# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/202 data_CRYSTALS_cif ## -----------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), (Psi correction), Acta Cryst, A24, 351-359 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, (1983) A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK( _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany' _computing_cell_refinement 'Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany' _computing_data_collection 'Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany' _computing_data_reduction 'Stoe and Cie (1996) IPDS Manual. Version 2.75. Stoe and Cie, Darmstadt, Germany' #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _refine_ls_matrix_type userblock _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #**************************************************************************** _cell_length_a 13.152(2) _cell_angle_alpha 90.0 _cell_length_b 18.720(3) _cell_angle_beta 99.40(2) _cell_length_c 20.918(3) _cell_angle_gamma 90.0 _cell_volume 5067(2) _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,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'Ta ' -1.2580 6.5230 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum [C11H12OTa][B(C6H3)(CF3)2]4;1.5(CH2Cl2) _chemical_formula_moiety [C11H12OTa][B(C6H3)(CF3)2]4;1.5(CH2Cl2) _chemical_formula_weight 1331.77 _diffrn_measurement_method 'rotation en' _diffrn_detector_area_resol_mean '(1.45 - 24.2)' _d(hkl)_range '(14.228 - 0.867)' _diffrn_standards_number 200 _cell_measurement_temperature 120K _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 24.2 _cell_formula_units_Z 4.00 _exptl_crystal_description ' rod ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.74 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2586.05 _exptl_absorpt_coefficient_mu 24.16 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5898 _exptl_absorpt_correction_T_max 0.7620 _absorpt_process_ref ; [X-Shape a Crystal Optimisation for Numerical Absorption Corrections Revision 1.01 July 1996 STOE and Cie GMBH 1996] ; _exptl_absorpt_process_details ; . Absorption corrections were applied on the data by using a set of symmetry equivalent reflections selected with the criterion [I>3((I)] such that all directions of the reciprocal space are equally represented. ; _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 7545 _reflns_number_total 39337 _diffrn_reflns_av_R_equivalents 0.044 # Number of reflections with Friedels Law is 7545 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8084 _diffrn_measured_fraction_theta_max 93.3% _reflns_number_observed 6322 _diffrn_reflns_2theta_min 2.9 _diffrn_reflns_2theta_max 48.4 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -1.67 _refine_diff_density_max 1.85 _refine_ls_number_reflns 6322 _refine_ls_number_parameters 694 _refine_ls_R_factor_obs 0.0512 _refine_ls_wR_factor_obs 0.0623 _refine_ls_goodness_of_fit_obs 0.9868 _refine_ls_shift/su_max 0.683701 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ta1 0.745734(18) 0.788182(12) 0.176678(12) 0.0257 1.0000 Uani O1 