Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name ' Moshe Kol' 'Israel Goldberg' 'Zeev Goldschmidt' 'Stanislav Groysman' 'Einat Hayut-Salant' 'Sharon Segal' 'Marina Shamis' _publ_contact_author_name 'Dr. M. Kol' _publ_contact_author_address ; Department of Chemistry Tel Aviv University Ramat Aviv Tel Aviv 69978 ISRAEL ; _publ_contact_author_email MOSHEKOL@POST.TAU.AC.IL #Crystallographic Information Files data_mk46 '1a' _database_code_CSD 189674 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C31 H40 N O5 Ta).1/2(C5 H12)' _chemical_formula_sum 'C33.50 H46 N O5 Ta' _chemical_formula_weight 723.66 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' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0690(2) _cell_length_b 20.5620(7) _cell_length_c 9.4240(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.849(2) _cell_angle_gamma 90.00 _cell_volume 3268.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 7547 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 28.27 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 3.402 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 degree Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7547 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7547 _reflns_number_gt 6303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'DIRDIF-96' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Scattered peaks C38 through C41 represent the location of a heavily disordered pentane solvent trapped in the crystal lattice. ; _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^)+(0.0440P)^2^+11.5442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7547 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.140 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta 0.177632(12) 0.077966(9) 0.09710(2) 0.02769(8) Uani 1 1 d . . . O1 O 0.1310(2) 0.01142(19) -0.0209(4) 0.0407(9) Uani 1 1 d . . . O2 O 0.1554(2) 0.04585(18) 0.2788(4) 0.0339(8) Uani 1 1 d . . . O3 O 0.2836(2) 0.04287(16) 0.1472(4) 0.0285(7) Uani 1 1 d . . . O4 O 0.2208(2) 0.12486(17) -0.0579(4) 0.0290(7) Uani 1 1 d . . . O5 O 0.0867(2) 0.13504(17) 0.0739(4) 0.0320(8) Uani 1 1 d . . . N6 N 0.2404(2) 0.16847(19) 0.2291(4) 0.0244(8) Uani 1 1 d . . . C7 C 0.2944(3) 0.1434(2) 0.3597(5) 0.0259(9) Uani 1 1 d . . . H7A H 0.3136 0.1802 0.4197 0.031 Uiso 1 1 calc R . . H7B H 0.2636 0.1162 0.4146 0.031 Uiso 1 1 calc R . . C8 C 0.2860(3) 0.2150(2) 0.1494(5) 0.0250(9) Uani 1 1 d . . . H8A H 0.2486 0.2457 0.0984 0.030 Uiso 1 1 calc R . . H8B H 0.3218 0.2395 0.2195 0.030 Uiso 1 1 calc R . . C9 C 0.1776(3) 0.2082(2) 0.2877(5) 0.0278(10) Uani 1 1 d . . . H9A H 0.1493 0.1802 0.3453 0.033 Uiso 1 1 calc R . . H9B H 0.2035 0.2419 0.3501 0.033 Uiso 1 1 calc R . . C10 C 0.3556(3) 0.0560(2) 0.2232(5) 0.0265(10) Uani 1 1 d . . . C11 C 0.4213(3) 0.0201(2) 0.1944(6) 0.0309(11) Uani 1 1 d . . . C12 C 0.4942(3) 0.0325(2) 0.2752(6) 0.0333(11) Uani 1 1 d . . . H12 H 0.5379 0.0088 0.2567 0.040 Uiso 1 1 calc R . . C13 C 0.5049(3) 0.0792(3) 0.3838(6) 0.0348(11) Uani 1 1 d . . . C14 C 0.4396(3) 0.1159(2) 0.4061(5) 0.0296(10) Uani 1 1 d . . . H14 H 0.4461 0.1485 0.4752 0.035 Uiso 1 1 calc R . . C15 C 0.3646(3) 0.1050(2) 0.3276(5) 0.0261(9) Uani 1 1 d . . . C16 C 0.2967(3) 0.1434(2) -0.0621(5) 0.0265(10) Uani 1 1 d . . . C17 C 0.3374(3) 0.1201(2) -0.1695(5) 0.0304(11) Uani 1 1 d . . . C18 C 0.4144(3) 0.1424(2) -0.1718(6) 0.0332(11) Uani 1 1 d . . . H18 H 0.4413 0.1283 -0.2448 0.040 Uiso 1 1 calc