# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Phillip E. Fanwick' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Dr. W. Lafayette IN 47907-2084 USA ; _publ_contact_author_email pfanwick@.purdue.edu _publ_contact_author_fax 1(765)4940239 _publ_contact_author_phone 1(765)4944572 _publ_section_title ; Regioselective insertion of 2-vinylpyridine in niobium and tantalum aryloxide complexes: an alternate route to pyridylalkyl metallacycles ; _publ_section_references ; P. T. Beurskens, G. Beurskens, R. deGelder,S. Garcia-Granda, R. O. Gould, R. Israel, J. M. M. Smits, '(1999). The DIRDIF-99 Program System. 'Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. 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. (1997). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of Gottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; loop_ _publ_author_name 'Rex Corbin' 'Brandon E. Dusick' 'Phillip E. Fanwick' 'Khamphee Phomphrai' 'Ian Rothwell' data_RCI035 _database_code_depnum_ccdc_archive 'CCDC 255067' _audit_creation_date 22-07-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C38 H48 Br2 Cl1 N2 O2 Ta1' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_weight 941.04 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2625(7) _cell_length_b 12.7572(8) _cell_length_c 14.0939(11) _cell_angle_alpha 111.989(3) _cell_angle_beta 101.730(4) _cell_angle_gamma 102.100(3) _cell_volume 1900.0(2) _cell_measurement_reflns_used 12828 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 5.046 _cell_measurement_temperature 150 _exptl_crystal_F_000 932 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.2517 _exptl_absorpt_correction_T_max 0.5322 _diffrn_reflns_number 12828 _diffrn_measured_fraction_theta_max 0.5174 _reflns_number_total 8833 _reflns_number_gt 7497 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 17 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.60' # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.084 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 8833 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.46 _refine_diff_density_min -2.04 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta 0.197612(17) 0.425452(18) 0.248876(17) 0.02028(7) Uani 1 1 d . . . Br(34) Br 0.39838(6) -0.13436(6) 0.17527(6) 0.05144(18) Uani 1 1 d . . . Br(44) Br 0.20032(5) 1.06373(5) 0.63312(5) 0.03658(14) Uani 1 1 d . . . Cl Cl 0.28946(10) 0.43330(11) 0.42836(10) 0.0271(3) Uani 1 1 d . . . O(3) O 0.2094(3) 0.2691(3) 0.1880(3) 0.0224(7) Uani 1 1 d . . . O(4) O 0.2008(3) 0.5851(3) 0.3216(3) 0.0229(7) Uani 1 1 d . . . N(11) N 0.3857(3) 0.4903(4) 0.2581(3) 0.0236(9) Uani 1 1 d . . . N(21) N 0.0336(3) 0.3739(4) 0.2924(3) 0.0238(9) Uani 1 1 d . . . C(12) C 0.3694(4) 0.5227(4) 0.1783(4) 0.0262(11) Uani 1 1 d . . . C(13) C 0.4644(5) 0.5934(5) 0.1653(5) 0.0366(14) Uani 1 1 d . . . C(14) C 0.5757(5) 0.6207(5) 0.2340(5) 0.0387(14) Uani 1 1 d . . . C(15) C 0.5909(5) 0.5831(5) 0.3141(5) 0.0357(14) Uani 1 1 d . . . C(16) C 0.4938(4) 0.5179(5) 0.3254(4) 0.0291(12) Uani 1 1 d . . . C(17) C 0.2414(4) 0.4724(5) 0.1169(4) 0.0254(11) Uani 1 1 d . . . C(18) C 0.1900(5) 0.5523(5) 0.0783(5) 0.0375(14) Uani 1 1 d . . . C(22) C -0.0446(4) 0.3240(5) 0.1940(4) 0.0300(12) Uani 1 1 d . . . C(23) C -0.1600(5) 0.2625(6) 0.1768(5) 0.0454(16) Uani 1 1 d . . . C(24) C -0.1933(5) 0.2577(6) 0.2623(6) 0.0484(17) Uani 1 1 d . . . C(25) C -0.1114(5) 0.3124(5) 0.3645(5) 0.0383(14) Uani 1 1 d . . . C(26) C 0.0025(5) 0.3690(5) 0.3769(4) 0.0299(12) Uani 1 1 d . . . C(27) C 0.0191(4) 0.3503(5) 0.1207(4) 0.0265(11) Uani 1 1 d . . . C(28) C -0.0078(5) 0.2423(5) 0.0152(4) 0.0402(15) Uani 1 1 d . . . C(31) C 0.2492(4) 0.1747(4) 0.1815(4) 0.0226(11) Uani 1 1 d . . . C(32) C 0.3309(4) 0.1500(4) 0.1257(4) 0.0253(11) Uani 1 1 d . . . C(33) C 0.3707(4) 0.0550(5) 0.1219(4) 0.0323(13) Uani 1 1 d . . . C(34) C 0.3332(4) -0.0118(4) 0.1733(5) 0.0324(13) Uani 1 1 d . . . C(35) C 0.2511(5) 0.0105(4) 0.2261(5) 0.0323(13) Uani 1 1 d . . . C(36) C 0.2074(4) 0.1034(4) 0.2303(4) 0.0254(11) Uani 1 1 d . . . C(41) C 0.2026(4) 0.6949(4) 0.3910(4) 0.0213(10) Uani 1 1 d . . . C(42) C 0.0988(4) 0.7278(4) 0.3769(4) 0.0233(11) Uani 1 1 d . . . C(43) C 0.0995(4) 0.8376(4) 0.4490(4) 0.0255(11) Uani 1 1 d . . . C(44) C 0.2000(4) 0.9141(4) 0.5333(4) 0.0271(11) Uani 1 1 d . . . C(45) C 0.3027(4) 0.8843(4) 0.5462(4) 0.0275(12) Uani 1 1 d . . . C(46) C 0.3059(4) 0.7748(5) 0.4762(4) 0.0265(11) Uani 1 1 d . . . C(321) C 0.5074(5) 0.2626(5) 0.0969(5) 0.0427(15) Uani 1 1 d . . . C(322) C 0.3731(5) 0.2235(5) 0.0687(4) 0.0306(12) Uani 1 1 d . . . C(323) C 0.3155(6) 0.1558(7) -0.0530(5) 0.058(2) Uani 1 1 d . . . C(361) C 0.1317(5) 0.1129(6) 0.3864(5) 0.0431(15) Uani 1 1 d . . . C(362) C 0.1123(4) 0.1234(4) 0.2821(4) 0.0276(12) Uani 1 1 d . . . C(363) C -0.0072(5) 0.0377(5) 0.2012(5) 0.0401(15) Uani 1 1 d . . . C(421) C -0.0488(6) 0.7059(6) 0.2132(5) 0.0462(16) Uani 1 1 d . . . C(422) C -0.0112(4) 0.6459(4) 0.2848(4) 0.0253(11) Uani 1 1 d . . . C(423) C -0.1110(5) 0.6043(5) 0.3244(5) 0.0417(15) Uani 1 1 d . . . C(461) C 0.5152(5) 0.8346(5) 0.4796(5) 0.0454(16) Uani 1 1 d . . . C(462) C 0.4197(5) 0.7457(5) 0.4912(5) 0.0333(13) Uani 1 1 d . . . C(463) C 0.4594(5) 0.7418(5) 0.5993(5) 0.0450(16) Uani 1 1 d . . . H(13) H 0.4529 0.6214 0.1116 0.044 Uiso 1 1 calc R . . H(14) H 0.6421 0.6659 0.2256 0.046 Uiso 1 1 calc R . . H(15) H 0.6672 0.6018 0.3608 0.043 Uiso 1 1 calc R . . H(16) H 0.5029 0.4923 0.3809 0.035 Uiso 1 1 calc R . . H(17) H 0.231(4) 0.401(4) 0.062(4) 0.020(13) Uiso 1 1 d . . . H(23) H -0.2150 0.2243 0.1066 0.054 Uiso 1 1 calc R . . H(24) H -0.2722 0.2171 0.2520 0.058 Uiso 1 1 calc R . . H(25) H -0.1338 0.3106 0.4247 0.046 Uiso 1 1 calc R . . H(26) H 0.0598 0.4050 0.4460 0.036 Uiso 1 1 calc R . . H(27) H 0.001(4) 0.417(4) 0.104(4) 0.020(13) Uiso 1 1 d . . . H(33) H 0.4245 0.0357 0.0835 0.039 Uiso 1 1 calc R . . H(35) H 0.2246 -0.0379 0.2594 0.039 Uiso 1 1 calc R . . H(43) H 0.0306 0.8605 0.4405 0.031 Uiso 1 1 calc R . . H(45) H 0.3714 0.9391 0.6033 0.033 Uiso 1 1 calc R . . H(18A) H 0.1940 0.6233 0.1405 0.056 Uiso 1 1 calc R . . H(18B) H 0.1079 0.5093 0.0339 0.056 Uiso 1 1 calc R . . H(18C) H 0.2347 0.5763 0.0355 0.056 Uiso 1 1 calc R . . H(28A) H 0.0061 0.1761 0.0297 0.060 Uiso 1 1 calc R . . H(28B) H 0.0431 0.2615 -0.0253 0.060 Uiso 1 1 calc R . . H(28C) H -0.0901 0.2195 -0.0272 0.060 Uiso 1 1 calc R . . H(322) H 0.3492 0.2970 0.0942 0.037 Uiso 1 1 calc R . . H(32A) H 0.5429 0.3030 0.1753 0.064 Uiso 1 1 calc R . . H(32B) H 0.5322 0.3172 0.0659 0.064 Uiso 1 1 calc R . . H(32C) H 0.5328 0.1924 0.0674 0.064 Uiso 1 1 calc R . . H(32D) H 0.3400 0.0848 -0.0806 0.087 Uiso 1 1 calc R . . H(32E) H 0.3395 0.2073 -0.0870 0.087 Uiso 1 1 calc R . . H(32F) H 0.2299 0.1319 -0.0695 0.087 Uiso 1 1 calc R . . H(362) H 0.1110 0.2063 0.2978 0.033 Uiso 1 1 calc R . . H(36A) H 0.1236 0.0300 0.3725 0.065 Uiso 1 1 calc R . . H(36B) H 0.0735 0.1380 0.4203 0.065 Uiso 1 1 calc R . . H(36C) H 0.2107 0.1639 0.4346 0.065 Uiso 1 1 calc R . . H(36D) H -0.0093 -0.0446 0.1849 0.060 Uiso 1 1 calc R . . H(36E) H -0.0190 0.0481 0.1348 0.060 Uiso 1 1 calc R . . H(36F) H -0.0697 0.0548 0.2323 0.060 Uiso 1 1 calc R . . H(422) H 0.0069 0.5740 0.2399 0.030 Uiso 1 1 calc R . . H(42A) H -0.0725 0.7736 0.2539 0.069 Uiso 1 1 calc R . . H(42B) H -0.1151 0.6483 0.1498 0.069 Uiso 1 1 calc R . . H(42C) H 0.0170 0.7341 0.1901 0.069 Uiso 1 1 calc R . . H(42D) H -0.0867 0.5630 0.3672 0.063 Uiso 1 1 calc R . . H(42E) H -0.1800 0.5497 0.2625 0.063 Uiso 1 1 calc R . . H(42F) H -0.1303 0.6733 0.3690 0.063 Uiso 1 1 calc R . . H(462) H 0.4056 0.6648 0.4332 0.040 Uiso 1 1 calc R . . H(46A) H 0.5346 0.9138 0.5387 0.068 Uiso 1 1 calc R . . H(46B) H 0.4868 0.8375 0.4107 0.068 Uiso 1 1 calc R . . H(46C) H 0.5855 0.8093 0.4819 0.068 Uiso 1 1 calc R . . H(46D) H 0.4731 0.8200 0.6577 0.068 Uiso 1 1 calc R . . H(46E) H 0.5323 0.7210 0.6061 0.068 Uiso 1 1 calc R . . H(46F) H 0.3985 0.6818 0.6035 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.01846(10) 0.02254(10) 0.01943(11) 0.00546(7) 0.00433(7) 0.01006(8) Br(34) 0.0589(4) 0.0368(3) 0.0700(5) 0.0295(3) 0.0263(4) 0.0241(3) Br(44) 0.0403(3) 0.0286(3) 0.0336(3) 0.0110(2) 0.0128(3) 0.0054(2) Cl 0.0271(6) 0.0311(6) 0.0220(7) 0.0066(5) 0.0026(5) 0.0142(5) O(3) 0.0202(17) 0.0277(18) 0.0184(18) 0.0053(14) 0.0067(14) 0.0099(15) O(4) 0.0192(17) 0.0287(18) 0.0173(18) 0.0063(14) 0.0021(14) 0.0089(15) N(11) 0.018(2) 0.028(2) 0.022(2) 0.0052(17) 0.0049(17) 0.0107(19) N(21) 0.018(2) 0.032(2) 0.027(2) 0.0091(18) 0.0109(18) 0.015(2) C(12) 0.025(3) 0.028(3) 0.027(3) 0.009(2) 0.009(2) 0.013(2) C(13) 0.036(3) 0.039(3) 0.045(4) 0.012(3) 0.018(3) 0.026(3) C(14) 0.028(3) 0.040(3) 0.047(4) 0.004(3) 0.015(3) 0.020(3) C(15) 0.022(3) 0.042(3) 0.038(4) 0.009(2) 0.009(2) 0.013(3) C(16) 0.023(3) 0.035(3) 0.029(3) 0.011(2) 0.005(2) 0.015(2) C(17) 0.028(3) 0.028(3) 0.023(3) 0.009(2) 0.007(2) 0.015(2) C(18) 0.037(3) 0.041(3) 0.044(4) 0.010(3) 0.012(3) 0.029(3) C(22) 0.028(3) 0.040(3) 0.027(3) 0.016(2) 0.010(2) 0.016(3) C(23) 0.028(3) 0.055(4) 0.038(4) 0.004(3) 0.005(3) 0.011(3) C(24) 0.025(3) 0.061(4) 0.066(5) 0.009(3) 0.018(3) 0.035(4) C(25) 0.041(3) 0.054(4) 0.039(4) 0.022(3) 0.023(3) 0.031(3) C(26) 0.030(3) 0.041(3) 0.023(3) 0.015(2) 0.010(2) 0.015(3) C(27) 0.019(2) 0.028(3) 0.017(3) 0.001(2) -0.0098(19) 0.005(2) C(28) 0.035(3) 0.045(3) 0.026(3) 0.001(3) 0.004(3) 0.010(3) C(31) 0.024(3) 0.019(2) 0.020(3) 0.005(2) 0.005(2) 0.006(2) C(32) 0.026(3) 0.025(3) 0.020(3) 0.006(2) 0.005(2) 0.007(2) C(33) 0.026(3) 0.030(3) 0.032(3) 0.008(2) 0.009(2) 0.005(2) C(34) 0.025(3) 0.022(3) 0.041(3) 0.006(2) 0.007(2) 0.006(2) C(35) 0.033(3) 0.022(3) 0.037(3) 0.006(2) 0.010(3) 0.010(2) C(36) 0.023(3) 0.020(2) 0.024(3) 0.001(2) 0.003(2) 0.006(2) C(41) 0.026(3) 0.018(2) 0.019(3) 0.0038(19) 0.006(2) 0.009(2) C(42) 0.026(3) 0.027(3) 0.019(3) 0.010(2) 0.008(2) 0.011(2) C(43) 0.023(3) 0.025(3) 0.030(3) 0.007(2) 0.009(2) 0.013(2) C(44) 0.031(3) 0.030(3) 0.025(3) 0.011(2) 0.012(2) 0.014(2) C(45) 0.029(3) 0.022(2) 0.022(3) 0.000(2) 0.005(2) 0.007(2) C(46) 0.026(3) 0.032(3) 0.022(3) 0.007(2) 0.007(2) 0.013(2) C(321) 0.035(3) 