0.8696(5) 0.7253(3) 0.3091(3) 0.0657 1.0000 Uani C1 0.6971(6) 0.9055(4) 0.1430(4) 0.0504 1.0000 Uani C2 0.6726(5) 0.8974(4) 0.2048(4) 0.0468 1.0000 Uani C3 0.7649(7) 0.8873(4) 0.2476(4) 0.0511 1.0000 Uani C4 0.8458(5) 0.8884(4) 0.2082(5) 0.0506 1.0000 Uani C5 0.8007(6) 0.8995(4) 0.1434(4) 0.0492 1.0000 Uani C6 0.6424(6) 0.6895(4) 0.1974(3) 0.0381 1.0000 Uani C7 0.7087(6) 0.6680(4) 0.1530(4) 0.0422 1.0000 Uani C8 0.6757(7) 0.7080(4) 0.0947(3) 0.0483 1.0000 Uani C9 0.5969(6) 0.7518(4) 0.1052(4) 0.0491 1.0000 Uani C10 0.5763(5) 0.7414(4) 0.1679(3) 0.0399 1.0000 Uani C11 0.8255(6) 0.7476(4) 0.2619(3) 0.0436 1.0000 Uani H1 0.832(4) 0.776(3) 0.122(2) 0.026(16) 1.0000 Uiso H2 0.871(3) 0.761(4) 0.170(3) 0.046(18) 1.0000 Uiso B1 0.3975(5) 0.5687(3) 0.2854(3) 0.0163 1.0000 Uani C111 0.4083(4) 0.5773(3) 0.2087(2) 0.0159 1.0000 Uani C112 0.3515(5) 0.6262(3) 0.1673(3) 0.0212 1.0000 Uani C113 0.3673(5) 0.6347(3) 0.1033(3) 0.0230 1.0000 Uani C114 0.4436(5) 0.5956(3) 0.0793(2) 0.0256 1.0000 Uani C115 0.5011(5) 0.5479(3) 0.1201(3) 0.0213 1.0000 Uani C116 0.4846(4) 0.5396(3) 0.1840(2) 0.0189 1.0000 Uani C117 0.3051(5) 0.6879(3) 0.0605(3) 0.0312 1.0000 Uani C118 0.5818(6) 0.5031(3) 0.0975(3) 0.0310 1.0000 Uani C121 0.4897(4) 0.6186(3) 0.3239(2) 0.0172 1.0000 Uani C122 0.4772(5) 0.6925(3) 0.3291(2) 0.0199 1.0000 Uani C123 0.5565(5) 0.7365(3) 0.3577(3) 0.0230 1.0000 Uani C124 0.6537(5) 0.7087(3) 0.3818(3) 0.0236 1.0000 Uani C125 0.6677(4) 0.6360(3) 0.3766(2) 0.0194 1.0000 Uani C126 0.5875(4) 0.5923(3) 0.3473(2) 0.0162 1.0000 Uani C127 0.5398(6) 0.8152(3) 0.3628(3) 0.0336 1.0000 Uani C128 0.7701(5) 0.6032(3) 0.4025(3) 0.0314 1.0000 Uani C131 0.4075(4) 0.4843(3) 0.3080(2) 0.0151 1.0000 Uani C132 0.4365(4) 0.4646(3) 0.3729(3) 0.0201 1.0000 Uani C133 0.4354(5) 0.3943(3) 0.3936(3) 0.0245 1.0000 Uani C134 0.4055(5) 0.3400(3) 0.3500(3) 0.0267 1.0000 Uani C135 0.3755(4) 0.3576(3) 0.2861(3) 0.0231 1.0000 Uani C136 0.3759(4) 0.4281(3) 0.2652(3) 0.0188 1.0000 Uani C137 0.4667(5) 0.3768(4) 0.4633(3) 0.0360 1.0000 Uani C138 0.3423(6) 0.3001(3) 0.2371(3) 0.0337 1.0000 Uani C141 0.2828(4) 0.5902(3) 0.3007(2) 0.0162 1.0000 Uani C142 0.2681(4) 0.6207(3) 0.3591(2) 0.0199 1.0000 Uani C143 0.1704(5) 0.6317(3) 0.3741(3) 0.0243 1.0000 Uani C144 0.0828(5) 0.6126(3) 0.3316(3) 0.0251 1.0000 Uani C145 0.0957(5) 0.5825(3) 0.2732(3) 0.0216 1.0000 Uani C146 0.1938(4) 0.5710(3) 0.2585(2) 0.0182 1.0000 Uani C147 0.1622(6) 0.6637(4) 0.4387(3) 0.0382 1.0000 Uani C148 0.0038(5) 0.5640(3) 0.2234(3) 0.0301 1.0000 Uani F1 0.2068(6) 0.6851(6) 0.0644(4) 0.1460 1.0000 Uani F2 0.3092(8) 0.6818(5) 0.0010(2) 0.1411 1.0000 Uani F3 0.3249(8) 0.7524(3) 0.0757(4) 0.1518 1.0000 Uani F4 0.6059(3) 0.5250(2) 0.04076(17) 0.0448 1.0000 Uani F5 0.6711(3) 0.5024(2) 0.13975(17) 0.0386 1.0000 Uani F6 0.8346(3) 0.6472(2) 0.4384(2) 0.0476 1.0000 Uani F7 0.4951(9) 0.8311(3) 0.4102(4) 0.1590 1.0000 Uani F8 0.4830(7) 0.8412(3) 0.3124(4) 0.1160 1.0000 Uani F9 0.6230(5) 0.8524(3) 0.3717(5) 0.1131 1.0000 Uani F10 0.8183(3) 0.5781(2) 0.3550(2) 0.0496 1.0000 Uani F11 0.5540(4) 0.43500(19) 0.0890(2) 0.0492 1.0000 