R . . C19 C 0.4523(3) 0.1847(3) -0.0689(6) 0.0343(11) Uani 1 1 d . . . C20 C 0.4112(3) 0.2056(2) 0.0395(5) 0.0288(10) Uani 1 1 d . . . H20 H 0.4362 0.2332 0.1107 0.035 Uiso 1 1 calc R . . C21 C 0.3336(3) 0.1861(2) 0.0434(5) 0.0257(10) Uani 1 1 d . . . C22 C 0.0723(3) 0.2004(2) 0.0719(5) 0.0292(10) Uani 1 1 d . . . C23 C 0.0132(3) 0.2270(3) -0.0311(5) 0.0338(11) Uani 1 1 d . . . C24 C 0.0042(3) 0.2942(3) -0.0322(6) 0.0345(11) Uani 1 1 d . . . H24 H -0.0347 0.3126 -0.1003 0.041 Uiso 1 1 calc R . . C25 C 0.0501(3) 0.3348(3) 0.0626(6) 0.0339(11) Uani 1 1 d . . . C26 C 0.1080(3) 0.3066(3) 0.1670(5) 0.0310(11) Uani 1 1 d . . . H26 H 0.1394 0.3331 0.2328 0.037 Uiso 1 1 calc R . . C27 C 0.1189(3) 0.2394(2) 0.1724(5) 0.0275(10) Uani 1 1 d . . . C28 C 0.4094(4) -0.0300(3) 0.0764(6) 0.0395(13) Uani 1 1 d . . . H28A H 0.4595 -0.0490 0.0659 0.059 Uiso 1 1 calc R . . H28B H 0.3868 -0.0096 -0.0121 0.059 Uiso 1 1 calc R . . H28C H 0.3742 -0.0633 0.1003 0.059 Uiso 1 1 calc R . . C29 C 0.5846(4) 0.0900(3) 0.4739(7) 0.0445(14) Uani 1 1 d . . . H29A H 0.5845 0.1307 0.5235 0.067 Uiso 1 1 calc R . . H29B H 0.6249 0.0907 0.4130 0.067 Uiso 1 1 calc R . . H29C H 0.5954 0.0554 0.5425 0.067 Uiso 1 1 calc R . . C30 C 0.2972(4) 0.0733(3) -0.2804(6) 0.0377(12) Uani 1 1 d . . . H30A H 0.3326 0.0625 -0.3467 0.056 Uiso 1 1 calc R . . H30B H 0.2502 0.0931 -0.3315 0.056 Uiso 1 1 calc R . . H30C H 0.2831 0.0345 -0.2337 0.056 Uiso 1 1 calc R . . C31 C 0.5356(3) 0.2084(3) -0.0741(8) 0.0458(15) Uani 1 1 d . . . H31A H 0.5573 0.1853 -0.1474 0.069 Uiso 1 1 calc R . . H31B H 0.5679 0.2010 0.0172 0.069 Uiso 1 1 calc R . . H31C H 0.5344 0.2541 -0.0953 0.069 Uiso 1 1 calc R . . C32 C -0.0382(3) 0.1834(3) -0.1329(6) 0.0407(13) Uani 1 1 d . . . H32A H -0.0809 0.1671 -0.0875 0.061 Uiso 1 1 calc R . . H32B H -0.0073 0.1476 -0.1593 0.061 Uiso 1 1 calc R . . H32C H -0.0595 0.2074 -0.2174 0.061 Uiso 1 1 calc R . . C33 C 0.0397(4) 0.4082(3) 0.0562(7) 0.0455(14) Uani 1 1 d . . . H33A H 0.0587 0.4247 -0.0275 0.068 Uiso 1 1 calc R . . H33B H 0.0694 0.4274 0.1406 0.068 Uiso 1 1 calc R . . H33C H -0.0154 0.4187 0.0514 0.068 Uiso 1 1 calc R . . C34 C 0.1911(4) -0.0019(3) 0.3784(6) 0.0365(12) Uani 1 1 d . . . H34A H 0.1682 0.0011 0.4662 0.044 Uiso 1 1 calc R . . H34B H 0.2474 0.0069 0.4020 0.044 Uiso 1 1 calc R . . C35 C 0.1795(5) -0.0691(3) 0.3194(8) 0.0587(19) Uani 1 1 d . . . H35A H 0.1242 -0.0763 0.2854 0.088 Uiso 1 1 calc R . . H35B H 0.1977 -0.1001 0.3935 0.088 Uiso 1 1 calc R . . H35C H 0.2091 -0.0743 0.2414 0.088 Uiso 1 1 calc R . . C36 C 0.0685(8) -0.0273(5) -0.0844(10) 0.112(5) Uani 1 1 d . . . H36A H 0.0490 -0.0521 -0.0095 0.134 Uiso 1 1 calc R . . H36B H 0.0258 0.0009 -0.1274 0.134 Uiso 1 1 calc R . . C37 C 0.0854(10) -0.0691(7) -0.1855(18) 0.146(6) Uiso 1 1 d . . . H37A H 0.0741 -0.0488 -0.2783 0.219 Uiso 1 1 calc R . . H37B H 0.0535 -0.1075 -0.1843 0.219 Uiso 1 1 calc R . . H37C H 0.1405 -0.0806 -0.1662 0.219 Uiso 1 1 calc R . . C38 C 0.2511(13) 0.7327(11) 0.106(2) 0.091(6) Uiso 0.50 1 d P . . C39 C 0.2428(16) 0.7769(13) -0.009(3) 0.117(8) Uiso 0.50 1 d P . . C40 C 0.2537(17) 0.7547(14) -0.182(3) 0.130(9) Uiso 0.50 1 d P . . C41 C 0.250(2) 0.6999(19) 0.221(4) 0.079(10) Uiso 0.25 1 d P . . 