000(3) -0.004(3) 0.001(3) C(151) 0.026(3) 0.016(3) 0.026(4) -0.002(2) 0.000(3) 0.007(2) C(152) 0.046(3) 0.023(2) 0.023(3) 0.004(2) -0.002(6) 0.000(5) C(153) 0.055(4) 0.023(3) 0.035(6) 0.010(3) 0.002(4) -0.002(3) C(154) 0.032(4) 0.024(3) 0.047(5) 0.008(3) -0.005(3) 0.007(3) C(155) 0.029(3) 0.028(3) 0.028(4) 0.002(3) -0.009(3) 0.007(3) C(156) 0.031(3) 0.024(3) 0.027(3) -0.004(3) -0.006(3) 0.005(2) C(161) 0.026(3) 0.020(3) 0.023(3) -0.001(3) -0.002(3) 0.010(2) C(162) 0.021(3) 0.030(3) 0.034(3) -0.002(3) -0.003(3) 0.004(3) C(163) 0.029(4) 0.032(4) 0.052(5) 0.000(3) -0.003(3) 0.013(3) C(164) 0.034(4) 0.034(4) 0.057(5) -0.005(4) -0.014(4) 0.005(4) C(165) 0.069(6) 0.023(4) 0.034(5) -0.009(4) -0.018(4) 0.010(3) C(166) 0.032(4) 0.019(3) 0.033(4) -0.002(3) -0.006(3) 0.006(2) C(221) 0.026(3) 0.021(3) 0.016(3) -0.006(2) 0.003(3) 0.000(2) C(222) 0.034(3) 0.021(3) 0.023(3) 0.004(3) -0.001(3) -0.005(2) C(223) 0.046(4) 0.036(4) 0.027(4) 0.001(3) 0.006(3) -0.004(3) C(224) 0.043(3) 0.039(3) 0.023(5) -0.011(3) -0.007(4) -0.009(3) C(225) 0.039(4) 0.035(3) 0.024(4) -0.009(3) -0.006(3) 0.000(3) C(226) 0.035(4) 0.026(3) 0.025(3) -0.003(3) 0.004(3) -0.004(2) C(231) 0.036(4) 0.021(3) 0.025(4) -0.010(3) 0.005(3) -0.009(2) C(232) 0.034(4) 0.037(4) 0.033(4) -0.005(3) 0.005(3) -0.009(3) C(233) 0.034(4) 0.046(4) 0.048(5) -0.004(3) 0.014(4) -0.010(4) C(234) 0.052(4) 0.051(3) 0.036(4) -0.021(3) 0.017(7) -0.006(6) C(235) 0.057(4) 0.048(3) 0.023(3) -0.021(3) -0.002(6) 0.001(5) C(236) 0.046(4) 0.038(4) 0.020(4) -0.011(3) 0.005(3) -0.001(3) C(251) 0.029(3) 0.017(3) 0.023(3) -0.004(2) 0.006(3) -0.002(2) C(252) 0.030(4) 0.032(3) 0.022(3) 0.000(3) 0.005(3) -0.004(3) C(253) 0.033(4) 0.044(4) 0.027(4) -0.008(3) -0.003(3) -0.009(3) C(254) 0.058(5) 0.035(4) 0.020(4) -0.013(3) 0.003(3) -0.007(3) C(255) 0.055(5) 0.024(3) 0.028(4) -0.006(3) 0.006(3) -0.006(3) C(256) 0.036(4) 0.019(3) 0.027(4) -0.007(3) 0.001(3) -0.007(2) C(261) 0.025(3) 0.017(3) 0.020(3) -0.007(2) 0.004(2) -0.004(2) C(262) 0.033(4) 0.027(3) 0.023(4) 0.001(3) 0.001(3) -0.004(2) C(263) 0.037(4) 0.027(3) 0.029(4) 0.000(3) 0.007(3) -0.006(3) C(264) 0.042(4) 0.035(4) 0.020(4) -0.006(3) 0.010(3) -0.008(3) C(265) 0.050(4) 0.030(3) 0.022(4) -0.009(3) 0.000(3) -0.003(3) C(266) 0.034(4) 0.024(3) 0.022(4) -0.004(3) -0.003(3) 0.001(3) C(901) 0.086(7) 0.063(5) 0.052(7) -0.011(5) 0.014(4) 0.012(4) C(902) 0.084(7) 0.059(5) 0.070(9) -0.004(5) 0.032(6) 0.004(4) C(903) 0.070(6) 0.032(4) 0.095(8) -0.004(4) 0.034(6) 0.008(5) C(904) 0.090(7) 0.052(5) 0.069(7) -0.021(5) 0.011(5) 0.017(5) C(905) 0.093(7) 0.037(5) 0.079(7) -0.003(5) 0.041(6) -0.005(5) C(906) 0.077(7) 0.035(5) 0.104(8) -0.006(4) 0.044(6) 0.015(5) C(911) 0.065(5) 0.076(5) 0.054(5) -0.017(4) 0.005(8) 0.006(8) C(912) 0.070(5) 0.071(5) 0.056(6) 0.002(4) -0.003(7) 0.019(7) C(913) 0.091(7) 0.035(4) 0.079(7) -0.006(4) -0.003(6) 0.007(4) C(914) 0.077(7) 0.077(6) 0.074(7) -0.009(5) -0.025(5) 0.000(5) C(915) 0.050(5) 0.073(6) 0.085(7) 0.009(5) -0.004(5) 0.026(5) C(916) 0.049(5) 