Uani F12 0.7604(3) 0.54521(19) 0.43980(18) 0.0382 1.0000 Uani F13 0.5596(6) 0.3995(5) 0.4872(3) 0.1149 1.0000 Uani F14 0.4536(13) 0.3165(4) 0.4798(3) 0.2351 1.0000 Uani F15 0.4189(7) 0.4178(6) 0.5016(3) 0.1340 1.0000 Uani F16 0.3268(7) 0.2389(3) 0.2623(3) 0.1062 1.0000 Uani F17 0.2575(6) 0.3153(3) 0.1976(4) 0.1036 1.0000 Uani F18 0.4094(5) 0.2907(3) 0.1980(3) 0.0920 1.0000 Uani F19 0.2143(6) 0.7233(3) 0.4497(3) 0.0927 1.0000 Uani F20 0.1970(5) 0.6214(4) 0.4873(2) 0.0860 1.0000 Uani F21 0.0658(4) 0.6785(4) 0.4456(3) 0.0973 1.0000 Uani F22 -0.0790(4) 0.5493(4) 0.2497(2) 0.0882 1.0000 Uani F23 0.0177(4) 0.5097(3) 0.1872(2) 0.0663 1.0000 Uani F24 -0.0235(5) 0.6182(3) 0.1836(3) 0.0767 1.0000 Uani C100 0.3402(6) 0.9335(4) 0.1010(4) 0.0521 1.0000 Uani Cl101 0.37821(16) 0.89252(11) 0.17670(11) 0.0577 1.0000 Uani Cl102 0.44736(16) 0.96146(14) 0.0665(1) 0.0638 1.0000 Uani C200 0.8534(15) 1.5238(11) -0.0359(8) 0.1587 0.5000 Uani Cl201 0.8842(5) 1.5733(6) 0.03551(19) 0.1527 0.5000 Uani Cl202 0.7481(6) 1.5576(6) -0.0792(2) 0.1538 0.5000 Uani H11 0.6472 0.9152 0.1048 0.0591 1.0000 Uiso H21 0.6045 0.8985 0.2159 0.0481 1.0000 Uiso H31 0.7741 0.8814 0.2942 0.0610 1.0000 Uiso H41 0.9194 0.8824 0.2241 0.0516 1.0000 Uiso H51 0.8359 0.9028 0.1063 0.0542 1.0000 Uiso H61 0.6455 0.6713 0.2409 0.0429 1.0000 Uiso H71 0.7626 0.6338 0.1601 0.0502 1.0000 Uiso H81 0.7040 0.7049 0.0555 0.0566 1.0000 Uiso H91 0.5611 0.7840 0.0739 0.0588 1.0000 Uiso H101 0.5241 0.7660 0.1867 0.0458 1.0000 Uiso H1121 0.2988 0.6543 0.1824 0.0264 1.0000 Uiso H1141 0.4552 0.6016 0.0357 0.0285 1.0000 Uiso H1161 0.5270 0.5067 0.2118 0.0228 1.0000 Uiso H1221 0.4112 0.7136 0.3122 0.0247 1.0000 Uiso H1241 0.7089 0.7391 0.4015 0.0278 1.0000 Uiso H1261 0.6010 0.5422 0.3431 0.0209 1.0000 Uiso H1321 0.4590 0.5013 0.4041 0.0264 1.0000 Uiso H1341 0.4047 0.2914 0.3637 0.0316 1.0000 Uiso H1361 0.3533 0.4389 0.2200 0.0228 1.0000 Uiso H1421 0.3274 0.6340 0.3901 0.0243 1.0000 Uiso H1441 0.0157 0.6199 0.3429 0.0307 1.0000 Uiso H1461 0.2009 0.5492 0.2180 0.0223 1.0000 Uiso H1001 0.2989 0.9744 0.1066 0.0563 1.0000 Uiso H1002 0.3012 0.9001 0.0724 0.0563 1.0000 Uiso H2001 0.9177 1.5281 -0.0554 0.1509 0.5000 Uiso H2002 0.8530 1.4770 -0.0184 0.1509 0.5000 Uiso 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 0.02255(15) 0.02317(13) 0.03211(13) 0.00497(9) 0.00642(11) -0.00431(9) O1 0.053(4) 0.072(4) 0.068(4) 0.019(3) -0.003(3) -0.005(3) C1 0.050(5) 0.032(4) 0.070(5) 0.006(3) 0.011(4) 0.003(3) C2 0.027(4) 0.028(3) 0.087(6) -0.007(3) 0.015(4) -0.004(3) C3 0.060(6) 0.035(4) 0.058(5) -0.014(3) 0.008(4) -0.010(3) C4 0.025(4) 0.029(4) 0.099(6) -0.010(4) 0.012(4) -0.009(3) C5 0.047(5) 0.031(4) 0.071(5) 0.015(3) 0.015(4) -0.001(3) C6 0.055(5) 0.036(3) 0.023(3) 0.003(3) 0.005(3) -0.021(3) C7 0.042(4) 0.031(3) 0.054(4) -0.009(3) 0.012(4) -0.009(3) C8 0.065(6) 0.055(5) 0.027(3) -0.002(3) 0.015(4) -0.025(4) C9 0.051(5) 0.049(4) 0.044(4) 0.011(3) -0.001(4) -0.018(4) C10 0.035(4) 0.034(3) 0.049(4) -0.007(3) 0.004(3) -0.014(3) C11 0.047(5) 0.045(4) 0.039(4) 0.008(3) 0.007(4) -0.008(3) B1 0.021(3) 0.018(3) 