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 Ta 0.02916(12) 0.02664(11) 0.02707(12) -0.00295(8) 0.00369(8) -0.00596(8) O1 0.037(2) 0.040(2) 0.043(2) -0.0059(17) 0.0017(17) -0.0132(17) O2 0.0309(19) 0.034(2) 0.037(2) 0.0004(15) 0.0077(16) -0.0041(15) O3 0.0309(18) 0.0269(17) 0.0271(18) -0.0038(13) 0.0020(14) -0.0018(14) O4 0.0285(18) 0.0332(18) 0.0247(17) -0.0026(13) 0.0025(14) -0.0036(14) O5 0.0254(18) 0.0355(19) 0.0335(19) -0.0009(14) -0.0002(15) -0.0044(15) N6 0.0217(19) 0.028(2) 0.024(2) -0.0010(15) 0.0040(15) 0.0002(15) C7 0.028(2) 0.028(2) 0.022(2) -0.0002(17) 0.0017(19) 0.0013(19) C8 0.025(2) 0.024(2) 0.026(2) 0.0000(17) 0.0046(18) -0.0001(18) C9 0.026(2) 0.033(2) 0.024(2) -0.0035(19) 0.0045(19) 0.002(2) C10 0.032(3) 0.023(2) 0.025(2) 0.0048(17) 0.0047(19) -0.0017(19) C11 0.035(3) 0.027(2) 0.032(3) 0.0040(19) 0.009(2) 0.001(2) C12 0.033(3) 0.031(3) 0.038(3) 0.006(2) 0.011(2) 0.008(2) C13 0.036(3) 0.031(3) 0.037(3) 0.009(2) 0.004(2) 0.003(2) C14 0.032(3) 0.029(2) 0.027(2) 0.0026(18) 0.001(2) -0.002(2) C15 0.030(2) 0.024(2) 0.025(2) 0.0041(18) 0.0062(19) 0.0010(19) C16 0.026(2) 0.024(2) 0.029(2) 0.0054(18) 0.0047(19) -0.0009(18) C17 0.043(3) 0.024(2) 0.024(2) 0.0038(18) 0.006(2) 0.006(2) C18 0.044(3) 0.027(2) 0.031(3) 0.001(2) 0.016(2) 0.007(2) C19 0.031(3) 0.031(3) 0.043(3) 0.007(2) 0.012(2) 0.005(2) C20 0.031(3) 0.025(2) 0.030(3) 0.0015(18) 0.003(2) 0.0001(19) C21 0.029(2) 0.022(2) 0.027(2) 0.0032(17) 0.0056(19) 0.0008(18) C22 0.026(2) 0.033(3) 0.030(3) -0.0019(19) 0.008(2) -0.002(2) C23 0.025(2) 0.050(3) 0.027(3) 0.001(2) 0.005(2) -0.004(2) C24 0.027(3) 0.046(3) 0.030(3) 0.004(2) 0.003(2) 0.007(2) C25 0.028(3) 0.043(3) 0.032(3) 0.003(2) 0.010(2) 0.007(2) C26 0.028(3) 0.040(3) 0.025(3) -0.004(2) 0.006(2) 0.001(2) C27 0.024(2) 0.033(2) 0.026(2) -0.0002(19) 0.0061(19) 0.0033(19) C28 0.044(3) 0.034(3) 0.041(3) -0.007(2) 0.008(3) 0.010(2) C29 0.034(3) 0.042(3) 0.056(4) 0.004(3) 0.000(3) 0.003(2) C30 0.054(4) 0.035(3) 0.024(3) -0.004(2) 0.009(2) 0.002(2) C31 0.035(3) 0.041(3) 0.066(4) 0.002(3) 0.022(3) 0.001(2) C32 0.027(3) 0.059(4) 0.035(3) -0.001(3) 0.002(2) -0.004(3) C33 0.041(3) 0.043(3) 0.052(4) 0.004(3) 0.006(3) 0.012(3) C34 0.046(3) 0.032(3) 0.032(3) 0.006(2) 0.007(2) -0.005(2) C35 0.082(5) 0.033(3) 0.058(4) 0.001(3) 0.000(4) -0.010(3) C36 0.155(11) 0.097(7) 0.068(6) 0.013(5) -0.031(6) -0.076(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta O1 1.863(4) . ? Ta O2 1.927(4) . ? Ta O5 1.931(4) . ? Ta O3 1.938(3) . ? Ta O4 1.984(3) . ? Ta N6 2.398(4) . ? O1 C36 1.391(9) . ? O2 C34 1.429(6) . ? O3 C10 1.350(6) . ? O4 C16 1.358(6) . ? O5 C22 1.366(6) . ? N6 C8 1.505(6) . ? N6 C7 1.510(6) . ? N6 C9 1.518(6) . ? C7 C15 1.504(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C21 1.503(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C27 1.504(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C15 1.401(7) . ? C10 C11 1.404(7) . ? C11 C12 1.379(8) . ? C11 C28 1.506(7) . ? C12 C13 1.395(8) . ? C12 H12 0.9300 . ? C13 C14 1.388(7) . ? C13 C29 1.506(8) . ? C14 C15 1.395(7) . ? C14 H14 0.9300 . ? C16 C17 1.397(7) . ? C16 C21 1.401(7) . ? C17 C18 1.395(8) . ? C17 C30 1.506(7) . ? C18 C19 1.387(8) . ? C18 H18 0.9300 . ? C19 C20 1.393(7) . ? C19 C31 1.511(7) . ? C20 C21 1.390(7) . ? C20 H20 0.9300 . ? C22 C27 1.393(7) . ? C22 C23 1.398(7) . ? C23 C24 1.390(8) . ? C23 C32 1.496(7) . ? C24 C25 1.376(8) . ? C24 H24 0.9300 . ? C25 C26 1.408(7) . ? C25 C33 1.519(8) . ? C26 C27 1.394(7) . ? C26 H26 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.491(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C37 1.346(17) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? 