0.062(5) 0.065(6) -0.005(4) 0.015(5) 0.004(4) C(921) 0.033(4) 0.043(4) 0.087(7) -0.007(3) -0.004(5) 0.014(4) C(922) 0.054(5) 0.031(4) 0.059(5) 0.000(3) 0.003(4) 0.000(3) C(923) 0.062(5) 0.030(4) 0.044(4) -0.001(3) -0.012(4) 0.006(3) C(924) 0.037(4) 0.034(4) 0.059(5) 0.002(3) -0.006(4) 0.012(3) C(925) 0.057(5) 0.048(5) 0.055(5) 0.001(4) 0.002(4) 0.012(4) C(926) 0.048(5) 0.057(5) 0.061(6) -0.015(4) -0.020(4) 0.018(4) C(931) 0.075(7) 0.109(8) 0.095(11) -0.017(6) -0.011(6) 0.000(7) C(932) 0.082(6) 0.104(6) 0.071(6) 0.013(5) -0.001(10) -0.026(10) C(933) 0.077(6) 0.094(6) 0.101(7) -0.005(5) -0.009(9) -0.061(8) C(934) 0.066(5) 0.061(5) 0.097(10) -0.007(5) -0.005(5) -0.001(5) C(935) 0.086(8) 0.065(6) 0.125(9) -0.007(6) -0.032(7) 0.015(6) C(936) 0.113(10) 0.080(8) 0.116(9) -0.016(7) -0.057(8) 0.001(7) C(941) 0.062(7) 0.087(7) 0.091(9) -0.007(5) 0.018(7) 0.014(7) C(942) 0.114(10) 0.052(6) 0.099(9) 0.007(6) -0.044(8) -0.016(6) C(943) 0.181(12) 0.059(5) 0.049(8) 0.005(7) 0.049(9) -0.012(5) C(944) 0.064(8) 0.120(10) 0.123(11) -0.025(7) 0.050(7) -0.035(8) C(945) 0.063(8) 0.183(13) 0.119(12) 0.003(8) -0.032(8) -0.055(10) C(946) 0.091(9) 0.128(9) 0.047(7) 0.027(7) -0.010(7) 0.016(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) 1.927(3) ? Ta N(31) 1.929(5) ? Ta O(2) 1.932(4) ? Ta Cl(1) 2.3696(14) ? Ta Cl(2) 2.3862(14) ? Ta N(41) 2.400(5) ? O(1) C(11) 1.367(6) ? O(2) C(21) 1.360(6) ? N(31) C(32) 1.465(7) ? N(31) C(31) 1.472(7) ? N(41) C(46) 1.331(7) ? N(41) C(42) 1.368(7) ? C(11) C(12) 1.391(7) ? C(11) C(16) 1.423(7) ? C(12) C(13) 1.397(7) ? C(12) C(121) 1.504(7) ? C(13) C(14) 1.389(7) ? C(13) C(131) 1.499(8) ? C(14) C(15) 1.371(7) ? C(15) C(16) 1.421(7) ? C(15) C(151) 1.510(7) ? C(16) C(161) 1.475(7) ? C(21) C(26) 1.410(7) ? C(21) C(22) 1.418(7) ? C(22) C(23) 1.402(7) ? C(22) C(221) 1.483(7) ? C(23) C(24) 1.392(8) ? C(23) C(231) 1.505(8) ? C(24) C(25) 1.392(10) ? C(25) C(26) 1.418(7) ? C(25) C(251) 1.501(9) ? C(26) C(261) 1.501(8) ? C(42) C(43) 1.366(9) ? C(43) C(44) 1.370(9) ? C(44) C(45) 1.380(9) ? C(45) C(46) 1.394(8) ? C(121) C(122) 1.374(7) ? C(121) C(126) 1.396(8) ? C(122) C(123) 1.398(8) ? C(123) C(124) 1.356(14) ? C(124) C(125) 1.383(10) ? C(125) C(126) 1.366(8) ? C(131) C(132) 1.390(8) ? C(131) C(136) 1.402(9) ? C(132) C(133) 1.382(8) ? C(133) C(134) 1.391(9) ? C(134) C(135) 1.392(9) ? C(135) C(136) 1.393(9) ? C(151) C(156) 1.373(8) ? C(151) C(152) 1.387(9) ? C(152) C(153) 1.388(7) ? C(153) C(154) 1.403(9) ? C(154) C(155) 1.395(8) ? C(155) C(156) 1.395(8) ? C(161) C(166) 1.390(8) ? C(161) C(162) 1.405(8) ? C(162) C(163) 1.391(8) ? C(163) C(164) 1.372(9) ? C(164) C(165) 1.383(10) ? C(165) C(166) 1.388(9) ? C(221) C(222) 1.384(7) ? C(221) C(226) 1.397(8) ? C(222) C(223) 1.386(8) ? C(223) C(224) 1.369(9) ? C(224) C(225) 1.379(9) ? C(225) C(226) 1.389(8) ? C(231) C(236) 1.387(8) ? C(231) C(232) 1.402(8) ? C(232) C(233) 1.393(9) ? C(233) C(234) 1.358(12) ? C(234) C(235) 1.366(8) ? C(235) C(236) 1.383(10) ? C(251) C(252) 1.378(8) ? C(251) C(256) 