0.011(3) 0.000(2) 0.007(2) 0.001(2) C111 0.022(3) 0.017(2) 0.009(2) -0.0006(18) -0.000(2) -0.003(2) C112 0.026(3) 0.021(3) 0.017(3) -0.003(2) 0.006(2) -0.001(2) C113 0.033(3) 0.023(3) 0.012(2) 0.002(2) 0.002(2) 0.003(2) C114 0.039(4) 0.029(3) 0.009(2) -0.002(2) 0.003(2) -0.008(3) C115 0.029(3) 0.021(3) 0.016(3) 0.000(2) 0.009(2) -0.005(2) C116 0.025(3) 0.021(3) 0.012(2) -0.002(2) 0.005(2) 0.001(2) C117 0.038(4) 0.035(3) 0.020(3) 0.007(2) 0.004(3) 0.010(3) C118 0.047(4) 0.032(3) 0.018(3) 0.001(2) 0.017(3) 0.003(3) C121 0.024(3) 0.021(3) 0.007(2) 0.0012(19) 0.006(2) 0.002(2) C122 0.028(3) 0.021(3) 0.012(2) 0.001(2) 0.005(2) 0.001(2) C123 0.036(4) 0.019(3) 0.014(2) -0.003(2) 0.003(2) -0.001(2) C124 0.028(3) 0.027(3) 0.015(3) -0.001(2) 0.002(2) -0.008(2) C125 0.023(3) 0.027(3) 0.009(2) 0.001(2) 0.005(2) -0.004(2) C126 0.024(3) 0.016(2) 0.011(2) -0.0012(18) 0.007(2) -0.003(2) C127 0.048(4) 0.019(3) 0.033(3) -0.001(2) 0.005(3) -0.006(3) C128 0.026(4) 0.034(3) 0.034(3) -0.009(3) 0.003(3) -0.005(3) C131 0.015(3) 0.019(3) 0.013(2) 0.0013(19) 0.006(2) 0.002(2) C132 0.022(3) 0.022(3) 0.017(3) 0.002(2) 0.006(2) -0.000(2) C133 0.021(3) 0.029(3) 0.025(3) 0.008(2) 0.007(3) -0.003(2) C134 0.029(4) 0.020(3) 0.031(3) 0.007(2) 0.006(3) -0.001(2) C135 0.023(3) 0.022(3) 0.025(3) -0.004(2) 0.005(2) -0.000(2) C136 0.017(3) 0.021(3) 0.019(3) -0.003(2) 0.004(2) 0.000(2) C137 0.031(4) 0.047(4) 0.027(3) 0.015(3) -0.001(3) -0.005(3) C138 0.038(4) 0.027(3) 0.037(4) -0.007(3) 0.008(3) -0.008(3) C141 0.020(3) 0.019(3) 0.010(2) 0.0020(19) 0.003(2) 0.001(2) C142 0.022(3) 0.023(3) 0.013(3) 0.001(2) -0.001(2) 0.003(2) C143 0.030(3) 0.028(3) 0.016(3) -0.002(2) 0.009(3) 0.003(2) C144 0.026(3) 0.028(3) 0.023(3) 0.004(2) 0.009(3) 0.004(2) C145 0.024(3) 0.022(3) 0.019(3) 0.003(2) 0.003(2) 0.001(2) C146 0.023(3) 0.020(3) 0.010(2) 0.0020(19) 0.002(2) 0.002(2) C147 0.036(4) 0.056(4) 0.024(3) -0.015(3) 0.009(3) 0.005(3) C148 0.025(4) 0.034(3) 0.031(3) 0.001(3) 0.002(3) -0.001(3) F1 0.066(5) 0.216(9) 0.157(7) 0.146(7) 0.021(5) 0.054(5) F2 0.221(9) 0.175(7) 0.027(3) 0.035(3) 0.020(4) 0.145(7) F3 0.21(1) 0.035(3) 0.160(7) 0.011(4) -0.117(7) 0.021(4) F4 0.058(3) 0.057(2) 0.0253(18) 0.0079(17) 0.0271(19) 0.015(2) F5 0.038(2) 0.050(2) 0.0297(19) -0.0001(16) 0.0108(18) 0.0140(17) F6 0.033(2) 0.039(2) 0.062(3) -0.0081(19) -0.018(2) -0.0056(17) F7 0.321(13) 0.037(3) 0.165(7) -0.004(4) 0.178(9) 0.034(5) F8 0.161(7) 0.025(2) 0.128(5) 0.001(3) -0.078(5) 0.013(3) F9 0.069(4) 0.025(3) 0.234(9) -0.016(3) -0.009(5) -0.011(2) F10 0.032(2) 0.066(3) 0.055(2) -0.002(2) 0.018(2) 0.0078(19) F11 0.072(3) 0.027(2) 0.056(3) -0.0148(17) 0.034(2) -0.0014(19) F12 0.037(2) 0.0316(19) 0.041(2) 0.0081(16) -0.0070(18) 0.0020(15) F13 0.077(5) 0.219(9) 0.039(3) 0.044(4) -0.019(3) -0.026(5) F14 0.55(2) 0.075(4) 0.041(3) 0.036(3) -0.077(7) -0.131(9) F15 0.145(7) 0.23(1) 0.030(3) 0.029(4) 0.029(4) 0.076(7) F16 0.225(9) 0.033(3) 0.065(3) -0.017(2) 0.039(4) -0.057(4) F17 0.092(5) 0.075(4) 0.119(5) -0.060(4) -0.056(4) 0.011(3) F18 0.101(5) 0.097(4) 0.094(4) -0.071(4) 0.060(4) -0.045(3) F19 0.131(6) 0.091(4) 