# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2067 # Polynuclear tantalum oxoalkoxides. Crystal Structures of # [Ta8O10(OEt)20], [Ta7O9(OPri)17] and [Ta5O7(OBut)11] # # Isaac Abrahams, D.C.Bradley, H.Chudzynska, M.Motevalli # and P.O'Shaughnessy # Name and address of author for correspondence data_global _publ_contact_author_name 'Dr. Isaac Abrahams' _publ_contact_author_address ; Department of Chemistry Queen Mary and Westfield College Mile End Road London E1 4NS UK ; _publ_contact_author_email i.abrahams@qmw.ac.uk _publ_contact_author_fax '44(0)207 882 7794' _publ_contact_author_phone '44(0)207 882 3235' _publ_requested_journal 'J. Chem. Soc Dalton Trans' _publ_section_title ; Polynuclear tantalum oxoalkoxides. Crystal Structures of [Ta8O10(OEt)20], [Ta7O9(OPri)17] and [Ta5O7(OBut)11] ; loop_ _publ_author_name _publ_author_address 'Isaac Abrahams' ; Department of Chemistry Queen Mary and Westfield College Mile End Road London E1 4NS UK ; 'Donald C. Bradley' ; Department of Chemistry Queen Mary and Westfield College Mile End Road London E1 4NS UK ; 'Halina Chudzynska' ; Department of Chemistry Queen Mary and Westfield College Mile End Road London E1 4NS UK ; 'Majid Motevalli' ; Department of Chemistry Queen Mary and Westfield College Mile End Road London E1 4NS UK ; 'Paul O'Shaugnessy' ; Department of Chemistry Queen Mary and Westfield College Mile End Road London E1 4NS UK ; _publ_section_exptl_refinement ; Due to rapid sample decomposition, data for structures 1 and 4 were collected sequentially on two and three similar sized crystals respectively. Data for structure 3 were initially corrected for absorption by empirical methods (psi-scans). The structures were solved by Patterson methods using the SHELXS-97 program and developed by difference Fourier techniques with subsequent refinement on F-squared by full matrix least squares using SHELXL-97. Initial refinements of structures 1 and 4 were carried out using individual batch scale factors with no merging of equivalent reflections. In the final stages of refinement, data were corrected for absorption against a refined isotropic model with the program DIFABS. In all cases merging of equivalent reflections was carried out after absorption correction. The H atoms were calculated geometrically and thermal parameters refined with a riding model. Anisotropic thermal parameters were refined for all non-hydrogen atoms. Soft bond length constraints were applied to C-C bonds and in the case of structure 1 also to C-O bonds. ; #----------------------------- COMPOUND(S) DETAILS -------------------------# #--Structure 1 data_h-ta2j _audit_creation_date 2000-02-29T20:08:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H100 O30 Ta8' _chemical_formula_structural 'C40 H100 O30 TA8' _chemical_formula_sum 'C40 H100 O30 Ta8' _chemical_formula_weight 2508.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 16.956(2) _cell_length_b 14.1310(10) _cell_length_c 14.927(2) _cell_angle_alpha 90 _cell_angle_beta 90.090(10) _cell_angle_gamma 90 _cell_volume 3576.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.48 _cell_measurement_theta_max 14.42 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 2.33 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_special_details ; Due to decomposition, intensity data were collected sequentially on two similar sized crystals. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.252 _exptl_absorpt_factor_muR 3.063 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.0052 _exptl_absorpt_correction_T_max 0.0468 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4 _diffrn_standards_decay_corr_max 1.058 _diffrn_standards_decay_corr_min 0.961 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -9 3 6 -4 1 8 _diffrn_reflns_number 6535 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.16 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 6277 _reflns_number_gt 4001 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4/PC (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4/PC (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Initial refinement was carried out using unmerged data with individual batch scale factors. Rescaling and merging of equivalent reflections was carried out after absorption correction using DIFABS (Walker & Stuart, 1983). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6277 _refine_ls_number_parameters 355 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.115 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1799 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.083 _refine_ls_shift/su_mean 0.005 _refine_diff_density_max 1.453 _refine_diff_density_min -2.269 _refine_diff_density_rms 0.321 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ta1 Ta 0.53754(4) 0.84933(5) 0.48228(5) 0.0636(3) Uani 1 1 d . . . Ta2 Ta 0.46365(5) 0.81697(6) 0.68456(6) 0.0730(3) Uani 1 1 d . . . Ta3 Ta 0.34623(5) 0.79955(6) 0.50015(6) 0.0741(3) Uani 1 1 d . . . Ta4 Ta 0.60107(5) 1.01426(6) 0.65944(5) 0.0698(3) Uani 1 1 d . . . O1 O 0.4401(8) 0.8687(7) 0.5611(7) 0.065(3) Uani 1 1 d . . . O2 O 0.5467(8) 0.7582(9) 0.5992(8) 0.072(3) Uani 1 1 d . . . O3 O 0.4940(7) 0.9232(9) 0.3888(8) 0.068(3) Uani 1 1 d . . . O4 O 0.6146(8) 0.7801(10) 0.4239(9) 0.087(4) Uani 1 1 d D . . O5 O 0.5967(6) 0.9369(8) 0.5443(8) 0.066(3) Uani 1 1 d . . . O6 O 0.5369(8) 0.9088(10) 0.7105(9) 0.078(4) Uani 1 1 d . . . O7 O 0.3821(9) 0.8816(12) 0.7453(10) 0.099(5) Uani 1 1 d D . . O8 O 0.4868(11) 0.7235(11) 0.7704(11) 0.109(5) Uani 1 1 d D . . O9 O 0.3811(9) 0.7271(9) 0.6217(9) 0.080(4) Uani 1 1 d . . . O10 O 0.2643(9) 0.8530(12) 0.5636(11) 0.103(5) Uani 1 1 d D . . O11 O 0.2926(9) 0.6958(11) 0.4558(12) 0.104(5) Uani 1 1 d D . . O12 O 0.4518(8) 0.7426(9) 0.4487(9) 0.079(4) Uani 1 1 d . . . O13 O 0.5964(10) 1.0821(13) 0.7673(10) 0.101(5) Uani 1 1 d D . . O14 O 0.6574(7) 1.1158(9) 0.5942(9) 0.072(3) Uani 1 1 d . . . O15 O 0.6988(9) 0.9617(13) 0.6854(11) 0.096(5) Uani 1 1 d D . . C1 C 0.6258(14) 0.7223(12) 0.6327(16) 0.094(7) Uani 1 1 d D . . H1A H 0.6312 0.7326 0.6967 0.113 Uiso 1 1 calc R . . H1B H 0.6689 0.7539 0.6022 0.113 Uiso 1 1 calc R . . C2 C 0.625(2) 0.6156(14) 0.611(2) 0.144(12) Uani 1 1 d D . . H2A H 0.5979 0.582 0.6575 0.217 Uiso 1 1 calc R . . H2B H 0.678 0.5928 0.6062 0.217 Uiso 1 1 calc R . . H2C H 0.598 0.6056 0.5548 0.217 Uiso 1 1 calc R . . C3 C 0.6744(18) 0.748(3) 0.367(2) 0.171(16) Uani 1 1 d D . . H3A H 0.6641 0.7708 0.3066 0.205 Uiso 1 1 calc R . . H3B H 0.6739 0.6796 0.3654 0.205 Uiso 1 1 calc R . . C4 C 0.7541(19) 0.781(4) 0.396(3) 0.27(3) Uani 1 1 d D . . H4A H 0.7541 0.7915 0.4598 0.408 Uiso 1 1 calc R . . H4B H 0.7666 0.8398 0.3663 0.408 Uiso 1 1 calc R . . H4C H 0.7929 0.7346 0.3812 0.408 Uiso 1 1 calc R . . C5 C 0.3593(19) 0.9787(18) 0.759(3) 0.169(17) Uani 1 1 d D . . H5A H 0.3033 0.9879 0.7488 0.203 Uiso 1 1 calc R . . H5B H 0.3889 1.0213 0.7211 0.203 Uiso 1 1 calc R . . C6 C 0.380(3) 0.992(4) 0.857(3) 0.34(5) Uani 1 1 d D . . H6A H 0.4364 0.9868 0.864 0.514 Uiso 1 1 calc R . . H6B H 0.3548 0.9438 0.8917 0.514 Uiso 1 1 calc R . . H6C H 0.3631 1.0531 0.8763 0.514 Uiso 1 1 calc R . . C7 C 0.511(2) 0.652(2) 0.832(2) 0.173(16) Uani 1 1 d D . . H7A H 0.5669 0.6585 0.8453 0.208 Uiso 1 1 calc R . . H7B H 0.5024 0.5897 0.8064 0.208 Uiso 1 1 calc R . . C8 C 0.464(3) 0.663(3) 0.915(3) 0.27(3) Uani 1 1 d D . . H8A H 0.4656 0.7277 0.9342 0.399 Uiso 1 1 calc R . . H8B H 0.4861 0.6233 0.9614 0.399 Uiso 1 1 calc R . . H8C H 0.4106 0.6444 0.9039 0.399 Uiso 1 1 calc R . . C9 C 0.3376(15) 0.6457(15) 0.6600(18) 0.108(8) Uani 1 1 d D . . H9A H 0.2827 0.648 0.6418 0.13 Uiso 1 1 calc R . . H9B H 0.3399 0.6478 0.725 0.13 Uiso 1 1 calc R . . C10 C 0.375(2) 0.5572(17) 0.627(2) 0.143(13) Uani 1 1 d D . . H10A H 0.3808 0.5607 0.5628 