1.382(8) ? C(252) C(253) 1.390(8) ? C(253) C(254) 1.379(9) ? C(254) C(255) 1.380(9) ? C(255) C(256) 1.393(8) ? C(261) C(266) 1.382(8) ? C(261) C(262) 1.383(8) ? C(262) C(263) 1.369(8) ? C(263) C(264) 1.405(9) ? C(264) C(265) 1.365(9) ? C(265) C(266) 1.385(8) ? C(901) C(902) 1.360(11) ? C(901) C(906) 1.377(12) ? C(902) C(903) 1.375(12) ? C(903) C(904) 1.392(12) ? C(904) C(905) 1.366(12) ? C(905) C(906) 1.361(12) ? C(911) C(916) 1.334(12) ? C(911) C(912) 1.389(10) ? C(912) C(913) 1.338(13) ? C(913) C(914) 1.364(12) ? C(914) C(915) 1.382(11) ? C(915) C(916) 1.375(12) ? C(921) C(926) 1.363(11) ? C(921) C(922) 1.382(10) ? C(922) C(923) 1.359(10) ? C(923) C(924) 1.372(10) ? C(924) C(925) 1.384(10) ? C(925) C(926) 1.366(10) ? C(931) C(936) 1.327(14) ? C(931) C(932) 1.348(12) ? C(932) C(933) 1.361(11) ? C(933) C(934) 1.347(11) ? C(934) C(935) 1.342(12) ? C(935) C(936) 1.395(15) ? C(941) C(942) 1.322(14) ? C(941) C(946) 1.322(13) ? C(942) C(943) 1.374(14) ? C(943) C(944) 1.334(15) ? C(944) C(945) 1.323(16) ? C(945) C(946) 1.328(15) ? 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 N(31) 96.61(16) ? O(1) Ta O(2) 167.28(15) ? N(31) Ta O(2) 96.11(17) ? O(1) Ta Cl(1) 90.05(11) ? N(31) Ta Cl(1) 94.46(15) ? O(2) Ta Cl(1) 88.93(12) ? O(1) Ta Cl(2) 90.11(11) ? N(31) Ta Cl(2) 94.79(15) ? O(2) Ta Cl(2) 88.86(12) ? Cl(1) Ta Cl(2) 170.66(5) ? O(1) Ta N(41) 83.51(15) ? N(31) Ta N(41) 179.8(2) ? O(2) Ta N(41) 83.77(15) ? Cl(1) Ta N(41) 85.67(13) ? Cl(2) Ta N(41) 85.08(12) ? C(11) O(1) Ta 160.9(3) ? C(21) O(2) Ta 154.0(3) ? C(32) N(31) C(31) 112.2(5) ? C(32) N(31) Ta 123.5(4) ? C(31) N(31) Ta 124.3(4) ? C(46) N(41) C(42) 117.4(5) ? C(46) N(41) Ta 122.4(4) ? C(42) N(41) Ta 120.2(4) ? O(1) C(11) C(12) 120.3(4) ? O(1) C(11) C(16) 117.8(5) ? C(12) C(11) C(16) 121.9(4) ? C(11) C(12) C(13) 119.2(4) ? C(11) C(12) C(121) 122.0(4) ? C(13) C(12) C(121) 118.7(5) ? C(14) C(13) C(12) 119.1(5) ? C(14) C(13) C(131) 118.1(4) ? C(12) C(13) C(131) 122.8(5) ? C(15) C(14) C(13) 123.1(4) ? C(14) C(15) C(16) 119.2(5) ? C(14) C(15) C(151) 118.0(5) ? C(16) C(15) C(151) 122.8(5) ? C(15) C(16) C(11) 117.6(5) ? C(15) C(16) C(161) 120.8(5) ? C(11) C(16) C(161) 121.6(5) ? O(2) C(21) C(26) 119.0(5) ? O(2) C(21) C(22) 118.5(5) ? C(26) C(21) C(22) 122.5(5) ? C(23) C(22) C(21) 118.1(5) ? C(23) C(22) C(221) 120.4(5) ? C(21) C(22) C(221) 121.4(5) ? C(24) C(23) C(22) 119.9(5) ? C(24) C(23) C(231) 116.7(5) ? C(22) C(23) C(231) 123.3(5) ? C(25) C(24) C(23) 121.8(5) ? C(24) C(25) C(26) 120.1(6) ? C(24) C(25) C(251) 117.6(4) ? C(26) C(25) C(251) 122.2(6) ? C(21) C(26) C(25) 117.3(6) ? C(21) C(26) C(261) 122.5(4) ? C(25) C(26) C(261) 120.2(5) ? C(43) C(42) N(41) 123.0(6) ? C(42) C(43) C(44) 119.2(7) ? C(43) C(44) C(45) 118.8(6) ? C(44) C(45) C(46) 119.4(6) ? N(41) C(46) C(45) 122.1(6) ? C(122) C(121) C(126) 118.3(5) ? C(122) C(121) C(12) 120.4(5) ? C(126) C(121) C(12) 121.2(6) ? C(121) C(122) C(123) 119.8(7) ? C(124) C(123) C(122) 121.5(9) ? C(123) C(124) C(125) 118.7(7) ? C(126) C(125) C(124) 