0.071(4) -0.061(3) 0.065(4) -0.046(4) F20 0.119(5) 0.121(5) 0.018(2) -0.003(3) 0.011(3) 0.031(4) F21 0.039(3) 0.202(7) 0.053(3) -0.064(4) 0.013(3) 0.025(4) F22 0.034(3) 0.180(7) 0.052(3) -0.025(3) 0.013(2) -0.041(3) F23 0.049(3) 0.071(3) 0.070(3) -0.043(3) -0.018(3) 0.010(2) F24 0.075(4) 0.064(3) 0.072(3) 0.016(3) -0.046(3) -0.003(3) C100 0.026(4) 0.059(5) 0.067(5) -0.015(4) -0.004(4) 0.003(3) Cl101 0.0438(12) 0.0601(12) 0.0685(13) -0.0090(9) 0.007(1) 0.0051(9) Cl102 0.0379(12) 0.0990(17) 0.0535(11) -0.0169(11) 0.0041(9) -0.001(1) C200 0.109(7) 0.332(11) 0.028(6) -0.013(7) -0.011(6) -0.090(8) Cl201 0.078(4) 0.36(1) 0.0155(18) -0.046(3) -0.003(2) -0.067(5) Cl202 0.121(5) 0.303(9) 0.026(2) 0.029(3) -0.023(3) -0.131(6) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ta1 . C1 . 2.363(7) yes Ta1 . C2 . 2.373(7) yes Ta1 . C3 . 2.364(7) yes Ta1 . C4 . 2.324(7) yes Ta1 . C5 . 2.349(7) yes Ta1 . C6 . 2.374(6) yes Ta1 . C7 . 2.338(6) yes Ta1 . C8 . 2.352(7) yes Ta1 . C9 . 2.361(8) yes Ta1 . C10 . 2.373(7) yes Ta1 . C11 . 2.061(7) yes Ta1 . H1 . 1.75(3) no Ta1 . H2 . 1.75(3) no O1 . C11 . 1.138(9) yes C1 . C2 . 1.390(12) yes C1 . C5 . 1.366(11) yes C1 . H11 . 0.965(9) no C2 . C3 . 1.399(12) yes C2 . H21 . 0.962(7) no C3 . C4 . 1.449(11) yes C3 . H31 . 0.968(8) no C4 . C5 . 1.403(12) yes C4 . H41 . 0.978(8) no C5 . H51 . 0.969(8) no C6 . C7 . 1.43(1) yes C6 . C10 . 1.379(11) yes C6 . H61 . 0.967(6) no C7 . C8 . 1.437(11) yes C7 . H71 . 0.950(8) no C8 . C9 . 1.368(12) yes C8 . H81 . 0.955(7) no C9 . C10 . 1.40(1) yes C9 . H91 . 0.956(8) no C10 . H101 . 0.962(7) no B1 . C111 . 1.642(7) yes B1 . C121 . 1.635(8) yes B1 . C131 . 1.648(7) yes B1 . C141 . 1.642(7) yes C111 . C112 . 1.391(8) yes C111 . C116 . 1.393(8) yes C112 . C113 . 1.397(8) yes C112 . H1121 . 0.964(5) no C113 . C114 . 1.399(9) yes C113 . C117 . 1.491(8) yes C114 . C115 . 1.372(9) yes C114 . H1141 . 0.956(5) no C115 . C116 . 1.398(7) yes C115 . C118 . 1.489(8) yes C116 . H1161 . 0.960(5) no C117 . F1 . 1.31(1) yes C117 . F2 . 1.260(8) yes C117 . F3 . 1.265(9) yes C118 . F4 . 1.341(7) yes C118 . F5 . 1.350(8) yes C118 . F11 . 1.330(7) yes C121 . C122 . 1.400(8) yes C121 . C126 . 1.389(8) yes C122 . C123 . 1.387(8) yes C122 . H1221 . 0.967(6) no C123 . C124 . 1.396(9) yes C123 . C127 . 1.495(8) yes C124 . C125 . 1.380(8) yes C124 . H1241 . 0.960(6) no C125 . C126 . 1.395(8) yes C125 . C128 . 1.499(9) yes C126 . H1261 . 0.960(5) no C127 . F7 . 1.268(9) yes C127 . F8 . 1.285(9) yes C127 . F9 . 1.285(9) yes C128 . F6 . 1.324(7) yes C128 . F10 . 1.348(7) yes C128 . F12 . 1.354(8) yes C131 . C132 . 1.399(8) yes C131 . C136 . 1.399(7) yes C132 . C133 . 1.385(8) yes C132 . H1321 . 0.961(5) no C133 . C134 . 1.380(9) yes C133 . C137 . 1.486(9) yes C134 . C135 . 1.371(9) yes C134 . H1341 . 0.955(5) no C135 . C136 . 1.391(8) yes C135 . C138 . 1.501(8) yes C136 . H1361 . 0.966(5) no C137 . F13 . 1.31(1) yes C137 . F14 . 1.201(9) yes C137 . F15 . 1.34(1) yes C138 . F16 . 1.291(8) yes C138 . F17 . 1.31(1) yes C138 . F18 . 1.310(9) yes C141 . C142 . 1.390(7) yes C141 . C146 . 