0.215 Uiso 1 1 calc R . . H10B H 0.3423 0.504 0.6418 0.215 Uiso 1 1 calc R . . H10C H 0.4258 0.5497 0.654 0.215 Uiso 1 1 calc R . . C11 C 0.2066(17) 0.895(4) 0.619(3) 0.24(3) Uani 1 1 d D . . H11A H 0.2088 0.963 0.6103 0.289 Uiso 1 1 calc R . . H11B H 0.221 0.8828 0.681 0.289 Uiso 1 1 calc R . . C12 C 0.124(2) 0.864(5) 0.606(4) 0.42(7) Uani 1 1 d D . . H12A H 0.1227 0.7998 0.5858 0.632 Uiso 1 1 calc R . . H12B H 0.0986 0.904 0.5622 0.632 Uiso 1 1 calc R . . H12C H 0.0957 0.869 0.6618 0.632 Uiso 1 1 calc R . . C13 C 0.2419(18) 0.632(3) 0.413(3) 0.23(3) Uani 1 1 d D . . H13A H 0.2324 0.5799 0.4543 0.281 Uiso 1 1 calc R . . H13B H 0.2695 0.606 0.3619 0.281 Uiso 1 1 calc R . . C14 C 0.164(3) 0.667(4) 0.382(3) 0.27(3) Uani 1 1 d D . . H14A H 0.1377 0.699 0.4297 0.403 Uiso 1 1 calc R . . H14B H 0.1324 0.6144 0.362 0.403 Uiso 1 1 calc R . . H14C H 0.1715 0.7099 0.3326 0.403 Uiso 1 1 calc R . . C15 C 0.471(2) 0.642(3) 0.401(2) 0.166(16) Uani 1 1 d D . . H15A H 0.5245 0.6208 0.4111 0.199 Uiso 1 1 calc R . . H15B H 0.4339 0.5926 0.4172 0.199 Uiso 1 1 calc R . . C16 C 0.458(3) 0.677(3) 0.308(3) 0.21(2) Uani 1 1 d D . . H16A H 0.4074 0.7062 0.3038 0.311 Uiso 1 1 calc R . . H16B H 0.4611 0.6248 0.2669 0.311 Uiso 1 1 calc R . . H16C H 0.4984 0.7223 0.2935 0.311 Uiso 1 1 calc R . . C17 C 0.584(5) 1.055(5) 0.859(2) 0.43(6) Uani 1 1 d DU . . H17A H 0.6247 1.0127 0.8818 0.52 Uiso 1 1 calc R . . H17B H 0.5322 1.0289 0.87 0.52 Uiso 1 1 calc R . . C18 C 0.593(5) 1.155(5) 0.892(4) 0.31(4) Uani 1 1 d D . . H18A H 0.5897 1.1981 0.8421 0.466 Uiso 1 1 calc R . . H18B H 0.6436 1.1625 0.9207 0.466 Uiso 1 1 calc R . . H18C H 0.5521 1.1694 0.934 0.466 Uiso 1 1 calc R . . C19 C 0.764(2) 0.930(3) 0.631(3) 0.21(2) Uani 1 1 d D . . H19A H 0.7539 0.9427 0.5685 0.253 Uiso 1 1 calc R . . H19B H 0.7727 0.8629 0.6391 0.253 Uiso 1 1 calc R . . C20 C 0.834(3) 0.984(4) 0.662(4) 0.32(4) Uani 1 1 d DU . . H20A H 0.8252 1.0508 0.6526 0.478 Uiso 1 1 calc R . . H20B H 0.8797 0.9645 0.6295 0.478 Uiso 1 1 calc R . . H20C H 0.8422 0.9731 0.7251 0.478 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0607(4) 0.0605(4) 0.0696(5) -0.0093(3) 0.0291(3) 0.0013(3) Ta2 0.0787(6) 0.0696(5) 0.0708(5) 0.0051(4) 0.0301(4) -0.0036(4) Ta3 0.0656(5) 0.0715(5) 0.0854(6) -0.0069(4) 0.0279(4) -0.0134(4) Ta4 0.0685(5) 0.0759(5) 0.0650(5) -0.0059(4) 0.0163(4) -0.0059(4) O1 0.095(9) 0.044(6) 0.057(7) -0.010(5) 0.027(6) 0.002(5) O2 0.078(8) 0.068(7) 0.069(8) -0.004(6) 0.024(7) 0.006(6) O3 0.073(8) 0.074(7) 0.058(7) -0.013(6) 0.017(6) -0.010(6) O4 0.083(9) 0.089(9) 0.090(10) -0.011(7) 0.043(8) 0.022(7) O5 0.034(5) 0.080(7) 0.085(8) 0.003(7) 0.026(5) 0.001(5) O6 0.069(8) 0.091(9) 0.074(8) 0.001(7) 0.021(6) 0.007(7) O7 0.092(11) 0.108(11) 0.098(11) -0.011(9) 0.047(9) -0.004(9) O8 0.136(15) 0.089(10) 0.104(12) 0.026(9) 0.030(11) -0.004(10) O9 0.099(10) 0.066(7) 0.076(8) 0.011(7) 0.022(8) -0.010(7) O10 0.080(10) 0.126(13) 0.105(11) 0.004(10) 0.045(9) -0.006(9) O11 0.087(10) 0.095(11) 0.131(14) -0.001(10) 0.008(10) -0.026(8) O12 0.088(9) 0.062(7) 0.087(9) -0.024(7) 0.038(8) -0.002(6) O13 0.117(13) 0.122(12) 0.065(8) -0.004(9) 0.024(9) -0.017(10) O14 0.044(6) 0.091(8) 0.082(8) -0.003(7) 0.018(6) -0.018(6) O15 0.072(9) 0.131(13) 0.084(10) -0.009(9) 0.006(8) 0.004(9) C1 0.106(17) 0.066(11) 0.112(17) 0.015(12) 0.052(15) 0.015(11) C2 0.17(3) 0.073(15) 0.19(3) -0.002(18) -0.04(3) 0.031(17) C3 0.15(3) 0.22(4) 0.14(3) -0.02(3) 0.09(2) 0.07(3) C4 0.10(3) 0.47(9) 0.25(5) 0.11(6) 0.10(3) 0.09(4) C5 0.11(3) 0.16(3) 0.23(5) -0.04(3) 0.08(3) -0.01(2) C6 0.43(10) 0.29(6) 0.32(8) -0.20(6) 0.21(8) -0.16(7) C7 0.20(4) 0.12(3) 0.20(4) 0.04(3) 0.01(3) 0.01(3) C8 0.29(7) 0.34(7) 0.16(4) 0.18(5) 0.04(4) 0.00(6) C9 0.110(19) 0.093(16) 0.12(2) 0.004(15) 0.029(16) -0.048(14) C10 0.21(4) 0.082(17) 0.14(3) 0.003(17) 0.05(2) -0.02(2) C11 0.09(2) 0.46(8) 0.17(4) -0.14(5) 0.03(2) 0.00(4) C12 0.17(5) 0.76(18) 0.34(9) 0.25(11) 0.15(6) 0.13(8) C13 0.11(3) 0.21(4) 0.38(7) -0.20(5) 0.06(4) -0.05(3) C14 0.19(5) 0.29(6) 0.33(7) -0.20(6) 0.02(5) 0.06(4) C15 0.14(3) 0.21(4) 0.15(3) -0.01(3) 0.05(3) -0.08(3) C16 0.25(6) 0.19(4) 0.18(4) 0.01(3) 0.01(4) -0.10(4) C17 0.40(9) 0.46(9) 0.44(9) 0.06(8) -0.09(7) 0.16(8) C18 0.47(13) 0.21(6) 0.25(6) 0.03(5) -0.15(7) -0.08(7) C19 0.29(7) 0.14(3) 0.21(5) 0.01(3) -0.09(5) -0.01(4) C20 0.23(6) 0.29(6) 0.44(9) 0.04(6) 0.04(6) -0.03(5) #----------------------------------------------------------------------------# # 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 Ta1 O5 1.842(12) . ? Ta1 O4 1.851(11) . ? Ta1 O3 1.891(13) . ? Ta1 O1 2.047(11) . ? Ta1 O12 2.154(13) . ? Ta1 O2 2.174(13) . ? Ta1 Ta2 3.3026(11) . ? Ta1 Ta3 3.3304(11) . ? Ta2 O6 1.838(14) . ? Ta2 O8 1.881(16) . ? Ta2 O7 1.891(14) . ? Ta2 O1 2.022(12) . ? Ta2 O2 2.074(12) . ? Ta2 O9 2.109(15) . ? Ta3 O10 1.845(14) . ? Ta3 O11 1.848(14) . ? Ta3 O14 1.848(13) 3_676 ? Ta3 O1 2.076(13) . ? Ta3 O12 2.108(12) . ? Ta3 O9 2.166(14) . ? Ta4 O15 1.857(16) . ? Ta4 O13 1.875(15) . ? Ta4 O3 1.974(13) 3_676 ? Ta4 O14 1.981(12) . ? Ta4 O6 1.997(13) . ? Ta4 O5 2.038(13) . ? O2 C1 1.52(3) . ? O3 Ta4 1.974(13) 3_676 ? O4 C3 1.400(16) . ? O7 C5 1.440(18) . ? O8 C7 1.429(18) . ? O9 C9 1.48(2) . ? O10 C11 1.414(18) . ? O11 C13 1.399(18) . ? O12 C15 1.63(4) . ? O13 C17 1.44(2) . ? O14 Ta3 1.848(13) 3_676 ? O15 C19 1.442(19) . ? C1 C2 1.544(17) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 C4 1.50(2) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 C6 1.51(2) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 C8 1.483(19) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 C10 1.488(18) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 C12 1.49(2) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C14 1.49(2) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 C16 1.482(19) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C17 C18 1.51(2) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C19 C20 1.48(2) . ? C19 H19A 0.97 . ? C19 H19B 0.97 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? 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 O5 Ta1 O4 102.0(6) . . ? O5 Ta1 O3 102.2(5) . . ? O4 Ta1 O3 102.7(6) . . ? O5 Ta1 O1 93.5(5) . . ? O4 Ta1 O1 155.7(5) . . ? O3 Ta1 O1 92.1(5) . . ? O5 Ta1 O12 162.7(5) . . ? O4 Ta1 O12 89.8(6) . . ? O3 Ta1 O12 87.3(5) . . ? O1 Ta1 O12 71.5(4) . . ? O5 Ta1 O2 87.5(5) . . ? O4 Ta1 O2 90.9(6) . . ? O3 Ta1 O2 161.1(5) . . ? O1 Ta1 O2 71.0(5) . . ? O12 Ta1 O2 79.6(5) . . ? O5 Ta1 Ta2 80.8(3) . . ? O4 Ta1 Ta2 128.8(5) . . ? O3 Ta1 Ta2 127.1(3) . . ? O1 Ta1 Ta2 35.5(4) . . ? O12 Ta1 Ta2 81.9(3) . . ? O2 Ta1 Ta2 37.9(3) . . ? O5 Ta1 Ta3 129.2(3) . . ? O4 Ta1 Ta3 127.9(5) . . ? O3 Ta1 Ta3 78.3(4) . . ? O1 Ta1 Ta3 36.4(3) . . ? O12 Ta1 Ta3 38.1(3) . . ? O2 Ta1 Ta3 83.1(4) . . ? Ta2 Ta1 Ta3 61.74(3) . . ? O6 Ta2 O8 102.3(7) . . ? O6 Ta2 O7 93.0(6) . . ? O8 Ta2 O7 99.4(7) . . ? O6 Ta2 O1 94.0(5) . . ? O8 Ta2 O1 156.2(6) . . ? O7 Ta2 O1 96.9(6) . . ? O6 Ta2 O2 87.3(5) . . ? O8 Ta2 O2 89.8(6) . . ? O7 Ta2 O2 170.5(7) . . ? O1 Ta2 O2 73.6(5) . . ? O6 Ta2 O9 165.3(5) . . ? O8 Ta2 O9 91.0(7) . . ? O7 Ta2 O9 91.1(6) . . ? O1 Ta2 O9 71.5(5) . . ? O2 Ta2 O9 86.4(5) . . ? O6 Ta2 Ta1 80.6(4) . . ? O8 Ta2 Ta1 129.9(5) . . ? O7 Ta2 Ta1 130.6(5) . . ? O1 Ta2 Ta1 36.0(3) . . ? O2 Ta2 Ta1 40.1(4) . . ? O9 Ta2 Ta1 86.0(3) . . ? O10 Ta3 O11 98.0(7) . . ? O10 Ta3 O14 95.9(7) . 3_676 ? O11 Ta3 O14 103.0(7) . 3_676 ? O10 Ta3 O1 99.2(6) . . ? O11 Ta3 O1 155.1(6) . . ? O14 Ta3 O1 93.1(5) 3_676 . ? O10 Ta3 O12 169.7(7) . . ? O11 Ta3 O12 89.1(6) . . ? O14 Ta3 O12 89.8(5) 3_676 . ? O1 Ta3 O12 71.8(5) . . ? O10 Ta3 O9 88.2(7) . . ? O11 Ta3 O9 93.4(6) . . ? O14 Ta3 O9 162.4(5) 3_676 . ? O1 Ta3 O9 69.4(5) . . ? O12 Ta3 O9 83.9(6) . . ? O10 Ta3 Ta1 133.6(5) . . ? O11 Ta3 Ta1 128.1(5) . . ? O14 Ta3 Ta1 80.4(3) 3_676 . ? O1 Ta3 Ta1 35.8(3) . . ? O12 Ta3 Ta1 39.1(4) . . ? O9 Ta3 Ta1 84.4(4) . . ? O15 Ta4 O13 93.7(8) . . ? O15 Ta4 O3 169.7(6) . 