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 O1 Ta O2 98.87(16) . . ? O1 Ta O5 96.69(16) . . ? O2 Ta O5 92.52(15) . . ? O1 Ta O3 99.74(16) . . ? O2 Ta O3 87.70(15) . . ? O5 Ta O3 163.34(14) . . ? O1 Ta O4 95.18(16) . . ? O2 Ta O4 165.26(14) . . ? O5 Ta O4 90.23(15) . . ? O3 Ta O4 85.55(14) . . ? O1 Ta N6 174.66(15) . . ? O2 Ta N6 86.46(14) . . ? O5 Ta N6 82.79(14) . . ? O3 Ta N6 80.59(13) . . ? O4 Ta N6 79.52(13) . . ? C36 O1 Ta 155.1(7) . . ? C34 O2 Ta 134.2(3) . . ? C10 O3 Ta 142.5(3) . . ? C16 O4 Ta 128.4(3) . . ? C22 O5 Ta 137.6(3) . . ? C8 N6 C7 109.0(4) . . ? C8 N6 C9 106.7(4) . . ? C7 N6 C9 105.3(3) . . ? C8 N6 Ta 117.3(3) . . ? C7 N6 Ta 109.0(3) . . ? C9 N6 Ta 108.8(3) . . ? C15 C7 N6 114.9(4) . . ? C15 C7 H7A 108.6 . . ? N6 C7 H7A 108.6 . . ? C15 C7 H7B 108.6 . . ? N6 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? C21 C8 N6 117.0(4) . . ? C21 C8 H8A 108.1 . . ? N6 C8 H8A 108.1 . . ? C21 C8 H8B 108.1 . . ? N6 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C27 C9 N6 113.4(4) . . ? C27 C9 H9A 108.9 . . ? N6 C9 H9A 108.9 . . ? C27 C9 H9B 108.9 . . ? N6 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? O3 C10 C15 120.6(4) . . ? O3 C10 C11 118.7(4) . . ? C15 C10 C11 120.6(5) . . ? C12 C11 C10 118.4(5) . . ? C12 C11 C28 122.8(5) . . ? C10 C11 C28 118.8(5) . . ? C11 C12 C13 122.5(5) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C12 117.9(5) . . ? C14 C13 C29 120.7(5) . . ? C12 C13 C29 121.3(5) . . ? C13 C14 C15 121.7(5) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 118.7(5) . . ? C14 C15 C7 120.3(4) . . ? C10 C15 C7 120.9(4) . . ? O4 C16 C17 120.6(4) . . ? O4 C16 C21 118.8(4) . . ? C17 C16 C21 120.7(5) . . ? C18 C17 C16 118.3(5) . . ? C18 C17 C30 121.9(5) . . ? C16 C17 C30 119.8(5) . . ? C19 C18 C17 122.3(5) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 118.2(5) . . ? C18 C19 C31 121.3(5) . . ? C20 C19 C31 120.4(5) . . ? C21 C20 C19 121.3(5) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C16 119.2(5) . . ? C20 C21 C8 121.2(4) . . ? C16 C21 C8 119.4(4) . . ? O5 C22 C27 118.4(4) . . ? O5 C22 C23 120.2(5) . . ? C27 C22 C23 121.4(5) . . ? C24 C23 C22 117.5(5) . . ? C24 C23 C32 122.5(5) . . ? C22 C23 C32 120.0(5) . . ? C25 C24 C23 123.1(5) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 C26 118.2(5) . . ? C24 C25 C33 121.7(5) . . ? C26 C25 C33 120.1(5) . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C22 119.2(5) . . ? C26 C27 C9 121.3(4) . . ? C22 C27 C9 119.5(4) . . ? C11 C28 H28A 109.5 . . ? C11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C13 C29 H29A 109.5 . . ? C13 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C13 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C17 C30 H30A 109.5 . . ? C17 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C17 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C19 C31 H31A 109.5 . . ? C19 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C19 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 C32 H32A 109.5 . . ? C23 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C23 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C33 H33A 109.5 . . ? C25 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C25 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C34 C35 111.9(5) . . ? O2 C34 H34A 109.2 . . ? C35 C34 H34A 109.2 . . ? O2 C34 H34B 109.2 . . ? C35 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 O1 115.9(13) . . ? C37 C36 H36A 108.3 . . ? O1 C36 H36A 108.3 . . ? C37 C36 H36B 108.3 . . ? O1 C36 H36B 108.3 . . ? H36A C36 H36B 107.4 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.114 _refine_diff_density_min -2.076 _refine_diff_density_rms 0.140 #=================================================================END #Revised Crystallographic Information File for 1b data_mk47a '1b' _database_code_CSD 189675 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C29 H35 Cl N O4 Ta).