1.394(8) yes C142 . C143 . 1.387(8) yes C142 . H1421 . 0.961(6) no C143 . C144 . 1.382(9) yes C143 . C147 . 1.499(8) yes C144 . C145 . 1.380(8) yes C144 . H1441 . 0.961(6) no C145 . C146 . 1.391(8) yes C145 . C148 . 1.502(9) yes C146 . H1461 . 0.959(5) no C147 . F19 . 1.310(9) yes C147 . F20 . 1.310(9) yes C147 . F21 . 1.329(8) yes C148 . F22 . 1.326(8) yes C148 . F23 . 1.298(8) yes C148 . F24 . 1.325(8) yes C100 . Cl101 . 1.758(9) yes C100 . Cl102 . 1.763(8) yes C100 . H1001 . 0.958(8) no C100 . H1002 . 0.955(8) no C200 . Cl201 . 1.749(12) yes C200 . Cl202 . 1.652(13) yes C200 . H2001 . 1.00(2) no C200 . H2002 . 0.95(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Ta1 . C2 . 34.1(3) yes C1 . Ta1 . C3 . 56.9(3) yes C2 . Ta1 . C3 . 34.3(3) yes C1 . Ta1 . C4 . 56.5(3) yes C2 . Ta1 . C4 . 57.9(2) yes C3 . Ta1 . C4 . 36.0(3) yes C1 . Ta1 . C5 . 33.7(3) yes C2 . Ta1 . C5 . 57.7(3) yes C3 . Ta1 . C5 . 58.8(3) yes C4 . Ta1 . C5 . 34.9(3) yes C1 . Ta1 . C6 . 130.0(3) yes C2 . Ta1 . C6 . 111.0(3) yes C3 . Ta1 . C6 . 120.1(3) yes C4 . Ta1 . C6 . 152.9(3) yes C5 . Ta1 . C6 . 163.2(3) yes C1 . Ta1 . C7 . 142.6(3) yes C2 . Ta1 . C7 . 143.4(2) yes C3 . Ta1 . C7 . 152.4(3) yes C4 . Ta1 . C7 . 157.8(3) yes C5 . Ta1 . C7 . 148.8(3) yes C1 . Ta1 . C8 . 108.7(3) yes C2 . Ta1 . C8 . 127.2(3) yes C3 . Ta1 . C8 . 161.5(3) yes C4 . Ta1 . C8 . 149.1(3) yes C5 . Ta1 . C8 . 117.0(3) yes C1 . Ta1 . C9 . 85.6(3) yes C2 . Ta1 . C9 . 94.5(3) yes C3 . Ta1 . C9 . 128.1(3) yes C4 . Ta1 . C9 . 141.7(3) yes C5 . Ta1 . C9 . 109.4(3) yes C1 . Ta1 . C10 . 96.6(3) yes C2 . Ta1 . C10 . 85.6(2) yes C3 . Ta1 . C10 . 109.9(3) yes C4 . Ta1 . C10 . 143.2(2) yes C5 . Ta1 . C10 . 129.4(3) yes C1 . Ta1 . C11 . 132.5(3) yes C2 . Ta1 . C11 . 105.9(3) yes C3 . Ta1 . C11 . 76.1(3) yes C4 . Ta1 . C11 . 82.4(3) yes C5 . Ta1 . C11 . 116.5(3) yes C1 . Ta1 . H1 . 95.6(19) no C2 . Ta1 . H1 . 127.2(20) no C3 . Ta1 . H1 . 119.9(20) no C4 . Ta1 . H1 . 83.9(20) no C5 . Ta1 . H1 . 70.0(20) no C1 . Ta1 . H2 . 117.0(22) no C2 . Ta1 . H2 . 133.8(23) no C3 . Ta1 . H2 . 105.9(23) no C4 . Ta1 . H2 . 76.0(23) no C5 . Ta1 . H2 . 83.7(23) no C6 . Ta1 . C7 . 35.3(2) yes C6 . Ta1 . C8 . 57.9(2) yes C7 . Ta1 . C8 . 35.7(3) yes C6 . Ta1 . C9 . 56.7(2) yes C7 . Ta1 . C9 . 57.7(3) yes C8 . Ta1 . C9 . 33.7(3) yes C6 . Ta1 . C10 . 33.8(3) yes C7 . Ta1 . C10 . 57.8(3) yes C8 . Ta1 . C10 . 57.1(3) yes C9 . Ta1 . C10 . 34.3(2) yes C6 . Ta1 . C11 . 77.3(3) yes C7 . Ta1 . C11 . 83.5(3) yes C8 . Ta1 . C11 . 118.6(3) yes C9 . Ta1 . C11 . 133.9(3) yes C10 . Ta1 . C11 . 105.6(3) yes C6 . Ta1 . H1 . 118.0(20) no C7 . Ta1 . H1 . 82.6(20) no C8 . Ta1 . H1 . 70.0(20) no C9 . Ta1 . H1 . 96.1(20) no C10 . Ta1 . H1 . 126.9(20) no C6 . Ta1 . H2 . 111.5(23) no C7 . Ta1 . H2 . 82.7(24) no C8 . Ta1 . H2 . 90.9(22) no C9 . Ta1 . H2 . 123.9(21) no C10 . Ta1 . H2 . 140.5(24) no C11 . Ta1 . H1 . 103.1(19) no C11 . Ta1 . H2 . 67.4(19) no H1 . Ta1 . H2 . 35.9(8) no Ta1 . C1 . C2 . 73.3(4) yes Ta1 . C1 . C5 . 72.6(4) yes C2 . C1 . C5 . 111.5(8) yes Ta1 . C1 . H11 . 122.5(6) no C2 . C1 . H11 . 124.2(8) no C5 . C1 . H11 . 