# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1778 data_monb1m _audit_creation_method SHELXL-97 _chemical_name_systematic tetramolybdenumdiniobiumoctaoxotetradecaisopropoxide _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H98 Mo4 Nb2 O22' _chemical_formula_sum 'C42 H98 Mo4 Nb2 O22' _chemical_formula_weight 1524.78 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0293(12) _cell_length_b 10.9976(13) _cell_length_c 15.7176(18) _cell_angle_alpha 94.154(2) _cell_angle_beta 93.941(2) _cell_angle_gamma 107.329(2) _cell_volume 1643.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used '999 with I>10sigma(I) ' _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 28.31 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type 'Bruker SADABS ' _exptl_absorpt_correction_T_min 0.5247 _exptl_absorpt_correction_T_max 0.8477 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K ' _diffrn_measurement_method 'Bruker SMART ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9739 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.1236 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.31 _reflns_number_total 7114 _reflns_number_gt 3116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART ' _computing_cell_refinement 'Bruker SMART ' _computing_data_reduction 'Bruker SAINTPLUS ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' Bruker SHELXTL 5.3 ' _computing_publication_material 'Bruker SHELXTL 5.3 ' _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^)+(0.0495P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00031(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7114 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1403 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.808 _refine_ls_shift/su_max 3.448 _refine_ls_shift/su_mean 0.046 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 Mo1 Mo 0.60143(6) 0.07418(5) 0.25818(4) 0.05436(18) Uani 1 1 d . . . Mo2 Mo 0.50958(5) -0.02770(5) 0.39417(3) 0.05347(18) Uani 1 1 d . . . Nb1 Nb 0.76065(6) 0.35386(5) 0.21162(4) 0.05946(19) Uani 1 1 d . . . O1 O 0.4418(4) 0.0748(4) 0.3195(2) 0.0573(11) Uani 1 1 d . . . O2 O 0.5665(4) 0.2058(3) 0.1769(2) 0.0554(10) Uani 1 1 d . . . O3 O 0.6946(4) 0.0302(4) 0.3575(2) 0.0571(11) Uani 1 1 d . . . O4 O 0.7936(4) 0.1709(4) 0.2165(2) 0.0598(11) Uani 1 1 d . . . O5 O 0.6053(4) -0.0291(4) 0.5157(2) 0.0601(11) Uani 1 1 d . . . O6 O 0.8011(5) 0.3415(4) 0.0977(3) 0.0728(13) Uani 1 1 d . . . O7 O 0.6804(5) 0.4829(4) 0.2044(3) 0.0834(14) Uani 1 1 d . . . O8 O 0.4310(4) -0.1823(4) 0.3617(3) 0.0756(13) Uani 1 1 d . . . O9 O 0.9393(5) 0.4485(4) 0.2563(3) 0.0808(13) Uani 1 1 d . . . O10 O 0.5547(5) -0.0546(4) 0.1872(3) 0.0730(13) Uani 1 1 d . . . O11 O 0.6948(4) 0.2958(4) 0.3226(3) 