120.7(7) ? C(125) C(126) C(121) 121.0(6) ? C(132) C(131) C(136) 119.1(6) ? C(132) C(131) C(13) 121.7(5) ? C(136) C(131) C(13) 119.2(5) ? C(133) C(132) C(131) 120.9(6) ? C(132) C(133) C(134) 120.0(6) ? C(133) C(134) C(135) 119.8(6) ? C(134) C(135) C(136) 120.1(6) ? C(135) C(136) C(131) 120.0(6) ? C(156) C(151) C(152) 118.5(6) ? C(156) C(151) C(15) 123.2(5) ? C(152) C(151) C(15) 118.1(5) ? C(151) C(152) C(153) 122.0(8) ? C(152) C(153) C(154) 119.6(7) ? C(155) C(154) C(153) 118.0(5) ? C(154) C(155) C(156) 121.2(6) ? C(151) C(156) C(155) 120.7(6) ? C(166) C(161) C(162) 118.6(6) ? C(166) C(161) C(16) 120.9(5) ? C(162) C(161) C(16) 120.5(5) ? C(163) C(162) C(161) 120.0(6) ? C(164) C(163) C(162) 121.2(7) ? C(163) C(164) C(165) 118.9(7) ? C(164) C(165) C(166) 121.2(7) ? C(165) C(166) C(161) 120.2(6) ? C(222) C(221) C(226) 118.0(5) ? C(222) C(221) C(22) 121.8(5) ? C(226) C(221) C(22) 120.1(5) ? C(221) C(222) C(223) 120.9(6) ? C(224) C(223) C(222) 121.3(6) ? C(223) C(224) C(225) 118.3(7) ? C(224) C(225) C(226) 121.4(6) ? C(225) C(226) C(221) 120.1(6) ? C(236) C(231) C(232) 118.9(6) ? C(236) C(231) C(23) 121.8(6) ? C(232) C(231) C(23) 119.2(5) ? C(233) C(232) C(231) 119.5(6) ? C(234) C(233) C(232) 120.6(7) ? C(233) C(234) C(235) 120.2(9) ? C(234) C(235) C(236) 120.9(9) ? C(235) C(236) C(231) 119.9(7) ? C(252) C(251) C(256) 118.4(5) ? C(252) C(251) C(25) 120.7(5) ? C(256) C(251) C(25) 120.8(5) ? C(251) C(252) C(253) 121.4(6) ? C(254) C(253) C(252) 119.2(6) ? C(253) C(254) C(255) 120.7(6) ? C(254) C(255) C(256) 119.0(6) ? C(251) C(256) C(255) 121.3(6) ? C(266) C(261) C(262) 118.9(5) ? C(266) C(261) C(26) 120.8(5) ? C(262) C(261) C(26) 120.1(5) ? C(263) C(262) C(261) 121.0(6) ? C(262) C(263) C(264) 120.0(6) ? C(265) C(264) C(263) 118.7(6) ? C(264) C(265) C(266) 121.2(6) ? C(261) C(266) C(265) 120.1(6) ? C(902) C(901) C(906) 119.6(9) ? C(901) C(902) C(903) 120.6(9) ? C(902) C(903) C(904) 119.3(9) ? C(905) C(904) C(903) 119.7(10) ? C(906) C(905) C(904) 120.2(9) ? C(905) C(906) C(901) 120.6(9) ? C(916) C(911) C(912) 120.1(11) ? C(913) C(912) C(911) 120.3(10) ? C(912) C(913) C(914) 120.6(8) ? C(913) C(914) C(915) 118.8(9) ? C(916) C(915) C(914) 120.4(8) ? C(911) C(916) C(915) 119.6(9) ? C(926) C(921) C(922) 119.6(7) ? C(923) C(922) C(921) 120.0(7) ? C(922) C(923) C(924) 120.9(7) ? C(923) C(924) C(925) 118.7(7) ? C(926) C(925) C(924) 120.4(8) ? C(921) C(926) C(925) 120.3(8) ? C(936) C(931) C(932) 118.9(10) ? C(931) C(932) C(933) 121.0(9) ? C(934) C(933) C(932) 119.2(8) ? C(935) C(934) C(933) 121.8(9) ? C(934) C(935) C(936) 117.1(10) ? C(931) C(936) C(935) 122.0(11) ? C(942) C(941) C(946) 120.6(11) ? C(941) C(942) C(943) 119.5(11) ? C(944) C(943) C(942) 119.0(11) ? C(945) C(944) C(943) 119.7(10) ? C(944) C(945) C(946) 121.1(11) ? C(941) C(946) C(945) 119.9(11) ? #===END #============================================================================== data_SS3217 _database_code_CSD 159030 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C35 