124.3(8) no Ta1 . C2 . C1 . 72.5(4) yes Ta1 . C2 . C3 . 72.5(4) yes C1 . C2 . C3 . 107.6(6) yes Ta1 . C2 . H21 . 120.6(5) no C1 . C2 . H21 . 126.2(9) no C3 . C2 . H21 . 126.3(9) no Ta1 . C3 . C2 . 73.2(4) yes Ta1 . C3 . C4 . 70.5(4) yes C2 . C3 . C4 . 105.9(7) yes Ta1 . C3 . H31 . 121.6(5) no C2 . C3 . H31 . 127.8(8) no C4 . C3 . H31 . 126.3(9) no Ta1 . C4 . C3 . 73.5(4) yes Ta1 . C4 . C5 . 73.5(4) yes C3 . C4 . C5 . 108.5(7) yes Ta1 . C4 . H41 . 119.2(5) no C3 . C4 . H41 . 125.6(9) no C5 . C4 . H41 . 125.8(8) no Ta1 . C5 . C1 . 73.7(4) yes Ta1 . C5 . C4 . 71.5(4) yes C1 . C5 . C4 . 106.4(7) yes Ta1 . C5 . H51 . 120.3(6) no C1 . C5 . H51 . 126.6(9) no C4 . C5 . H51 . 127.0(8) no Ta1 . C6 . C7 . 70.9(4) yes Ta1 . C6 . C10 . 73.1(4) yes C7 . C6 . C10 . 108.3(6) yes Ta1 . C6 . H61 . 120.6(5) no C7 . C6 . H61 . 125.1(8) no C10 . C6 . H61 . 126.6(7) no Ta1 . C7 . C6 . 73.7(4) yes Ta1 . C7 . C8 . 72.7(4) yes C6 . C7 . C8 . 105.9(7) yes Ta1 . C7 . H71 . 119.5(5) no C6 . C7 . H71 . 127.4(7) no C8 . C7 . H71 . 126.7(7) no Ta1 . C8 . C7 . 71.6(4) yes Ta1 . C8 . C9 . 73.5(4) yes C7 . C8 . C9 . 107.9(6) yes Ta1 . C8 . H81 . 120.2(5) no C7 . C8 . H81 . 126.2(9) no C9 . C8 . H81 . 125.9(8) no Ta1 . C9 . C8 . 72.8(5) yes Ta1 . C9 . C10 . 73.3(4) yes C8 . C9 . C10 . 109.7(7) yes Ta1 . C9 . H91 . 121.1(5) no C8 . C9 . H91 . 124.7(8) no C10 . C9 . H91 . 125.7(9) no Ta1 . C10 . C6 . 73.1(4) yes Ta1 . C10 . C9 . 72.4(4) yes C6 . C10 . C9 . 108.2(7) yes Ta1 . C10 . H101 . 121.1(5) no C6 . C10 . H101 . 126.5(7) no C9 . C10 . H101 . 125.3(8) no Ta1 . C11 . O1 . 179.8(7) yes C111 . B1 . C121 . 104.4(4) yes C111 . B1 . C131 . 111.0(4) yes C121 . B1 . C131 . 112.9(4) yes C111 . B1 . C141 . 113.3(4) yes C121 . B1 . C141 . 113.3(4) yes C131 . B1 . C141 . 102.2(4) yes B1 . C111 . C112 . 123.3(4) yes B1 . C111 . C116 . 119.7(5) yes C112 . C111 . C116 . 116.6(4) yes C111 . C112 . C113 . 121.5(5) yes C111 . C112 . H1121 . 119.8(5) no C113 . C112 . H1121 . 118.6(6) no C112 . C113 . C114 . 120.7(5) yes C112 . C113 . C117 . 119.9(5) yes C114 . C113 . C117 . 119.4(5) yes C113 . C114 . C115 . 118.2(5) yes C113 . C114 . H1141 . 121.0(6) no C115 . C114 . H1141 . 120.8(6) no C114 . C115 . C116 . 120.7(5) yes C114 . C115 . C118 . 121.2(5) yes C116 . C115 . C118 . 118.1(5) yes C111 . C116 . C115 . 122.1(5) yes C111 . C116 . H1161 . 118.8(5) no C115 . C116 . H1161 . 119.1(5) no C113 . C117 . F1 . 112.7(6) yes C113 . C117 . F2 . 115.1(6) yes F1 . C117 . F2 . 105.1(8) yes C113 . C117 . F3 . 114.7(6) yes F1 . C117 . F3 . 100.8(8) yes F2 . C117 . F3 . 107.1(8) yes C115 . C118 . F4 . 113.1(5) yes C115 . C118 . F5 . 112.7(5) yes F4 . C118 . F5 . 106.1(5) yes C115 . C118 . F11 . 112.8(5) yes F4 . C118 . F11 . 105.9(5) yes F5 . C118 . F11 . 105.6(5) yes B1 . C121 . C122 . 121.0(5) yes B1 . C121 . C126 . 122.7(4) yes C122 . C121 . C126 . 115.9(5) yes C121 . C122 . C123 . 122.1(5) yes C121 . C122 . H1221 . 119.1(5) no C123 . C122 . H1221 . 118.8(5) no C122 . C123 . C124 . 120.9(5) yes C122 . C123 . C127 . 120.5(6) yes C124 . C123 . C127 . 118.6(5) yes C123 . C124 . C125 . 