(C5 H12)' _chemical_formula_sum 'C34 H47 Cl N O4 Ta' _chemical_formula_weight 750.13 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' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.1150(4) _cell_length_b 20.2450(10) _cell_length_c 9.5900(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.766(4) _cell_angle_gamma 90.00 _cell_volume 3321.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used '6046' _cell_measurement_theta_min '2.01' _cell_measurement_theta_max '25.64' _exptl_crystal_description ? _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.426 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3411 _exptl_absorpt_correction_T_max 0.6275 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '1 degree phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6046 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.64 _reflns_number_total 6046 _reflns_number_gt 4940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B. V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'DIRDIF-96' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0446P)^2^+32.3659P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6046 _refine_ls_number_parameters 377 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 1.578 _refine_ls_shift/su_mean 0.065 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta 0.161351(14) 0.084420(10) 0.05680(2) 0.02637(6) Uani 1 1 d . . . Cl2 Cl 0.11213(9) 0.04970(7) 0.27674(15) 0.0389(4) Uani 1 1 d . . . O3 O 0.2580(2) 0.04179(18) 0.1053(4) 0.0302(10) Uani 1 1 d . . . O4 O 0.2142(2) 0.12785(18) -0.0954(4) 0.0299(10) Uani 1 1 d . . . O5 O 0.0773(2) 0.14658(17) 0.0374(4) 0.0260(9) Uani 1 1 d . . . O1 O 0.1138(2) 0.0153(2) -0.0425(4) 0.0400(11) Uani 1 1 d . . . N6 N 0.2241(2) 0.1718(2) 0.1867(4) 0.0195(10) Uani 1 1 d . . . C7 C 0.1624(3) 0.2146(2) 0.2522(5) 0.0227(12) Uani 1 1 d . . . H7A H 0.1891 0.2488 0.3101 0.027 Uiso 1 1 calc R . . H7B H 0.1316 0.1867 0.3151 0.027 Uiso 1 1 calc R . . C8 C 0.2729(3) 0.2171(3) 0.1000(5) 0.0281(13) Uani 1 1 d . . . H8A H 0.2370 0.2483 0.0509 0.034 Uiso 1 1 calc R . . H8B H 0.3066 0.2435 0.1646 0.034 Uiso 1 1 calc R . . C9 C 0.2724(3) 0.1455(3) 0.3075(5) 0.0246(13) Uani 1 1 d . . . H9A H 0.2933 0.1833 0.3626 0.029 Uiso 1 1 calc R . . H9B H 0.2379 0.1199 0.3686 0.029 Uiso 1 1 calc R . . C10 C 0.3295(3) 0.0512(3) 0.1730(6) 0.0295(14) Uani 1 1 d . . . C11 C 0.3900(4) 0.0081(3) 0.1403(7) 0.0388(16) Uani 1 1 d . . . C12 C 0.4609(4) 0.0180(3) 0.2097(7) 0.0433(17) Uani 1 1 d . . . H12 H 0.5032 -0.0105 0.1897 0.052 Uiso 1 1 calc R . . C13 C 0.4732(4) 0.0681(3) 0.3081(7) 0.0435(18) Uani 1 1 d . . . C14 C 0.4128(3) 0.1104(3) 0.3337(6) 0.0376(16) Uani 1 1 d . . . H14 H 0.4211 0.1459 0.3972 0.045 Uiso 1 1 calc R . . C15 C 0.3392(3) 0.1025(3) 0.2686(6) 0.0304(14) Uani 1 1 d . . . C16 C 0.2908(3) 0.1448(3) -0.1050(5) 0.0274(13) Uani 1 1 d . . . C17 C 0.3326(4) 0.1201(3) -0.2168(6) 0.0351(15) Uani 1 1 d . . . C18 C 0.4102(4) 0.1417(3) -0.2252(7) 0.0435(17) Uani 1 1 d . . . H18 H 0.4402 0.1263 -0.3003 0.052 Uiso 1 1 