H37 Cl2 N2 O2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 769.55 _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 10.0975(2) _cell_length_b 11.1400(2) _cell_length_c 15.5664(3) _cell_angle_alpha 80.5543(8) _cell_angle_beta 84.6022(8) _cell_angle_gamma 67.3869(7) _cell_volume 1593.55(8) _cell_measurement_reflns_used 16611 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.60 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.610 _cell_measurement_temperature 150 _exptl_crystal_F_000 768 # 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 0.3673 _exptl_absorpt_correction_T_max 0.5819 _diffrn_reflns_number 16611 _reflns_number_total 7190 _reflns_number_gt 6802 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 14 _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 0.027 _refine_ls_wR_factor_ref 0.058 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding, U=1.3*Ueq of bonding atom ; _refine_ls_number_reflns 7189 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0168P)^2^+0.6727P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.017 _refine_diff_density_max 1.11 _refine_diff_density_min -1.24 _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 0.098940(13) 0.191788(11) 0.319929(7) 0.01696(4) Uani ? Cl(1) -0.14055(9) 0.27628(8) 0.38323(5) 0.0293(2) Uani ? Cl(2) 0.02357(9) 0.05002(8) 0.25127(5) 0.0258(2) Uani ? O(1) 0.2684(2) 0.1455(2) 0.24808(12) 0.0226(7) Uani ? O(2) 0.1399(2) 0.32408(19) 0.36035(13) 0.0197(6) Uani ? N(4) 0.1725(3) 0.0577(2) 0.42083(15) 0.0212(8) Uani ? N(3A) -0.0154(8) 0.3759(7) 0.2148(5) 0.024(2) Uani ? N(3B) 0.0154(8) 0.3307(7) 0.1876(4) 0.024(2) Uani ? C(11) 0.3997(3) 0.1479(3) 0.21840(18) 0.0186(9) Uani ? C(12) 0.4396(3) 0.1422(3) 0.12922(18) 0.0210(9) Uani ? C(13) 0.5773(4) 0.1376(3) 0.1030(2) 0.0256(10) Uani ? C(14) 0.6712(4) 0.1407(3) 0.1607(2) 0.0286(11) Uani ? C(15) 0.6265(3) 0.1534(3) 0.2469(2) 0.0237(10) Uani ? C(16) 0.4919(3) 0.1575(3) 0.27745(18) 0.0195(9) Uani ? C(1B) 0.4451(3) 0.1770(3) 0.37112(19) 0.0236(10) Uani ? C(21) 0.2245(3) 0.3899(3) 0.37315(17) 0.0191(9) Uani ? C(22) 0.1599(4) 0.5260(3) 0.37727(18) 0.0218(10) Uani ? C(23) 0.2475(4) 0.5895(3) 0.3941(2) 0.0285(11) Uani ? C(24) 0.3924(4) 0.5223(4) 0.4063(2) 0.0363(12) Uani ? C(25) 0.4549(4) 0.3893(4) 0.3995(2) 0.0310(11) Uani ? C(26) 0.3726(3) 0.3209(3) 0.38260(18) 0.0221(10) Uani ? C(31) -0.1288(6) 0.3777(5) 0.1645(4) 0.0592(18) Uani ? C(32) 0.0820(4) 0.4309(4) 0.1633(2) 0.0309(12) Uani ? C(41) 0.2654(4) -0.0790(3) 0.4158(2) 0.0323(11) Uani ? C(42) 0.1493(4) 0.0863(3) 0.51083(19) 0.0300(11) Uani ? C(121) 0.3393(3) 0.1497(3) 0.06258(18) 0.0221(10) Uani ? C(122) 0.2431(4) 0.0859(3) 0.0774(2) 0.0274(11) Uani ? C(123) 0.1472(4) 0.1004(4) 0.0143(2) 0.0354(12) Uani ? C(124) 0.1490(4) 0.1760(4) -0.0652(2) 0.0397(12) Uani ? C(125) 0.2447(5) 0.2372(4) -0.0819(2) 0.0391(14) Uani ? C(126) 0.3392(4) 0.2254(3) -0.0187(2) 0.0314(11) Uani ? C(221) 0.0051(4) 0.6032(3) 0.36211(18) 0.0206(10) Uani ? C(222) -0.0364(4) 