3_676 ? O13 Ta4 O3 92.8(6) . 3_676 ? O15 Ta4 O14 87.8(7) . . ? O13 Ta4 O14 94.2(6) . . ? O3 Ta4 O14 83.7(5) 3_676 . ? O15 Ta4 O6 96.2(7) . . ? O13 Ta4 O6 91.7(6) . . ? O3 Ta4 O6 91.6(5) 3_676 . ? O14 Ta4 O6 172.6(5) . . ? O15 Ta4 O5 89.6(6) . . ? O13 Ta4 O5 175.2(6) . . ? O3 Ta4 O5 84.5(5) 3_676 . ? O14 Ta4 O5 89.5(5) . . ? O6 Ta4 O5 84.4(5) . . ? Ta2 O1 Ta1 108.5(6) . . ? Ta2 O1 Ta3 112.3(5) . . ? Ta1 O1 Ta3 107.7(5) . . ? C1 O2 Ta2 122.1(12) . . ? C1 O2 Ta1 121.6(11) . . ? Ta2 O2 Ta1 102.0(5) . . ? Ta1 O3 Ta4 146.5(6) . 3_676 ? C3 O4 Ta1 166(2) . . ? Ta1 O5 Ta4 143.4(5) . . ? Ta2 O6 Ta4 144.6(8) . . ? C5 O7 Ta2 136.5(16) . . ? C7 O8 Ta2 175(2) . . ? C9 O9 Ta2 128.8(14) . . ? C9 O9 Ta3 123.7(15) . . ? Ta2 O9 Ta3 105.5(5) . . ? C11 O10 Ta3 175(2) . . ? C13 O11 Ta3 168(2) . . ? C15 O12 Ta3 131.7(14) . . ? C15 O12 Ta1 125.5(14) . . ? Ta3 O12 Ta1 102.8(5) . . ? C17 O13 Ta4 133(3) . . ? Ta3 O14 Ta4 145.9(7) 3_676 . ? C19 O15 Ta4 134(2) . . ? O2 C1 C2 104(2) . . ? O2 C1 H1A 110.9 . . ? C2 C1 H1A 110.9 . . ? O2 C1 H1B 110.9 . . ? C2 C1 H1B 110.9 . . ? H1A C1 H1B 108.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C3 C4 112(2) . . ? O4 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O4 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O7 C5 C6 101(3) . . ? O7 C5 H5A 111.6 . . ? C6 C5 H5A 111.6 . . ? O7 C5 H5B 111.5 . . ? C6 C5 H5B 111.5 . . ? H5A C5 H5B 109.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O8 C7 C8 108(2) . . ? O8 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O8 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O9 C9 C10 108.1(18) . . ? O9 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? O9 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O10 C11 C12 117(3) . . ? O10 C11 H11A 108 . . ? C12 C11 H11A 108 . . ? O10 C11 H11B 108 . . ? C12 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.4 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O11 C13 C14 118(3) . . ? O11 C13 H13A 107.7 . . ? C14 C13 H13A 107.7 . . ? O11 C13 H13B 107.8 . . ? C14 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.4 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 O12 95(3) . . ? C16 C15 H15A 112.7 . . ? O12 C15 H15A 112.7 . . ? C16 C15 H15B 112.7 . . ? O12 C15 H15B 112.7 . . ? H15A C15 H15B 110.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O13 C17 C18 93(4) . . ? O13 C17 H17A 113 . . ? C18 C17 H17A 112.8 . . ? O13 C17 H17B 113.4 . . ? C18 C17 H17B 113.6 . . ? H17A C17 H17B 110.5 . . ? C17 C18 H18A 109.4 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.1 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O15 C19 C20 106(3) . . ? O15 C19 H19A 110.5 . . ? C20 C19 H19A 110.5 . . ? O15 C19 H19B 110.5 . . ? C20 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? #===END #--Structure 3 data_haltan _audit_creation_date 2000-02-29T20:23:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C51 H119 O26 Ta7' _chemical_formula_structural 'C51 H119 O26 TA7' _chemical_formula_sum 'C51 H119 O26 Ta7' _chemical_formula_weight 2415.11 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.847(9) _cell_length_b 13.626(5) _cell_length_c 27.917(9) _cell_angle_alpha 90 _cell_angle_beta 98.56(6) _cell_angle_gamma 90 _cell_volume 8218(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.94 _cell_measurement_theta_max 13.91 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.341 _exptl_absorpt_factor_muR 1.868 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.0479 _exptl_absorpt_correction_T_max 0.1544 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.9484E-2 _diffrn_orient_matrix_ub_12 -0.70712E-1 _diffrn_orient_matrix_ub_13 -0.7195E-2 _diffrn_orient_matrix_ub_21 0.9317E-2 _diffrn_orient_matrix_ub_22 -0.15498E-1 _diffrn_orient_matrix_ub_23 0.35374E-1 _diffrn_orient_matrix_ub_31 -0.44339E-1 _diffrn_orient_matrix_ub_32 0.11878E-1 _diffrn_orient_matrix_ub_33 0.00331 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 29 _diffrn_standards_decay_corr_max 1.518 _diffrn_standards_decay_corr_min 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -14 0 2 -13 1 3 _diffrn_reflns_number 7433 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7228 _reflns_number_gt 4128 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4/PC (Enraf Nonius, 1992)' _computing_cell_refinement 'CAD4/PC (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7228 _refine_ls_number_parameters 382 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1425 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.005 _refine_diff_density_max 1.875 _refine_diff_density_min -1.359 _refine_diff_density_rms 0.22 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ta1 Ta 0 0.82503(7) 0.25 0.0493(3) Uani 1 2 d S . . Ta2 Ta 0.00447(4) 0.57537(5) 0.30626(3) 0.0535(2) Uani 1 1 d . . . Ta3 Ta 0.06103(4) 0.79306(6) 0.15725(3) 0.0577(2) Uani 1 1 d . . . Ta4 Ta 0.09612(4) 0.76353(6) 0.37440(3) 0.0629(3) Uani 1 1 d . . . O1 O 0 0.6778(10) 0.25 0.037(3) Uani 1 2 d S . . O2 O -0.0263(5) 0.8131(7) 0.1802(4) 0.043(3) Uani 1 1 d . . . O3 O -0.0074(5) 0.7621(9) 0.0989(4) 0.061(3) Uani 1 1 d . . . O4 O 0.0794(5) 0.8198(9) 0.2245(4) 0.063(3) Uani 1 1 d . . . O5 O 0 0.9630(11) 0.25 0.051(4) Uani 1 2 d S . . O6 O -0.0561(5) 0.6471(8) 0.3313(4) 0.055(3) Uani 1 1 d . . . O7 O 0.0567(5) 0.5158(8) 0.2539(4) 0.057(3) Uani 1 1 d . . . O8 O 0.0718(5) 0.6323(9) 0.3438(4) 0.058(3) Uani 1 1 d . . . O9 O 0.1592(6) 0.7793(9) 0.3382(5) 0.076(4) Uani 1 1 d . . . O10 O 0.1366(6) 0.7630(10) 0.1357(5) 0.083(4) Uani 1 1 d . . . O11 O 0.0673(6) 0.9238(9) 0.1356(5) 0.074(4) Uani 1 1 d . . . O12 O 0.0004(6) 0.4577(9) 0.3398(5) 0.073(4) Uani 1 1 d . . . O13 O 0.1344(6) 0.6931(11) 0.4283(5) 0.085(4) Uani 1 1 d . . . O14 O 0.1085(6) 0.8895(9) 0.4038(5) 0.079(4) Uani 1 1 d . . . C1 C -0.0004(11) 0.7355(15) 0.0499(7) 0.085(7) Uani 1 1 d D . . H1 H -0.0422 0.7378 0.0313 0.102 Uiso 1 1 calc R . . C2 C 0.0188(12) 0.6347(16) 0.0491(10) 0.122(10) Uani 1 1 d D . . H2A H 0.0061 0.6079 0.0174 0.183 Uiso 1 1 calc R . . H2B H 0.0003 0.5979 0.0725 0.183 Uiso 1 1 calc R . . H2C H 0.0631 0.631 0.0568 0.183 Uiso 1 1 calc R . . C3 C 0.0354(13) 0.8032(18) 0.0272(9) 0.132(11) Uani 1 1 d D . . H3A H 0.0181 0.8678 0.0284 0.198 Uiso 1 1 calc R . . H3B H 0.0352 0.7844 -0.006 0.198 Uiso 1 1 calc R . . H3C H 0.0772 0.8034 0.0438 0.198 Uiso 1 1 calc R . . C4 C 0.1856(12) 0.695(2) 0.1383(9) 0.104(8) Uani 1 1 d D . . H4 H 0.1701 0.631 0.1476 0.125 Uiso 1 1 calc R . . C5 C 0.2019(17) 0.685(4) 0.0912(11) 0.34(4) Uani 1 1 d D . . H5A H 0.2281 0.6287 0.0902 0.516 Uiso 1 1 calc R . . H5B H 0.2235 0.7428 0.0834 0.516 Uiso 1 1 calc R . . H5C H 0.165 0.6769 0.0681 0.516 Uiso 1 1 calc R . . C6 C 0.2365(14) 0.722(4) 0.1737(14) 0.27(3) Uani 1 1 d D . . H6A H 0.2655 0.6683 0.1784 0.4 Uiso 1 1 calc R . . H6B H 0.2219 0.7361 0.2037 0.4 Uiso 1 1 calc R . . H6C H 0.2564 0.7785 0.1628 0.4 Uiso 1 1 calc R . . C7 C 0.1171(10) 0.4809(16) 0.2543(11) 0.132(11) Uani 1 1 d D . . H7 H 0.1213 0.4681 0.2204 0.159 Uiso 1 1 calc R . . C8 C 0.1625(11) 0.553(2) 0.2709(13) 0.185(19) Uani 1 1 d D . . H8A H 0.1445 0.6169 0.2668 0.277 Uiso 1 1 calc R . . H8B H 0.1963 0.5478 0.2526 0.277 Uiso 1 1 calc R . . H8C H 0.1775 0.5418 0.3046 0.277 Uiso 1 1 calc R . . C9 C 0.1294(18) 0.390(2) 0.2790(16) 0.28(3) Uani 1 1 d D . . H9A H 0.1731 0.3777 0.2837 0.417 Uiso 1 1 calc R . . H9B H 0.1082 0.3382 0.26 0.417 Uiso 1 1 calc R . . H9C H 0.1152 0.3933 0.3099 0.417 Uiso 1 1 calc R . . C10 C -0.0048(16) 0.3683(17) 0.3614(12) 0.20(2) Uani 1 1 d D . . H10 H -0.0142 0.3213 0.3348 0.237 Uiso 1 1 calc R . . C11 C -0.0587(16) 0.372(3) 0.3845(16) 0.21(2) Uani 1 1 d D . . H11A H -0.062 0.4351 0.3987 0.317 Uiso 1 1 calc