117.7(5) yes C123 . C124 . H1241 . 121.2(5) no C125 . C124 . H1241 . 121.1(6) no C124 . C125 . C126 . 120.8(5) yes C124 . C125 . C128 . 120.0(5) yes C126 . C125 . C128 . 119.2(5) yes C121 . C126 . C125 . 122.4(5) yes C121 . C126 . H1261 . 119.1(5) no C125 . C126 . H1261 . 118.4(5) no C123 . C127 . F7 . 112.2(5) yes C123 . C127 . F8 . 112.8(5) yes F7 . C127 . F8 . 105.7(8) yes C123 . C127 . F9 . 114.4(6) yes F7 . C127 . F9 . 104.6(8) yes F8 . C127 . F9 . 106.3(7) yes C125 . C128 . F6 . 113.8(5) yes C125 . C128 . F10 . 112.3(5) yes F6 . C128 . F10 . 107.4(5) yes C125 . C128 . F12 . 111.9(5) yes F6 . C128 . F12 . 106.5(5) yes F10 . C128 . F12 . 104.2(5) yes B1 . C131 . C132 . 121.9(4) yes B1 . C131 . C136 . 122.4(4) yes C132 . C131 . C136 . 115.3(5) yes C131 . C132 . C133 . 122.6(5) yes C131 . C132 . H1321 . 118.4(5) no C133 . C132 . H1321 . 119.0(5) no C132 . C133 . C134 . 120.6(5) yes C132 . C133 . C137 . 120.1(5) yes C134 . C133 . C137 . 119.3(5) yes C133 . C134 . C135 . 118.3(5) yes C133 . C134 . H1341 . 121.3(6) no C135 . C134 . H1341 . 120.4(6) no C134 . C135 . C136 . 121.2(5) yes C134 . C135 . C138 . 119.9(5) yes C136 . C135 . C138 . 118.8(5) yes C131 . C136 . C135 . 121.9(5) yes C131 . C136 . H1361 . 118.8(5) no C135 . C136 . H1361 . 119.3(5) no C133 . C137 . F13 . 113.1(5) yes C133 . C137 . F14 . 117.3(6) yes F13 . C137 . F14 . 111.4(9) yes C133 . C137 . F15 . 112.2(6) yes F13 . C137 . F15 . 94.9(7) yes F14 . C137 . F15 . 105.3(9) yes C135 . C138 . F16 . 113.9(6) yes C135 . C138 . F17 . 113.5(6) yes F16 . C138 . F17 . 106.0(7) yes C135 . C138 . F18 . 111.9(6) yes F16 . C138 . F18 . 107.7(6) yes F17 . C138 . F18 . 103.1(7) yes B1 . C141 . C142 . 122.4(5) yes B1 . C141 . C146 . 121.1(4) yes C142 . C141 . C146 . 116.1(5) yes C141 . C142 . C143 . 121.8(5) yes C141 . C142 . H1421 . 119.0(5) no C143 . C142 . H1421 . 119.3(5) no C142 . C143 . C144 . 121.5(5) yes C142 . C143 . C147 . 118.0(6) yes C144 . C143 . C147 . 120.6(5) yes C143 . C144 . C145 . 117.7(5) yes C143 . C144 . H1441 . 120.5(5) no C145 . C144 . H1441 . 121.7(6) no C144 . C145 . C146 . 120.7(5) yes C144 . C145 . C148 . 120.4(5) yes C146 . C145 . C148 . 118.8(5) yes C141 . C146 . C145 . 122.2(5) yes C141 . C146 . H1461 . 118.5(5) no C145 . C146 . H1461 . 119.3(5) no C143 . C147 . F19 . 112.7(6) yes C143 . C147 . F20 . 113.0(6) yes F19 . C147 . F20 . 105.8(7) yes C143 . C147 . F21 . 113.1(6) yes F19 . C147 . F21 . 106.5(7) yes F20 . C147 . F21 . 105.1(6) yes C145 . C148 . F22 . 112.6(5) yes C145 . C148 . F23 . 114.3(5) yes F22 . C148 . F23 . 106.4(6) yes C145 . C148 . F24 . 111.4(5) yes F22 . C148 . F24 . 105.2(7) yes F23 . C148 . F24 . 106.3(6) yes Cl101 . C100 . Cl102 . 111.7(4) yes Cl101 . C100 . H1001 . 108.7(7) no Cl102 . C100 . H1001 . 108.7(7) no Cl101 . C100 . H1002 . 108.8(7) no Cl102 . C100 . H1002 . 108.8(6) no H1001 . C100 . H1002 . 110.1(7) no Cl201 . C200 . Cl202 . 108.8(5) yes Cl201 . C200 . H2001 . 102.2(15) no Cl202 . C200 . H2001 . 115.7(17) no Cl201 . C200 . H2002 . 100.0(13) no Cl202 . C200 . H2002 . 120.5(20) no H2001 . C200 . H2002 . 106.9(11) no