0.7251(3) 0.3094(2) 0.0303(11) Uani ? C(223) -0.1798(5) 0.8013(3) 0.2964(2) 0.0395(14) Uani ? C(224) -0.2844(4) 0.7572(4) 0.3354(2) 0.0390(12) Uani ? C(225) -0.2459(4) 0.6375(3) 0.3881(2) 0.0321(12) Uani ? C(226) -0.1019(3) 0.5605(3) 0.40123(18) 0.0216(10) Uani ? C(901) 0.5327(7) 0.4009(9) 0.8107(4) 0.108(3) Uani ? C(902) 0.6404(7) 0.2789(6) 0.8200(3) 0.083(3) Uani ? C(903) 0.7453(6) 0.2499(4) 0.8761(3) 0.0548(16) Uani ? C(904) 0.7453(7) 0.3390(6) 0.9257(4) 0.075(2) Uani ? C(905) 0.6395(9) 0.4593(7) 0.9180(8) 0.138(5) Uani ? C(906) 0.5334(9) 0.4915(6) 0.8587(8) 0.141(4) Uani ? H(13) 0.6067 0.1322 0.0448 0.0330 Uiso calc H(14) 0.7635 0.1345 0.1420 0.0370 Uiso calc H(15) 0.6886 0.1592 0.2851 0.0310 Uiso calc H(23) 0.2075 0.6792 0.3971 0.0370 Uiso calc H(24) 0.4484 0.5662 0.4192 0.0470 Uiso calc H(25) 0.5532 0.3453 0.4064 0.0400 Uiso calc H(3A) -0.0636 0.4392 0.2490 0.0310 Uiso calc H(3B) 0.0588 0.2749 0.1478 0.0310 Uiso calc H(122) 0.2429 0.0329 0.1302 0.0360 Uiso calc H(123) 0.0818 0.0592 0.0257 0.0460 Uiso calc H(124) 0.0851 0.1852 -0.1074 0.0520 Uiso calc H(125) 0.2465 0.2871 -0.1357 0.0510 Uiso calc H(126) 0.4032 0.2682 -0.0306 0.0410 Uiso calc H(1B1) 0.5284 0.1367 0.4073 0.0310 Uiso calc H(1B2) 0.3792 0.1330 0.3909 0.0310 Uiso calc H(222) 0.0334 0.7554 0.2827 0.0400 Uiso calc H(223) -0.2058 0.8824 0.2613 0.0510 Uiso calc H(224) -0.3808 0.8081 0.3262 0.0500 Uiso calc H(225) -0.3164 0.6083 0.4148 0.0420 Uiso calc H(226) -0.0767 0.4797 0.4365 0.0280 Uiso calc H(31A) -0.163(6) 0.438(5) 0.213(3) 0.0760 Uiso ? H(31B) -0.183(6) 0.328(5) 0.187(3) 0.0760 Uiso ? H(31C) -0.152(6) 0.436(5) 0.119(3) 0.0760 Uiso ? H(32A) 0.182(5) 0.388(4) 0.167(2) 0.0400 Uiso ? H(32B) 0.068(4) 0.488(4) 0.201(3) 0.0400 Uiso ? H(32C) 0.051(4) 0.484(4) 0.110(3) 0.0400 Uiso ? H(41A) 0.3591 -0.0952 0.4350 0.0420 Uiso calc H(41B) 0.2727 -0.0959 0.3567 0.0420 Uiso calc H(41C) 0.2255 -0.1358 0.4524 0.0420 Uiso calc H(42A) 0.1054 0.0307 0.5450 0.0390 Uiso calc H(42B) 0.0875 0.1766 0.5117 0.0390 Uiso calc H(42C) 0.2397 0.0703 0.5347 0.0390 Uiso calc H(901) 0.4600 0.4211 0.7720 0.1420 Uiso calc H(902) 0.6410 0.2159 0.7873 0.1080 Uiso calc H(903) 0.8189 0.1674 0.8810 0.0710 Uiso calc H(904) 0.8177 0.3174 0.9649 0.0980 Uiso calc H(905) 0.6380 0.5206 0.9525 0.1800 Uiso calc H(906) 0.4625 0.5754 0.8518 0.1830 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 0.01477(7) 0.01901(7) 0.01965(7) -0.00892(5) 0.00012(5) -0.00366(4) Cl(1) 0.0179(4) 0.0325(4) 0.0429(4) -0.0133(3) 0.0073(3) -0.0150(3) Cl(2) 0.0249(4) 0.0310(4) 0.0290(4) -0.0165(3) -0.0001(3) -0.0102(3) O(1) 0.0201(12) 0.0305(12) 0.0192(10) -0.0122(10) -0.0016(9) -0.0016(8) O(2) 0.0146(11) 0.0193(10) 0.0267(10) -0.0083(9) -0.0013(8) -0.0025(8) N(4) 0.0238(15) 0.0227(13) 0.0186(12) -0.0100(11) 0.0017(10) -0.0050(10) N(3A) 0.019(4) 0.023(4) 0.029(4) -0.008(3) -0.005(3) -0.002(3) N(3B) 0.025(4) 0.021(4) 0.025(4) -0.007(3) -0.009(3) -0.004(2) C(11) 0.0129(15) 0.0166(14) 0.0252(14) -0.0052(12) 0.0038(12) -0.0033(11) C(12) 