R . . H11B H -0.0557 0.3223 0.4093 0.317 Uiso 1 1 calc R . . H11C H -0.0947 0.3594 0.361 0.317 Uiso 1 1 calc R . . C12 C 0.051(2) 0.334(3) 0.3896(16) 0.30(3) Uani 1 1 d D . . H12A H 0.0858 0.3619 0.3774 0.443 Uiso 1 1 calc R . . H12B H 0.0526 0.2637 0.3876 0.443 Uiso 1 1 calc R . . H12C H 0.0517 0.3532 0.4228 0.443 Uiso 1 1 calc R . . C13 C 0.1542(14) 0.603(3) 0.4460(11) 0.147(12) Uani 1 1 d D . . H13 H 0.1211 0.5585 0.4323 0.177 Uiso 1 1 calc R . . C14 C 0.1585(17) 0.590(3) 0.4969(11) 0.25(3) Uani 1 1 d D . . H14A H 0.1814 0.6431 0.5134 0.372 Uiso 1 1 calc R . . H14B H 0.1794 0.529 0.5059 0.372 Uiso 1 1 calc R . . H14C H 0.1177 0.5878 0.5057 0.372 Uiso 1 1 calc R . . C15 C 0.2072(17) 0.568(3) 0.4274(13) 0.24(3) Uani 1 1 d D . . H15A H 0.1972 0.5589 0.3931 0.366 Uiso 1 1 calc R . . H15B H 0.2199 0.5067 0.4426 0.366 Uiso 1 1 calc R . . H15C H 0.2402 0.615 0.4342 0.366 Uiso 1 1 calc R . . C16 C 0 1.062(3) 0.25 0.28(5) Uani 1 2 d SD . . H16 H -0.0103 1.0621 0.283 0.331 Uiso 0.5 1 calc PR . . C17 C 0.0558(17) 1.111(3) 0.2666(19) 0.37(4) Uani 1 1 d D . . H17A H 0.0482 1.1806 0.2678 0.553 Uiso 1 1 calc R . . H17B H 0.0851 1.0987 0.2449 0.553 Uiso 1 1 calc R . . H17C H 0.0722 1.0882 0.2984 0.553 Uiso 1 1 calc R . . C18 C 0.1111(14) 0.992(2) 0.1256(13) 0.185(19) Uani 1 1 d D . . H18 H 0.1317 0.9569 0.1018 0.223 Uiso 1 1 calc R . . C19 C 0.0839(17) 1.073(2) 0.0980(14) 0.21(2) Uani 1 1 d D . . H19A H 0.0515 1.1003 0.1136 0.318 Uiso 1 1 calc R . . H19B H 0.067 1.0509 0.0661 0.318 Uiso 1 1 calc R . . H19C H 0.1149 1.1219 0.0957 0.318 Uiso 1 1 calc R . . C20 C 0.1611(18) 1.011(3) 0.1629(13) 0.22(2) Uani 1 1 d D . . H20A H 0.1462 1.0131 0.1936 0.331 Uiso 1 1 calc R . . H20B H 0.1794 1.0734 0.1571 0.331 Uiso 1 1 calc R . . H20C H 0.1916 0.9604 0.1634 0.331 Uiso 1 1 calc R . . C21 C 0.1016(15) 0.971(2) 0.4314(12) 0.155(13) Uani 1 1 d D . . H21 H 0.0615 0.9683 0.443 0.186 Uiso 1 1 calc R . . C22 C 0.150(2) 0.969(3) 0.4715(15) 0.31(4) Uani 1 1 d D . . H22A H 0.1402 0.9201 0.4942 0.464 Uiso 1 1 calc R . . H22B H 0.1533 1.0318 0.4869 0.464 Uiso 1 1 calc R . . H22C H 0.1881 0.9523 0.4606 0.464 Uiso 1 1 calc R . . C23 C 0.102(2) 1.053(2) 0.3996(17) 0.28(3) Uani 1 1 d D . . H23A H 0.1407 1.0868 0.4069 0.416 Uiso 1 1 calc R . . H23B H 0.0687 1.0962 0.4037 0.416 Uiso 1 1 calc R . . H23C H 0.0969 1.0297 0.3667 0.416 Uiso 1 1 calc R . . C24 C 0.2116(13) 0.814(2) 0.3185(16) 0.20(2) Uani 1 1 d D . . H24 H 0.2139 0.7758 0.2892 0.239 Uiso 1 1 calc R . . C25 C 0.2033(17) 0.913(2) 0.3037(18) 0.24(2) Uani 1 1 d D . . H25A H 0.2344 0.953 0.3223 0.361 Uiso 1 1 calc R . . H25B H 0.163 0.9348 0.3087 0.361 Uiso 1 1 calc R . . H25C H 0.207 0.9182 0.2699 0.361 Uiso 1 1 calc R . . C26 C 0.2659(13) 0.792(4) 0.351(2) 0.41(5) Uani 1 1 d D . . H26A H 0.2635 0.823 0.3821 0.61 Uiso 1 1 calc R . . H26B H 0.3015 0.8166 0.3388 0.61 Uiso 1 1 calc R . . H26C H 0.2694 0.7225 0.3558 0.61 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0598(6) 0.0376(6) 0.0518(7) 0 0.0122(5) 0 Ta2 0.0650(5) 0.0420(4) 0.0542(5) 0.0069(4) 0.0115(4) 0.0022(4) Ta3 0.0588(5) 0.0589(5) 0.0587(5) 0.0000(4) 0.0196(4) -0.0074(4) Ta4 0.0610(5) 0.0730(6) 0.0530(5) -0.0062(4) 0.0026(4) -0.0014(4) O1 0.034(8) 0.054(9) 0.023(8) 0 0.002(6) 0 O2 0.050(6) 0.037(6) 0.046(7) 0.014(5) 0.023(5) 0.004(5) O3 0.068(8) 0.070(8) 0.047(7) -0.001(6) 0.015(6) -0.013(6) O4 0.046(7) 0.077(9) 0.068(9) -0.003(7) 0.014(6) 0.000(6) O5 0.063(10) 0.048(9) 0.039(10) 0 0.002(8) 0 O6 0.046(6) 0.069(8) 0.049(7) 0.005(6) 0.009(5) -0.011(6) O7 0.059(7) 0.047(7) 0.068(8) 0.004(6) 0.015(6) 0.016(6) O8 0.066(7) 0.068(8) 0.040(7) 0.007(6) 0.007(6) 0.005(6) O9 0.073(9) 0.073(9) 0.078(10) -0.004(7) 0.004(7) -0.008(7) O10 0.085(10) 0.084(10) 0.093(11) -0.006(8) 0.052(9) -0.011(8) O11 0.091(9) 0.060(8) 0.073(9) 0.020(7) 0.014(8) -0.022(7) O12 0.095(10) 0.051(8) 0.068(9) 0.011(7) 0.001(7) 0.001(7) O13 0.079(9) 0.099(11) 0.073(10) 0.008(9) 0.000(8) 0.014(8) O14 0.068(8) 0.061(9) 0.112(12) -0.029(8) 0.022(8) -0.025(7) C1 0.116(19) 0.089(17) 0.052(13) -0.005(12) 0.018(12) -0.015(15) C2 0.13(2) 0.12(2) 0.13(2) -0.049(19) 0.062(19) -0.040(18) C3 0.19(3) 0.12(2) 0.09(2) 0.007(18) 0.05(2) 0.01(2) C4 0.10(2) 0.12(2) 0.10(2) -0.019(17) 0.039(17) -0.002(17) C5 0.15(4) 0.64(12) 0.23(5) -0.17(6) -0.01(3) 0.18(5) C6 0.10(3) 0.44(8) 0.24(5) -0.14(5) -0.03(3) 0.06(4) C7 0.055(15) 0.14(3) 0.21(3) 0.00(2) 0.027(18) 0.025(16) C8 0.066(18) 0.22(4) 0.27(5) -0.14(3) 0.02(2) 0.00(2) C9 0.31(5) 0.19(4) 0.40(7) 0.21(4) 0.24(5) 0.21(4) C10 0.39(7) 0.030(14) 0.21(4) 0.024(18) 0.16(4) -0.04(3) C11 0.19(4) 0.16(4) 0.29(6) 0.03(4) 0.05(4) -0.07(3) C12 0.34(7) 0.28(6) 0.26(6) 0.21(5) 0.05(5) 0.17(5) C13 0.13(3) 0.16(3) 0.15(3) 0.05(3) 0.00(2) 0.04(2) C14 0.18(4) 0.39(7) 0.16(4) 0.18(4) -0.01(3) 0.00(4) C15 0.22(4) 0.37(7) 0.15(4) 0.05(4) 0.03(3) 0.19(5) C16 0.19(6) 0.03(2) 0.61(15) 0 0.05(7) 0 C17 0.58(11) 0.19(4) 0.32(8) -0.04(5) -0.01(7) -0.28(6) C18 0.16(3) 0.12(3) 0.26(5) 0.11(3) -0.04(3) -0.09(2) C19 0.27(5) 0.13(3) 0.23(5) 0.09(3) 0.01(4) -0.05(3) C20 0.21(4) 0.16(4) 0.28(6) 0.01(3) -0.01(4) -0.13(3) C21 0.16(3) 0.11(3) 0.19(4) -0.06(3) 0.02(3) -0.01(2) C22 0.28(6) 0.33(7) 0.25(6) -0.21(5) -0.15(5) 0.04(5) C23 0.36(7) 0.06(2) 0.45(9) 0.02(3) 0.16(6) -0.03(3) C24 0.08(2) 0.10(2) 0.42(7) 0.08(3) 0.06(3) 0.003(18) C25 0.16(4) 0.15(4) 0.41(8) 0.03(4) 0.04(4) -0.04(3) C26 0.037(19) 0.35(7) 0.83(15) 0.17(8) 0.04(4) -0.05(3) #----------------------------------------------------------------------------# # 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 Ta1 O5 1.880(15) . ? Ta1 O2 1.955(10) 2 ? Ta1 O2 1.955(10) . ? Ta1 O4 1.972(11) 2 ? Ta1 O4 1.972(11) . ? Ta1 O1 2.007(14) . ? Ta1 Ta3 3.1144(16) . ? Ta1 Ta3 3.1144(16) 2 ? Ta2 O8 1.845(12) . ? Ta2 O6 1.863(11) . ? Ta2 O12 1.866(12) . ? Ta2 O1 2.092(9) . ? Ta2 O7 2.143(11) . ? Ta2 O7 2.145(12) 2 ? Ta2 Ta2 3.1182(19) 2 ? Ta3 O10 1.886(13) . ? Ta3 O11 1.892(11) . ? Ta3 O4 1.897(12) . ? Ta3 O6 2.020(11) 2 ? Ta3 O3 2.083(12) . ? Ta3 O2 2.118(9) . ? Ta4 O9 1.838(13) . ? Ta4 O13 1.874(15) . ? Ta4 O14 1.905(12) . ? Ta4 O8 2.019(12) . ? Ta4 O2 2.100(11) 2 ? Ta4 O3 2.179(11) 2 ? O1 Ta2 2.092(9) 2 ? O2 Ta4 2.100(11) 2 ? O3 C1 1.44(2) . ? O3 Ta4 2.179(11) 2 ? O5 C16 1.35(4) . ? O6 Ta3 2.020(11) 2 ? O7 C7 1.40(2) . ? O7 Ta2 2.145(12) 2 ? O9 C24 1.43(3) . ? O10 C4 1.41(3) . ? O11 C18 1.39(3) . ? O12 C10 1.37(2) . ? O13 C13 1.37(3) . ? O14 C21 1.38(3) . ? C1 C3 1.420(12) . ? C1 C2 1.438(12) . ? C1 H1 0.98 . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 C5 1.418(13) . ? C4 C6 1.421(13) . ? C4 H4 0.98 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 C9 1.421(13) . ? C7 C8 1.421(13) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 C11 1.423(13) . ? C10 C12 1.426(13) . ? C10 H10 0.98 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C15 1.419(13) . ? C13 C14 1.422(13) . ? C13 H13 0.98 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 C17 1.409(13) . ? C16 C17 1.409(13) 2 ? C16 H16 0.98 . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C17 H17C 0.96 . ? C18 C20 1.418(13) . ? C18 C19 1.422(13) . ? C18 H18 0.98 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 C22 1.417(13) . ? C21 C23 1.419(13) . ? C21 H21 0.98 . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 C25 1.410(13) . ? C24 C26 1.421(13) . ? C24 H24 0.98 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? 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 O5 Ta1 O2 94.8(3) . 2 ? O5 Ta1 O2 94.8(3) . . ? O2 Ta1 O2 170.4(5) 2 . ? O5 Ta1 O4 92.1(3) . 2 ? O2 Ta1 O4 77.3(5) 2 2 ? O2 Ta1 O4 102.3(5) . 2 ? O5 Ta1 O4 92.1(3) . . ? O2 Ta1 O4 102.3(5) 2 . ? O2 Ta1 O4 77.3(5) . . ? O4 Ta1 O4 175.9(7) 2 . ? O5 Ta1 O1 180.000(4) . . ? O2 Ta1 O1 85.2(3) 2 . ? O2 Ta1 O1 85.2(3) . . ? O4 Ta1 O1 87.9(3) 2 . ? O4 Ta1 O1 87.9(3) . . ? O5 Ta1 Ta3 98.04(2) . . ? O2 Ta1 Ta3 135.9(3) 2 . ? O2 Ta1 Ta3 42.1(3) . . ? O4 Ta1 Ta3 143.5(4) 2 . ? O4 Ta1 Ta3 35.6(4) . . ? O1 Ta1 Ta3 81.96(2) . . ? O5 Ta1 Ta3 98.04(2) . 