calc R . . C19 C 0.4451(3) 0.1844(3) -0.1294(7) 0.0413(17) Uani 1 1 d . . . C20 C 0.4012(3) 0.2060(3) -0.0169(6) 0.0348(15) Uani 1 1 d . . . H20 H 0.4248 0.2337 0.0523 0.042 Uiso 1 1 calc R . . C21 C 0.3239(3) 0.1872(3) -0.0057(6) 0.0284(13) Uani 1 1 d . . . C22 C 0.0628(3) 0.2124(2) 0.0525(5) 0.0227(12) Uani 1 1 d . . . C23 C 0.0028(3) 0.2426(3) -0.0285(5) 0.0316(14) Uani 1 1 d . . . C24 C -0.0079(3) 0.3099(3) -0.0140(5) 0.0293(14) Uani 1 1 d . . . H24 H -0.0482 0.3307 -0.0681 0.035 Uiso 1 1 calc R . . C25 C 0.0380(3) 0.3483(3) 0.0765(5) 0.0295(14) Uani 1 1 d . . . C26 C 0.0952(3) 0.3166(3) 0.1588(5) 0.0272(13) Uani 1 1 d . . . H26 H 0.1269 0.3418 0.2222 0.033 Uiso 1 1 calc R . . C27 C 0.1066(3) 0.2485(3) 0.1495(5) 0.0248(12) Uani 1 1 d . . . C28 C 0.3768(4) -0.0450(3) 0.0317(7) 0.0488(19) Uani 1 1 d . . . H28A H 0.3346 -0.0743 0.0603 0.073 Uiso 1 1 calc R . . H28B H 0.4249 -0.0707 0.0222 0.073 Uiso 1 1 calc R . . H28C H 0.3623 -0.0246 -0.0581 0.073 Uiso 1 1 calc R . . C29 C 0.5522(4) 0.0760(4) 0.3846(9) 0.061(2) Uani 1 1 d . . . H29A H 0.5557 0.1202 0.4260 0.092 Uiso 1 1 calc R . . H29B H 0.5942 0.0703 0.3185 0.092 Uiso 1 1 calc R . . H29C H 0.5573 0.0427 0.4584 0.092 Uiso 1 1 calc R . . C30 C 0.2944(4) 0.0742(3) -0.3215(6) 0.0443(18) Uani 1 1 d . . . H30A H 0.2805 0.0329 -0.2753 0.067 Uiso 1 1 calc R . . H30B H 0.3308 0.0649 -0.3960 0.067 Uiso 1 1 calc R . . H30C H 0.2471 0.0950 -0.3615 0.067 Uiso 1 1 calc R . . C31 C 0.5274(4) 0.2084(4) -0.1464(9) 0.063(2) Uani 1 1 d . . . H31A H 0.5529 0.2141 -0.0543 0.094 Uiso 1 1 calc R . . H31B H 0.5264 0.2508 -0.1957 0.094 Uiso 1 1 calc R . . H31C H 0.5565 0.1760 -0.2002 0.094 Uiso 1 1 calc R . . C32 C -0.0503(3) 0.2030(3) -0.1247(6) 0.0377(16) Uani 1 1 d . . . H32A H -0.1021 0.1995 -0.0845 0.057 Uiso 1 1 calc R . . H32B H -0.0285 0.1587 -0.1366 0.057 Uiso 1 1 calc R . . H32C H -0.0550 0.2250 -0.2156 0.057 Uiso 1 1 calc R . . C33 C 0.0232(4) 0.4211(3) 0.0938(6) 0.0413(16) Uani 1 1 d . . . H33A H 0.0042 0.4295 0.1875 0.062 Uiso 1 1 calc R . . H33B H -0.0161 0.4357 0.0240 0.062 Uiso 1 1 calc R . . H33C H 0.0719 0.4455 0.0812 0.062 Uiso 1 1 calc R . . C34 C 0.0809(6) -0.0442(4) -0.0759(10) 0.087(3) Uani 1 1 d . . . H34A H 0.0312 -0.0360 -0.1287 0.104 Uiso 1 1 calc R . . H34B H 0.0679 -0.0670 0.0116 0.104 Uiso 1 1 calc R . . C35 C 0.1267(8) -0.0864(5) -0.1542(12) 0.128(4) Uani 1 1 d . . . H35A H 0.1333 -0.0675 -0.2472 0.192 Uiso 1 1 calc R . . H35B H 0.1009 -0.1295 -0.1631 0.192 Uiso 1 1 calc R . . H35C H 0.1780 -0.0919 -0.1074 0.192 Uiso 1 1 calc R . . C36 C 0.2414(7) 0.5722(5) 0.9563(12) 0.109(4) Uani 1 1 d . . . C37 C 0.2140(8) 0.6170(7) 0.8468(15) 0.128(5) Uani 1 1 d . . . C38 C 0.2644(7) 0.6738(6) 0.827(2) 0.179(7) Uani 1 1 d D . . C39 C 0.2491(9) 0.7388(7) 0.8635(18) 0.172(7) Uani 1 1 d D . . C40 C 0.2989(7) 0.7969(6) 0.8352(14) 0.113(4) Uani 1 1 d . . . 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 Ta 0.03510(12) 0.02005(10) 0.02406(11) -0.00094(9) 0.00266(8) -0.00027(10) Cl2 0.0475(8) 0.0348(7) 0.0350(7) 0.0087(6) 0.0123(6) -0.0054(7) O3 0.039(2) 0.0254(19) 0.0265(19) 0.0015(15) 0.0087(17) 0.0097(17) O4 0.030(2) 0.0288(19) 0.031(2) -0.0049(16) -0.0017(16) 0.0005(16) O5 0.0286(19) 0.0242(18) 0.0251(19) -0.0038(15) -0.0027(15) -0.0052(16) O1 0.048(2) 0.033(2) 0.040(2) 0.0027(18) 0.009(2) -0.0034(19) N6 0.020(2) 0.021(2) 0.018(2) 0.0004(16) 0.0060(17) 0.0014(17) C7 0.028(3) 0.022(2) 0.018(2) -0.008(2) 0.003(2) 0.000(2) C8 