0.0238(17) 0.0165(14) 0.0216(14) -0.0064(12) 0.0024(12) -0.0043(11) C(13) 0.0227(18) 0.0261(16) 0.0276(15) -0.0093(14) 0.0079(13) -0.0075(13) C(14) 0.0174(17) 0.0267(17) 0.0412(18) -0.0077(14) 0.0067(14) -0.0089(14) C(15) 0.0156(16) 0.0219(15) 0.0326(16) -0.0050(13) -0.0010(13) -0.0062(12) C(16) 0.0143(15) 0.0175(14) 0.0251(14) -0.0041(12) -0.0007(12) -0.0035(11) C(1B) 0.0152(16) 0.0313(17) 0.0236(15) -0.0071(13) -0.0048(12) -0.0034(12) C(21) 0.0204(16) 0.0270(16) 0.0160(13) -0.0153(13) 0.0016(11) -0.0048(11) C(22) 0.0285(18) 0.0262(16) 0.0173(13) -0.0175(14) 0.0043(12) -0.0056(11) C(23) 0.035(2) 0.0315(18) 0.0306(16) -0.0233(16) 0.0077(15) -0.0139(13) C(24) 0.036(2) 0.054(2) 0.0379(19) -0.0333(19) 0.0064(16) -0.0217(17) C(25) 0.0188(18) 0.051(2) 0.0319(17) -0.0186(16) 0.0041(14) -0.0186(15) C(26) 0.0188(17) 0.0338(17) 0.0182(13) -0.0132(14) 0.0005(12) -0.0081(12) C(31) 0.054(3) 0.053(3) 0.072(3) -0.025(2) -0.042(3) 0.022(2) C(32) 0.036(2) 0.0283(19) 0.0278(17) -0.0137(16) -0.0057(16) 0.0047(14) C(41) 0.042(2) 0.0210(17) 0.0301(17) -0.0076(15) -0.0049(16) -0.0020(13) C(42) 0.039(2) 0.0329(18) 0.0187(14) -0.0143(16) 0.0012(14) -0.0043(13) C(121) 0.0206(17) 0.0210(15) 0.0214(14) -0.0028(13) 0.0014(12) -0.0077(11) C(122) 0.030(2) 0.0347(18) 0.0207(14) -0.0144(15) 0.0021(13) -0.0085(13) C(123) 0.031(2) 0.051(2) 0.0299(17) -0.0182(18) 0.0010(15) -0.0151(16) C(124) 0.038(2) 0.049(2) 0.0286(17) -0.0077(19) -0.0089(16) -0.0131(16) C(125) 0.054(3) 0.035(2) 0.0224(16) -0.0097(18) -0.0071(16) -0.0019(14) C(126) 0.039(2) 0.0280(18) 0.0265(16) -0.0122(16) 0.0026(15) -0.0049(13) C(221) 0.0268(18) 0.0196(15) 0.0178(13) -0.0102(13) 0.0014(12) -0.0071(11) C(222) 0.046(2) 0.0221(17) 0.0223(15) -0.0129(16) 0.0044(15) -0.0045(12) C(223) 0.058(3) 0.0248(18) 0.0233(16) -0.0013(17) -0.0058(17) -0.0025(13) C(224) 0.035(2) 0.037(2) 0.0319(18) 0.0056(17) -0.0086(16) -0.0126(15) C(225) 0.0229(19) 0.039(2) 0.0334(17) -0.0087(15) -0.0001(14) -0.0104(15) C(226) 0.0226(17) 0.0219(15) 0.0204(14) -0.0079(13) 0.0001(12) -0.0048(11) C(901) 0.062(4) 0.128(6) 0.077(4) -0.001(5) 0.019(3) 0.047(4) C(902) 0.080(4) 0.102(5) 0.046(3) -0.009(4) 0.012(3) -0.023(3) C(903) 0.061(3) 0.036(2) 0.057(3) -0.011(2) 0.011(2) -0.0036(19) C(904) 0.064(4) 0.076(4) 0.100(4) -0.042(3) 0.033(3) -0.036(3) C(905) 0.085(6) 0.082(5) 0.280(12) -0.059(5) 0.103(7) -0.106(7) C(906) 0.060(5) 0.033(3) 0.272(13) 0.007(3) 0.060(6) 0.036(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 Ta O(2) 1.8868(19) ? Ta O(1) 1.896(2) ? Ta N(4) 1.961(2) ? Ta N(3B) 2.372(7) ? Ta N(3A) 2.377(7) ? Ta Cl(1) 2.4105(8) ? Ta Cl(2) 2.4180(7) ? O(1) C(11) 1.371(4) ? O(2) C(21) 1.367(3) ? N(3A) C(31) 1.439(8) ? N(3A) C(32) 1.462(8) ? N(3B) C(31) 1.405(9) ? N(3B) C(32) 1.494(8) ? N(4) C(41) 1.460(4) ? N(4) C(42) 1.465(4) ? C(11) C(16) 1.412(4) ? C(11) C(12) 1.413(4) ? C(12) C(13) 1.396(4) ? C(12) C(121) 1.487(4) ? C(13) C(14) 1.380(5) ? C(14) C(15) 1.387(4) ? C(15) C(16) 1.383(4) ? C(16) C(1B) 1.514(4) ? C(1B) C(26) 