2 ? O2 Ta1 Ta3 42.1(3) 2 2 ? O2 Ta1 Ta3 135.9(3) . 2 ? O4 Ta1 Ta3 35.6(4) 2 2 ? O4 Ta1 Ta3 143.5(4) . 2 ? O1 Ta1 Ta3 81.96(2) . 2 ? Ta3 Ta1 Ta3 163.92(5) . 2 ? O8 Ta2 O6 96.7(5) . . ? O8 Ta2 O12 99.7(5) . . ? O6 Ta2 O12 100.0(5) . . ? O8 Ta2 O1 95.2(4) . . ? O6 Ta2 O1 88.6(4) . . ? O12 Ta2 O1 161.7(5) . . ? O8 Ta2 O7 95.0(5) . . ? O6 Ta2 O7 159.2(5) . . ? O12 Ta2 O7 94.9(5) . . ? O1 Ta2 O7 73.2(4) . . ? O8 Ta2 O7 162.8(4) . 2 ? O6 Ta2 O7 95.6(4) . 2 ? O12 Ta2 O7 89.8(5) . 2 ? O1 Ta2 O7 73.2(4) . 2 ? O7 Ta2 O7 69.8(5) . 2 ? O8 Ta2 Ta2 119.8(3) . 2 ? O6 Ta2 Ta2 115.9(3) . 2 ? O12 Ta2 Ta2 120.3(4) . 2 ? O1 Ta2 Ta2 41.8(3) . 2 ? O7 Ta2 Ta2 43.4(3) . 2 ? O7 Ta2 Ta2 43.3(3) 2 2 ? O10 Ta3 O11 89.7(6) . . ? O10 Ta3 O4 107.0(6) . . ? O11 Ta3 O4 96.9(5) . . ? O10 Ta3 O6 84.6(5) . 2 ? O11 Ta3 O6 170.2(5) . 2 ? O4 Ta3 O6 92.4(5) . 2 ? O10 Ta3 O3 105.5(5) . . ? O11 Ta3 O3 91.1(5) . . ? O4 Ta3 O3 146.6(4) . . ? O6 Ta3 O3 82.9(5) 2 . ? O10 Ta3 O2 174.7(5) . . ? O11 Ta3 O2 95.0(5) . . ? O4 Ta3 O2 75.1(4) . . ? O6 Ta3 O2 90.4(4) 2 . ? O3 Ta3 O2 71.9(4) . . ? O10 Ta3 Ta1 143.1(5) . . ? O11 Ta3 Ta1 101.2(4) . . ? O4 Ta3 Ta1 37.2(3) . . ? O6 Ta3 Ta1 88.1(3) 2 . ? O3 Ta3 Ta1 109.4(3) . . ? O2 Ta3 Ta1 38.2(3) . . ? O9 Ta4 O13 102.7(6) . . ? O9 Ta4 O14 93.5(5) . . ? O13 Ta4 O14 95.6(7) . . ? O9 Ta4 O8 92.5(5) . . ? O13 Ta4 O8 86.8(6) . . ? O14 Ta4 O8 172.9(5) . . ? O9 Ta4 O2 95.0(5) . 2 ? O13 Ta4 O2 159.5(5) . 2 ? O14 Ta4 O2 93.7(5) . 2 ? O8 Ta4 O2 82.0(4) . 2 ? O9 Ta4 O3 165.3(5) . 2 ? O13 Ta4 O3 92.0(5) . 2 ? O14 Ta4 O3 86.4(5) . 2 ? O8 Ta4 O3 86.9(4) . 2 ? O2 Ta4 O3 70.3(4) 2 2 ? Ta1 O1 Ta2 131.8(3) . 2 ? Ta1 O1 Ta2 131.8(3) . . ? Ta2 O1 Ta2 96.4(6) 2 . ? Ta1 O2 Ta4 145.5(5) . 2 ? Ta1 O2 Ta3 99.7(4) . . ? Ta4 O2 Ta3 109.2(4) 2 . ? C1 O3 Ta3 128.8(12) . . ? C1 O3 Ta4 123.4(12) . 2 ? Ta3 O3 Ta4 107.6(5) . 2 ? Ta3 O4 Ta1 107.2(5) . . ? C16 O5 Ta1 180.000(9) . . ? Ta2 O6 Ta3 129.3(5) . 2 ? C7 O7 Ta2 136.0(15) . . ? C7 O7 Ta2 127.7(14) . 2 ? Ta2 O7 Ta2 93.3(4) . 2 ? Ta2 O8 Ta4 138.6(6) . . ? C24 O9 Ta4 164(2) . . ? C4 O10 Ta3 145.1(14) . . ? C18 O11 Ta3 141.0(16) . . ? C10 O12 Ta2 175.9(18) . . ? C13 O13 Ta4 145.9(18) . . ? C21 O14 Ta4 162.0(17) . . ? C3 C1 C2 116(2) . . ? C3 C1 O3 113.7(18) . . ? C2 C1 O3 109.2(17) . . ? C3 C1 H1 105.9 . . ? C2 C1 H1 105.9 . . ? O3 C1 H1 105.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O10 C4 C5 108(2) . . ? O10 C4 C6 112(3) . . ? C5 C4 C6 113(3) . . ? O10 C4 H4 108 . . ? C5 C4 H4 108 . . ? C6 C4 H4 108 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O7 C7 C9 114(2) . . ? O7 C7 C8 112(2) . . ? C9 C7 C8 112(3) . . ? O7 C7 H7 106 . . ? C9 C7 H7 106 . . ? C8 C7 H7 106 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O12 C10 C11 108(3) . . ? O12 C10 C12 114(3) . . ? C11 C10 C12 117(4) . . ? O12 C10 H10 105.6 . . ? C11 C10 H10 105.6 . . ? C12 C10 H10 105.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.4 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O13 C13 C15 114(3) . . ? O13 C13 C14 117(3) . . ? C15 C13 C14 113(3) . . ? O13 C13 H13 104 . . ? C15 C13 H13 104 . . ? C14 C13 H13 104 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.4 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 C17 118(3) . . ? O5 C16 C17 118(3) . 2 ? C17 C16 C17 123(5) . 2 ? O5 C16 H16 90 . . ? C17 C16 H16 90 . . ? C17 C16 H16 90 2 . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.4 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O11 C18 C20 117(2) . . ? O11 C18 C19 112(2) . . ? C20 C18 C19 118(3) . . ? O11 C18 H18 102 . . ? C20 C18 H18 102 . . ? C19 C18 H18 102 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O14 C21 C22 107(3) . . ? O14 C21 C23 106(3) . . ? C22 C21 C23 116(4) . . ? O14 C21 H21 109.2 . . ? C22 C21 H21 109.2 . . ? C23 C21 H21 109.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.4 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 117(4) . . ? C25 C24 O9 111(3) . . ? C26 C24 O9 109(3) . . ? C25 C24 H24 106.6 . . ? C26 C24 H24 106.7 . . ? O9 C24 H24 106.7 . . ? C24 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.6 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? #===END #--Structure 4 data_h-tan2j _audit_creation_date 2000-02-27T16:38:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H99 O18 Ta5 . C7 H8' _chemical_formula_structural 'C44 H99 O18 TA5 . C7 H8' _chemical_formula_sum 'C51 H107 O18 Ta5' _chemical_formula_weight 1913.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.421(3) _cell_length_b 12.854(2) _cell_length_c 22.921(4) _cell_angle_alpha 78.78(9) _cell_angle_beta 79.79(2) _cell_angle_gamma 80.63(3) _cell_volume 3501.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.48 _cell_measurement_theta_max 14.42 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_special_details ; Due to decomposition, intensity data were collected sequentially on three similar sized crystals. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.839 _exptl_absorpt_factor_muR 1.176 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166 ; _exptl_absorpt_correction_T_min 0.085 _exptl_absorpt_correction_T_max 0.3086 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 13 _diffrn_standards_decay_corr_max 1.215 _diffrn_standards_decay_corr_min 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 8 4 -2 -5 8 _diffrn_reflns_number 12901 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 12284 _reflns_number_gt 7245 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4/PC (Enraf Nonius, 1992)' _computing_cell_refinement 'CAD4/PC (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Initial refinement was carried out using unmerged data with individual batch scale factors. Rescaling and merging of equivalent reflections was carried out after absorption correction using DIFABS (Walker & Stuart, 1983). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1636P)^2^+0.1697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 12284 _refine_ls_number_parameters 657 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.1546 _refine_ls_R_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.2645 _refine_ls_wR_factor_gt 0.2345 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 4.332 _refine_diff_density_min -3.108 _refine_diff_density_rms 0.362 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ta1 Ta 0.23313(8) 0.20695(7) 0.13937(4) 0.0379(3) Uani 1 1 d . . . Ta2 Ta 0.12615(9) 0.29733(7) 0.29104(5) 0.0470(3) Uani 1 1 d . . . Ta3 Ta 0.25364(8) 0.02487(7) 0.25444(4) 0.0436(3) Uani 1 1 d . . . Ta4 Ta 0.04405(8) 0.39299(7) 0.17423(5) 0.0473(3) Uani 1 1 d . . . Ta5 Ta 0.00410(8) 0.10559(8) 0.25864(5) 0.0469(3) Uani 1 1 d . . . O1 O 0.1887(12) 0.3032(11) 0.2024(6) 0.041(4) Uani 1 1 d . . . O2 O 0.1438(12) 0.0961(11) 0.1952(8) 0.047(4) Uani 1 1 d . . . O3 O 0.3286(13) 0.1203(12) 0.1996(8) 0.051(4) Uani 1 1 d . . . O4 O 0.0976(13) 0.2942(11) 0.1192(7) 0.042(4) Uani 1 1 d . . . O5 O 0.1355(14) 0.1417(11) 0.2986(6) 0.048(4) Uani 1 1 d . . . O6 O 0.2481(14) 0.1237(11) 0.0794(7) 0.048(4) Uani 1 1 d . . . O7 O -0.0890(14) 0.0893(14) 0.3293(8) 0.057(4) Uani 1 1 d . . . O8 O 0.0481(16) 0.3119(13) 0.3684(9) 0.066(5) Uani 1 1 d . . . O9 O 0.3437(13) 0.2874(11) 0.0978(7) 0.047(4) Uani 1 1 d . . . O10 O 0.1037(14) -0.0452(12) 0.2867(8) 0.054(4) Uani 1 1 d . . . O11 O 0.1026(12) 0.5116(13) 0.1297(10) 0.065(5) Uani 1 1 d . . . O12 O 0.2626(16) 0.3317(15) 0.3041(9) 0.067(5) Uani 1 1 d . . . O13 O 0.3229(13) 0.0032(12) 0.3220(8) 0.055(4) Uani 1 1 d . . . O14 O 0.0479(13) 0.4271(14) 0.2550(8) 0.064(5) Uani 1 1 d . . . O15 O 0.3228(14) -0.0990(11) 0.2222(8) 0.052(4) Uani 1 1 d . . . O16 O -0.1056(14) 0.4391(14) 0.1667(9) 