0.035(3) 0.023(3) 0.026(3) 0.002(2) 0.001(2) -0.002(2) C9 0.025(3) 0.029(3) 0.020(3) 0.000(2) 0.000(2) 0.003(2) C10 0.022(3) 0.036(3) 0.030(3) 0.008(2) 0.002(2) 0.004(2) C11 0.040(3) 0.031(3) 0.046(4) 0.005(3) 0.004(3) 0.011(3) C12 0.040(3) 0.040(3) 0.051(4) 0.007(3) 0.016(3) 0.018(3) C13 0.033(3) 0.046(4) 0.052(4) 0.014(3) -0.001(3) 0.006(3) C14 0.036(3) 0.040(3) 0.037(3) 0.011(3) -0.004(3) 0.005(3) C15 0.036(3) 0.024(3) 0.031(3) 0.004(2) 0.003(2) 0.004(2) C16 0.038(3) 0.021(3) 0.024(3) 0.005(2) 0.006(2) 0.006(2) C17 0.047(3) 0.030(3) 0.029(3) 0.007(2) 0.012(3) 0.011(3) C18 0.040(3) 0.042(3) 0.050(4) 0.013(3) 0.020(3) 0.019(3) C19 0.028(3) 0.047(4) 0.050(4) 0.013(3) 0.015(3) 0.009(3) C20 0.032(3) 0.033(3) 0.040(3) 0.008(3) 0.002(3) 0.001(3) C21 0.028(3) 0.025(3) 0.033(3) 0.006(2) 0.007(2) 0.005(2) C22 0.024(3) 0.023(2) 0.022(3) 0.002(2) 0.001(2) 0.002(2) C23 0.035(3) 0.039(3) 0.022(3) 0.001(2) 0.005(2) 0.006(3) C24 0.027(3) 0.043(3) 0.018(3) 0.005(2) 0.003(2) 0.005(2) C25 0.038(3) 0.029(3) 0.022(3) 0.005(2) 0.007(2) 0.010(2) C26 0.035(3) 0.027(3) 0.020(3) -0.002(2) 0.004(2) 0.005(2) C27 0.027(3) 0.029(3) 0.019(2) -0.002(2) 0.004(2) 0.003(2) C28 0.048(4) 0.041(4) 0.058(4) -0.005(3) 0.013(3) 0.019(3) C29 0.037(4) 0.063(5) 0.083(6) 0.001(4) -0.011(4) 0.011(4) C30 0.061(4) 0.044(4) 0.029(3) -0.003(3) 0.009(3) 0.017(3) C31 0.033(4) 0.066(5) 0.090(5) 0.021(4) 0.023(4) 0.007(4) C32 0.028(3) 0.055(4) 0.030(3) -0.002(3) 0.000(2) 0.006(3) C33 0.054(4) 0.037(3) 0.034(3) 0.004(3) 0.013(3) 0.021(3) C34 0.109(7) 0.062(5) 0.092(6) -0.029(4) 0.037(5) -0.047(5) C35 0.201(11) 0.054(5) 0.135(8) -0.031(5) 0.105(7) -0.005(7) C36 0.132(8) 0.093(7) 0.098(8) 0.012(6) -0.056(6) -0.024(7) C37 0.120(10) 0.113(9) 0.149(11) 0.054(8) -0.006(8) -0.008(8) C38 0.081(8) 0.112(10) 0.35(2) 0.080(12) 0.070(11) 0.019(8) C39 0.116(10) 0.188(14) 0.210(15) -0.084(12) -0.008(10) -0.035(10) C40 0.088(8) 0.094(8) 0.157(11) -0.013(8) -0.016(8) 0.007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta O1 1.865(4) . ? Ta O3 1.910(4) . ? Ta O5 1.916(4) . ? Ta O4 1.950(4) . ? Ta N6 2.398(4) . ? Ta Cl2 2.4004(14) . ? O3 C10 1.380(6) . ? O4 C16 1.361(7) . ? O5 C22 1.364(6) . ? O1 C34 1.364(9) . ? N6 C9 1.501(6) . ? N6 C8 1.509(7) . ? N6 C7 1.515(6) . ? C7 C27 1.515(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C21 1.486(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C15 1.493(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.392(8) . ? C10 C11 1.397(8) . ? C11 C12 1.381(9) . ? C11 C28 1.510(9) . ? C12 C13 1.397(9) . ? C12 H12 0.9500 . ? C13 C14 1.371(9) . ? C13 C29 1.526(9) . ? C14 C15 1.397(8) . ? C14 H14 0.9500 . ? C16 C21 1.390(8) . ? C16 C17 1.401(8) . ? C17 C18 1.403(9) . ? C17 C30 1.503(9) . ? C18 C19 1.383(9) . ? C18 H18 0.9500 . ? C19 C20 1.403(9) . ? C19 C31 1.503(9) . ? C20 C21 1.385(8) . ? C20 H20 0.9500 . ? C22 C27 1.385(7) . ? C22 C23 1.408(7) . ? C23 C24 1.381(8) . ? C23 C32 1.507(8) . ? C24 C25 1.390(8) . ? C24 H24 0.9500 . ? C25 C26 1.396(8) . ? C25 C33 1.506(8) . ? C26 C27 1.396(7) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.395(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.456(16) . ? C37 C38 1.452(17) . ? C38 C39 1.388(17) . ? C39 C40 1.483(19) . ? 