1.517(4) ? C(21) C(26) 1.404(4) ? C(21) C(22) 1.411(4) ? C(22) C(23) 1.392(4) ? C(22) C(221) 1.486(5) ? C(23) C(24) 1.379(5) ? C(24) C(25) 1.387(5) ? C(25) C(26) 1.391(4) ? C(121) C(122) 1.392(5) ? C(121) C(126) 1.401(4) ? C(122) C(123) 1.390(5) ? C(123) C(124) 1.381(5) ? C(124) C(125) 1.366(6) ? C(125) C(126) 1.390(5) ? C(221) C(226) 1.393(4) ? C(221) C(222) 1.399(4) ? C(222) C(223) 1.382(5) ? C(223) C(224) 1.381(6) ? C(224) C(225) 1.379(5) ? C(225) C(226) 1.390(5) ? C(901) C(906) 1.353(13) ? C(901) C(902) 1.371(9) ? C(902) C(903) 1.345(7) ? C(903) C(904) 1.354(7) ? C(904) C(905) 1.350(10) ? C(905) C(906) 1.382(13) ? 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) 92.15(9) ? O(2) Ta N(4) 96.08(9) ? O(1) Ta N(4) 98.20(10) ? O(2) Ta N(3B) 90.84(18) ? O(1) Ta N(3B) 78.5(2) ? N(4) Ta N(3B) 172.47(18) ? O(2) Ta N(3A) 78.80(18) ? O(1) Ta N(3A) 90.05(19) ? N(4) Ta N(3A) 170.49(19) ? N(3B) Ta N(3A) 16.31(16) ? O(2) Ta Cl(1) 89.77(7) ? O(1) Ta Cl(1) 167.93(6) ? N(4) Ta Cl(1) 93.44(8) ? N(3B) Ta Cl(1) 89.55(19) ? N(3A) Ta Cl(1) 78.64(18) ? O(2) Ta Cl(2) 170.88(6) ? O(1) Ta Cl(2) 88.67(7) ? N(4) Ta Cl(2) 92.80(7) ? N(3B) Ta Cl(2) 80.42(17) ? N(3A) Ta Cl(2) 92.11(17) ? Cl(1) Ta Cl(2) 87.58(3) ? C(11) O(1) Ta 154.51(19) ? C(21) O(2) Ta 155.2(2) ? C(31) N(3A) C(32) 112.8(5) ? C(31) N(3A) Ta 120.3(4) ? C(32) N(3A) Ta 114.4(4) ? C(31) N(3B) C(32) 112.9(5) ? C(31) N(3B) Ta 122.4(5) ? C(32) N(3B) Ta 113.3(4) ? C(41) N(4) C(42) 111.7(2) ? C(41) N(4) Ta 124.81(19) ? C(42) N(4) Ta 123.3(2) ? O(1) C(11) C(16) 119.3(3) ? O(1) C(11) C(12) 119.4(3) ? C(16) C(11) C(12) 121.3(3) ? C(13) C(12) C(11) 117.4(3) ? C(13) C(12) C(121) 119.3(3) ? C(11) C(12) C(121) 123.2(3) ? C(14) C(13) C(12) 122.0(3) ? C(13) C(14) C(15) 119.4(3) ? C(16) C(15) C(14) 121.6(3) ? C(15) C(16) C(11) 118.2(3) ? C(15) C(16) C(1B) 119.9(3) ? C(11) C(16) C(1B) 121.8(3) ? C(16) C(1B) C(26) 112.6(2) ? O(2) C(21) C(26) 119.5(3) ? O(2) C(21) C(22) 118.9(3) ? C(26) C(21) C(22) 121.6(3) ? C(23) C(22) C(21) 117.7(3) ? C(23) C(22) C(221) 119.4(3) ? C(21) C(22) C(221) 122.8(3) ? C(24) C(23) C(22) 121.4(3) ? C(23) C(24) C(25) 120.2(3) ? C(24) C(25) C(26) 120.9(3) ? C(25) C(26) C(21) 118.2(3) ? C(25) C(26) C(1B) 119.7(3) ? C(21) C(26) C(1B) 122.1(3) ? N(3B) C(31) N(3A) 27.4(3) ? N(3A) C(32) N(3B) 26.3(3) ? C(122) C(121) C(126) 117.8(3) ? C(122) C(121) C(12) 123.0(3) ? C(126) C(121) C(12) 119.2(3) ? C(123) C(122) C(121) 120.8(3) ? C(124) C(123) C(122) 120.2(3) ? C(125) C(124) C(123) 120.0(3) ? C(124) C(125) C(126) 120.4(3) ? C(125) C(126) C(121) 120.8(3) ? C(226) C(221) C(222) 118.2(3) ? C(226) C(221) C(22) 122.2(3) ? C(222) C(221) C(22) 119.6(3) ? C(223) C(222) C(221) 120.9(3) ? C(224) C(223) C(222) 120.1(3) ? C(225) C(224) C(223) 120.0(4) ? C(224) C(225) C(226) 120.2(3) ? C(225) C(226) C(221) 120.7(3) ? C(906) C(901) C(902) 119.2(8) ? C(903) C(902) C(901) 120.3(7) ? C(902) C(903) C(904) 121.0(5) ? C(905) C(904) C(903) 119.6(7) ? C(904) C(905) C(906) 119.9(7) ? C(901) C(906) C(905) 120.0(6) ? #===END