0.068(5) Uani 1 1 d U . . O17 O -0.0116(16) 0.2583(14) 0.2399(9) 0.080(7) Uani 1 1 d . . . O18 O -0.0811(15) 0.0708(15) 0.2096(9) 0.066(5) Uani 1 1 d . . . C1 C 0.216(2) 0.0678(17) 0.0393(12) 0.059(8) Uani 1 1 d D . . C2 C 0.151(4) -0.021(3) 0.079(2) 0.16(2) Uani 1 1 d D . . H2A H 0.1987 -0.0875 0.0834 0.246 Uiso 1 1 calc R . . H2B H 0.0902 -0.0278 0.0596 0.246 Uiso 1 1 calc R . . H2C H 0.1231 -0.0014 0.1176 0.246 Uiso 1 1 calc R . . C3 C 0.317(3) 0.020(4) 0.0015(18) 0.127(16) Uani 1 1 d D . . H3A H 0.3536 0.0761 -0.0241 0.19 Uiso 1 1 calc R . . H3B H 0.2949 -0.0237 -0.0228 0.19 Uiso 1 1 calc R . . H3C H 0.3662 -0.0235 0.0272 0.19 Uiso 1 1 calc R . . C4 C 0.141(4) 0.149(3) 0.0026(17) 0.14(2) Uani 1 1 d D . . H4A H 0.0707 0.1632 0.0268 0.21 Uiso 1 1 calc R . . H4B H 0.1314 0.1213 -0.0319 0.21 Uiso 1 1 calc R . . H4C H 0.1734 0.2142 -0.0106 0.21 Uiso 1 1 calc R . . C5 C -0.153(2) 0.093(3) 0.3898(15) 0.094(12) Uani 1 1 d D . . C6 C -0.076(3) 0.065(3) 0.4329(15) 0.105(13) Uani 1 1 d D . . H6A H -0.0353 -0.0046 0.4293 0.157 Uiso 1 1 calc R . . H6B H -0.116 0.0629 0.4729 0.157 Uiso 1 1 calc R . . H6C H -0.026 0.1169 0.4251 0.157 Uiso 1 1 calc R . . C7 C -0.212(4) 0.206(3) 0.3850(16) 0.16(2) Uani 1 1 d D . . H7A H -0.1582 0.2549 0.3757 0.241 Uiso 1 1 calc R . . H7B H -0.2575 0.2149 0.4225 0.241 Uiso 1 1 calc R . . H7C H -0.2567 0.2192 0.3536 0.241 Uiso 1 1 calc R . . C8 C -0.241(3) 0.020(3) 0.4041(17) 0.118(15) Uani 1 1 d D . . H8A H -0.3032 0.0535 0.3851 0.177 Uiso 1 1 calc R . . H8B H -0.2627 0.0046 0.4469 0.177 Uiso 1 1 calc R . . H8C H -0.2117 -0.0461 0.3895 0.177 Uiso 1 1 calc R . . C9 C 0.025(3) 0.381(3) 0.4140(15) 0.091(11) Uani 1 1 d D . . C10 C 0.001(7) 0.311(4) 0.4726(19) 0.26(5) Uani 1 1 d D . . H10A H -0.0572 0.3482 0.4977 0.387 Uiso 1 1 calc R . . H10B H 0.0659 0.294 0.4916 0.387 Uiso 1 1 calc R . . H10C H -0.022 0.2467 0.4668 0.387 Uiso 1 1 calc R . . C11 C 0.109(5) 0.455(5) 0.402(3) 0.28(5) Uani 1 1 d D . . H11A H 0.175 0.4246 0.3788 0.424 Uiso 1 1 calc R . . H11B H 0.1265 0.4651 0.4396 0.424 Uiso 1 1 calc R . . H11C H 0.0812 0.5222 0.3802 0.424 Uiso 1 1 calc R . . C12 C -0.083(5) 0.444(6) 0.404(3) 0.29(5) Uani 1 1 d D . . H12A H -0.0821 0.5166 0.4092 0.438 Uiso 1 1 calc R . . H12B H -0.1404 0.4137 0.4327 0.438 Uiso 1 1 calc R . . H12C H -0.0955 0.4439 0.3641 0.438 Uiso 1 1 calc R . . C13 C 0.450(2) 0.298(2) 0.0583(12) 0.059(7) Uani 1 1 d D . . C14 C 0.520(3) 0.194(2) 0.077(2) 0.107(14) Uani 1 1 d D . . H14A H 0.4949 0.1658 0.1182 0.16 Uiso 1 1 calc R . . H14B H 0.5957 0.2058 0.0727 0.16 Uiso 1 1 calc R . . H14C H 0.5144 0.1441 0.0519 0.16 Uiso 1 1 calc R . . C15 C 0.507(3) 0.384(3) 0.074(2) 0.124(15) Uani 1 1 d D . . H15A H 0.4591 0.4504 0.0711 0.186 Uiso 1 1 calc R . . H15B H 0.5742 0.3921 0.0462 0.186 Uiso 1 1 calc R . . H15C H 0.524 0.3622 0.1141 0.186 Uiso 1 1 calc R . . C16 C 0.427(3) 0.310(4) -0.0036(12) 0.116(15) Uani 1 1 d D . . H16A H 0.4103 0.2429 -0.01 0.173 Uiso 1 1 calc R . . H16B H 0.4905 0.3298 -0.0315 0.173 Uiso 1 1 calc R . . H16C H 0.3651 0.3639 -0.0095 0.173 Uiso 1 1 calc R . . C17 C 0.130(2) 0.5935(19) 0.0814(19) 0.090(13) Uani 1 1 d D . . C18 C 0.235(3) 0.625(5) 0.081(3) 0.21(4) Uani 1 1 d D . . H18A H 0.2737 0.5744 0.1089 0.321 Uiso 1 1 calc R . . H18B H 0.2246 0.6947 0.0916 0.321 Uiso 1 1 calc R . . H18C H 0.2762 0.627 0.041 0.321 Uiso 1 1 calc R . . C19 C 0.150(7) 0.549(4) 0.025(2) 0.23(4) Uani 1 1 d D . . H19A H 0.1987 0.5891 -0.0048 0.342 Uiso 1 1 calc R . . H19B H 0.0812 0.5521 0.0107 0.342 Uiso 1 1 calc R . . H19C H 0.1832 0.4753 0.0327 0.342 Uiso 1 1 calc R . . C20 C 0.055(5) 0.693(4) 0.083(3) 0.26(5) Uani 1 1 d D . . H20A H 0.0037 0.6988 0.0557 0.395 Uiso 1 1 calc R . . H20B H 0.0967 0.7521 0.0722 0.395 Uiso 1 1 calc R . . H20C H 0.0157 0.6925 0.1233 0.395 Uiso 1 1 calc R . . C21 C 0.427(2) -0.1570(19) 0.2009(11) 0.059(7) Uani 1 1 d D . . C22 C 0.401(5) -0.228(5) 0.164(4) 0.29(5) Uani 1 1 d D . . H22A H 0.3231 -0.2327 0.1724 0.441 Uiso 1 1 calc R . . H22B H 0.441 -0.2979 0.1741 0.441 Uiso 1 1 calc R . . H22C H 0.4214 -0.2002 0.1225 0.441 Uiso 1 1 calc R . . C23 C 0.505(4) -0.087(4) 0.172(4) 0.26(5) Uani 1 1 d D . . H23A H 0.4677 -0.0232 0.1508 0.385 Uiso 1 1 calc R . . H23B H 0.5591 -0.1217 0.1445 0.385 Uiso 1 1 calc R . . H23C H 0.5402 -0.0679 0.2019 0.385 Uiso 1 1 calc R . . C24 C 0.464(5) -0.223(6) 0.255(2) 0.32(6) Uani 1 1 d D . . H24A H 0.4207 -0.1987 0.2898 0.475 Uiso 1 1 calc R . . H24B H 0.5401 -0.2189 0.2543 0.475 Uiso 1 1 calc R . . H24C H 0.454 -0.2964 0.2557 0.475 Uiso 1 1 calc R . . C25 C 0.349(3) -0.004(2) 0.3829(13) 0.081(10) Uani 1 1 d D . . C26 C 0.280(4) 0.086(3) 0.4097(16) 0.135(19) Uani 1 1 d D . . H26A H 0.3119 0.1511 0.3937 0.202 Uiso 1 1 calc R . . H26B H 0.2773 0.0713 0.4526 0.202 Uiso 1 1 calc R . . H26C H 0.2067 0.0946 0.4001 0.202 Uiso 1 1 calc R . . C27 C 0.469(3) -0.002(5) 0.378(2) 0.17(2) Uani 1 1 d D . . H27A H 0.5087 -0.0606 0.3591 0.25 Uiso 1 1 calc R . . H27B H 0.4885 -0.0085 0.4172 0.25 Uiso 1 1 calc R . . H27C H 0.4881 0.0643 0.3538 0.25 Uiso 1 1 calc R . . C28 C 0.311(5) -0.109(3) 0.4176(15) 0.21(4) Uani 1 1 d D . . H28A H 0.2555 -0.1274 0.3988 0.316 Uiso 1 1 calc R . . H28B H 0.2811 -0.1003 0.4583 0.316 Uiso 1 1 calc R . . H28C H 0.3728 -0.1644 0.4177 0.316 Uiso 1 1 calc R . . C29 C 0.078(3) -0.158(2) 0.2962(14) 0.084(10) Uani 1 1 d D . . C30 C 0.098(4) -0.188(2) 0.2342(14) 0.111(15) Uani 1 1 d D . . H30A H 0.1681 -0.1683 0.2134 0.166 Uiso 1 1 calc R . . H30B H 0.0406 -0.1507 0.2121 0.166 Uiso 1 1 calc R . . H30C H 0.099 -0.2637 0.2377 0.166 Uiso 1 1 calc R . . C31 C -0.041(3) -0.159(3) 0.3226(17) 0.096(12) Uani 1 1 d D . . H31A H -0.0601 -0.23 0.326 0.143 Uiso 1 1 calc R . . H31B H -0.0858 -0.1095 0.297 0.143 Uiso 1 1 calc R . . H31C H -0.0528 -0.1396 0.3617 0.143 Uiso 1 1 calc R . . C32 C 0.160(4) -0.224(3) 0.3324(19) 0.136(19) Uani 1 1 d D . . H32A H 0.2203 -0.1847 0.3303 0.205 Uiso 1 1 calc R . . H32B H 0.1866 -0.2891 0.317 0.205 Uiso 1 1 calc R . . H32C H 0.1258 -0.2403 0.3735 0.205 Uiso 1 1 calc R . . C33 C -0.210(2) 0.493(2) 0.1848(14) 0.079(9) Uani 1 1 d DU . . C34 C -0.279(3) 0.508(5) 0.136(2) 0.19(2) Uani 1 1 d DU . . H34A H -0.354 0.5341 0.1508 0.289 Uiso 1 1 calc R . . H34B H -0.2776 0.4406 0.1232 0.289 Uiso 1 1 calc R . . H34C H -0.2509 0.5584 0.1024 0.289 Uiso 1 1 calc R . . C35 C -0.254(4) 0.429(3) 0.245(2) 0.164(19) Uani 1 1 d DU . . H35A H -0.2366 0.3539 0.2439 0.246 Uiso 1 1 calc R . . H35B H -0.3329 0.4473 0.2533 0.246 Uiso 1 1 calc R . . H35C H -0.2212 0.446 0.2764 0.246 Uiso 1 1 calc R . . C36 C -0.196(3) 0.605(3) 0.195(3) 0.21(4) Uani 1 1 d D . . H36A H -0.1254 0.6031 0.2064 0.314 Uiso 1 1 calc R . . H36B H -0.2531 0.6265 0.2263 0.314 Uiso 1 1 calc R . . H36C H -0.2026 0.6555 0.1584 0.314 Uiso 1 1 calc R . . C37 C -0.178(3) 0.072(3) 0.1825(15) 0.084(10) Uani 1 1 d D . . C38 C -0.171(3) -0.031(3) 0.160(2) 0.121(15) Uani 1 1 d D . . H38A H -0.0955 -0.0535 0.1444 0.181 Uiso 1 1 calc R . . H38B H -0.2162 -0.0219 0.1295 0.181 Uiso 1 1 calc R . . H38C H -0.1957 -0.0849 0.1932 0.181 Uiso 1 1 calc R . . C39 C -0.281(3) 0.094(4) 0.227(2) 0.135(18) Uani 1 1 d D . . H39A H -0.2657 0.1368 0.2544 0.203 Uiso 1 1 calc R . . H39B H -0.302 0.0276 0.25 0.203 Uiso 1 1 calc R . . H39C H -0.3397 0.1321 0.2064 0.203 Uiso 1 1 calc R . . C40 C -0.171(4) 0.164(5) 0.131(2) 0.22(3) Uani 1 1 d D . . H40A H -0.2039 0.2295 0.1445 0.324 Uiso 1 1 calc R . . H40B H -0.2106 0.1524 0.1004 0.324 Uiso 1 1 calc R . . H40C H -0.0955 0.1684 0.1138 0.324 Uiso 1 1 calc R . . C41 C 0.363(2) 0.376(2) 0.2814(14) 0.070(9) Uani 1 1 d D . . C42 C 0.444(3) 0.294(3) 0.253(2) 0.117(15) Uani 1 1 d D . . H42A H 0.5006 0.2662 0.2773 0.176 Uiso 1 1 calc R . . H42B H 0.4765 0.3262 0.2136 0.176 Uiso 1 1 calc R . . H42C H 0.4065 0.2362 0.2488 0.176 Uiso 1 1 calc R . . C43 C 0.399(3) 0.412(3) 0.3311(16) 0.124(17) Uani 1 1 d D . . H43A H 0.3519 0.4756 0.34 0.186 Uiso 1 1 calc R . . H43B H 0.4736 0.4262 0.3197 0.186 Uiso 1 1 calc R . . H43C H 0.3937 0.3568 0.3661 0.186 Uiso 1 1 calc R . . C44 C 0.338(4) 0.466(3) 0.230(2) 0.19(3) Uani 1 1 d D . . H44A H 0.3248 0.4358 0.1966 0.278 Uiso 1 1 calc R . . H44B H 0.3995 0.5053 0.2169 0.278 Uiso 1 1 calc R . . H44C H 0.2734 0.5124 0.2428 0.278 Uiso 1 1 calc R . . C45 C 0.383(4) -0.401(4) 0.463(4) 0.31(5) Uani 1 1 d D . . H45A H 0.325 -0.3602 0.4865 0.471 Uiso 1 1 calc R . . H45B H 0.3888 -0.4746 0.4815 0.471 Uiso 1 1 calc R . . H45C H 0.365 -0.3936 0.4231 0.471 Uiso 1 1 calc R . . C46 C 0.486(3) -0.360(2) 0.4597(19) 0.19(4) Uani 1 1 d GD . . C47 C 0.532(4) -0.308(2) 0.4950(14) 0.18(3) Uani 1 1 d G . . H47 H 0.4944 -0.2957 0.5323 0.221 Uiso 1 1 calc R . . C48 C 0.636(4) -0.276(3) 0.475(2) 0.26(5) Uani 1 1 d GU . . H48 H 0.6669 -0.2408 0.4983 0.312 Uiso 1 1 calc R . . C49 C 0.693(3) -0.295(4) 0.419(2) 0.26(5) Uani 1 1 d G . . H49 H 0.762 -0.2727 0.4055 0.313 Uiso 1 1 calc R . . C50 C 0.646(4) -0.347(3) 0.3838(16) 0.35(9) Uani 1 1 d G . . H50 H 0.6846 -0.3593 0.3466 0.421 Uiso 1 1 calc R . . C51 C 0.543(4) -0.379(3) 0.4041(17) 0.22(4) Uani 1 1 d G . . H51 H 0.512 -0.4142 0.3805 0.262 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0366(5) 0.0335(5) 0.0395(5) -0.0087(4) -0.0012(4) 0.0050(4) Ta2 0.0527(6) 0.0414(5) 0.0461(6) -0.0182(4) -0.0027(5) 0.0038(4) Ta3 0.0451(6) 0.0342(5) 0.0475(6) -0.0068(4) -0.0068(5) 0.0063(4) Ta4 0.0410(6) 0.0407(5) 0.0557(6) -0.0109(4) -0.0095(5) 0.0132(4) Ta5 0.0416(6) 0.0453(5) 0.0512(6) -0.0107(4) -0.0002(5) -0.0026(4) O1 0.047(9) 0.039(8) 0.036(8) -0.013(6) 0.000(7) -0.003(7) O2 0.035(9) 0.041(8) 0.071(11) -0.029(8) -0.017(8) 0.011(7) O3 0.039(9) 0.053(9) 0.062(11) -0.018(8) -0.023(8) 0.022(7) O4 0.050(10) 0.040(8) 0.035(8) -0.005(6) -0.004(7) -0.007(7) O5 0.074(12) 0.044(8) 0.021(7) -0.007(6) 0.005(8) -0.008(8) O6 0.057(11) 0.043(9) 0.041(9) -0.015(7) -0.002(8) 0.007(7) O7 0.049(11) 0.074(12) 0.050(11) -0.004(9) -0.017(9) -0.010(9) O8 0.076(13) 0.052(10) 0.067(12) -0.025(9) 0.000(10) 0.005(9) O9 0.046(10) 0.036(8) 0.047(9) 0.001(7) 0.009(8) -0.002(7) O10 0.050(11) 0.042(9) 0.062(11) 0.000(8) -0.004(9) -0.001(7) O11 0.020(8) 0.043(9) 0.123(17) -0.009(10) -0.015(10) 0.016(7) O12 0.074(14) 0.078(12) 0.060(12) -0.022(10) -0.021(10) -0.014(10) O13 0.037(9) 0.047(9) 0.080(13) -0.006(8) -0.024(9) 0.013(7) O14 0.045(10) 0.088(13) 0.069(12) -0.054(10) -0.024(9) 0.032(9) O15 0.054(11) 0.029(8) 0.060(11) 0.007(7) -0.004(9) 0.008(7) O16 0.045(9) 0.066(11) 0.083(13) -0.024(10) -0.020(9) 0.050(9) O17 0.062(13) 0.061(11) 0.091(15) -0.025(10) 0.044(11) 0.021(9) O18 0.050(11) 0.075(12) 0.078(14) -0.028(10) -0.011(10) -0.002(9) C1 0.061(17) 0.047(13) 0.09(2) -0.039(13) -0.050(15) 0.021(12) C2 0.14(4) 0.15(4) 0.24(6) -0.11(4) 0.03(4) -0.10(4) C3 0.13(4) 0.16(4) 0.09(3) -0.06(3) 0.02(3) -0.01(3) C4 0.16(4) 0.17(4) 0.09(3) -0.05(3) -0.08(3) 0.07(3) C5 0.046(18) 0.16(4) 0.07(2) -0.01(2) -0.035(17) 0.01(2) C6 0.06(2) 0.16(4) 0.08(3) -0.02(2) 0.01(2) -0.03(2) C7 0.27(7) 0.11(3) 0.06(2) -0.01(2) 0.02(3) 0.07(4) C8 0.08(3) 0.20(4) 0.09(3) -0.03(3) 0.03(2) -0.07(3) C9 0.10(3) 0.08(2) 0.08(2) -0.041(19) 0.02(2) 0.02(2) C10 0.50(14) 0.17(5) 0.06(3) -0.05(3) -0.01(5) 0.06(7) C11 0.30(9) 0.32(9) 0.28(9) -0.26(8) 0.16(8) -0.17(8) C12 0.20(7) 0.42(12) 0.32(10) -0.33(10) -0.08(7) 0.11(8) C13 0.039(15) 0.079(18) 0.054(17) -0.008(14) 0.009(12) -0.011(13) C14 0.09(3) 0.055(19) 0.16(4) 0.01(2) 0.00(3) -0.022(18) C15 0.12(4) 0.13(4) 0.13(4) -0.04(3) -0.01(3) -0.03(3) C16 0.06(2) 0.22(5) 0.046(19) 0.00(2) 0.031(17) -0.04(3) C17 0.06(2) 0.025(13) 0.19(4) -0.017(18) -0.04(2) 0.004(12) C18 0.06(3) 0.32(8) 0.20(6) 0.15(6) -0.03(3) -0.02(4) C19 0.47(13) 0.14(5) 0.08(4) 0.00(3) -0.07(6) -0.06(6) C20 0.17(6) 0.12(4) 0.34(9) 0.11(5) 0.12(6) 0.07(4) C21 0.067(19) 0.051(14) 0.051(15) -0.018(12) -0.003(14) 0.022(13) C22 0.21(7) 0.20(6) 0.49(14) -0.26(8) -0.01(8) 0.09(5) C23 0.08(3) 0.16(5) 0.49(13) -0.12(7) 0.13(6) -0.01(3) C24 0.23(7) 0.45(11) 0.14(5) -0.01(6) -0.02(5) 0.31(8) C25 0.09(3) 0.09(2) 0.051(18) -0.016(16) -0.012(17) 0.022(19) C26 0.21(5) 0.10(3) 0.09(3) -0.03(2) -0.09(3) 0.07(3) C27 0.08(3) 0.35(8) 0.10(3) -0.05(4) -0.05(3) -0.07(4) C28 0.50(11) 0.07(3) 0.04(2) -0.004(18) -0.04(4) 0.03(4) C29 0.09(3) 0.041(15) 0.12(3) -0.027(16) -0.03(2) 0.017(15) C30 0.21(5) 0.07(2) 0.08(2) -0.034(18) 0.00(3) -0.08(2) C31 0.08(2) 0.08(2) 0.11(3) 0.00(2) 0.03(2) -0.032(19) C32 0.19(5) 0.06(2) 0.13(4) 0.02(2) -0.01(3) 0.02(3) C33 0.029(13) 0.075(19) 0.11(2) -0.006(16) 0.019(12) 0.011(12) C34 0.027(18) 0.33(6) 0.21(4) -0.08(4) -0.04(2) 0.07(3) C35 0.16(4) 0.10(3) 0.18(3) 0.01(3) 0.08(3) -0.04(3) C36 0.07(3) 0.10(3) 0.47(12) -0.10(5) -0.04(5) 0.02(2) C37 0.09(3) 0.11(3) 0.06(2) -0.006(19) -0.003(18) -0.05(2) C38 0.12(3) 0.16(4) 0.12(4) -0.06(3) -0.03(3) -0.05(3) C39 0.06(2) 0.18(4) 0.19(5) -0.07(4) -0.03(3) 0.00(3) C40 0.12(4) 0.42(11) 0.14(5) 0.00(6) -0.06(4) -0.11(6) C41 0.062(19) 0.061(17) 0.10(2) -0.001(16) -0.027(18) -0.038(15) C42 0.09(3) 0.10(3) 0.18(5) -0.05(3) -0.03(3) -0.05(2) C43 0.16(4) 0.14(3) 0.10(3) -0.09(3) 0.03(3) -0.10(3) C44 0.19(5) 0.07(2) 0.29(7) -0.04(4) 0.09(5) -0.10(3) C45 0.47(15) 0.09(4) 0.35(11) 0.17(5) -0.19(10) -0.06(6) C46 0.06(2) 0.06(3) 0.39(11) 0.10(4) -0.06(4) -0.006(19) C47 0.32(9) 0.06(3) 0.19(6) -0.05(3) -0.17(6) 0.08(4) C48 0.29(8) 0.22(7) 0.19(6) 0.09(5) 0.06(6) -0.08(6) C49 0.17(6) 0.23(8) 0.40(15) 0.02(9) -0.19(9) 0.01(6) C50 0.35(14) 0.28(11) 0.52(19) -0.23(12) -0.33(14) 0.17(10) C51 0.34(12) 0.22(7) 0.06(3) 0.03(4) -0.05(5) 0.01(8) #----------------------------------------------------------------------------# # 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 Ta1 O9 1.865(15) . ? Ta1 O6 1.866(14) . ? Ta1 O4 1.940(15) . ? Ta1 O3 2.026(15) . ? Ta1 O1 2.028(13) . ? Ta1 O2 2.049(17) . ? Ta1 Ta4 3.1815(18) . ? Ta1 Ta3 3.185(3) . ? Ta2 O8 1.893(18) . ? Ta2 O12 1.905(19) . ? Ta2 O14 1.906(17) . ? Ta2 O5 1.960(14) . ? Ta2 O1 2.034(14) . ? Ta2 O17 2.40(2) . ? Ta2 Ta4 3.000(2) . ? Ta2 Ta5 3.3544(18) . ? Ta3 O3 1.819(18) . ? Ta3 O13 1.856(17) . ? Ta3 O15 1.900(15) . ? Ta3 O2 2.076(15) . ? Ta3 O10 2.151(17) . ? Ta3 O5 2.186(15) . ? Ta3 Ta5 3.0949(17) . ? Ta4 O11 1.840(18) . ? Ta4 O16 1.884(16) . ? Ta4 O4 1.923(14) . ? Ta4 O14 1.993(16) . ? Ta4 O1 2.103(15) . ? Ta4 O17 2.18(2) . ? Ta5 O7 1.813(18) . ? Ta5 O18 1.832(18) . ? Ta5 O17 1.911(18) . ? Ta5 O2 2.060(16) . ? Ta5 O5 2.158(17) . ? Ta5 O10 2.172(15) . ? O6 C1 1.41(3) . ? O7 C5 1.48(4) . ? O8 C9 1.46(3) . ? O9 C13 1.48(3) . ? O10 C29 1.51(3) . ? O11 C17 1.41(4) . ? O12 C41 1.42(3) . ? O13 C25 1.47(3) . ? O15 C21 1.44(3) . ? O16 C33 1.40(3) . ? O18 C37 1.45(4) . ? C1 C3 1.50(3) . ? C1 C4 1.52(3) . ? C1 C2 1.55(4) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 C6 1.45(3) . ? C5 C8 1.50(3) . ? C5 C7 1.51(3) . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 C10 1.47(4) . ? C9 C12 1.48(4) . ? C9 C11 1.48(4) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C16 1.47(3) . ? C13 C14 1.50(3) . ? C13 C15 1.52(3) . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C17 C18 1.42(4) . ? C17 C20 1.45(4) . ? C17 C19 1.48(4) . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C18 H18C 0.96 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 H20A 0.96 . ? C20 H20B 0.96 . ? C20 H20C 0.96 . ? C21 C23 1.42(4) . ? C21 C22 1.46(4) . ? C21 C24 1.46(4) . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C27 1.48(4) . ? C25 C26 1.49(3) . ? C25 C28 1.52(4) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 C32 1.48(4) . ? C29 C31 1.49(3) . ? C29 C30 1.51(3) . ? C30 H30A 0.96 . ? C30 H30B 0.96 . ? C30 H30C 0.96 . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? C33 C34 1.50(4) . ? C33 C35 1.52(4) . ? C33 C36 1.55(4) . ? C34 H34A 0.96 . ? C34 H34B 0.96 . ? C34 H34C 0.96 . ? C35 H35A 0.96 . ? C35 H35B 0.96 . ? C35 H35C 0.96 . ? C36 H36A 0.96 . ? C36 H36B 0.96 . ? C36 H36C 0.96 . ? C37 C38 1.50(3) . ? C37 C40 1.50(4) . ? C37 C39 1.51(4) . ? C38 H38A 0.96 . ? C38 H38B 0.96 . ? C38 H38C 0.96 . ? C39 H39A 0.96 . ? C39 H39B 0.96 . ? C39 H39C 0.96 . ? C40 H40A 0.96 . ? C40 H40B 0.96 . ? C40 H40C 0.96 . ? C41 C43 1.47(3) . ? C41 C42 1.50(3) . ? C41 C44 1.52(4) . ? C42 H42A 0.96 . ? C42 H42B 0.96 . ? C42 H42C 0.96 . ? C43 H43A 0.96 . ? C43 H43B 0.96 . ? C43 H43C 0.96 . ? C44 H44A 0.96 . ? C44 H44B 0.96 . ? C44 H44C 0.96 . ? C45 C46 1.448(10) . ? C45 H45A 0.96 . ? C45 H45B 0.96 . ? C45 H45C 0.96 . ? C46 C47 1.39 . ? C46 C51 1.39 . ? C47 C48 1.39 . ? C47 H47 0.93 . ? C48 C49 1.39 . ? C48 H48 0.93 . ? C49 C50 1.39 . ? C49 H49 0.93 . ? C50 C51 1.39 . ? C50 H50 0.93 . ? C51 H51 0.93 . ? 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 O9 Ta1 O6 93.2(7) . . ? O9 Ta1 O4 104.0(6) . . ? O6 Ta1 O4 95.7(6) . . ? O9 Ta1 O3 94.1(7) . . ? O6 Ta1 O3 104.7(6) . . ? O4 Ta1 O3 151.9(6) . . ? O9 Ta1 O1 92.5(6) . . ? O6 Ta1 O1 170.0(7) . . ? O4 Ta1 O1 74.9(6) . . ? O3 Ta1 O1 83.1(6) . . ? O9 Ta1 O2 165.5(6) . . ? O6 Ta1 O2 88.0(6) . . ? O4 Ta1 O2 90.2(6) . . ? O3 Ta1 O2 71.7(6) . . ? O1 Ta1 O2 88.6(6) . . ? O9 Ta1 Ta4 100.4(4) . . ? O6 Ta1 Ta4 130.0(5) . . ? O4 Ta1 Ta4 34.4(4) . . ? O3 Ta1 Ta4 121.8(4) . . ? O1 Ta1 Ta4 40.5(4) . . ? O2 Ta1 Ta4 89.8(4) . . ? O9 Ta1 Ta3 126.1(5) . . ? O6 Ta1 Ta3 100.5(5) . . ? O4 Ta1 Ta3 125.7(4) . . ? O3 Ta1 Ta3 32.0(5) . . ? O1 Ta1 Ta3 82.7(4) . . ? O2 Ta1 Ta3 39.8(4) . . ? Ta4 Ta1 Ta3 108.96(5) . . ? O8 Ta2 O12 96.4(8) . . ? O8 Ta2 O14 92.0(7) . . ? O12 Ta2 O14 106.7(8) . . ? O8 Ta2 O5 98.3(7) . . ? O12 Ta2 O5 109.1(8) . . ? O14 Ta2 O5 141.2(7) . . ? O8 Ta2 O1 169.6(7) . . ? O12 Ta2 O1 88.8(7) . . ? O14 Ta2 O1 77.9(6) . . ? O5 Ta2 O1 88.4(6) . . ? O8 Ta2 O17 103.2(7) . . ? O12 Ta2 O17 160.1(7) . . ? O14 Ta2 O17 70.0(7) . . ? O5 Ta2 O17 71.2(7) . . ? O1 Ta2 O17 71.3(6) . . ? O8 Ta2 Ta4 125.4(6) . . ? O12 Ta2 Ta4 118.6(6) . . ? O14 Ta2 Ta4 40.8(5) . . ? O5 Ta2 Ta4 106.7(4) . . ? O1 Ta2 Ta4 44.4(4) . . ? O17 Ta2 Ta4 45.9(5) . . ? O8 Ta2 Ta5 100.8(6) . . ? O12 Ta2 Ta5 144.1(6) . . ? O14 Ta2 Ta5 103.9(5) . . ? O5 Ta2 Ta5 37.5(5) . . ? O1 Ta2 Ta5 79.7(4) . . ? O17 Ta2 Ta5 33.9(4) . . ? Ta4 Ta2 Ta5 75.21(7) . . ? O3 Ta3 O13 104.7(7) . . ? O3 Ta3 O15 96.6(7) . . ? O13 Ta3 O15 98.8(7) . . ? O3 Ta3 O2 75.3(6) . . ? O13 Ta3 O2 158.1(6) . . ? O15 Ta3 O2 103.0(6) . . ? O3 Ta3 O10 148.7(6) . . ? O13 Ta3 O10 103.9(7) . . ? O15 Ta3 O10 91.4(7) . . ? O2 Ta3 O10 73.4(6) . . ? O3 Ta3 O5 97.1(6) . . ? O13 Ta3 O5 85.6(6) . . ? O15 Ta3 O5 164.0(7) . . ? O2 Ta3 O5 72.8(6) . . ? O10 Ta3 O5 72.7(6) . . ? O3 Ta3 Ta5 107.8(4) . . ? O13 Ta3 Ta5 122.1(5) . . ? O15 Ta3 Ta5 122.9(5) . . ? O2 Ta3 Ta5 41.4(4) . . ? O10 Ta3 Ta5 44.6(4) . . ? O5 Ta3 Ta5 44.2(4) . . ? O3 Ta3 Ta1 36.2(5) . . ? O13 Ta3 Ta1 135.9(5) . . ? O15 Ta3 Ta1 104.3(5) . . ? O2 Ta3 Ta1 39.2(5) . . ? O10 Ta3 Ta1 112.5(4) . . ? O5 Ta3 Ta1 82.3(4) . . ? Ta5 Ta3 Ta1 74.13(4) . . ? O11 Ta4 O16 98.6(8) . . ? O11 Ta4 O4 99.0(7) . . ? O16 Ta4 O4 106.5(7) . . ? O11 Ta4 O14 96.7(9) . . ? O16 Ta4 O14 100.6(7) . . ? O4 Ta4 O14 146.0(6) . . ? O11 Ta4 O1 99.3(6) . . ? O16 Ta4 O1 161.9(7) . . ? O4 Ta4 O1 73.5(6) . . ? O14 Ta4 O1 74.4(6) . . ? O11 Ta4 O17 169.7(9) . . ? O16 Ta4 O17 87.0(8) . . ? O4 Ta4 O17 87.5(6) . . ? O14 Ta4 O17 73.7(8) . . ? O1 Ta4 O17 74.9(7) . . ? O11 Ta4 Ta2 117.6(6) . . ? O16 Ta4 Ta2 124.2(6) . . ? O4 Ta4 Ta2 107.7(4) . . ? O14 Ta4 Ta2 38.6(5) . . ? O1 Ta4 Ta2 42.6(4) . . ? O17 Ta4 Ta2 52.4(6) . . ? O11 Ta4 Ta1 100.9(5) . . ? O16 Ta4 Ta1 138.8(6) . . ? O4 Ta4 Ta1 34.7(5) . . ? O14 Ta4 Ta1 112.6(4) . . ? O1 Ta4 Ta1 38.8(4) . . ? O17 Ta4 Ta1 79.9(4) . . ? Ta2 Ta4 Ta1 76.40(6) . . ? O7 Ta5 O18 99.6(8) . . ? O7 Ta5 O17 99.6(7) . . ? O18 Ta5 O17 103.0(9) . . ? O7 Ta5 O2 162.1(7) . . ? O18 Ta5 O2 92.6(7) . . ? O17 Ta5 O2 90.3(6) . . ? O7 Ta5 O5 93.7(6) . . ? O18 Ta5 O5 166.3(7) . . ? O17 Ta5 O5 78.0(8) . . ? O2 Ta5 O5 73.7(6) . . ? O7 Ta5 O10 91.1(7) . . ? O18 Ta5 O10 103.4(7) . . ? O17 Ta5 O10 149.4(8) . . ? O2 Ta5 O10 73.3(6) . . ? O5 Ta5 O10 72.8(6) . . ? O7 Ta5 Ta3 120.5(5) . . ? O18 Ta5 Ta3 123.4(5) . . ? O17 Ta5 Ta3 107.3(6) . . ? O2 Ta5 Ta3 41.8(4) . . ? O5 Ta5 Ta3 44.9(4) . . ? O10 Ta5 Ta3 44.0(4) . . ? O7 Ta5 Ta2 95.2(5) . . ? O18 Ta5 Ta2 146.5(6) . . ? O17 Ta5 Ta2 44.6(7) . . ? O2 Ta5 Ta2 81.3(4) . . ? O5 Ta5 Ta2 33.5(4) . . ? O10 Ta5 Ta2 106.3(4) . . ? Ta3 Ta5 Ta2 71.79(4) . . ? Ta1 O1 Ta2 140.7(8) . . ? Ta1 O1 Ta4 100.7(6) . . ? Ta2 O1 Ta4 92.9(6) . . ? Ta1 O2 Ta5 134.2(7) . . ? Ta1 O2 Ta3 101.1(6) . . ? Ta5 O2 Ta3 96.9(7) . . ? Ta3 O3 Ta1 111.7(8) . . ? Ta4 O4 Ta1 110.9(7) . . ? Ta2 O5 Ta5 109.0(7) . . ? Ta2 O5 Ta3 131.9(8) . . ? Ta5 O5 Ta3 90.9(5) . . ? C1 O6 Ta1 158.7(15) . . ? C5 O7 Ta5 168.3(18) . . ? C9 O8 Ta2 144(2) . . ? C13 O9 Ta1 151.9(14) . . ? C29 O10 Ta3 132.7(15) . . ? C29 O10 Ta5 130.3(15) . . ? Ta3 O10 Ta5 91.4(6) . . ? C17 O11 Ta4 161.1(19) . . ? C41 O12 Ta2 150.0(17) . . ? C25 O13 Ta3 165.1(16) . . ? Ta2 O14 Ta4 100.6(7) . . ? C21 O15 Ta3 144.9(16) . . ? C33 O16 Ta4 152.5(19) . . ? Ta5 O17 Ta4 143.7(8) . . ? Ta5 O17 Ta2 101.5(9) . . ? Ta4 O17 Ta2 81.6(7) . . ? C37 O18 Ta5 157.9(18) . . ? O6 C1 C3 110(2) . . ? O6 C1 C4 106(2) . . ? C3 C1 C4 113(3) . . ? O6 C1 C2 106(2) . . ? C3 C1 C2 111(3) . . ? C4 C1 C2 110(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 O7 108(2) . . ? C6 C5 C8 111(3) . . ? O7 C5 C8 112(3) . . ? C6 C5 C7 115(4) . . ? O7 C5 C7 104(3) . . ? C8 C5 C7 107(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O8 C9 C10 107(3) . . ? O8 C9 C12 104(3) . . ? C10 C9 C12 104(5) . . ? O8 C9 C11 109(3) . . ? C10 C9 C11 122(5) . . ? C12 C9 C11 108(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 O9 106(2) . . ? C16 C13 C14 112(3) . . ? O9 C13 C14 103(2) . . ? C16 C13 C15 119(3) . . ? O9 C13 C15 111(2) . . ? C14 C13 C15 105(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O11 C17 C18 113(3) . . ? O11 C17 C20 113(3) . . ? C18 C17 C20 103(4) . . ? O11 C17 C19 108(3) . . ? C18 C17 C19 101(5) . . ? C20 C17 C19 118(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 O15 111(2) . . ? C23 C21 C22 116(5) . . ? O15 C21 C22 106(3) . . ? C23 C21 C24 110(5) . . ? O15 C21 C24 105(2) . . ? C22 C21 C24 108(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O13 C25 C27 108(3) . . ? O13 C25 C26 108(2) . . ? C27 C25 C26 114(4) . . ? O13 C25 C28 105(3) . . ? C27 C25 C28 114(4) . . ? C26 C25 C28 109(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 C31 117(3) . . ? C32 C29 O10 106(3) . . ? C31 C29 O10 108(2) . . ? C32 C29 C30 110(3) . . ? C31 C29 C30 110(3) . . ? O10 C29 C30 105(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O16 C33 C34 110(3) . . ? O16 C33 C35 106(3) . . ? C34 C33 C35 116(4) . . ? O16 C33 C36 109(3) . . ? C34 C33 C36 107(4) . . ? C35 C33 C36 108(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O18 C37 C38 109(3) . . ? O18 C37 C40 104(3) . . ? C38 C37 C40 111(4) . . ? O18 C37 C39 110(3) . . ? C38 C37 C39 113(3) . . ? C40 C37 C39 110(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O12 C41 C43 108(3) . . ? O12 C41 C42 109(2) . . ? C43 C41 C42 115(3) . . ? O12 C41 C44 106(2) . . ? C43 C41 C44 114(3) . . ? C42 C41 C44 105(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 120 . . ? C47 C46 C45 137(5) . . ? C51 C46 C45 103(5) . . ? C48 C47 C46 120 . . ? C48 C47 H47 120 . . ? C46 C47 H47 120 . . ? C47 C48 C49 120 . . ? C47 C48 H48 120 . . ? C49 C48 H48 120 . . ? C48 C49 C50 120 . . ? C48 C49 H49 120 . . ? C50 C49 H49 120 . . ? C49 C50 C51 120 . . ? C49 C50 H50 120 . . ? C51 C50 H50 120 . . ? C50 C51 C46 120 . . ? C50 C51 H51 120 . . ? C46 C51 H51 120 . . ? #===END