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 O1 Ta O3 98.39(17) . . ? O1 Ta O5 97.40(17) . . ? O3 Ta O5 164.20(15) . . ? O1 Ta O4 99.28(16) . . ? O3 Ta O4 88.18(15) . . ? O5 Ta O4 89.72(15) . . ? O1 Ta N6 178.90(16) . . ? O3 Ta N6 80.59(15) . . ? O5 Ta N6 83.62(14) . . ? O4 Ta N6 81.14(14) . . ? O1 Ta Cl2 93.98(13) . . ? O3 Ta Cl2 88.77(11) . . ? O5 Ta Cl2 89.70(11) . . ? O4 Ta Cl2 166.69(11) . . ? N6 Ta Cl2 85.58(10) . . ? C10 O3 Ta 143.2(3) . . ? C16 O4 Ta 129.4(3) . . ? C22 O5 Ta 140.3(3) . . ? C34 O1 Ta 162.4(5) . . ? C9 N6 C8 109.9(4) . . ? C9 N6 C7 104.9(4) . . ? C8 N6 C7 106.6(4) . . ? C9 N6 Ta 111.5(3) . . ? C8 N6 Ta 114.1(3) . . ? C7 N6 Ta 109.3(3) . . ? N6 C7 C27 115.0(4) . . ? N6 C7 H7A 108.5 . . ? C27 C7 H7A 108.5 . . ? N6 C7 H7B 108.5 . . ? C27 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C21 C8 N6 118.4(4) . . ? C21 C8 H8A 107.7 . . ? N6 C8 H8A 107.7 . . ? C21 C8 H8B 107.7 . . ? N6 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C15 C9 N6 115.0(4) . . ? C15 C9 H9A 108.5 . . ? N6 C9 H9A 108.5 . . ? C15 C9 H9B 108.5 . . ? N6 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? O3 C10 C15 119.9(5) . . ? O3 C10 C11 117.5(5) . . ? C15 C10 C11 122.6(5) . . ? C12 C11 C10 116.7(6) . . ? C12 C11 C28 123.1(6) . . ? C10 C11 C28 120.2(6) . . ? C11 C12 C13 122.9(6) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C14 C13 C12 118.4(6) . . ? C14 C13 C29 120.7(6) . . ? C12 C13 C29 120.9(6) . . ? C13 C14 C15 121.6(6) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C10 C15 C14 117.9(5) . . ? C10 C15 C9 121.5(5) . . ? C14 C15 C9 120.5(5) . . ? O4 C16 C21 118.9(5) . . ? O4 C16 C17 118.6(5) . . ? C21 C16 C17 122.5(5) . . ? C18 C17 C16 116.1(5) . . ? C18 C17 C30 123.2(5) . . ? C16 C17 C30 120.7(5) . . ? C19 C18 C17 123.2(6) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C18 C19 C20 118.3(6) . . ? C18 C19 C31 121.1(6) . . ? C20 C19 C31 120.5(6) . . ? C21 C20 C19 120.7(6) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C16 C21 C20 119.2(5) . . ? C16 C21 C8 118.9(5) . . ? C20 C21 C8 121.6(5) . . ? O5 C22 C27 119.4(4) . . ? O5 C22 C23 119.8(5) . . ? C27 C22 C23 120.8(5) . . ? C24 C23 C22 118.0(5) . . ? C24 C23 C32 120.5(5) . . ? C22 C23 C32 121.5(5) . . ? C23 C24 C25 122.7(5) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C24 C25 C26 118.0(5) . . ? C24 C25 C33 121.6(5) . . ? C26 C25 C33 120.3(5) . . ? C25 C26 C27 121.0(5) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.4(5) . . ? C22 C27 C7 121.0(5) . . ? C26 C27 C7 119.5(5) . . ? C11 C28 H28A 109.5 . . ? C11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C13 C29 H29A 109.5 . . ? C13 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C13 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C17 C30 H30A 109.5 . . ? C17 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C17 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C19 C31 H31A 109.5 . . ? C19 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C19 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 C32 H32A 109.5 . . ? C23 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C23 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C33 H33A 109.5 . . ? C25 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C25 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O1 C34 C35 115.7(8) . . ? O1 C34 H34A 108.4 . . ? C35 C34 H34A 108.4 . . ? O1 C34 H34B 108.4 . . ? C35 C34 H34B 108.4 . . ? H34A C34 H34B 107.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C37 C36 114.0(12) . . ? C39 C38 C37 126.8(13) . . ? C38 C39 C40 126.3(14) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 3.133 _refine_diff_density_min -1.947 _refine_diff_density_rms 0.150