0.0665(12) Uani 1 1 d . . . C1 C 0.4400(7) 0.2148(7) 0.1306(4) 0.074(2) Uani 1 1 d . . . H1A H 0.4680 0.2821 0.0920 0.088 Uiso 1 1 calc R . . C2 C 0.9253(7) 0.1452(7) 0.2193(5) 0.086(2) Uani 1 1 d . . . H2A H 0.9869 0.2055 0.1853 0.103 Uiso 1 1 calc R . . C3 C 0.7351(7) -0.0613(8) 0.5353(5) 0.082(2) Uani 1 1 d . . . H3A H 0.7198 -0.0950 0.5911 0.098 Uiso 1 1 calc R . . C4 C 0.7928(9) 0.2640(8) 0.0214(5) 0.092(2) Uani 1 1 d . . . H4A H 0.7485 0.1749 0.0320 0.111 Uiso 1 1 calc R . . C5 C 0.9948(8) 0.1643(10) 0.3086(6) 0.150(5) Uani 1 1 d . . . H5A H 1.0092 0.2507 0.3321 0.225 Uiso 1 1 calc R . . H5B H 1.0837 0.1481 0.3077 0.225 Uiso 1 1 calc R . . H5C H 0.9362 0.1062 0.3433 0.225 Uiso 1 1 calc R . . C6 C 0.3493(8) 0.2539(9) 0.1920(5) 0.117(3) Uani 1 1 d . . . H6A H 0.4016 0.3331 0.2245 0.176 Uiso 1 1 calc R . . H6B H 0.3193 0.1888 0.2302 0.176 Uiso 1 1 calc R . . H6C H 0.2687 0.2648 0.1607 0.176 Uiso 1 1 calc R . . C7 C 0.8502(8) 0.0528(8) 0.5581(6) 0.129(3) Uani 1 1 d . . . H7A H 0.9344 0.0303 0.5710 0.193 Uiso 1 1 calc R . . H7B H 0.8315 0.0994 0.6075 0.193 Uiso 1 1 calc R . . H7C H 0.8620 0.1050 0.5111 0.193 Uiso 1 1 calc R . . C8 C 0.6284(12) 0.5847(10) 0.1774(8) 0.142(4) Uani 1 1 d . . . H8B H 0.5290 0.5403 0.1602 0.170 Uiso 1 1 calc R . . C9 C 0.7447(9) -0.1704(8) 0.4843(6) 0.134(4) Uani 1 1 d . . . H9A H 0.8316 -0.1860 0.5009 0.201 Uiso 1 1 calc R . . H9B H 0.7412 -0.1549 0.4250 0.201 Uiso 1 1 calc R . . H9C H 0.6677 -0.2437 0.4927 0.201 Uiso 1 1 calc R . . C10 C 0.7017(9) 0.2972(9) -0.0472(5) 0.138(4) Uani 1 1 d . . . H10B H 0.6104 0.2873 -0.0282 0.206 Uiso 1 1 calc R . . H10C H 0.6931 0.2412 -0.0984 0.206 Uiso 1 1 calc R . . H10D H 0.7432 0.3842 -0.0588 0.206 Uiso 1 1 calc R . . C11 C 0.6812(13) 0.6257(9) 0.0983(7) 0.171(5) Uani 1 1 d . . . H11A H 0.6454 0.6931 0.0816 0.256 Uiso 1 1 calc R . . H11B H 0.6516 0.5550 0.0547 0.256 Uiso 1 1 calc R . . H11C H 0.7818 0.6565 0.1059 0.256 Uiso 1 1 calc R . . C12 C 0.3659(9) 0.0935(8) 0.0776(6) 0.144(4) Uani 1 1 d . . . H12A H 0.4279 0.0730 0.0390 0.217 Uiso 1 1 calc R . . H12B H 0.2853 0.1028 0.0453 0.217 Uiso 1 1 calc R . . H12C H 0.3363 0.0260 0.1141 0.217 Uiso 1 1 calc R . . C13 C 0.9377(10) 0.2757(10) -0.0040(5) 0.148(4) Uani 1 1 d . . . H13A H 0.9915 0.2531 0.0417 0.222 Uiso 1 1 calc R . . H13B H 0.9828 0.3622 -0.0153 0.222 Uiso 1 1 calc R . . H13C H 0.9311 0.2191 -0.0547 0.222 Uiso 1 1 calc R . . C14 C 0.8994(9) 0.0103(8) 0.1758(7) 0.161(5) Uani 1 1 d . . . H14A H 0.8550 0.0041 0.1189 0.242 Uiso 1 1 calc R . . H14B H 0.8397 -0.0508 0.2082 0.242 Uiso 1 1 calc R . . H14C H 0.9873 -0.0073 0.1729 0.242 Uiso 1 1 calc R . . C15 C 0.6890(11) 0.3454(10) 0.4071(7) 0.127(3) Uani 1 1 d . . . H15A H 0.6457 0.2675 0.4342 0.152 Uiso 1 