0.048(4) 0.045(4) 0.007(3) 0.013(3) 0.023(3) C(322) 0.031(3) 0.038(3) 0.024(3) 0.012(2) 0.012(2) 0.014(2) C(323) 0.053(4) 0.083(5) 0.027(4) 0.004(4) 0.007(3) 0.024(4) C(361) 0.040(3) 0.052(4) 0.040(4) 0.012(3) 0.017(3) 0.021(3) C(362) 0.025(3) 0.020(2) 0.038(3) 0.003(2) 0.014(2) 0.013(2) C(363) 0.029(3) 0.047(4) 0.047(4) 0.012(3) 0.014(3) 0.023(3) C(421) 0.051(4) 0.049(4) 0.034(4) 0.015(3) -0.001(3) 0.021(3) C(422) 0.026(3) 0.027(3) 0.022(3) 0.013(2) 0.003(2) 0.009(2) C(423) 0.026(3) 0.046(4) 0.037(4) -0.004(3) 0.004(3) 0.014(3) C(461) 0.030(3) 0.048(4) 0.057(4) 0.012(3) 0.017(3) 0.020(3) C(462) 0.029(3) 0.028(3) 0.038(3) 0.011(2) 0.009(2) 0.008(3) C(463) 0.037(3) 0.040(3) 0.044(4) 0.008(3) -0.010(3) 0.016(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_site_symmetry_2 _geom_bond_publ_flag Ta O(4) 1.894(3) . ? Ta O(3) 1.904(3) . ? Ta N(11) 2.240(4) . ? Ta N(21) 2.258(4) . ? Ta C(27) 2.278(5) . ? Ta C(17) 2.283(5) . ? Ta Cl 2.5064(13) . ? Br(34) C(34) 1.906(5) . ? Br(44) C(44) 1.899(5) . ? O(3) C(31) 1.371(6) . ? O(4) C(41) 1.367(5) . ? N(11) C(12) 1.329(7) . ? N(11) C(16) 1.351(6) . ? N(21) C(22) 1.338(7) . ? N(21) C(26) 1.342(6) . ? C(12) C(13) 1.404(7) . ? C(12) C(17) 1.495(7) . ? C(13) C(14) 1.390(8) . ? C(14) C(15) 1.378(8) . ? C(15) C(16) 1.377(7) . ? C(17) C(18) 1.509(7) . ? C(17) H(17) 0.91(5) . ? C(22) C(23) 1.389(7) . ? C(22) C(27) 1.506(7) . ? C(23) C(24) 1.367(8) . ? C(24) C(25) 1.392(9) . ? C(25) C(26) 1.373(7) . ? C(27) C(28) 1.515(7) . ? C(27) H(27) 1.02(5) . ? C(31) C(36) 1.406(7) . ? C(31) C(32) 1.411(6) . ? C(32) C(33) 1.385(7) . ? C(32) C(322) 1.523(7) . ? C(33) C(34) 1.376(8) . ? C(34) C(35) 1.384(7) . ? C(35) C(36) 1.386(7) . ? C(36) C(362) 1.513(6) . ? C(41) C(46) 1.418(7) . ? C(41) C(42) 1.421(7) . ? C(42) C(43) 1.386(7) . ? C(42) C(422) 1.509(7) . ? C(43) C(44) 1.384(7) . ? C(44) C(45) 1.387(7) . ? C(45) C(46) 1.390(7) . ? C(46) C(462) 1.511(7) . ? C(321) C(322) 1.537(7) . ? C(322) C(323) 1.526(8) . ? C(361) C(362) 1.502(8) . ? C(362) C(363) 1.536(7) . ? C(421) C(422) 1.535(8) . ? C(422) C(423) 1.522(7) . ? C(461) C(462) 1.532(8) . ? C(462) C(463) 1.525(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(4) Ta O(3) 173.78(15) . . ? O(4) Ta N(11) 89.74(14) . . ? O(3) Ta N(11) 86.33(14) . . ? O(4) Ta N(21) 86.35(14) . . ? O(3) Ta N(21) 95.98(14) . . ? N(11) Ta N(21) 162.59(15) . . ? O(4) Ta C(27) 99.76(17) . . ? O(3) Ta C(27) 86.40(17) . . ? N(11) Ta C(27) 136.83(17) . . ? N(21) Ta C(27) 60.58(17) . . ? O(4) Ta C(17) 87.47(17) . . ? O(3) Ta C(17) 94.76(16) . . ? N(11) Ta C(17) 60.56(17) . . ? N(21) Ta C(17) 136.02(17) . . ? C(27) Ta C(17) 77.77(19) . . ? O(4) Ta Cl 88.34(11) . . ? O(3) Ta Cl 86.35(11) . . ? N(11) Ta Cl 82.20(11) . . ? N(21) Ta Cl 80.73(12) . . ? C(27) Ta Cl 139.55(14) . . ? C(17) Ta Cl 142.52(13) . . ? C(31) O(3) Ta 158.3(3) . . ? C(41) O(4) Ta 168.6(3) . . ? C(12) N(11) C(16) 121.6(4) . . ? C(12) N(11) Ta 98.3(3) . . ? C(16) N(11) Ta 139.0(4) . . ? C(22) N(21) C(26) 121.4(4) . . ? C(22) N(21) Ta 98.6(3) . . ? C(26) N(21) Ta 139.4(4) . . ? N(11) C(12) C(13) 120.6(5) . . ? N(11) C(12) C(17) 107.6(4) . . ? C(13) C(12) C(17) 131.8(5) . . ? C(14) C(13) C(12) 117.6(6) . . ? C(15) C(14) C(13) 120.8(5) . . ? C(16) C(15) C(14) 118.9(5) . . ? N(11) C(16) C(15) 120.4(5) . . ? C(12) C(17) C(18) 115.5(4) . . ? C(12) C(17) Ta 91.7(3) . . ? C(18) C(17) Ta 123.5(4) . . ? C(12) C(17) H(17) 107(3) . . ? C(18) C(17) H(17) 112(3) . . ? Ta C(17) H(17) 105(3) . . ? N(21) C(22) C(23) 120.2(5) . . ? N(21) C(22) C(27) 107.0(4) . . ? C(23) C(22) C(27) 132.8(5) . . ? C(24) C(23) C(22) 119.1(6) . . ? C(23) C(24) C(25) 119.9(5) . . ? C(26) C(25) C(24) 118.9(5) . . ? N(21) C(26) C(25) 120.5(5) . . ? C(22) C(27) C(28) 112.8(4) . . ? C(22) C(27) Ta 92.8(3) . . ? C(28) C(27) Ta 121.1(4) . . ? C(22) C(27) H(27) 112(3) . . ? C(28) C(27) H(27) 108(3) . . ? Ta C(27) H(27) 109(3) . . ? O(3) C(31) C(36) 119.5(4) . . ? O(3) C(31) C(32) 119.6(4) . . ? C(36) C(31) C(32) 120.9(5) . . ? C(33) C(32) C(31) 118.2(5) . . ? C(33) C(32) C(322) 120.4(4) . . ? C(31) C(32) C(322) 121.4(5) . . ? C(34) C(33) C(32) 120.7(5) . . ? C(33) C(34) C(35) 121.2(5) . . ? C(33) C(34) Br(34) 119.6(4) . . ? C(35) C(34) Br(34) 119.3(4) . . ? C(34) C(35) C(36) 120.0(5) . . ? C(35) C(36) C(31) 118.8(4) . . ? C(35) C(36) C(362) 120.1(4) . . ? C(31) C(36) C(362) 121.0(5) . . ? O(4) C(41) C(46) 120.8(4) . . ? O(4) C(41) C(42) 119.0(4) . . ? C(46) C(41) C(42) 120.2(4) . . ? C(43) C(42) C(41) 119.0(5) . . ? C(43) C(42) C(422) 119.7(4) . . ? C(41) C(42) C(422) 121.2(4) . . ? C(44) C(43) C(42) 120.4(5) . . ? C(43) C(44) C(45) 121.1(5) . . ? C(43) C(44) Br(44) 120.4(4) . . ? C(45) C(44) Br(44) 118.6(4) . . ? C(44) C(45) C(46) 120.5(5) . . ? C(45) C(46) C(41) 118.7(5) . . ? C(45) C(46) C(462) 119.3(5) . . ? C(41) C(46) C(462) 122.0(5) . . ? C(32) C(322) C(323) 111.2(5) . . ? C(32) C(322) C(321) 111.6(5) . . ? C(323) C(322) C(321) 110.6(4) . . ? C(361) C(362) C(36) 114.0(5) . . ? C(361) C(362) C(363) 111.0(4) . . ? C(36) C(362) C(363) 109.2(4) . . ? C(42) C(422) C(423) 111.8(4) . . ? C(42) C(422) C(421) 110.9(4) . . ? C(423) C(422) C(421) 110.5(5) . . ? C(46) C(462) C(463) 111.3(4) . . ? C(46) C(462) C(461) 110.8(5) . . ? C(463) C(462) C(461) 111.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(4) Ta O(3) C(31) 10.3(17) . . . . ? N(11) Ta O(3) C(31) 61.2(8) . . . . ? N(21) Ta O(3) C(31) -101.5(8) . . . . ? C(27) Ta O(3) C(31) -161.4(8) . . . . ? C(17) Ta O(3) C(31) 121.2(8) . . . . ? Cl Ta O(3) C(31) -21.2(7) . . . . ? O(3) Ta O(4) C(41) -57(2) . . . . ? N(11) Ta O(4) C(41) -108.1(15) . . . . ? N(21) Ta O(4) C(41) 54.9(15) . . . . ? C(27) Ta O(4) C(41) 114.2(15) . . . . ? C(17) Ta O(4) C(41) -168.6(15) . . . . ? Cl Ta O(4) C(41) -25.9(15) . . . . ? O(4) Ta N(11) C(12) -78.2(3) . . . . ? O(3) Ta N(11) C(12) 106.7(3) . . . . ? N(21) Ta N(11) C(12) -155.0(4) . . . . ? C(27) Ta N(11) C(12) 25.9(4) . . . . ? C(17) Ta N(11) C(12) 9.1(3) . . . . ? Cl Ta N(11) C(12) -166.5(3) . . . . ? O(4) Ta N(11) C(16) 89.2(5) . . . . ? O(3) Ta N(11) C(16) -86.0(5) . . . . ? N(21) Ta N(11) C(16) 12.3(9) . . . . ? C(27) Ta N(11) C(16) -166.7(5) . . . . ? C(17) Ta N(11) C(16) 176.5(6) . . . . ? Cl Ta N(11) C(16) 0.9(5) . . . . ? O(4) Ta N(21) C(22) 109.9(3) . . . . ? O(3) Ta N(21) C(22) -75.9(3) . . . . ? N(11) Ta N(21) C(22) -172.7(4) . . . . ? C(27) Ta N(21) C(22) 6.6(3) . . . . ? C(17) Ta N(21) C(22) 27.4(4) . . . . ? Cl Ta N(21) C(22) -161.2(3) . . . . ? O(4) Ta N(21) C(26) -79.3(5) . . . . ? O(3) Ta N(21) C(26) 94.9(5) . . . . ? N(11) Ta N(21) C(26) -1.9(9) . . . . ? C(27) Ta N(21) C(26) 177.4(6) . . . . ? C(17) Ta N(21) C(26) -161.9(5) . . . . ? Cl Ta N(21) C(26) 9.6(5) . . . . ? C(16) N(11) C(12) C(13) -3.8(7) . . . . ? Ta N(11) C(12) C(13) 166.5(4) . . . . ? C(16) N(11) C(12) C(17) 177.0(4) . . . . ? Ta N(11) C(12) C(17) -12.7(4) . . . . ? N(11) C(12) C(13) C(14) 4.2(8) . . . . ? C(17) C(12) C(13) C(14) -176.7(5) . . . . ? C(12) C(13) C(14) C(15) -2.3(8) . . . . ? C(13) C(14) C(15) C(16) -0.1(9) . . . . ? C(12) N(11) C(16) C(15) 1.2(7) . . . . ? Ta N(11) C(16) C(15) -164.1(4) . . . . ? C(14) C(15) C(16) N(11) 0.8(8) . . . . ? N(11) C(12) C(17) C(18) 141.0(5) . . . . ? C(13) C(12) C(17) C(18) -38.1(8) . . . . ? N(11) C(12) C(17) Ta 12.4(4) . . . . ? C(13) C(12) C(17) Ta -166.8(5) . . . . ? O(4) Ta C(17) C(12) 83.1(3) . . . . ? O(3) Ta C(17) C(12) -91.0(3) . . . . ? N(11) Ta C(17) C(12) -8.0(3) . . . . ? N(21) Ta C(17) C(12) 165.2(3) . . . . ? C(27) Ta C(17) C(12) -176.3(3) . . . . ? Cl Ta C(17) C(12) -0.8(4) . . . . ? O(4) Ta C(17) C(18) -39.2(4) . . . . ? O(3) Ta C(17) C(18) 146.6(4) . . . . ? N(11) Ta C(17) C(18) -130.4(5) . . . . ? N(21) Ta C(17) C(18) 42.9(5) . . . . ? C(27) Ta C(17) C(18) 61.3(4) . . . . ? Cl Ta C(17) C(18) -123.2(4) . . . . ? C(26) N(21) C(22) C(23) -2.0(8) . . . . ? Ta N(21) C(22) C(23) 171.0(5) . . . . ? C(26) N(21) C(22) C(27) 177.9(5) . . . . ? Ta N(21) C(22) C(27) -9.1(4) . . . . ? N(21) C(22) C(23) C(24) 2.5(9) . . . . ? C(27) C(22) C(23) C(24) -177.4(6) . . . . ? C(22) C(23) C(24) C(25) -1.0(10) . . . . ? C(23) C(24) C(25) C(26) -0.9(10) . . . . ? C(22) N(21) C(26) C(25) -0.1(8) . . . . ? Ta N(21) C(26) C(25) -169.4(4) . . . . ? C(24) C(25) C(26) N(21) 1.5(9) . . . . ? N(21) C(22) C(27) C(28) 134.5(5) . . . . ? C(23) C(22) C(27) C(28) -45.6(9) . . . . ? N(21) C(22) C(27) Ta 8.9(4) . . . . ? C(23) C(22) C(27) Ta -171.2(6) . . . . ? O(4) Ta C(27) C(22) -85.9(3) . . . . ? O(3) Ta C(27) C(22) 93.2(3) . . . . ? N(11) Ta C(27) C(22) 173.9(3) . . . . ? N(21) Ta C(27) C(22) -5.8(3) . . . . ? C(17) Ta C(27) C(22) -171.2(3) . . . . ? Cl Ta C(27) C(22) 13.1(4) . . . . ? O(4) Ta C(27) C(28) 155.2(4) . . . . ? O(3) Ta C(27) C(28) -25.8(4) . . . . ? N(11) Ta C(27) C(28) 55.0(5) . . . . ? N(21) Ta C(27) C(28) -124.7(5) . . . . ? C(17) Ta C(27) C(28) 69.9(4) . . . . ? Cl Ta C(27) C(28) -105.8(4) . . . . ? Ta O(3) C(31) C(36) 80.0(9) . . . . ? Ta O(3) C(31) C(32) -100.3(8) . . . . ? O(3) C(31) C(32) C(33) 179.1(4) . . . . ? C(36) C(31) C(32) C(33) -1.3(7) . . . . ? O(3) C(31) C(32) C(322) -2.2(7) . . . . ? C(36) C(31) C(32) C(322) 177.5(5) . . . . ? C(31) C(32) C(33) C(34) -1.3(8) . . . . ? C(322) C(32) C(33) C(34) 179.9(5) . . . . ? C(32) C(33) C(34) C(35) 2.9(8) . . . . ? C(32) C(33) C(34) Br(34) -175.5(4) . . . . ? C(33) C(34) C(35) C(36) -1.7(8) . . . . ? Br(34) C(34) C(35) C(36) 176.6(4) . . . . ? C(34) C(35) C(36) C(31) -0.8(8) . . . . ? C(34) C(35) C(36) C(362) 176.3(5) . . . . ? O(3) C(31) C(36) C(35) -178.0(5) . . . . ? C(32) C(31) C(36) C(35) 2.3(7) . . . . ? O(3) C(31) C(36) C(362) 4.9(7) . . . . ? C(32) C(31) C(36) C(362) -174.8(5) . . . . ? Ta O(4) C(41) C(46) 74.8(16) . . . . ? Ta O(4) C(41) C(42) -104.9(15) . . . . ? O(4) C(41) C(42) C(43) 178.1(4) . . . . ? C(46) C(41) C(42) C(43) -1.6(7) . . . . ? O(4) C(41) C(42) C(422) -2.2(7) . . . . ? C(46) C(41) C(42) C(422) 178.1(4) . . . . ? C(41) C(42) C(43) C(44) 0.2(7) . . . . ? C(422) C(42) C(43) C(44) -179.4(5) . . . . ? C(42) C(43) C(44) C(45) 1.6(8) . . . . ? C(42) C(43) C(44) Br(44) -179.2(4) . . . . ? C(43) C(44) C(45) C(46) -1.9(8) . . . . ? Br(44) C(44) C(45) C(46) 