1 calc R . . C16 C 1.0638(11) 0.6682(10) 0.2612(8) 0.174(5) Uani 1 1 d . . . H16A H 1.1569 0.7273 0.2677 0.261 Uiso 1 1 calc R . . H16B H 1.0116 0.6891 0.3060 0.261 Uiso 1 1 calc R . . H16C H 1.0179 0.6735 0.2066 0.261 Uiso 1 1 calc R . . C17 C 1.0709(11) 0.5420(11) 0.2663(10) 0.190(6) Uani 1 1 d . . . H17 H 1.0693 0.5504 0.3287 0.228 Uiso 1 1 calc R . . C18 C 1.1857(11) 0.5071(10) 0.2733(10) 0.232(8) Uani 1 1 d . . . H18A H 1.1606 0.4157 0.2733 0.348 Uiso 1 1 calc R . . H18B H 1.2409 0.5470 0.3258 0.348 Uiso 1 1 calc R . . H18C H 1.2392 0.5329 0.2258 0.348 Uiso 1 1 calc R . . C19 C 0.5956(17) 0.4107(13) 0.4164(7) 0.245(9) Uani 1 1 d . . . H19A H 0.6000 0.4416 0.4755 0.368 Uiso 1 1 calc R . . H19B H 0.5029 0.3552 0.3979 0.368 Uiso 1 1 calc R . . H19C H 0.6176 0.4818 0.3823 0.368 Uiso 1 1 calc R . . C20 C 0.6238(16) 0.6674(11) 0.2446(8) 0.242(8) Uani 1 1 d . . . H20A H 0.5895 0.7338 0.2242 0.363 Uiso 1 1 calc R . . H20B H 0.7163 0.7047 0.2733 0.363 Uiso 1 1 calc R . . H20C H 0.5623 0.6224 0.2839 0.363 Uiso 1 1 calc R . . C21 C 0.8191(14) 0.3919(16) 0.4535(7) 0.292(11) Uani 1 1 d . . . H21A H 0.8084 0.4248 0.5101 0.437 Uiso 1 1 calc R . . H21B H 0.8787 0.4592 0.4253 0.437 Uiso 1 1 calc R . . H21C H 0.8605 0.3240 0.4575 0.437 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 Mo1 0.0463(4) 0.0558(4) 0.0647(4) 0.0147(3) 0.0069(3) 0.0187(3) Mo2 0.0411(3) 0.0548(4) 0.0669(4) 0.0159(3) 0.0066(3) 0.0156(3) Nb1 0.0562(4) 0.0567(4) 0.0679(4) 0.0147(3) 0.0110(3) 0.0178(3) O1 0.046(2) 0.066(3) 0.064(3) 0.020(2) 0.011(2) 0.019(2) O2 0.048(3) 0.057(3) 0.063(3) 0.015(2) 0.003(2) 0.017(2) O3 0.041(2) 0.066(3) 0.073(3) 0.025(2) 0.015(2) 0.023(2) O4 0.048(3) 0.063(3) 0.079(3) 0.023(2) 0.016(2) 0.025(2) O5 0.046(3) 0.075(3) 0.066(3) 0.015(2) 0.003(2) 0.027(2) O6 0.079(3) 0.067(3) 0.071(3) 0.017(2) 0.016(3) 0.017(3) O7 0.096(4) 0.062(3) 0.106(4) 0.019(3) 0.019(3) 0.039(3) O8 0.073(3) 0.052(3) 0.096(3) 0.008(2) 0.002(3) 0.012(2) O9 0.065(3) 0.075(3) 0.087(3) 0.007(3) 0.006(3) -0.002(3) O10 0.083(3) 0.059(3) 0.077(3) 0.003(2) 0.007(3) 0.023(2) O11 0.070(3) 0.071(3) 0.058(3) 0.001(2) 0.008(2) 0.022(2) C1 0.060(5) 0.093(6) 0.079(5) 0.017(4) -0.005(4) 0.039(4) C2 0.052(5) 0.101(6) 0.124(7) 0.044(5) 0.035(5) 0.038(4) C3 0.049(5) 0.123(7) 0.087(6) 0.016(5) 0.001(4) 0.049(5) C4 0.105(7) 0.091(6) 0.075(6) 0.005(5) 0.010(5) 0.021(5) C5 0.062(6) 0.265(13) 0.152(9) 0.130(9) 0.028(6) 0.064(7) C6 0.084(6) 0.153(8) 0.147(8) 0.062(6) 0.024(6) 0.070(6) C7 0.054(5) 0.128(8) 0.200(10) -0.002(7) -0.014(6) 0.030(5) C8 0.181(11) 0.105(8) 0.184(11) 0.054(8) 0.075(9) 0.089(8) C9 0.103(7) 0.106(7) 0.213(11) 0.002(7) -0.008(7) 0.071(6) C10 0.129(9) 0.185(10) 0.083(7) -0.001(6) -0.002(6) 0.030(8) C11 0.237(14) 0.138(9) 