178.8(4) . . . . ? C(44) C(45) C(46) C(41) 0.5(7) . . . . ? C(44) C(45) C(46) C(462) 179.1(5) . . . . ? O(4) C(41) C(46) C(45) -178.5(4) . . . . ? C(42) C(41) C(46) C(45) 1.2(7) . . . . ? O(4) C(41) C(46) C(462) 3.0(7) . . . . ? C(42) C(41) C(46) C(462) -177.3(5) . . . . ? C(33) C(32) C(322) C(323) 74.5(7) . . . . ? C(31) C(32) C(322) C(323) -104.3(6) . . . . ? C(33) C(32) C(322) C(321) -49.5(7) . . . . ? C(31) C(32) C(322) C(321) 131.8(5) . . . . ? C(35) C(36) C(362) C(361) 43.6(7) . . . . ? C(31) C(36) C(362) C(361) -139.3(5) . . . . ? C(35) C(36) C(362) C(363) -81.2(6) . . . . ? C(31) C(36) C(362) C(363) 95.9(5) . . . . ? C(43) C(42) C(422) C(423) -64.9(6) . . . . ? C(41) C(42) C(422) C(423) 115.5(5) . . . . ? C(43) C(42) C(422) C(421) 59.0(6) . . . . ? C(41) C(42) C(422) C(421) -120.6(5) . . . . ? C(45) C(46) C(462) C(463) 62.9(6) . . . . ? C(41) C(46) C(462) C(463) -118.6(5) . . . . ? C(45) C(46) C(462) C(461) -61.0(7) . . . . ? C(41) C(46) C(462) C(461) 117.5(6) . . . . ? #============================================================================== data_BD6111 _database_code_depnum_ccdc_archive 'CCDC 255068' _audit_creation_date 11-06-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C38 H50 Cl1 N2 O2 Ta1' _chemical_formula_moiety 'C38 H50 Cl1 N2 O2 Ta1' _chemical_formula_structural ? _chemical_formula_weight 783.24 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1330(3) _cell_length_b 12.3876(3) _cell_length_c 13.9642(4) _cell_angle_alpha 98.8630(10) _cell_angle_beta 115.4240(10) _cell_angle_gamma 101.1690(10) _cell_volume 1791.75(18) _cell_measurement_reflns_used 17886 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.139 _cell_measurement_temperature 150 _exptl_crystal_F_000 796 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.1822 _exptl_absorpt_correction_T_max 0.3333 _diffrn_reflns_number 17886 _diffrn_measured_fraction_theta_max 0.9837 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9837 _reflns_number_total 8312 _reflns_number_gt 7514 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 16 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.102 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 8299 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.68 _refine_diff_density_min -2.94 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta -0.000746(17) 0.263236(14) 0.227969(14) 0.02514(8) Uani 1 1 d . . . Cl Cl 0.04194(11) 0.20606(9) 0.07094(10) 0.0323(2) Uani 1 1 d . . . O(1) O -0.1650(3) 0.2665(3) 0.1210(3) 0.0257(6) Uani 1 1 d . . . O(2) O 0.1678(3) 0.2572(3) 0.3232(3) 0.0294(7) Uani 1 1 d . . . N(31) N -0.0654(4) 0.0737(3) 0.1980(3) 0.0267(8) Uani 1 1 d . . . N(41) N 0.0738(4) 0.4381(3) 0.2138(3) 0.0293(8) Uani 1 1 d . . . C(11) C -0.2622(4) 0.2782(4) 0.0318(4) 0.0285(9) Uani 1 1 d . . . C(12) C -0.2952(5) 0.3821(4) 0.0399(4) 0.0312(10) Uani 1 1 d . . . C(13) C -0.3977(5) 0.3925(4) -0.0514(5) 0.0404(12) Uani 1 1 d . . . C(14) C -0.4643(5) 0.3083(5) -0.1480(5) 0.0413(12) Uani 1 1 d . . . C(15) C -0.4295(5) 0.2082(5) -0.1552(4) 0.0400(12) Uani 1 1 d . . . C(16) C -0.3290(5) 0.1901(4) -0.0658(4) 0.0313(10) Uani 1 1 d . . . C(21) C 0.2790(5) 0.2322(4) 0.3637(4) 0.0294(9) Uani 1 1 d . . . C(22) C 0.2942(5) 0.1502(4) 0.4250(4) 0.0349(10) Uani 1 1 d . . . C(23) C 0.4090(5) 0.1254(5) 0.4671(5) 0.0402(12) Uani 1 1 d . . . C(24) C 0.5075(5) 0.1767(5) 0.4487(5) 0.0452(13) Uani 1 1 d . . . C(25) C 0.4916(5) 0.2564(4) 0.3894(5) 0.0402(12) Uani 1 1 d . . . C(26) C 0.3780(5) 0.2869(4) 0.3459(4) 0.0340(10) Uani 1 1 d . . . C(32) C -0.1450(5) 0.0723(4) 0.2418(4) 0.0305(10) Uani 1 1 d . . . C(33) C -0.2438(5) -0.0253(5) 0.2109(5) 0.0415(12) Uani 1 1 d . . . C(34) C -0.2500(6) -0.1242(4) 0.1443(5) 0.0453(13) Uani 1 1 d . . . C(35) C -0.1625(6) -0.1225(4) 0.1067(5) 0.0389(12) Uani 1 1 d . . . C(36) C -0.0715(5) -0.0202(4) 0.1325(4) 0.0329(10) Uani 1 1 d . . . C(42) C 0.1065(6) 0.5005(5) 0.3132(4) 0.0419(12) Uani 1 1 d . . . C(43) C 0.1782(8) 0.6108(6) 0.3503(6) 0.0639(18) Uani 1 1 d . . . C(44) C 0.2093(8) 0.6600(6) 0.2806(7) 0.071(2) Uani 1 1 d . . . C(45) C 0.1722(7) 0.5976(5) 0.1763(6) 0.0538(16) Uani 1 1 d . . . C(46) C 0.1052(6) 0.4834(5) 0.1445(4) 0.0396(12) Uani 1 1 d . . . C(121) C -0.3038(6) 0.4848(6) 0.2054(5) 0.0540(15) Uani 1 1 d . . . C(122) C -0.2243(5) 0.4781(4) 0.1450(4) 0.0343(10) Uani 1 1 d . . . C(123) C -0.1838(7) 0.5938(5) 0.1253(6) 0.0586(17) Uani 1 1 d . . . C(161) C -0.4115(6) -0.0223(5) -0.1004(6) 0.0516(14) Uani 1 1 d . . . C(162) C -0.2978(5) 0.0777(4) -0.0775(4) 0.0355(10) Uani 1 1 d . . . C(163) C -0.2573(6) 0.0548(6) -0.1669(5) 0.0533(15) Uani 1 1 d . . . C(221) C 0.1643(8) -0.0323(6) 0.4311(9) 0.087(3) Uani 1 1 d . . . C(222) C 0.1896(5) 0.0960(5) 0.4502(5) 0.0419(12) Uani 1 1 d . . . C(223) C 0.2175(8) 0.1561(8) 0.5652(6) 0.078(2) Uani 1 1 d . . . C(261) C 0.3782(6) 0.3352(5) 0.1779(5) 0.0501(14) Uani 1 1 d . . . C(262) C 0.3649(5) 0.3741(4) 0.2800(4) 0.0360(11) Uani 1 1 d . . . C(263) C 0.4612(6) 0.4911(5) 0.3490(5) 0.0545(15) Uani 1 1 d . . . C(321) C -0.1049(5) 0.1870(4) 0.3157(4) 0.0334(10) Uani 1 1 d . . . C(322) C -0.2126(6) 0.2253(5) 0.3263(5) 0.0423(12) Uani 1 1 d . . . C(421) C 0.0430(6) 0.4198(5) 0.3609(5) 0.0395(12) Uani 1 1 d . . . C(422) C 0.1260(6) 0.4308(5) 0.4810(5) 0.0509(14) Uani 1 1 d . . . H(13) H -0.4222 0.4606 -0.0462 0.049 Uiso 1 1 calc R . . H(14) H -0.5332 0.3181 -0.2093 0.050 Uiso 1 1 calc R . . H(15) H -0.4750 0.1500 -0.2227 0.048 Uiso 1 1 calc R . . H(23) H 0.4208 0.0718 0.5097 0.048 Uiso 1 1 calc R . . H(24) H 0.5851 0.1570 0.4769 0.054 Uiso 1 1 calc R . . H(25) H 0.5596 0.2919 0.3774 0.048 Uiso 1 1 calc R . . H(33) H -0.3062 -0.0245 0.2348 0.050 Uiso 1 1 calc R . . H(34) H -0.3148 -0.1930 0.1248 0.054 Uiso 1 1 calc R . . H(35) H -0.1640 -0.1905 0.0634 0.047 Uiso 1 1 calc R . . H(36) H -0.0135 -0.0172 0.1033 0.039 Uiso 1 1 calc R . . H(43) H 0.2064 0.6534 0.4235 0.077 Uiso 1 1 calc R . . H(44) H 0.2572 0.7382 0.3047 0.085 Uiso 1 1 calc R . . H(45) H 0.1918 0.6320 0.1270 0.065 Uiso 1 1 calc R . . H(46) H 0.0815 0.4372 0.0739 0.048 Uiso 1 1 calc R . . H(122) H -0.1451 0.4609 0.1943 0.041 Uiso 1 1 calc R . . H(12A) H -0.3829 0.5005 0.1585 0.081 Uiso 1 1 calc R . . H(12B) H -0.2549 0.5462 0.2739 0.081 Uiso 1 1 calc R . . H(12C) H -0.3243 0.4120 0.2222 0.081 Uiso 1 1 calc R . . H(12D) H -0.1322 0.5891 0.0876 0.088 Uiso 1 1 calc R . . H(12E) H -0.1335 0.6520 0.1960 0.088 Uiso 1 1 calc R . . H(12F) H -0.2599 0.6145 0.0796 0.088 Uiso 1 1 calc R . . H(162) H -0.2246 0.0814 -0.0058 0.043 Uiso 1 1 calc R . . H(16A) H -0.4358 -0.0076 -0.0423 0.077 Uiso 1 1 calc R . . H(16B) H -0.3872 -0.0932 -0.1020 0.077 Uiso 1 1 calc R . . H(16C) H -0.4840 -0.0296 -0.1717 0.077 Uiso 1 1 calc R . . H(16D) H -0.3255 0.0553 -0.2375 0.080 Uiso 1 1 calc R . . H(16E) H -0.2414 -0.0199 -0.1729 0.080 Uiso 1 1 calc R . . H(16F) H -0.1793 0.1143 -0.1474 0.080 Uiso 1 1 calc R . . H(222) H 0.1094 0.1092 0.3975 0.050 Uiso 1 1 calc R . . H(22A) H 0.2392 -0.0491 0.4841 0.131 Uiso 1 1 calc R . . H(22B) H 0.1469 -0.0667 0.3562 0.131 Uiso 1 1 calc R . . H(22C) H 0.0903 -0.0640 0.4407 0.131 Uiso 1 1 calc R . . H(22D) H 0.2926 0.1412 0.6200 0.118 Uiso 1 1 calc R . . H(22E) H 0.1438 0.1275 0.5762 0.118 Uiso 1 1 calc R . . H(22F) H 0.2339 0.2386 0.5734 0.118 Uiso 1 1 calc R . . H(262) H 0.2774 0.3830 0.2553 0.043 Uiso 1 1 calc R . . H(26A) H 0.3633 0.3911 0.1347 0.075 Uiso 1 1 calc R . . H(26B) H 0.3156 0.2607 0.1333 0.075 Uiso 1 1 calc R . . H(26C) H 0.4644 0.3285 0.1999 0.075 Uiso 1 1 calc R . . H(26D) H 0.5480 0.4846 0.3756 0.082 Uiso 1 1 calc R . . H(26E) H 0.4482 0.5185 0.4120 0.082 Uiso 1 1 calc R . . H(26F) H 0.4490 0.5453 0.3037 0.082 Uiso 1 1 calc R . . H(321) H 0.010(7) 0.203(6) 0.374(6) 0.07(2) Uiso 1 1 d . . . H(32A) H -0.266(6) 0.233(5) 0.252(5) 0.038(15) Uiso 1 1 d . . . H(32B) H -0.187(5) 0.303(5) 0.370(5) 0.038(15) Uiso 1 1 d . . . H(32C) H -0.245(7) 0.170(6) 0.361(6) 0.061(19) Uiso 1 1 d . . . H(421) H -0.017(7) 0.422(6) 0.351(6) 0.06(2) Uiso 1 1 d . . . H(42A) H 0.211(3) 0.403(3) 0.4914(7) 0.042(15) Uiso 1 1 calc R . . H(42B) H 0.072(2) 0.377(3) 0.5110(14) 0.09(2) Uiso 1 1 calc R . . H(42C) H 0.156(3) 0.521(3) 0.5284(17) 0.10(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02347(11) 0.02607(11) 0.02581(11) 0.00897(7) 0.01095(8) 0.00671(7) Cl 0.0330(6) 0.0327(5) 0.0335(6) 0.0070(5) 0.0202(5) 0.0041(5) O(1) 0.0221(15) 0.0293(15) 0.0268(16) 0.0102(12) 0.0105(13) 0.0104(13) O(2) 0.0250(16) 0.0313(16) 0.0321(17) 0.0112(13) 0.0116(14) 0.0105(14) N(31) 0.028(2) 0.0236(18) 0.028(2) 0.0061(15) 0.0139(17) 0.0090(15) N(41) 0.031(2) 0.0234(18) 0.039(2) 0.0100(16) 0.0197(19) 0.0125(16) C(11) 0.026(2) 0.034(2) 0.031(2) 0.0100(19) 0.015(2) 0.015(2) C(12) 0.025(2) 0.031(2) 0.037(3) 0.0068(19) 0.014(2) 0.013(2) C(13) 0.034(3) 0.037(3) 0.048(3) 0.015(2) 0.013(3) 0.021(2) C(14) 0.030(3) 0.043(3) 0.041(3) 0.010(2) 0.006(2) 0.021(2) C(15) 0.033(3) 0.045(3) 0.034(3) 0.005(2) 0.011(2) 0.013(2) C(16) 0.029(2) 0.036(2) 0.032(2) 0.010(2) 0.017(2) 0.012(2) C(21) 0.029(2) 0.032(2) 0.024(2) 0.0081(19) 0.011(2) 0.0032(18) C(22) 0.030(3) 0.038(3) 0.033(3) 0.013(2) 0.011(2) 0.009(2) C(23) 0.035(3) 0.039(3) 0.042(3) 0.015(2) 0.011(2) 0.014(2) C(24) 0.029(3) 0.047(3) 0.053(3) 0.018(2) 0.012(3) 0.012(3) C(25) 0.027(3) 0.043(3) 0.050(3) 0.012(2) 0.017(2) 0.015(2) C(26) 0.026(2) 0.039(3) 0.034(3) 0.009(2) 0.011(2) 0.009(2) C(32) 0.036(3) 0.036(2) 0.028(2) 0.018(2) 0.019(2) 0.015(2) C(33) 0.043(3) 0.049(3) 0.051(3) 0.017(2) 0.035(3) 0.021(3) C(34) 0.050(3) 0.030(2) 0.062(4) 0.003(2) 0.035(3) 0.013(2) C(35) 0.052(3) 0.026(2) 0.045(3) 0.011(2) 0.029(3) 0.009(2) C(36) 0.037(3) 0.035(2) 0.039(3) 0.016(2) 0.024(2) 0.017(2) C(42) 0.053(3) 0.046(3) 0.032(3) 0.023(3) 0.021(3) 0.011(2) C(43) 0.072(5) 0.054(4) 0.042(4) 0.001(3) 0.019(4) -0.006(3) C(44) 0.073(5) 0.036(3) 0.075(5) -0.012(3) 0.028(4) -0.004(3) C(45) 0.064(4) 0.050(3) 0.067(4) 0.018(3) 0.041(4) 0.034(3) C(46) 0.056(3) 0.040(3) 0.031(3) 0.022(3) 0.022(3) 0.016(2) C(121) 0.052(4) 0.068(4) 0.052(4) 0.025(3) 0.030(3) 0.016(3) C(122) 0.033(3) 0.033(2) 0.042(3) 0.017(2) 0.018(2) 0.014(2) C(123) 0.069(4) 0.036(3) 0.059(4) 0.004(3) 0.024(4) 0.014(3) C(161) 0.052(4) 0.041(3) 0.062(4) 0.015(3) 0.026(3) 0.014(3) C(162) 0.028(3) 0.040(3) 0.028(2) 0.009(2) 0.007(2) 0.002(2) C(163) 0.043(3) 0.069(4) 0.042(3) 0.016(3) 0.021(3) 0.000(3) C(221) 0.066(5) 0.058(4) 0.163(10) 0.027(4) 0.064(6) 0.055(5) C(222) 0.036(3) 0.050(3) 0.044(3) 0.020(2) 0.016(3) 0.025(3) C(223) 0.064(5) 0.132(7) 0.045(4) 0.021(5) 0.029(4) 0.037(4) C(261) 0.046(3) 0.059(4) 0.045(3) 0.011(3) 0.022(3) 0.016(3) C(262) 0.031(3) 0.040(3) 0.038(3) 0.010(2) 0.015(2) 0.015(2) C(263) 0.061(4) 0.038(3) 0.051(4) 0.008(3) 0.016(3) 0.015(3) C(321) 0.038(3) 0.037(2) 0.034(3) 0.017(2) 0.021(2) 0.012(2) C(322) 0.055(4) 0.045(3) 0.046(3) 0.024(3) 0.035(3) 0.017(3) C(421) 0.039(3) 0.037(3) 0.034(3) 0.014(2) 0.014(3) -0.006(2) C(422) 0.056(4) 0.055(3) 0.036(3) 0.012(3) 0.021(3) 0.003(3) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ta O(1) 1.923(3) YES Ta O(2) 1.927(3) YES Ta N(31) 2.237(4) YES Ta N(41) 2.253(4) YES Ta C(421) 2.266(5) YES Ta C(321) 2.284(5) YES Ta Cl 2.4934(11) YES Ta H(321) 2.24(7) YES O(1) C(11) 1.350(5) YES O(2) C(21) 1.340(6) YES N(31) C(36) 1.334(6) YES N(31) C(32) 1.346(6) YES N(41) C(42) 1.325(7) YES N(41) C(46) 1.341(6) YES C(11) C(16) 1.399(7) YES C(11) C(12) 1.422(6) YES C(12) C(13) 1.393(7) YES C(12) C(122) 1.514(7) YES C(13) C(14) 1.366(8) YES C(14) C(15) 1.388(7) YES C(15) C(16) 1.408(7) YES C(16) C(162) 1.515(7) YES C(21) C(26) 1.398(7) YES C(21) C(22) 1.415(7) YES C(22) C(23) 1.377(7) YES C(22) C(222) 1.521(7) YES C(23) C(24) 1.384(8) YES C(24) C(25) 1.374(8) YES C(25) C(26) 1.402(7) YES C(26) C(262) 1.512(7) YES C(32) C(33) 1.384(7) YES C(32) C(321) 1.473(7) YES C(33) C(34) 1.388(8) YES C(34) C(35) 1.370(8) YES C(35) C(36) 1.389(7) YES C(43) C(42) 1.352(9) YES C(43) C(44) 1.368(11) YES C(44) C(45) 1.370(10) YES C(45) C(46) 1.382(8) YES C(121) C(122) 1.535(7) YES C(122) C(123) 1.528(7) YES C(161) C(162) 1.543(8) YES C(162) C(163) 1.533(7) YES C(221) C(222) 1.516(8) YES C(222) C(223) 1.521(9) YES C(261) C(262) 1.519(8) YES C(262) C(263) 1.531(8) YES C(321) C(322) 1.529(7) YES C(321) H(321) 1.23(7) YES C(322) H(32A) 0.99(6) YES C(322) H(32B) 0.97(6) YES C(322) H(32C) 1.01(7) YES C(421) C(422) 1.507(8) YES C(421) C(42) 1.544(8) YES C(421) H(421) 0.69(7) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ta O(2) 174.26(12) YES O(1) Ta N(31) 92.75(13) YES O(2) Ta N(31) 86.99(14) YES O(1) Ta N(41) 85.77(14) YES O(2) Ta N(41) 92.76(14) YES N(31) Ta N(41) 162.55(14) YES O(1) Ta C(421) 98.53(18) YES O(2) Ta C(421) 85.52(18) YES N(31) Ta C(421) 136.76(18) YES N(41) Ta C(421) 60.48(19) YES O(1) Ta C(321) 85.99(15) YES O(2) Ta C(321) 98.81(16) YES N(31) Ta C(321) 60.10(15) YES N(41) Ta C(321) 136.90(15) YES C(421) Ta C(321) 79.1(2) YES O(1) Ta Cl 87.07(9) YES O(2) Ta Cl 87.22(10) YES N(31) Ta Cl 81.58(10) YES N(41) Ta Cl 80.99(10) YES C(421) Ta Cl 140.28(17) YES C(321) Ta Cl 140.59(13) YES O(1) Ta H(321) 117.3(19) YES O(2) Ta H(321) 67.7(19) YES N(31) Ta H(321) 64.7(18) YES N(41) Ta H(321) 131.0(18) YES C(421) Ta H(321) 73.1(18) YES C(321) Ta H(321) 31.4(19) YES Cl Ta H(321) 138.0(17) YES C(11) O(1) Ta 164.4(3) YES C(21) O(2) Ta 163.8(3) YES C(36) N(31) C(32) 121.6(4) YES C(36) N(31) Ta 138.5(3) YES C(32) N(31) Ta 96.7(3) YES C(42) N(41) C(46) 121.3(4) YES C(42) N(41) Ta 99.9(3) YES C(46) N(41) Ta 137.9(3) YES O(1) C(11) C(16) 120.8(4) YES O(1) C(11) C(12) 118.3(4) YES C(16) C(11) C(12) 120.9(4) YES C(13) C(12) C(11) 118.1(5) YES C(13) C(12) C(122) 120.3(4) YES C(11) C(12) C(122) 121.6(4) YES C(14) C(13) C(12) 122.4(5) YES C(13) C(14) C(15) 118.8(5) YES C(14) C(15) C(16) 122.1(5) YES C(11) C(16) C(15) 117.7(4) YES C(11) C(16) C(162) 122.6(4) YES C(15) C(16) C(162) 119.8(5) YES O(2) C(21) C(26) 120.4(4) YES O(2) C(21) C(22) 118.7(4) YES C(26) C(21) C(22) 120.9(4) YES C(23) C(22) C(21) 118.5(5) YES C(23) C(22) C(222) 120.4(5) YES C(21) C(22) C(222) 121.0(4) YES C(22) C(23) C(24) 121.6(5) YES C(25) C(24) C(23) 119.2(5) YES C(24) C(25) C(26) 121.9(5) YES C(21) C(26) C(25) 117.7(4) YES C(21) C(26) C(262) 122.4(4) YES C(25) C(26) C(262) 119.8(4) YES N(31) C(32) C(33) 120.1(4) YES N(31) C(32) C(321) 106.8(4) YES C(33) C(32) C(321) 133.1(4) YES C(32) C(33) C(34) 118.7(5) YES C(35) C(34) C(33) 119.8(5) YES C(34) C(35) C(36) 119.3(5) YES N(31) C(36) C(35) 120.1(4) YES C(42) C(43) C(44) 118.7(6) YES C(43) C(44) C(45) 120.7(6) YES C(44) C(45) C(46) 118.2(5) YES N(41) C(46) C(45) 119.8(5) YES C(12) C(122) C(123) 112.6(4) YES C(12) C(122) C(121) 111.1(4) YES C(123) C(122) C(121) 110.0(5) YES C(16) C(162) C(163) 112.9(4) YES C(16) C(162) C(161) 110.7(4) YES C(163) C(162) C(161) 110.0(5) YES C(221) C(222) C(22) 112.8(5) YES C(221) C(222) C(223) 112.8(6) YES C(22) C(222) C(223) 110.6(5) YES C(26) C(262) C(261) 111.8(4) YES C(26) C(262) C(263) 112.0(5) YES C(261) C(262) C(263) 109.6(5) YES C(32) C(321) C(322) 114.8(5) YES C(32) C(321) Ta 91.2(3) YES C(322) C(321) Ta 124.2(3) YES C(32) C(321) H(321) 103(3) YES C(322) C(321) H(321) 137(3) YES Ta C(321) H(321) 72(4) YES C(321) C(322) H(32A) 104(3) YES C(321) C(322) H(32B) 114(3) YES H(32A) C(322) H(32B) 100(5) YES C(321) C(322) H(32C) 105(4) YES H(32A) C(322) H(32C) 123(5) YES H(32B) C(322) H(32C) 111(5) YES C(422) C(421) C(42) 113.6(5) YES C(422) C(421) Ta 121.7(4) YES C(42) C(421) Ta 92.8(3) YES C(422) C(421) H(421) 111(7) YES C(42) C(421) H(421) 114(6) YES Ta C(421) H(421) 102(6) YES N(41) C(42) C(43) 121.1(5) YES N(41) C(42) C(421) 104.7(5) YES C(43) C(42) C(421) 134.2(5) YES #============================================================================== data_RCI016 _database_code_depnum_ccdc_archive 'CCDC 255069' _audit_creation_date 14-07-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C55 H46 Cl2 N1 O2 Ta1' _chemical_formula_moiety 'C43 H34 Cl2 N1 O2 Ta1,2(C6 H6)' _chemical_formula_structural ? _chemical_formula_weight 1004.84 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4442(4) _cell_length_b 11.7997(4) _cell_length_c 17.5214(5) _cell_angle_alpha 82.0975(19) _cell_angle_beta 84.3171(18) _cell_angle_gamma 75.1193(17) _cell_volume 2259.97(13) _cell_measurement_reflns_used 22282 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.48 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.563 _cell_measurement_temperature 150 _exptl_crystal_F_000 1012 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.2092 _exptl_absorpt_correction_T_max 0.4635 _diffrn_reflns_number 22282 _diffrn_measured_fraction_theta_max 0.7261 _diffrn_reflns_theta_full 18.3 _diffrn_measured_fraction_theta_full 0.9608 _reflns_number_total 10513 _reflns_number_gt 9668 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 22 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.40' # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_gt 0.030 _refine_ls_wR_factor_ref 0.063 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 10509 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.69 _refine_diff_density_min -1.76 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta 0.092689(10) 0.280413(9) 0.272410(6) 0.02050(4) Uani 1 1 d . . . Cl(1) Cl 0.15540(7) 0.26789(6) 0.40006(4) 0.03202(16) Uani 1 1 d . . . Cl(2) Cl 0.30410(6) 0.24740(6) 0.23262(4) 0.03005(15) Uani 1 1 d . . . O(1) O 0.06122(16) 0.27471(16) 0.16936(10) 0.0234(4) Uani 1 1 d . . . O(2) O 0.00118(16) 0.43548(16) 0.27794(10) 0.0232(4) Uani 1 1 d . . . N(1) N 0.1301(2) 0.0853(2) 0.29077(14) 0.0271(5) Uani 1 1 d . . . C(2) C 0.0287(3) 0.0789(2) 0.33519(16) 0.0288(6) Uani 1 1 d . . . C(3) C 0.0191(3) -0.0264(3) 0.3790(2) 0.0421(8) Uani 1 1 d . . . C(4) C 0.1141(4) -0.1252(3) 0.3710(2) 0.0469(9) Uani 1 1 d . . . C(5) C 0.2142(3) -0.1179(3) 0.3217(2) 0.0414(8) Uani 1 1 d . . . C(6) C 0.2213(3) -0.0107(3) 0.28265(18) 0.0331(7) Uani 1 1 d . . . C(7) C -0.0539(3) 0.1993(3) 0.32982(17) 0.0292(6) Uani 1 1 d . . . C(8) C -0.1270(3) 0.2352(3) 0.40364(18) 0.0395(8) Uani 1 1 d . . . C(11) C 0.1046(2) 0.2354(2) 0.09925(15) 0.0237(6) Uani 1 1 d . . . C(12) C 0.1739(2) 0.2988(2) 0.04941(16) 0.0272(6) Uani 1 1 d . . . C(13) C 0.2267(3) 0.2532(3) -0.01925(17) 0.0341(7) Uani 1 1 d . . . C(14) C 0.2087(3) 0.1495(3) -0.03795(18) 0.0385(8) Uani 1 1 d . . . C(15) C 0.1366(3) 0.0905(3) 0.01113(18) 0.0356(7) Uani 1 1 d . . . C(16) C 0.0825(2) 0.1309(3) 0.08071(16) 0.0283(6) Uani 1 1 d . . . C(21) C -0.0751(3) 0.5222(2) 0.31689(15) 0.0247(6) Uani 1 1 d . . . C(22) C -0.0263(3) 0.5853(2) 0.36220(16) 0.0253(6) Uani 1 1 d . . . C(23) C -0.1077(3) 0.6659(2) 0.40606(17) 0.0308(7) Uani 1 1 d . . . C(24) C -0.2318(3) 0.6824(3) 0.40492(18) 0.0365(7) Uani 1 1 d . . . C(25) C -0.2772(3) 0.6213(3) 0.35783(17) 0.0330(7) Uani 1 1 d . . . C(26) C -0.2001(3) 0.5413(2) 0.31189(16) 0.0266(6) Uani 1 1 d . . . C(121) C 0.1929(3) 0.4139(3) 0.06485(15) 0.0279(6) Uani 1 1 d . . . C(122) C 0.3087(3) 0.4303(3) 0.06539(17) 0.0354(7) Uani 1 1 d . . . C(123) C 0.3265(3) 0.5393(3) 0.07367(19) 0.0404(8) Uani 1 1 d . . . C(124) C 0.2280(3) 0.6354(3) 0.08044(19) 0.0405(8) Uani 1 1 d . . . C(125) C 0.1120(3) 0.6210(3) 0.07995(17) 0.0358(7) Uani 1 1 d . . . C(126) C 0.0947(3) 0.5106(3) 0.07300(16) 0.0303(6) Uani 1 1 d . . . C(161) C 0.0048(3) 0.0641(3) 0.13109(17) 0.0303(7) Uani 1 1 d . . . C(162) C -0.1134(3) 0.1178(3) 0.15537(19) 0.0383(8) Uani 1 1 d . . . C(163) C -0.1861(3) 0.0548(3) 0.2006(2) 0.0500(9) Uani 1 1 d . . . C(164) C -0.1408(4) -0.0647(3) 0.2228(2) 0.0527(10) Uani 1 1 d . . . C(165) C -0.0239(4) -0.1196(3) 0.1988(2) 0.0470(9) Uani 1 1 d . . . C(166) C 0.0486(3) -0.0571(3) 0.15353(19) 0.0382(8) Uani 1 1 d . . . C(221) C 0.1058(3) 0.5701(2) 0.36631(16) 0.0254(6) Uani 1 1 d . . . C(222) C 0.1843(3) 0.5669(2) 0.29953(17) 0.0295(6) Uani 1 1 d . . . C(223) C 0.3061(3) 0.5592(3) 0.30454(19) 0.0358(7) Uani 1 1 d . . . C(224) C 0.3517(3) 0.5551(3) 0.3756(2) 0.0403(8) Uani 1 1 d . . . C(225) C 0.2755(3) 0.5573(3) 0.44190(19) 0.0380(8) Uani 1 1 d . . . C(226) C 0.1536(3) 0.5644(2) 0.43762(17) 0.0308(7) Uani 1 1 d . . . C(261) C -0.2522(2) 0.4817(2) 0.25880(16) 0.0275(6) Uani 1 1 d . . . C(262) C -0.3446(3) 0.4261(3) 0.28398(19) 0.0353(7) Uani 1 1 d . . . C(263) C -0.3983(3) 0.3788(3) 0.2324(2) 0.0408(8) Uani 1 1 d . . . C(264) C -0.3585(3) 0.3851(3) 0.1551(2) 0.0388(8) Uani 1 1 d . . . C(265) C -0.2652(3) 0.4376(3) 0.12961(18) 0.0368(7) Uani 1 1 d . . . C(266) C -0.2123(3) 0.4860(3) 0.18114(17) 0.0312(6) Uani 1 1 d . . . C(911) C 0.4677(4) -0.2143(4) 0.1233(3) 0.0751(14) Uani 1 1 d . . . C(912) C 0.5298(4) -0.2260(4) 0.1884(3) 0.0730(13) Uani 1 1 d . . . C(913) C 0.5502(3) -0.1301(4) 0.2132(3) 0.0650(12) Uani 1 1 d . . . C(914) C 0.5101(3) -0.0217(4) 0.1736(3) 0.0601(11) Uani 1 1 d . . . C(915) C 0.4472(3) -0.0083(4) 0.1095(2) 0.0569(10) Uani 1 1 d . . . C(916) C 0.4259(4) -0.1039(4) 0.0839(3) 0.0651(12) Uani 1 1 d . . . C(921) C 0.5110(4) -0.2168(4) 0.5903(2) 0.0572(10) Uani 1 1 d . . . C(922) C 0.4585(5) -0.1116(5) 0.6136(3) 0.0718(13) Uani 1 1 d . . . C(923) C 0.3724(5) -0.0275(4) 0.5678(4) 0.0905(19) Uani 1 1 d . . . C(924) C 0.3489(4) -0.0619(4) 0.4980(3) 0.0703(13) Uani 1 1 d . . . C(925) C 0.4062(4) -0.1701(4) 0.4796(2) 0.0615(11) Uani 1 1 d . . . C(926) C 0.4834(3) -0.2451(4) 0.5244(2) 0.0572(10) Uani 1 1 d . . . H(3) H -0.0500 -0.0304 0.4131 0.051 Uiso 1 1 calc R . . H(4) H 0.1102 -0.1986 0.3998 0.056 Uiso 1 1 calc R . . H(5) H 0.2775 -0.1865 0.3149 0.050 Uiso 1 1 calc R . . H(6) H 0.2910 -0.0043 0.2497 0.040 Uiso 1 1 calc R . . H(7) H -0.106(3) 0.213(3) 0.2891(18) 0.035(8) Uiso 1 1 d . . . H(13) H 0.2756 0.2945 -0.0534 0.041 Uiso 1 1 calc R . . H(14) H 0.2457 0.1190 -0.0843 0.046 Uiso 1 1 calc R . . H(15) H 0.1232 0.0201 -0.0027 0.043 Uiso 1 1 calc R . . H(23) H -0.0771 0.7101 0.4372 0.037 Uiso 1 1 calc R . . H(24) H -0.2855 0.7355 0.4363 0.044 Uiso 1 1 calc R . . H(25) H -0.3624 0.6338 0.3567 0.040 Uiso 1 1 calc R . . H(8A) H -0.1914 0.1931 0.4147 0.059 Uiso 1 1 calc R . . H(8B) H -0.1631 0.3205 0.3973 0.059 Uiso 1 1 calc R . . H(8C) H -0.0737 0.2152 0.4465 0.059 Uiso 1 1 calc R . . H(122) H 0.3768 0.3654 0.0600 0.042 Uiso 1 1 calc R . . H(123) H 0.4064 0.5484 0.0747 0.048 Uiso 1 1 calc R . . H(124) H 0.2402 0.7106 0.0854 0.049 Uiso 1 1 calc R . . H(125) H 0.0442 0.6865 0.0844 0.043 Uiso 1 1 calc R . . H(126) H 0.0146 0.5010 0.0738 0.036 Uiso 1 1 calc R . . H(162) H -0.1448 0.1997 0.1404 0.046 Uiso 1 1 calc R . . H(163) H -0.2667 0.0930 0.2165 0.060 Uiso 1 1 calc R . . H(164) H -0.1901 -0.1086 0.2544 0.063 Uiso 1 1 calc R . . H(165) H 0.0068 -0.2016 0.2138 0.056 Uiso 1 1 calc R . . H(166) H 0.1288 -0.0962 0.1373 0.046 Uiso 1 1 calc R . . H(222) H 0.1538 0.5700 0.2506 0.035 Uiso 1 1 calc R . . H(223) H 0.3587 0.5568 0.2590 0.043 Uiso 1 1 calc R . . H(224) H 0.4352 0.5508 0.3786 0.048 Uiso 1 1 calc R . . H(225) H 0.3068 0.5539 0.4906 0.046 Uiso 1 1 calc R . . H(226) H 0.1019 0.5654 0.4836 0.037 Uiso 1 1 calc R . . H(262) H -0.3716 0.4205 0.3371 0.042 Uiso 1 1 calc R . . H(263) H -0.4623 0.3420 0.2502 0.049 Uiso 1 1 calc R . . H(264) H -0.3955 0.3533 0.1197 0.047 Uiso 1 1 calc R . . H(265) H -0.2369 0.4409 0.0767 0.044 Uiso 1 1 calc R . . H(266) H -0.1482 0.5224 0.1631 0.037 Uiso 1 1 calc R . . H(911) H 0.4537 -0.2820 0.1056 0.090 Uiso 1 1 calc R . . H(912) H 0.5584 -0.3018 0.2159 0.088 Uiso 1 1 calc R . . H(913) H 0.5927 -0.1382 0.2584 0.078 Uiso 1 1 calc R . . H(914) H 0.5260 0.0454 0.1908 0.072 Uiso 1 1 calc R . . H(915) H 0.4184 0.0680 0.0827 0.068 Uiso 1 1 calc R . . H(916) H 0.3824 -0.0949 0.0392 0.078 Uiso 1 1 calc R . . H(921) H 0.5687 -0.2722 0.6209 0.069 Uiso 1 1 calc R . . H(922) H 0.4785 -0.0926 0.6609 0.086 Uiso 1 1 calc R . . H(923) H 0.3329 0.0477 0.5835 0.109 Uiso 1 1 calc R . . H(924) H 0.2935 -0.0094 0.4645 0.084 Uiso 1 1 calc R . . H(925) H 0.3903 -0.1931 0.4326 0.074 Uiso 1 1 calc R . . H(926) H 0.5204 -0.3213 0.5095 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta 0.02332(7) 0.01829(6) 0.01895(6) -0.00349(4) -0.00028(4) -0.00292(4) Cl(1) 0.0445(4) 0.0305(4) 0.0210(3) -0.0070(3) -0.0069(3) -0.0035(3) Cl(2) 0.0238(4) 0.0344(4) 0.0305(4) -0.0046(3) -0.0022(3) -0.0035(3) O(1) 0.0228(10) 0.0235(9) 0.0239(10) -0.0045(8) -0.0001(8) -0.0056(8) O(2) 0.0218(10) 0.0222(9) 0.0239(10) -0.0037(8) 0.0029(8) -0.0039(8) N(1) 0.0305(14) 0.0210(12) 0.0283(13) -0.0033(10) -0.0041(10) -0.0022(10) C(2) 0.0384(17) 0.0241(14) 0.0269(15) -0.0115(13) -0.0047(13) -0.0041(12) C(3) 0.053(2) 0.0343(18) 0.0415(19) -0.0197(16) -0.0046(16) 0.0052(15) C(4) 0.067(3) 0.0243(16) 0.053(2) -0.0173(17) -0.0202(19) 0.0062(15) C(5) 0.052(2) 0.0204(15) 0.051(2) -0.0007(14) -0.0212(17) -0.0052(14) C(6) 0.0358(17) 0.0273(15) 0.0336(16) -0.0001(13) -0.0053(13) -0.0065(13) C(7) 0.0326(17) 0.0301(16) 0.0259(15) -0.0116(13) 0.0023(12) -0.0026(13) C(8) 0.043(2) 0.0358(17) 0.0375(18) -0.0119(15) 0.0122(14) -0.0023(14) C(11) 0.0207(14) 0.0287(14) 0.0197(13) 0.0002(11) -0.0045(11) -0.0062(11) C(12) 0.0234(15) 0.0315(15) 0.0231(14) 0.0001(12) -0.0040(11) -0.0024(12) C(13) 0.0288(16) 0.0461(19) 0.0227(15) -0.0013(14) 0.0008(12) -0.0046(14) C(14) 0.0362(18) 0.049(2) 0.0261(16) 0.0046(15) -0.0031(13) -0.0166(15) C(15) 0.0324(17) 0.0369(17) 0.0373(17) 0.0015(14) -0.0104(14) -0.0168(15) C(16) 0.0234(15) 0.0315(15) 0.0290(15) 0.0005(12) -0.0080(12) -0.0095(13) C(21) 0.0303(16) 0.0178(13) 0.0224(14) -0.0029(11) 0.0047(11) -0.0003(11) C(22) 0.0325(16) 0.0176(13) 0.0233(14) -0.0058(11) 0.0053(11) 0.0010(11) C(23) 0.0397(18) 0.0220(14) 0.0297(15) -0.0082(13) 0.0097(13) -0.0076(12) C(24) 0.0424(19) 0.0265(15) 0.0349(17) -0.0021(14) 0.0126(14) -0.0068(14) C(25) 0.0269(16) 0.0314(16) 0.0345(16) -0.0002(13) 0.0073(13) -0.0022(13) C(26) 0.0290(16) 0.0232(14) 0.0246(14) -0.0058(12) 0.0036(11) 0.0022(12) C(121) 0.0314(16) 0.0327(16) 0.0180(13) -0.0068(13) -0.0021(11) 0.0015(12) C(122) 0.0294(17) 0.0386(18) 0.0338(17) -0.0027(14) -0.0046(13) 0.0019(14) C(123) 0.0354(19) 0.0445(19) 0.0435(19) -0.0142(15) -0.0072(15) -0.0014(16) C(124) 0.046(2) 0.0393(18) 0.0382(18) -0.0144(16) -0.0052(15) -0.0027(15) C(125) 0.0361(18) 0.0365(17) 0.0300(16) -0.0008(14) 0.0011(13) -0.0053(14) C(126) 0.0305(16) 0.0368(16) 0.0221(14) -0.0071(13) 0.0008(12) -0.0026(13) C(161) 0.0307(16) 0.0313(16) 0.0321(16) -0.0060(13) -0.0103(13) -0.0119(13) C(162) 0.0353(18) 0.0369(18) 0.047(2) -0.0126(14) -0.0062(15) -0.0108(15) C(163) 0.038(2) 0.059(2) 0.060(2) -0.0214(18) -0.0006(17) -0.018(2) C(164) 0.061(3) 0.054(2) 0.055(2) -0.035(2) -0.0049(19) -0.0068(19) C(165) 0.066(3) 0.0334(18) 0.049(2) -0.0191(18) -0.0158(19) -0.0082(16) C(166) 0.046(2) 0.0322(17) 0.0396(18) -0.0078(15) -0.0140(15) -0.0124(15) C(221) 0.0340(16) 0.0153(13) 0.0268(14) -0.0071(11) 0.0024(12) -0.0030(11) C(222) 0.0347(17) 0.0228(14) 0.0299(15) -0.0066(12) 0.0025(12) -0.0037(12) C(223) 0.0349(18) 0.0294(16) 0.0424(18) -0.0101(13) 0.0097(14) -0.0070(14) C(224) 0.0353(18) 0.0305(17) 0.056(2) -0.0078(14) -0.0039(16) -0.0079(16) C(225) 0.045(2) 0.0272(16) 0.0419(19) -0.0056(14) -0.0123(15) -0.0056(14) C(226) 0.0450(19) 0.0184(14) 0.0283(15) -0.0085(13) 0.0011(13) -0.0015(12) C(261) 0.0217(15) 0.0265(15) 0.0297(15) -0.0004(11) 0.0008(11) 0.0003(12) C(262) 0.0274(16) 0.0356(17) 0.0387(18) -0.0046(13) 0.0058(13) -0.0018(14) C(263) 0.0268(17) 0.0399(18) 0.054(2) -0.0091(14) -0.0001(15) -0.0013(16) C(264) 0.0312(18) 0.0380(18) 0.046(2) -0.0011(14) -0.0122(15) -0.0066(15) C(265) 0.0373(18) 0.0391(18) 0.0290(16) -0.0018(14) -0.0046(13) 0.0004(14) C(266) 0.0269(16) 0.0309(16) 0.0316(16) -0.0038(12) -0.0006(12) 0.0028(13) C(911) 0.047(3) 0.060(3) 0.127(4) -0.019(2) -0.001(3) -0.032(3) C(912) 0.039(2) 0.063(3) 0.098(4) 0.002(2) 0.000(2) 0.026(3) C(913) 0.034(2) 0.087(3) 0.068(3) -0.004(2) -0.0046(19) -0.004(3) C(914) 0.039(2) 0.064(3) 0.078(3) -0.0118(19) 0.009(2) -0.022(2) C(915) 0.043(2) 0.051(2) 0.061(3) 0.0035(18) 0.0078(19) 0.010(2) C(916) 0.044(2) 0.090(4) 0.060(3) -0.007(2) -0.007(2) -0.019(3) C(921) 0.048(2) 0.072(3) 0.051(2) -0.024(2) -0.0048(18) 0.011(2) C(922) 0.096(4) 0.081(3) 0.054(3) -0.048(3) -0.005(3) -0.010(3) C(923) 0.088(4) 0.044(3) 0.144(5) -0.036(3) 0.052(4) -0.030(3) C(924) 0.039(2) 0.068(3) 0.096(4) -0.018(2) -0.012(2) 0.032(3) C(925) 0.057(3) 0.078(3) 0.051(2) -0.022(2) -0.006(2) -0.001(2) C(926) 0.039(2) 0.070(3) 0.057(2) -0.012(2) 0.0071(18) -0.002(2) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta O(2) 1.8705(18) . ? Ta O(1) 1.8891(17) . ? Ta N(1) 2.215(2) . ? Ta C(7) 2.229(3) . ? Ta Cl(1) 2.3900(7) . ? Ta Cl(2) 2.3976(7) . ? O(1) C(11) 1.374(3) . ? O(2) C(21) 1.375(3) . ? N(1) C(6) 1.341(4) . ? N(1) C(2) 1.345(4) . ? C(2) C(3) 1.391(4) . ? C(2) C(7) 1.487(4) . ? C(3) C(4) 1.388(5) . ? C(4) C(5) 1.378(5) . ? C(5) C(6) 1.372(4) . ? C(7) C(8) 1.519(4) . ? C(7) H(7) 0.94(3) . ? C(11) C(12) 1.392(4) . ? C(11) C(16) 1.406(4) . ? C(12) C(13) 1.403(4) . ? C(12) C(121) 1.494(4) . ? C(13) C(14) 1.379(4) . ? C(14) C(15) 1.376(5) . ? C(15) C(16) 1.398(4) . ? C(16) C(161) 1.485(4) . ? C(21) C(26) 1.399(4) . ? C(21) C(22) 1.401(4) . ? C(22) C(23) 1.403(4) . ? C(22) C(221) 1.484(4) . ? C(23) C(24) 1.385(4) . ? C(24) C(25) 1.383(4) . ? C(25) C(26) 1.399(4) . ? C(26) C(261) 1.491(4) . ? C(121) C(122) 1.388(4) . ? C(121) C(126) 1.393(4) . ? C(122) C(123) 1.381(4) . ? C(123) C(124) 1.388(5) . ? C(124) C(125) 1.382(4) . ? C(125) C(126) 1.389(4) . ? C(161) C(162) 1.391(4) . ? C(161) C(166) 1.403(4) . ? C(162) C(163) 1.377(5) . ? C(163) C(164) 1.387(5) . ? C(164) C(165) 1.380(5) . ? C(165) C(166) 1.372(5) . ? C(221) C(226) 1.399(4) . ? C(221) C(222) 1.402(4) . ? C(222) C(223) 1.384(4) . ? C(223) C(224) 1.387(5) . ? C(224) C(225) 1.381(5) . ? C(225) C(226) 1.385(4) . ? C(261) C(262) 1.388(4) . ? C(261) C(266) 1.390(4) . ? C(262) C(263) 1.390(4) . ? C(263) C(264) 1.384(5) . ? C(264) C(265) 1.375(5) . ? C(265) C(266) 1.390(4) . ? C(911) C(912) 1.376(7) . ? C(911) C(916) 1.379(6) . ? C(912) C(913) 1.347(6) . ? C(913) C(914) 1.358(6) . ? C(914) C(915) 1.364(6) . ? C(915) C(916) 1.354(6) . ? C(921) C(926) 1.332(5) . ? C(921) C(922) 1.333(6) . ? C(922) C(923) 1.427(7) . ? C(923) C(924) 1.411(7) . ? C(924) C(925) 1.343(6) . ? C(925) C(926) 1.314(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(2) Ta O(1) 95.57(8) . . ? O(2) Ta N(1) 156.15(9) . . ? O(1) Ta N(1) 88.55(8) . . ? O(2) Ta C(7) 94.25(10) . . ? O(1) Ta C(7) 97.33(9) . . ? N(1) Ta C(7) 61.91(10) . . ? O(2) Ta Cl(1) 91.19(6) . . ? O(1) Ta Cl(1) 172.63(6) . . ? N(1) Ta