0.176(11) 0.082(8) 0.040(10) 0.096(9) C12 0.122(8) 0.105(7) 0.180(10) -0.015(7) -0.078(7) 0.022(6) C13 0.157(10) 0.232(12) 0.099(7) 0.046(7) 0.051(7) 0.109(10) C14 0.111(8) 0.100(7) 0.308(15) 0.026(8) 0.077(9) 0.070(6) C15 0.112(8) 0.131(8) 0.121(9) -0.047(7) 0.015(7) 0.025(7) C16 0.131(10) 0.115(9) 0.232(13) 0.005(9) 0.004(9) -0.026(8) C17 0.075(8) 0.109(9) 0.36(2) 0.031(11) -0.028(10) -0.006(7) C18 0.061(7) 0.153(11) 0.46(2) -0.055(12) 0.011(11) 0.022(7) C19 0.42(3) 0.273(17) 0.146(11) 0.014(10) 0.096(13) 0.254(19) C20 0.45(2) 0.146(11) 0.230(14) 0.075(10) 0.184(15) 0.199(14) C21 0.156(14) 0.50(3) 0.120(11) -0.141(14) -0.004(10) 0.002(16) _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 Mo1 O10 1.665(4) . ? Mo1 O1 1.926(4) . ? Mo1 O3 1.929(4) . ? Mo1 O4 2.081(4) . ? Mo1 O2 2.088(4) . ? Mo1 O11 2.448(4) . ? Mo1 Mo2 2.5836(8) . ? Mo1 Nb1 3.1791(8) . ? Mo2 O8 1.671(4) . ? Mo2 O1 1.910(4) . ? Mo2 O3 1.917(4) . ? Mo2 O5 2.061(4) 2_656 ? Mo2 O5 2.082(4) . ? Nb1 O7 1.835(4) . ? Nb1 O9 1.843(5) . ? Nb1 O6 1.867(4) . ? Nb1 O11 1.989(4) . ? Nb1 O2 2.140(4) . ? Nb1 O4 2.140(4) . ? O2 C1 1.451(6) . ? O4 C2 1.428(7) . ? O5 C3 1.466(7) . ? O5 Mo2 2.061(4) 2_656 ? O6 C4 1.404(8) . ? O7 C8 1.445(9) . ? O9 C17 1.402(10) . ? O11 C15 1.410(9) . ? C1 C12 1.480(9) . ? C1 C6 1.496(9) . ? C2 C5 1.495(10) . ? C2 C14 1.529(10) . ? C3 C9 1.425(9) . ? C3 C7 1.432(10) . ? C4 C10 1.500(10) . ? C4 C13 1.505(10) . ? C8 C20 1.356(12) . ? C8 C11 1.434(12) . ? C15 C19 1.348(12) . ? C15 C21 1.384(13) . ? C16 C17 1.418(12) . ? C17 C18 1.318(12) . ? 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 O10 Mo1 O1 108.15(19) . . ? O10 Mo1 O3 106.71(18) . . ? O1 Mo1 O3 91.30(15) . . ? O10 Mo1 O4 99.52(19) . . ? O1 Mo1 O4 150.31(16) . . ? O3 Mo1 O4 90.88(15) . . ? O10 Mo1 O2 98.09(17) . . ? O1 Mo1 O2 92.67(15) . . ? O3 Mo1 O2 152.24(16) . . ? O4 Mo1 O2 72.59(14) . . ? O10 Mo1 O11 162.11(17) . . ? O1 Mo1 O11 83.53(15) . . ? O3 Mo1 O11 86.01(15) . . ? O4 Mo1 O11 67.09(15) . . ? O2 Mo1 O11 67.19(14) . . ? O10 Mo1 Mo2 100.47(15) . . ? O1 Mo1 Mo2 47.39(10) . . ? O3 Mo1 Mo2 47.61(11) . . ? O4 Mo1 Mo2 137.67(11) . . ? O2 Mo1 Mo2 139.57(10) . . ? O11 Mo1 Mo2 97.40(10) . . ? O10 Mo1 Nb1 123.40(15) . . ? O1 Mo1 Nb1 110.85(11) . . ? O3 Mo1 Nb1 111.65(11) . . ? O4 Mo1 Nb1 41.85(10) . . ? O2 Mo1 Nb1 41.85(10) . . ? O11 Mo1 Nb1 38.73(10) . . ? Mo2 Mo1 Nb1 136.13(3) . . ? O8 Mo2 O1 109.23(18) . . ? O8 Mo2 O3 111.52(19) . . ? O1 Mo2 O3 92.15(15) . . ? O8 Mo2 O5 108.24(19) . 2_656 ? O1 Mo2 O5 86.38(15) . 2_656 ? O3 Mo2 O5 138.27(16) . 