Cl(1) 86.43(6) . . ? C(7) Ta Cl(1) 85.05(8) . . ? O(2) Ta Cl(2) 118.76(6) . . ? O(1) Ta Cl(2) 88.69(6) . . ? N(1) Ta Cl(2) 84.74(7) . . ? C(7) Ta Cl(2) 145.79(8) . . ? Cl(1) Ta Cl(2) 85.48(3) . . ? C(11) O(1) Ta 147.38(16) . . ? C(21) O(2) Ta 152.12(17) . . ? C(6) N(1) C(2) 121.5(3) . . ? C(6) N(1) Ta 140.4(2) . . ? C(2) N(1) Ta 96.78(17) . . ? N(1) C(2) C(3) 120.6(3) . . ? N(1) C(2) C(7) 107.5(2) . . ? C(3) C(2) C(7) 131.7(3) . . ? C(4) C(3) C(2) 117.6(3) . . ? C(5) C(4) C(3) 120.6(3) . . ? C(6) C(5) C(4) 119.3(3) . . ? N(1) C(6) C(5) 120.2(3) . . ? C(2) C(7) C(8) 116.2(3) . . ? C(2) C(7) Ta 92.04(18) . . ? C(8) C(7) Ta 124.4(2) . . ? C(2) C(7) H(7) 112.1(19) . . ? C(8) C(7) H(7) 110.0(19) . . ? Ta C(7) H(7) 100.3(19) . . ? O(1) C(11) C(12) 118.4(2) . . ? O(1) C(11) C(16) 119.9(2) . . ? C(12) C(11) C(16) 121.6(2) . . ? C(11) C(12) C(13) 118.4(3) . . ? C(11) C(12) C(121) 123.1(2) . . ? C(13) C(12) C(121) 118.5(3) . . ? C(14) C(13) C(12) 121.1(3) . . ? C(15) C(14) C(13) 119.4(3) . . ? C(14) C(15) C(16) 122.2(3) . . ? C(15) C(16) C(11) 117.3(3) . . ? C(15) C(16) C(161) 119.8(3) . . ? C(11) C(16) C(161) 122.9(2) . . ? O(2) C(21) C(26) 118.4(2) . . ? O(2) C(21) C(22) 119.4(2) . . ? C(26) C(21) C(22) 122.2(2) . . ? C(21) C(22) C(23) 117.5(3) . . ? C(21) C(22) C(221) 123.4(2) . . ? C(23) C(22) C(221) 119.1(2) . . ? C(24) C(23) C(22) 121.4(3) . . ? C(25) C(24) C(23) 119.6(3) . . ? C(24) C(25) C(26) 121.3(3) . . ? C(21) C(26) C(25) 117.8(3) . . ? C(21) C(26) C(261) 122.3(2) . . ? C(25) C(26) C(261) 119.8(3) . . ? C(122) C(121) C(126) 118.2(3) . . ? C(122) C(121) C(12) 121.1(3) . . ? C(126) C(121) C(12) 120.6(3) . . ? C(123) C(122) C(121) 121.2(3) . . ? C(122) C(123) C(124) 120.1(3) . . ? C(125) C(124) C(123) 119.6(3) . . ? C(124) C(125) C(126) 120.0(3) . . ? C(125) C(126) C(121) 121.0(3) . . ? C(162) C(161) C(166) 118.1(3) . . ? C(162) C(161) C(16) 121.7(3) . . ? C(166) C(161) C(16) 120.2(3) . . ? C(163) C(162) C(161) 121.4(3) . . ? C(162) C(163) C(164) 119.6(4) . . ? C(165) C(164) C(163) 119.8(4) . . ? C(166) C(165) C(164) 120.8(3) . . ? C(165) C(166) C(161) 120.3(3) . . ? C(226) C(221) C(222) 118.5(3) . . ? C(226) C(221) C(22) 120.0(3) . . ? C(222) C(221) C(22) 121.4(3) . . ? C(223) C(222) C(221) 120.3(3) . . ? C(222) C(223) C(224) 120.4(3) . . ? C(225) C(224) C(223) 119.9(3) . . ? C(224) C(225) C(226) 120.2(3) . . ? C(225) C(226) C(221) 120.6(3) . . ? C(262) C(261) C(266) 118.4(3) . . ? C(262) C(261) C(26) 121.6(3) . . ? C(266) C(261) C(26) 119.9(3) . . ? C(261) C(262) C(263) 120.8(3) . . ? C(264) C(263) C(262) 120.0(3) . . ? C(265) C(264) C(263) 119.9(3) . . ? C(264) C(265) C(266) 120.1(3) . . ? C(261) C(266) C(265) 120.8(3) . . ? C(912) C(911) C(916) 119.6(4) . . ? C(913) C(912) C(911) 120.2(4) . . ? C(912) C(913) C(914) 120.0(4) . . ? C(913) C(914) C(915) 120.7(4) . . ? C(916) C(915) C(914) 120.0(4) . . ? C(915) C(916) C(911) 119.6(4) . . ? C(926) C(921) C(922) 120.6(4) . . ? C(921) C(922) C(923) 120.2(4) . . ? C(924) C(923) C(922) 116.4(4) . . ? C(925) C(924) C(923) 119.0(4) . . ? C(926) C(925) C(924) 122.2(4) . . ? C(925) C(926) C(921) 121.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(2) Ta O(1) C(11) 143.0(3) . . . . ? N(1) Ta O(1) C(11) -60.5(3) . . . . ? C(7) Ta O(1) C(11) -121.9(3) . . . . ? Cl(1) Ta O(1) C(11) -13.5(7) . . . . ? Cl(2) Ta O(1) C(11) 24.3(3) . . . . ? O(1) Ta O(2) C(21) 143.5(4) . . . . ? N(1) Ta O(2) C(21) 44.4(5) . . . . ? C(7) Ta O(2) C(21) 45.7(4) . . . . ? Cl(1) Ta O(2) C(21) -39.5(4) . . . . ? Cl(2) Ta O(2) C(21) -124.9(3) . . . . ? O(2) Ta N(1) C(6) -172.8(3) . . . . ? O(1) Ta N(1) C(6) 86.6(3) . . . . ? C(7) Ta N(1) C(6) -174.3(3) . . . . ? Cl(1) Ta N(1) C(6) -88.0(3) . . . . ? Cl(2) Ta N(1) C(6) -2.2(3) . . . . ? O(2) Ta N(1) C(2) -7.2(3) . . . . ? O(1) Ta N(1) C(2) -107.79(17) . . . . ? C(7) Ta N(1) C(2) -8.69(16) . . . . ? Cl(1) Ta N(1) C(2) 77.61(16) . . . . ? Cl(2) Ta N(1) C(2) 163.39(16) . . . . ? C(6) N(1) C(2) C(3) 5.0(4) . . . . ? Ta N(1) C(2) C(3) -164.3(2) . . . . ? C(6) N(1) C(2) C(7) -178.6(2) . . . . ? Ta N(1) C(2) C(7) 12.1(2) . . . . ? N(1) C(2) C(3) C(4) -4.2(4) . . . . ? C(7) C(2) C(3) C(4) -179.6(3) . . . . ? C(2) C(3) C(4) C(5) 0.4(5) . . . . ? C(3) C(4) C(5) C(6) 2.6(5) . . . . ? C(2) N(1) C(6) C(5) -1.9(4) . . . . ? Ta N(1) C(6) C(5) 161.3(2) . . . . ? C(4) C(5) C(6) N(1) -1.9(4) . . . . ? N(1) C(2) C(7) C(8) -142.3(3) . . . . ? C(3) C(2) C(7) C(8) 33.6(5) . . . . ? N(1) C(2) C(7) Ta -11.9(2) . . . . ? C(3) C(2) C(7) Ta 163.9(3) . . . . ? O(2) Ta C(7) C(2) -171.60(16) . . . . ? O(1) Ta C(7) C(2) 92.21(17) . . . . ? N(1) Ta C(7) C(2) 7.81(15) . . . . ? Cl(1) Ta C(7) C(2) -80.77(16) . . . . ? Cl(2) Ta C(7) C(2) -6.3(3) . . . . ? O(2) Ta C(7) C(8) -47.6(3) . . . . ? O(1) Ta C(7) C(8) -143.8(3) . . . . ? N(1) Ta C(7) C(8) 131.8(3) . . . . ? Cl(1) Ta C(7) C(8) 43.3(3) . . . . ? Cl(2) Ta C(7) C(8) 117.7(2) . . . . ? Ta O(1) C(11) C(12) -81.5(4) . . . . ? Ta O(1) C(11) C(16) 96.0(3) . . . . ? O(1) C(11) C(12) C(13) 174.7(2) . . . . ? C(16) C(11) C(12) C(13) -2.8(4) . . . . ? O(1) C(11) C(12) C(121) -6.5(4) . . . . ? C(16) C(11) C(12) C(121) 176.1(3) . . . . ? C(11) C(12) C(13) C(14) 1.3(4) . . . . ? C(121) C(12) C(13) C(14) -177.6(3) . . . . ? C(12) C(13) C(14) C(15) 0.8(5) . . . . ? C(13) C(14) C(15) C(16) -1.4(5) . . . . ? C(14) C(15) C(16) C(11) 0.0(4) . . . . ? C(14) C(15) C(16) C(161) 179.5(3) . . . . ? O(1) C(11) C(16) C(15) -175.3(2) . . . . ? C(12) C(11) C(16) C(15) 2.2(4) . . . . ? O(1) C(11) C(16) C(161) 5.2(4) . . . . ? C(12) C(11) C(16) C(161) -177.4(3) . . . . ? Ta O(2) C(21) C(26) -92.5(4) . . . . ? Ta O(2) C(21) C(22) 85.3(4) . . . . ? O(2) C(21) C(22) C(23) -174.8(2) . . . . ? C(26) C(21) C(22) C(23) 2.9(4) . . . . ? O(2) C(21) C(22) C(221) 4.7(4) . . . . ? C(26) C(21) C(22) C(221) -177.6(3) . . . . ? C(21) C(22) C(23) C(24) 0.2(4) . . . . ? C(221) C(22) C(23) C(24) -179.3(3) . . . . ? C(22) C(23) C(24) C(25) -2.1(5) . . . . ? C(23) C(24) C(25) C(26) 1.0(5) . . . . ? O(2) C(21) C(26) C(25) 173.7(2) . . . . ? C(22) C(21) C(26) C(25) -4.0(4) . . . . ? O(2) C(21) C(26) C(261) -7.5(4) . . . . ? C(22) C(21) C(26) C(261) 174.8(3) . . . . ? C(24) C(25) C(26) C(21) 2.0(4) . . . . ? C(24) C(25) C(26) C(261) -176.8(3) . . . . ? C(11) C(12) C(121) C(122) 125.2(3) . . . . ? C(13) C(12) C(121) C(122) -55.9(4) . . . . ? C(11) C(12) C(121) C(126) -59.9(4) . . . . ? C(13) C(12) C(121) C(126) 118.9(3) . . . . ? C(126) C(121) C(122) C(123) -0.1(4) . . . . ? C(12) C(121) C(122) C(123) 174.9(3) . . . . ? C(121) C(122) C(123) C(124) -1.0(5) . . . . ? C(122) C(123) C(124) C(125) 0.9(5) . . . . ? C(123) C(124) C(125) C(126) 0.2(5) . . . . ? C(124) C(125) C(126) C(121) -1.3(4) . . . . ? C(122) C(121) C(126) C(125) 1.2(4) . . . . ? C(12) C(121) C(126) C(125) -173.8(3) . . . . ? C(15) C(16) C(161) C(162) -125.3(3) . . . . ? C(11) C(16) C(161) C(162) 54.2(4) . . . . ? C(15) C(16) C(161) C(166) 52.7(4) . . . . ? C(11) C(16) C(161) C(166) -127.8(3) . . . . ? C(166) C(161) C(162) C(163) 0.4(4) . . . . ? C(16) C(161) C(162) C(163) 178.5(3) . . . . ? C(161) C(162) C(163) C(164) 0.2(5) . . . . ? C(162) C(163) C(164) C(165) -0.6(5) . . . . ? C(163) C(164) C(165) C(166) 0.4(5) . . . . ? C(164) C(165) C(166) C(161) 0.2(5) . . . . ? C(162) C(161) C(166) C(165) -0.6(4) . . . . ? C(16) C(161) C(166) C(165) -178.7(3) . . . . ? C(21) C(22) C(221) C(226) -137.0(3) . . . . ? C(23) C(22) C(221) C(226) 42.4(4) . . . . ? C(21) C(22) C(221) C(222) 46.1(4) . . . . ? C(23) C(22) C(221) C(222) -134.4(3) . . . . ? C(226) C(221) C(222) C(223) -0.5(4) . . . . ? C(22) C(221) C(222) C(223) 176.4(2) . . . . ? C(221) C(222) C(223) C(224) -0.2(4) . . . . ? C(222) C(223) C(224) C(225) 0.7(5) . . . . ? C(223) C(224) C(225) C(226) -0.4(5) . . . . ? C(224) C(225) C(226) C(221) -0.3(4) . . . . ? C(222) C(221) C(226) C(225) 0.8(4) . . . . ? C(22) C(221) C(226) C(225) -176.1(2) . . . . ? C(21) C(26) C(261) C(262) 131.7(3) . . . . ? C(25) C(26) C(261) C(262) -49.5(4) . . . . ? C(21) C(26) C(261) C(266) -51.6(4) . . . . ? C(25) C(26) C(261) C(266) 127.2(3) . . . . ? C(266) C(261) C(262) C(263) -1.7(4) . . . . ? C(26) C(261) C(262) C(263) 175.1(3) . . . . ? C(261) C(262) C(263) C(264) 0.9(5) . . . . ? C(262) C(263) C(264) C(265) 0.5(5) . . . . ? C(263) C(264) C(265) C(266) -1.0(5) . . . . ? C(262) C(261) C(266) C(265) 1.1(4) . . . . ? C(26) C(261) C(266) C(265) -175.8(3) . . . . ? C(264) C(265) C(266) C(261) 0.3(5) . . . . ? C(916) C(911) C(912) C(913) -0.3(7) . . . . ? C(911) C(912) C(913) C(914) -0.5(7) . . . . ? C(912) C(913) C(914) C(915) 1.2(6) . . . . ? C(913) C(914) C(915) C(916) -1.1(6) . . . . ? C(914) C(915) C(916) C(911) 0.2(6) . . . . ? C(912) C(911) C(916) C(915) 0.5(7) . . . . ? C(926) C(921) C(922) C(923) -0.4(7) . . . . ? C(921) C(922) C(923) C(924) -0.8(7) . . . . ? C(922) C(923) C(924) C(925) 1.1(6) . . . . ? C(923) C(924) C(925) C(926) 0.0(7) . . . . ? C(924) C(925) C(926) C(921) -1.3(7) . . . . ? C(922) C(921) C(926) C(925) 1.6(6) . . . . ? #============================================================================ data_RCI054 _database_code_depnum_ccdc_archive 'CCDC 255070' _audit_creation_date 21-10-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.33 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C43 H59 Cl1 N1 Nb1 O3' _chemical_formula_moiety 'C43 H59 Cl1 N1 Nb1 O3' _chemical_formula_structural ? _chemical_formula_weight 766.31 _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 16.4650(10) _cell_length_b 13.6886(7) _cell_length_c 18.7548(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.699(3) _cell_angle_gamma 90.00 _cell_volume 4026.9(4) _cell_measurement_reflns_used 37822 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_meas ? loop_ _atom_type_symbol _atom_type_radius_bond Nb 1.34 Cl 0.99 O 0.73 N 0.75 C 0.77 H 0.32 _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.388 _cell_measurement_temperature 150 _exptl_crystal_F_000 1624 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1997 _exptl_absorpt_correction_T_min 0.7618 _exptl_absorpt_correction_T_max 0.8815 _diffrn_reflns_number 37822 _diffrn_measured_fraction_theta_max 0.9850 _diffrn_reflns_theta_full 26.7 _diffrn_measured_fraction_theta_full 0.9980 _reflns_number_total 9506 _reflns_number_gt 7516 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.095 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.92 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_max 23 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.55' # 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_all 0.095 _refine_ls_R_factor_gt 0.064 _refine_ls_wR_factor_ref 0.179 _refine_ls_wR_factor_gt 0.162 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 9471 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.1159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.54 _refine_diff_density_min -1.90 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb Nb 0.07089(2) 0.09148(2) 0.307208(17) 0.02309(12) Uani 1 1 d . . . Cl Cl 0.11513(6) 0.12086(7) 0.43964(5) 0.0327(2) Uani 1 1 d . . . O(1) O 0.11773(16) -0.03634(17) 0.33141(14) 0.0275(5) Uani 1 1 d . . . O(2) O -0.03972(16) 0.04137(17) 0.26841(14) 0.0277(5) Uani 1 1 d . . . O(3) O 0.02905(16) 0.22111(17) 0.28319(14) 0.0280(5) Uani 1 1 d . . . N(1) N 0.20161(19) 0.1606(2) 0.32072(17) 0.0286(7) Uani 1 1 d . . . C(2) C 0.2056(2) 0.1369(3) 0.2526(2) 0.0295(8) Uani 1 1 d . . . C(3) C 0.2808(3) 0.1519(3) 0.2340(2) 0.0384(10) Uani 1 1 d . . . C(4) C 0.3482(3) 0.1955(3) 0.2854(3) 0.0430(10) Uani 1 1 d . . . C(5) C 0.3426(3) 0.2225(3) 0.3556(3) 0.0404(10) Uani 1 1 d . . . C(6) C 0.2675(2) 0.2019(3) 0.3716(2) 0.0345(9) Uani 1 1 d . . . C(7) C 0.1227(3) 0.0927(3) 0.2083(2) 0.0317(8) Uani 1 1 d . . . C(8) C 0.1301(3) 0.0014(4) 0.1654(3) 0.0488(12) Uani 1 1 d . . . C(11) C 0.1486(2) -0.1203(3) 0.3691(2) 0.0270(8) Uani 1 1 d . . . C(12) C 0.2369(2) -0.1357(3) 0.3964(2) 0.0312(8) Uani 1 1 d . . . C(13) C 0.2656(3) -0.2208(3) 0.4362(2) 0.0363(9) Uani 1 1 d . . . C(14) C 0.2093(3) -0.2892(3) 0.4487(2) 0.0388(9) Uani 1 1 d . . . C(15) C 0.1230(3) -0.2738(3) 0.4208(2) 0.0342(9) Uani 1 1 d . . . C(16) C 0.0898(2) -0.1896(3) 0.3801(2) 0.0282(8) Uani 1 1 d . . . C(21) C -0.1255(2) 0.0255(3) 0.2386(2) 0.0270(7) Uani 1 1 d . . . C(22) C -0.1541(2) -0.0298(3) 0.1730(2) 0.0320(8) Uani 1 1 d . . . C(23) C -0.2419(3) -0.0412(3) 0.1417(3) 0.0427(10) Uani 1 1 d . . . C(24) C -0.2988(3) -0.0023(3) 0.1743(3) 0.0466(11) Uani 1 1 d . . . C(25) C -0.2681(3) 0.0481(3) 0.2409(3) 0.0415(10) Uani 1 1 d . . . C(26) C -0.1818(2) 0.0629(3) 0.2755(2) 0.0314(8) Uani 1 1 d . . . C(31) C 0.0065(2) 0.3142(3) 0.2608(2) 0.0271(8) Uani 1 1 d . . . C(32) C -0.0512(2) 0.3309(3) 0.1891(2) 0.0308(8) Uani 1 1 d . . . C(33) C -0.0709(3) 0.4272(3) 0.1672(2) 0.0356(9) Uani 1 1 d . . . C(34) C -0.0364(3) 0.5045(3) 0.2136(2) 0.0379(9) Uani 1 1 d . . . C(35) C 0.0176(3) 0.4866(3) 0.2844(2) 0.0365(9) Uani 1 1 d . . . C(36) C 0.0399(3) 0.3921(3) 0.3100(2) 0.0298(8) Uani 1 1 d . . . C(121) C 0.3671(4) -0.0325(4) 0.4527(3) 0.0684(16) Uani 1 1 d . . . C(122) C 0.3000(3) -0.0636(3) 0.3817(2) 0.0362(9) Uani 1 1 d . . . C(123) C 0.3405(3) -0.1060(4) 0.3252(3) 0.0560(14) Uani 1 1 d . . . C(161) C -0.0290(3) -0.1123(3) 0.4138(3) 0.0451(11) Uani 1 1 d . . . C(162) C -0.0048(2) -0.1703(3) 0.3542(2) 0.0313(8) Uani 1 1 d . . . C(163) C -0.0591(3) -0.2623(3) 0.3347(3) 0.0453(11) Uani 1 1 d . . . C(221) C -0.0990(3) -0.0328(4) 0.0611(3) 0.0477(11) Uani 1 1 d . . . C(222) C -0.0921(3) -0.0773(3) 0.1376(2) 0.0406(10) Uani 1 1 d . . . C(223) C -0.1046(3) -0.1888(3) 0.1312(3) 0.0478(11) Uani 1 1 d . . . C(261) C -0.1606(3) 0.2274(3) 0.3381(3) 0.0461(11) Uani 1 1 d . . . C(262) C -0.1504(3) 0.1172(3) 0.3498(2) 0.0357(9) Uani 1 1 d . . . C(263) C -0.1966(3) 0.0840(3) 0.4056(3) 0.0435(10) Uani 1 1 d . . . C(321) C -0.1900(3) 0.2493(4) 0.1184(3) 0.0564(13) Uani 1 1 d . . . C(322) C -0.0919(3) 0.2485(3) 0.1364(2) 0.0382(9) Uani 1 1 d . . . C(323) C -0.0679(3) 0.2531(3) 0.0637(2) 0.0477(11) Uani 1 1 d . . . C(361) C 0.0500(4) 0.3975(5) 0.4461(3) 0.0639(15) Uani 1 1 d . . . C(362) C 0.0972(3) 0.3735(3) 0.3891(2) 0.0349(9) Uani 1 1 d . . . C(363) C 0.1808(3) 0.4306(3) 0.4067(3) 0.0505(12) Uani 1 1 d . . . H(3) H 0.2848 0.1321 0.1867 0.046 Uiso 1 1 calc R . . H(4) H 0.3993 0.2076 0.2732 0.052 Uiso 1 1 calc R . . H(5) H 0.3888 0.2541 0.3912 0.049 Uiso 1 1 calc R . . H(6) H 0.2630 0.2174 0.4196 0.041 Uiso 1 1 calc R . . H(7) H 0.087(3) 0.143(3) 0.169(3) 0.050(13) Uiso 1 1 d . . . H(13) H 0.3251 -0.2326 0.4553 0.044 Uiso 1 1 calc R . . H(14) H 0.2304 -0.3467 0.4765 0.047 Uiso 1 1 calc R . . H(15) H 0.0850 -0.3213 0.4293 0.041 Uiso 1 1 calc R . . H(23) H -0.2630 -0.0769 0.0964 0.051 Uiso 1 1 calc R . . H(24) H -0.3585 -0.0100 0.1514 0.056 Uiso 1 1 calc R . . H(25) H -0.3077 0.0736 0.2638 0.050 Uiso 1 1 calc R . . H(33) H -0.1092 0.4401 0.1189 0.043 Uiso 1 1 calc R . . H(34) H -0.0499 0.5697 0.1969 0.046 Uiso 1 1 calc R . . H(35) H 0.0402 0.5402 0.3165 0.044 Uiso 1 1 calc R . . H(8A) H 0.1621 0.0162 0.1304 0.073 Uiso 1 1 calc R . . H(8B) H 0.0730 -0.0218 0.1375 0.073 Uiso 1 1 calc R . . H(8C) H 0.1600 -0.0493 0.2005 0.073 Uiso 1 1 calc R . . H(122) H 0.2675 -0.0039 0.3587 0.043 Uiso 1 1 calc R . . H(12A) H 0.3394 -0.0066 0.4881 0.103 Uiso 1 1 calc R . . H(12B) H 0.4031 0.0183 0.4410 0.103 Uiso 1 1 calc R . . H(12C) H 0.4024 -0.0889 0.4749 0.103 Uiso 1 1 calc R . . H(12D) H 0.3776 -0.0568 0.3131 0.084 Uiso 1 1 calc R . . H(12E) H 0.2957 -0.1247 0.2796 0.084 Uiso 1 1 calc R . . H(12F) H 0.3743 -0.1637 0.3468 0.084 Uiso 1 1 calc R . . H(162) H -0.0178 -0.1289 0.3082 0.038 Uiso 1 1 calc R . . H(16A) H -0.0148 -0.1502 0.4603 0.068 Uiso 1 1 calc R . . H(16B) H -0.0904 -0.0989 0.3968 0.068 Uiso 1 1 calc R . . H(16C) H 0.0024 -0.0505 0.4227 0.068 Uiso 1 1 calc R . . H(16D) H -0.0390 -0.3026 0.3003 0.068 Uiso 1 1 calc R . . H(16E) H -0.1188 -0.2442 0.3108 0.068 Uiso 1 1 calc R . . H(16F) H -0.0544 -0.2994 0.3805 0.068 Uiso 1 1 calc R . . H(222) H -0.0331 -0.0645 0.1712 0.049 Uiso 1 1 calc R . . H(22A) H -0.1579 -0.0383 0.0284 0.072 Uiso 1 1 calc R . . H(22B) H -0.0609 -0.0678 0.0387 0.072 Uiso 1 1 calc R . . H(22C) H -0.0825 0.0362 0.0673 0.072 Uiso 1 1 calc R . . H(22D) H -0.0956 -0.2166 0.1812 0.072 Uiso 1 1 calc R . . H(22E) H -0.0634 -0.2173 0.1088 0.072 Uiso 1 1 calc R . . H(22F) H -0.1626 -0.2036 0.0996 0.072 Uiso 1 1 calc R . . H(262) H -0.0883 0.1028 0.3723 0.043 Uiso 1 1 calc R . . H(26A) H -0.2211 0.2433 0.3161 0.069 Uiso 1 1 calc R . . H(26B) H -0.1290 0.2489 0.3042 0.069 Uiso 1 1 calc R . . H(26C) H -0.1382 0.2607 0.3863 0.069 Uiso 1 1 calc R . . H(26D) H -0.1685 0.1126 0.4548 0.065 Uiso 1 1 calc R . . H(26E) H -0.1947 0.0126 0.4095 0.065 Uiso 1 1 calc R . . H(26F) H -0.2562 0.1056 0.3880 0.065 Uiso 1 1 calc R . . H(322) H -0.0701 0.1853 0.1619 0.046 Uiso 1 1 calc R . . H(32A) H -0.2049 0.2479 0.1652 0.085 Uiso 1 1 calc R . . H(32B) H -0.2141 0.1917 0.0883 0.085 Uiso 1 1 calc R . . H(32C) H -0.2132 0.3086 0.0903 0.085 Uiso 1 1 calc R . . H(32D) H -0.0876 0.3152 0.0382 0.071 Uiso 1 1 calc R . . H(32E) H -0.0949 0.1988 0.0310 0.071 Uiso 1 1 calc R . . H(32F) H -0.0058 0.2484 0.0752 0.071 Uiso 1 1 calc R . . H(362) H 0.1115 0.3023 0.3936 0.042 Uiso 1 1 calc R . . H(36A) H 0.0352 0.4670 0.4428 0.096 Uiso 1 1 calc R . . H(36B) H 0.0869 0.3825 0.4967 0.096 Uiso 1 1 calc R . . H(36C) H -0.0021 0.3583 0.4351 0.096 Uiso 1 1 calc R . . H(36D) H 0.1688 0.5007 0.4070 0.076 Uiso 1 1 calc R . . H(36E) H 0.2086 0.4167 0.3685 0.076 Uiso 1 1 calc R . . H(36F) H 0.2184 0.4109 0.4559 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb 0.02151(18) 0.02213(17) 0.02543(19) 0.00048(12) 0.00686(13) 0.00009(12) Cl 0.0362(5) 0.0361(5) 0.0259(5) -0.0019(4) 0.0094(4) 0.0002(4) O(1) 0.0284(13) 0.0226(12) 0.0329(14) 0.0028(10) 0.0114(11) 0.0011(10) O(2) 0.0250(13) 0.0260(13) 0.0313(14) 0.0024(10) 0.0075(11) -0.0013(10) O(3) 0.0312(14) 0.0194(12) 0.0333(14) 0.0022(10) 0.0095(12) 0.0015(10) N(1) 0.0230(15) 0.0318(17) 0.0299(17) -0.0044(12) 0.0065(13) 0.0000(13) C(2) 0.032(2) 0.0289(19) 0.028(2) 0.0026(15) 0.0102(17) 0.0056(15) C(3) 0.033(2) 0.049(3) 0.036(2) 0.0033(18) 0.0161(19) 0.0083(18) C(4) 0.030(2) 0.050(3) 0.053(3) -0.0028(19) 0.018(2) 0.007(2) C(5) 0.027(2) 0.040(2) 0.052(3) -0.0064(17) 0.0098(19) 0.004(2) C(6) 0.032(2) 0.035(2) 0.037(2) -0.0018(16) 0.0106(18) -0.0010(17) C(7) 0.032(2) 0.039(2) 0.0249(19) 0.0008(17) 0.0093(16) 0.0014(16) C(8) 0.039(2) 0.060(3) 0.053(3) -0.004(2) 0.021(2) -0.019(2) C(11) 0.0315(19) 0.0240(17) 0.0257(19) 0.0030(14) 0.0091(16) -0.0010(14) C(12) 0.032(2) 0.0300(19) 0.030(2) 0.0051(16) 0.0074(17) -0.0017(15) C(13) 0.033(2) 0.035(2) 0.038(2) 0.0070(17) 0.0067(18) 0.0037(17) C(14) 0.046(2) 0.031(2) 0.036(2) 0.0091(18) 0.007(2) 0.0073(17) C(15) 0.046(2) 0.0278(19) 0.031(2) -0.0017(17) 0.0135(18) -0.0013(15) C(16) 0.037(2) 0.0240(17) 0.0239(19) 0.0034(15) 0.0103(16) -0.0020(14) C(21) 0.0214(17) 0.0260(18) 0.032(2) -0.0021(14) 0.0050(15) 0.0011(14) C(22) 0.0259(18) 0.0298(19) 0.039(2) -0.0009(15) 0.0083(17) -0.0072(16) C(23) 0.029(2) 0.052(3) 0.043(2) -0.0047(19) 0.0037(19) -0.013(2) C(24) 0.023(2) 0.058(3) 0.055(3) -0.0061(19) 0.006(2) -0.014(2) C(25) 0.026(2) 0.046(3) 0.052(3) 0.0005(18) 0.011(2) -0.006(2) C(26) 0.0264(19) 0.0300(19) 0.038(2) 0.0014(15) 0.0103(17) -0.0005(16) C(31) 0.0237(18) 0.0256(18) 0.034(2) 0.0041(14) 0.0125(16) 0.0065(15) C(32) 0.0275(19) 0.030(2) 0.034(2) 0.0008(15) 0.0087(17) 0.0046(16) C(33) 0.030(2) 0.038(2) 0.038(2) 0.0055(16) 0.0090(18) 0.0090(17) C(34) 0.043(2) 0.026(2) 0.049(3) 0.0075(17) 0.019(2) 0.0066(17) C(35) 0.039(2) 0.0245(19) 0.050(3) 0.0013(16) 0.020(2) -0.0009(17) C(36) 0.0307(19) 0.0243(19) 0.038(2) 0.0023(15) 0.0152(17) 0.0027(15) C(121) 0.068(4) 0.060(4) 0.063(4) -0.020(3) -0.003(3) -0.003(3) C(122) 0.0258(19) 0.032(2) 0.047(2) 0.0036(15) 0.0060(18) 0.0043(18) C(123) 0.047(3) 0.053(3) 0.079(4) -0.003(2) 0.036(3) 0.002(3) C(161) 0.045(3) 0.040(2) 0.057(3) 0.0065(19) 0.026(2) 0.000(2) C(162) 0.033(2) 0.0274(19) 0.036(2) -0.0010(15) 0.0134(17) 0.0039(15) C(163) 0.039(2) 0.036(2) 0.059(3) -0.0036(18) 0.012(2) 0.004(2) C(221) 0.049(3) 0.047(3) 0.051(3) -0.008(2) 0.020(2) -0.006(2) C(222) 0.030(2) 0.054(3) 0.035(2) -0.0021(18) 0.0055(18) -0.0127(19) C(223) 0.054(3) 0.041(2) 0.045(3) 0.012(2) 0.010(2) -0.005(2) C(261) 0.043(3) 0.044(3) 0.056(3) -0.006(2) 0.021(2) -0.012(2) C(262) 0.028(2) 0.042(2) 0.038(2) 0.0002(17) 0.0118(18) -0.0056(17) C(263) 0.043(3) 0.050(3) 0.041(2) 0.001(2) 0.019(2) 0.000(2) C(321) 0.036(2) 0.058(3) 0.064(3) -0.005(2) -0.002(2) 0.006(3) C(322) 0.040(2) 0.034(2) 0.034(2) 0.0007(17) 0.0021(19) 0.0074(17) C(323) 0.060(3) 0.043(3) 0.036(2) 0.004(2) 0.009(2) 0.0027(19) C(361) 0.062(4) 0.095(5) 0.035(3) 0.004(3) 0.015(3) -0.002(3) C(362) 0.037(2) 0.0303(19) 0.036(2) -0.0032(17) 0.0086(18) -0.0028(17) C(363) 0.045(3) 0.041(3) 0.056(3) -0.011(2) 0.001(2) -0.001(2) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb O(2) 1.874(3) . . ? Nb O(3) 1.907(2) . . ? Nb O(1) 1.910(2) . . ? Nb C(7) 2.266(4) . . ? Nb N(1) 2.293(3) . . ? Nb Cl 2.4003(10) . . ? O(1) C(11) 1.365(4) . . ? O(2) C(21) 1.369(4) . . ? O(3) C(31) 1.357(4) . . ? N(1) C(6) 1.333(5) . . ? N(1) C(2) 1.340(5) . . ? C(2) C(3) 1.398(5) . . ? C(2) C(7) 1.493(5) . . ? C(3) C(4) 1.366(6) . . ? C(4) C(5) 1.398(6) . . ? C(5) C(6) 1.387(5) . . ? C(7) C(8) 1.511(6) . . ? C(7) H(7) 1.04(5) . . ? C(11) C(12) 1.401(5) . . ? C(11) C(16) 1.415(5) . . ? C(12) C(13) 1.387(5) . . ? C(12) C(122) 1.518(5) . . ? C(13) C(14) 1.387(6) . . ? C(14) C(15) 1.373(6) . . ? C(15) C(16) 1.398(5) . . ? C(16) C(162) 1.507(5) . . ? C(21) C(22) 1.399(5) . . ? C(21) C(26) 1.411(5) . . ? C(22) C(23) 1.393(5) . . ? C(22) C(222) 1.522(5) . . ? C(23) C(24) 1.373(6) . . ? C(24) C(25) 1.380(6) . . ? C(25) C(26) 1.387(6) . . ? C(26) C(262) 1.524(6) . . ? C(31) C(36) 1.408(5) . . ? C(31) C(32) 1.410(5) . . ? C(32) C(33) 1.389(5) . . ? C(32) C(322) 1.515(6) . . ? C(33) C(34) 1.377(6) . . ? C(34) C(35) 1.377(6) . . ? C(35) C(36) 1.390(5) . . ? C(36) C(362) 1.517(6) . . ? C(121) C(122) 1.510(7) . . ? C(122) C(123) 1.526(6) . . ? C(161) C(162) 1.519(5) . . ? C(162) C(163) 1.524(5) . . ? C(221) C(222) 1.530(6) . . ? C(222) C(223) 1.541(6) . . ? C(261) C(262) 1.527(6) . . ? C(262) C(263) 1.538(5) . . ? C(321) C(322) 1.547(6) . . ? C(322) C(323) 1.533(6) . . ? C(361) C(362) 1.536(6) . . ? C(362) C(363) 1.528(6) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(2) Nb O(3) 90.58(11) . . . ? O(2) Nb O(1) 91.80(11) . . . ? O(3) Nb O(1) 177.45(10) . . . ? O(2) Nb C(7) 104.38(13) . . . ? O(3) Nb C(7) 89.93(13) . . . ? O(1) Nb C(7) 88.62(12) . . . ? O(2) Nb N(1) 164.28(11) . . . ? O(3) Nb N(1) 84.37(11) . . . ? O(1) Nb N(1) 93.10(11) . . . ? C(7) Nb N(1) 60.86(13) . . . ? O(2) Nb Cl 114.61(8) . . . ? O(3) Nb Cl 93.60(8) . . . ? O(1) Nb Cl 86.22(8) . . . ? C(7) Nb Cl 140.78(11) . . . ? N(1) Nb Cl 80.63(8) . . . ? C(11) O(1) Nb 162.7(2) . . . ? C(21) O(2) Nb 167.7(2) . . . ? C(31) O(3) Nb 172.6(2) . . . ? C(6) N(1) C(2) 121.3(3) . . . ? C(6) N(1) Nb 141.9(3) . . . ? C(2) N(1) Nb 96.4(2) . . . ? N(1) C(2) C(3) 120.4(4) . . . ? N(1) C(2) C(7) 109.1(3) . . . ? C(3) C(2) C(7) 130.5(4) . . . ? C(4) C(3) C(2) 118.7(4) . . . ? C(3) C(4) C(5) 120.4(4) . . . ? C(6) C(5) C(4) 118.0(4) . . . ? N(1) C(6) C(5) 121.1(4) . . . ? C(2) C(7) C(8) 115.0(3) . . . ? C(2) C(7) Nb 93.2(2) . . . ? C(8) C(7) Nb 122.8(3) . . . ? C(2) C(7) H(7) 110(3) . . . ? C(8) C(7) H(7) 107(3) . . . ? Nb C(7) H(7) 108(2) . . . ? O(1) C(11) C(12) 119.8(3) . . . ? O(1) C(11) C(16) 118.4(3) . . . ? C(12) C(11) C(16) 121.8(3) . . . ? C(13) C(12) C(11) 117.9(4) . . . ? C(13) C(12) C(122) 120.2(4) . . . ? C(11) C(12) C(122) 121.9(3) . . . ? C(14) C(13) C(12) 121.5(4) . . . ? C(15) C(14) C(13) 119.9(4) . . . ? C(14) C(15) C(16) 121.5(4) . . . ? C(15) C(16) C(11) 117.4(4) . . . ? C(15) C(16) C(162) 121.0(3) . . . ? C(11) C(16) C(162) 121.5(3) . . . ? O(2) C(21) C(22) 118.4(3) . . . ? O(2) C(21) C(26) 119.5(3) . . . ? C(22) C(21) C(26) 122.1(3) . . . ? C(23) C(22) C(21) 117.4(3) . . . ? C(23) C(22) C(222) 121.0(4) . . . ? C(21) C(22) C(222) 121.5(3) . . . ? C(24) C(23) C(22) 122.0(4) . . . ? C(23) C(24) C(25) 119.0(4) . . . ? C(24) C(25) C(26) 122.6(4) . . . ? C(25) C(26) C(21) 116.7(4) . . . ? C(25) C(26) C(262) 121.0(3) . . . ? C(21) C(26) C(262) 122.3(3) . . . ? O(3) C(31) C(36) 119.5(3) . . . ? O(3) C(31) C(32) 119.3(3) . . . ? C(36) C(31) C(32) 121.2(3) . . . ? C(33) C(32) C(31) 117.7(4) . . . ? C(33) C(32) C(322) 119.8(4) . . . ? C(31) C(32) C(322) 122.5(3) . . . ? C(34) C(33) C(32) 121.8(4) . . . ? C(35) C(34) C(33) 119.6(4) . . . ? C(34) C(35) C(36) 121.6(4) . . . ? C(35) C(36) C(31) 117.9(4) . . . ? C(35) C(36) C(362) 121.0(4) . . . ? C(31) C(36) C(362) 121.1(3) . . . ? C(121) C(122) C(12) 112.4(4) . . . ? C(121) C(122) C(123) 111.2(4) . . . ? C(12) C(122) C(123) 110.3(4) . . . ? C(16) C(162) C(161) 109.4(3) . . . ? C(16) C(162) C(163) 113.9(3) . . . ? C(161) C(162) C(163) 110.1(3) . . . ? C(22) C(222) C(221) 111.8(4) . . . ? C(22) C(222) C(223) 111.4(4) . . . ? C(221) C(222) C(223) 110.6(4) . . . ? C(26) C(262) C(261) 111.0(4) . . . ? C(26) C(262) C(263) 112.2(3) . . . ? C(261) C(262) C(263) 109.5(3) . . . ? C(32) C(322) C(323) 111.6(3) . . . ? C(32) C(322) C(321) 111.2(4) . . . ? C(323) C(322) C(321) 109.9(4) . . . ? C(36) C(362) C(363) 112.1(4) . . . ? C(36) C(362) C(361) 110.4(4) . . . ? C(363) C(362) C(361) 110.6(4) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(2) Nb O(1) C(11) -95.4(8) . . . . ? O(3) Nb O(1) C(11) 105(2) . . . . ? C(7) Nb O(1) C(11) 160.2(8) . . . . ? N(1) Nb O(1) C(11) 99.5(8) . . . . ? Cl Nb O(1) C(11) 19.1(8) . . . . ? O(3) Nb O(2) C(21) -6.3(11) . . . . ? O(1) Nb O(2) C(21) 174.6(11) . . . . ? C(7) Nb O(2) C(21) -96.3(11) . . . . ? N(1) Nb O(2) C(21) -77.2(12) . . . . ? Cl Nb O(2) C(21) 88.0(11) . . . . ? O(2) Nb O(3) C(31) -123(2) . . . . ? O(1) Nb O(3) C(31) 36(4) . . . . ? C(7) Nb O(3) C(31) -19(2) . . . . ? N(1) Nb O(3) C(31) 42(2) . . . . ? Cl Nb O(3) C(31) 122(2) . . . . ? O(2) Nb N(1) C(6) 162.6(4) . . . . ? O(3) Nb N(1) C(6) 90.8(4) . . . . ? O(1) Nb N(1) C(6) -89.4(4) . . . . ? C(7) Nb N(1) C(6) -176.1(5) . . . . ? Cl Nb N(1) C(6) -3.8(4) . . . . ? O(2) Nb N(1) C(2) -25.8(5) . . . . ? O(3) Nb N(1) C(2) -97.6(2) . . . . ? O(1) Nb N(1) C(2) 82.2(2) . . . . ? C(7) Nb N(1) C(2) -4.5(2) . . . . ? Cl Nb N(1) C(2) 167.8(2) . . . . ? C(6) N(1) C(2) C(3) 2.3(6) . . . . ? Nb N(1) C(2) C(3) -171.6(3) . . . . ? C(6) N(1) C(2) C(7) -179.7(3) . . . . ? Nb N(1) C(2) C(7) 6.3(3) . . . . ? N(1) C(2) C(3) C(4) -3.2(6) . . . . ? C(7) C(2) C(3) C(4) 179.3(4) . . . . ? C(2) C(3) C(4) C(5) 1.4(7) . . . . ? C(3) C(4) C(5) C(6) 1.2(7) . . . . ? C(2) N(1) C(6) C(5) 0.5(6) . . . . ? Nb N(1) C(6) C(5) 170.7(3) . . . . ? C(4) C(5) C(6) N(1) -2.3(6) . . . . ? N(1) C(2) C(7) C(8) -135.0(4) . . . . ? C(3) C(2) C(7) C(8) 42.7(6) . . . . ? N(1) C(2) C(7) Nb -6.3(3) . . . . ? C(3) C(2) C(7) Nb 171.3(4) . . . . ? O(2) Nb C(7) C(2) 178.2(2) . . . . ? O(3) Nb C(7) C(2) 87.6(2) . . . . ? O(1) Nb C(7) C(2) -90.3(2) . . . . ? N(1) Nb C(7) C(2) 4.0(2) . . . . ? Cl Nb C(7) C(2) -8.0(3) . . . . ? O(2) Nb C(7) C(8) -59.1(4) . . . . ? O(3) Nb C(7) C(8) -149.7(3) . . . . ? O(1) Nb C(7) C(8) 32.4(3) . . . . ? N(1) Nb C(7) C(8) 126.7(4) . . . . ? Cl Nb C(7) C(8) 114.7(3) . . . . ? Nb O(1) C(11) C(12) -100.8(8) . . . . ? Nb O(1) C(11) C(16) 78.8(9) . . . . ? O(1) C(11) C(12) C(13) 178.3(3) . . . . ? C(16) C(11) C(12) C(13) -1.3(5) . . . . ? O(1) C(11) C(12) C(122) -3.3(5) . . . . ? C(16) C(11) C(12) C(122) 177.2(3) . . . . ? C(11) C(12) C(13) C(14) 0.3(6) . . . . ? C(122) C(12) C(13) C(14) -178.2(4) . . . . ? C(12) C(13) C(14) C(15) 0.6(6) . . . . ? C(13) C(14) C(15) C(16) -0.5(6) . . . . ? C(14) C(15) C(16) C(11) -0.5(5) . . . . ? C(14) C(15) C(16) C(162) -175.8(4) . . . . ? O(1) C(11) C(16) C(15) -178.2(3) . . . . ? C(12) C(11) C(16) C(15) 1.4(5) . . . . ? O(1) C(11) C(16) C(162) -2.8(5) . . . . ? C(12) C(11) C(16) C(162) 176.7(3) . . . . ? Nb O(2) C(21) C(22) 123.4(10) . . . . ? Nb O(2) C(21) C(26) -58.2(12) . . . . ? O(2) C(21) C(22) C(23) -177.0(4) . . . . ? C(26) C(21) C(22) C(23) 4.5(6) . . . . ? O(2) C(21) C(22) C(222) 3.9(5) . . . . ? C(26) C(21) C(22) C(222) -174.5(4) . . . . ? C(21) C(22) C(23) C(24) -1.7(7) . . . . ? C(222) C(22) C(23) C(24) 177.4(4) . . . . ? C(22) C(23) C(24) C(25) -1.2(7) . . . . ? C(23) C(24) C(25) C(26) 1.4(7) . . . . ? C(24) C(25) C(26) C(21) 1.3(7) . . . . ? C(24) C(25) C(26) C(262) -178.7(4) . . . . ? O(2) C(21) C(26) C(25) 177.3(3) . . . . ? C(22) C(21) C(26) C(25) -4.3(6) . . . . ? O(2) C(21) C(26) C(262) -2.7(5) . . . . ? C(22) C(21) C(26) C(262) 175.7(4) . . . . ? Nb O(3) C(31) C(36) -100.2(19) . . . . ? Nb O(3) C(31) C(32) 81(2) . . . . ? O(3) C(31) C(32) C(33) -178.1(3) . . . . ? C(36) C(31) C(32) C(33) 3.0(5) . . . . ? O(3) C(31) C(32) C(322) 2.2(5) . . . . ? C(36) C(31) C(32) C(322) -176.8(3) . . . . ? C(31) C(32) C(33) C(34) -0.7(6) . . . . ? C(322) C(32) C(33) C(34) 179.1(4) . . . . ? C(32) C(33) C(34) C(35) -1.5(6) . . . . ? C(33) C(34) C(35) C(36) 1.4(6) . . . . ? C(34) C(35) C(36) C(31) 0.9(6) . . . . ? C(34) C(35) C(36) C(362) -178.0(3) . . . . ? O(3) C(31) C(36) C(35) 178.0(3) . . . . ? C(32) C(31) C(36) C(35) -3.1(5) . . . . ? O(3) C(31) C(36) C(362) -3.2(5) . . . . ? C(32) C(31) C(36) C(362) 175.7(3) . . . . ? C(13) C(12) C(122) C(121) -54.2(5) . . . . ? C(11) C(12) C(122) C(121) 127.4(4) . . . . ? C(13) C(12) C(122) C(123) 70.6(5) . . . . ? C(11) C(12) C(122) C(123) -107.9(4) . . . . ? C(15) C(16) C(162) C(161) 90.3(4) . . . . ? C(11) C(16) C(162) C(161) -84.9(4) . . . . ? C(15) C(16) C(162) C(163) -33.3(5) . . . . ? C(11) C(16) C(162) C(163) 151.5(4) . . . . ? C(23) C(22) C(222) C(221) 66.8(5) . . . . ? C(21) C(22) C(222) C(221) -114.2(4) . . . . ? C(23) C(22) C(222) C(223) -57.5(5) . . . . ? C(21) C(22) C(222) C(223) 121.5(4) . . . . ? C(25) C(26) C(262) C(261) -78.5(5) . . . . ? C(21) C(26) C(262) C(261) 101.5(4) . . . . ? C(25) C(26) C(262) C(263) 44.3(5) . . . . ? C(21) C(26) C(262) C(263) -135.7(4) . . . . ? C(33) C(32) C(322) C(323) 61.5(5) . . . . ? C(31) C(32) C(322) C(323) -118.7(4) . . . . ? C(33) C(32) C(322) C(321) -61.6(5) . . . . ? C(31) C(32) C(322) C(321) 118.2(4) . . . . ? C(35) C(36) C(362) C(363) -53.8(5) . . . . ? C(31) C(36) C(362) C(363) 127.4(4) . . . . ? C(35) C(36) C(362) C(361) 70.0(5) . . . . ? C(31) C(36) C(362) C(361) -108.8(4) . . . . ?