2_656 ? O8 Mo2 O5 104.17(18) . . ? O1 Mo2 O5 144.28(16) . . ? O3 Mo2 O5 87.08(15) . . ? O5 Mo2 O5 71.26(16) 2_656 . ? O8 Mo2 Mo1 104.99(15) . . ? O1 Mo2 Mo1 47.92(11) . . ? O3 Mo2 Mo1 48.00(11) . . ? O5 Mo2 Mo1 130.42(10) 2_656 . ? O5 Mo2 Mo1 133.02(11) . . ? O7 Nb1 O9 99.6(2) . . ? O7 Nb1 O6 97.23(19) . . ? O9 Nb1 O6 96.4(2) . . ? O7 Nb1 O11 98.54(18) . . ? O9 Nb1 O11 95.60(18) . . ? O6 Nb1 O11 158.28(18) . . ? O7 Nb1 O2 93.64(18) . . ? O9 Nb1 O2 165.01(17) . . ? O6 Nb1 O2 88.79(17) . . ? O11 Nb1 O2 75.41(16) . . ? O7 Nb1 O4 163.80(18) . . ? O9 Nb1 O4 95.88(18) . . ? O6 Nb1 O4 85.63(16) . . ? O11 Nb1 O4 75.16(16) . . ? O2 Nb1 O4 70.42(14) . . ? O7 Nb1 Mo1 124.43(15) . . ? O9 Nb1 Mo1 124.54(14) . . ? O6 Nb1 Mo1 108.09(13) . . ? O11 Nb1 Mo1 50.35(12) . . ? O2 Nb1 Mo1 40.63(9) . . ? O4 Nb1 Mo1 40.43(10) . . ? Mo2 O1 Mo1 84.69(14) . . ? C1 O2 Mo1 132.1(4) . . ? C1 O2 Nb1 128.2(4) . . ? Mo1 O2 Nb1 97.51(15) . . ? Mo2 O3 Mo1 84.38(14) . . ? C2 O4 Mo1 132.2(4) . . ? C2 O4 Nb1 126.7(4) . . ? Mo1 O4 Nb1 97.72(15) . . ? C3 O5 Mo2 124.9(4) . 2_656 ? C3 O5 Mo2 126.3(4) . . ? Mo2 O5 Mo2 108.74(16) 2_656 . ? C4 O6 Nb1 148.3(4) . . ? C8 O7 Nb1 165.7(5) . . ? C17 O9 Nb1 160.8(6) . . ? C15 O11 Nb1 140.4(5) . . ? C15 O11 Mo1 128.6(5) . . ? Nb1 O11 Mo1 90.91(16) . . ? O2 C1 C12 110.8(6) . . ? O2 C1 C6 109.9(5) . . ? C12 C1 C6 112.6(7) . . ? O4 C2 C5 111.9(6) . . ? O4 C2 C14 107.6(6) . . ? C5 C2 C14 113.4(7) . . ? C9 C3 C7 123.9(7) . . ? C9 C3 O5 114.2(6) . . ? C7 C3 O5 110.3(7) . . ? O6 C4 C10 110.0(7) . . ? O6 C4 C13 110.1(7) . . ? C10 C4 C13 112.7(7) . . ? C20 C8 C11 123.0(10) . . ? C20 C8 O7 111.9(10) . . ? C11 C8 O7 110.8(8) . . ? C19 C15 C21 118.6(11) . . ? C19 C15 O11 115.4(10) . . ? C21 C15 O11 113.4(9) . . ? C18 C17 O9 119.6(11) . . ? C18 C17 C16 126.6(11) . . ? O9 C17 C16 113.6(9) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 0.513 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.085 #=END data_tamopr2t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ' Molybdenum-tantalum oxoisopropoxide ' _chemical_melting_point ? _chemical_formula_moiety 'C21 H49 Mo2 O11 Ta' _chemical_formula_sum 'C42 H98 Mo4 O22 Ta2' _chemical_formula_weight 1700.86 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0444(17) _cell_length_b 11.0070(19) _cell_length_c 15.769(3) _cell_angle_alpha 94.159(5) _cell_angle_beta 94.091(7) _cell_angle_gamma 107.143(4) _cell_volume 1653.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used '998 with I > 10 sigma(I) ' _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 28.36 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max '0.60 mm ' _exptl_crystal_size_mid '0.50 mm ' _exptl_crystal_size_min '0.20 mm ' _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 4.091 _exptl_absorpt_correction_type 'Bruker SADABS ' _exptl_absorpt_correction_T_min 0.1927 _exptl_absorpt_correction_T_max 0.4950 _exptl_absorpt_process_details ' Bruker SADABS ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' SMART CCD' _diffrn_measurement_method 'CCD area Detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9792 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.36 _reflns_number_total 7141 _reflns_number_gt 3909 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Bruker SMART ' _computing_cell_refinement ' Bruker SMART ' _computing_data_reduction ' Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' Bruker SHELXTL 5.3 ' _computing_publication_material ' Bruker SHELXTL 5.3 ' _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^)+(0.0444P)^2^+0.0000P] 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 7141 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.737 _refine_ls_restrained_S_all 0.737 _refine_ls_shift/su_max 0.080 _refine_ls_shift/su_mean 0.003 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 0.74049(3) 0.64895(3) 0.28884(2) 0.05114(12) Uani 1 1 d . . . Mo1 Mo 0.89938(6) 0.92647(6) 0.24102(4) 0.04569(18) Uani 1 1 d . . . Mo2 Mo 0.99063(6) 1.02793(6) 0.10552(4) 0.04544(18) Uani 1 1 d . . . O1 O 0.7087(4) 0.8319(4) 0.2837(3) 0.0471(12) Uani 1 1 d . . . O2 O 0.9340(4) 0.7954(4) 0.3237(3) 0.0499(13) Uani 1 1 d . . . O3 O 1.0596(4) 0.9257(4) 0.1813(3) 0.0472(12) Uani 1 1 d . . . O4 O 1.1058(5) 0.9706(5) 0.0158(3) 0.0539(13) Uani 1 1 d . . . O5 O 0.8073(4) 0.9710(5) 0.1422(3) 0.0494(13) Uani 1 1 d . . . O6 O 0.8047(5) 0.7058(5) 0.1769(3) 0.0583(14) Uani 1 1 d . . . O7 O 0.9477(5) 1.0553(5) 0.3132(3) 0.0629(14) Uani 1 1 d . . . O8 O 1.0685(5) 1.1826(5) 0.1376(3) 0.0649(15) Uani 1 1 d . . . O9 O 0.6991(5) 0.6560(5) 0.4027(3) 0.0633(15) Uani 1 1 d . . . O10 O 0.8191(6) 0.5163(5) 0.2958(4) 0.0800(18) Uani 1 1 d . . . O11 O 0.5618(6) 0.5558(6) 0.2433(4) 0.0789(18) Uani 1 1 d . . . C1 C 1.0598(9) 0.7860(10) 0.3699(6) 0.077(3) Uani 1 1 d . . . H1A H 1.0321 0.7173 0.4072 0.092 Uiso 1 1 calc R . . C2 C 0.5774(8) 0.8620(9) 0.2833(6) 0.079(3) Uani 1 1 d . . . H2A H 0.5164 0.8014 0.3170 0.095 Uiso 1 1 calc R . . C3 C 1.2373(8) 0.9413(10) 0.0381(6) 0.078(3) Uani 1 1 d . . . H3A H 1.2229 0.9078 0.0937 0.093 Uiso 1 1 calc R . . C4 C 0.7063(11) 0.7345(10) 0.4796(6) 0.087(3) Uani 1 1 d . . . H4A H 0.7495 0.8236 0.4692 0.105 Uiso 1 1 calc R . . C5 C 1.1541(9) 0.7526(12) 0.3114(7) 0.116(4) Uani 1 1 d . . . H5A H 1.1059 0.6733 0.2779 0.174 Uiso 1 1 calc R . . H5B H 1.2348 0.7437 0.3438 0.174 Uiso 1 1 calc R . . H5C H 1.1833 0.8188 0.2742 0.174 Uiso 1 1 calc R . . C6 C 0.5062(10) 0.8397(13) 0.1921(7) 0.144(6) Uani 1 1 d . . . H6A H 0.4941 0.7534 0.1694 0.217 Uiso 1 1 calc R . . H6B H 0.5633 0.8978 0.1572 0.217 Uiso 1 1 calc R . . H6C H 0.4164 0.8540 0.1926 0.217 Uiso 1 1 calc R . . C7 C 1.3508(9) 1.0528(11) 0.0581(7) 0.117(4) Uani 1 1 d . . . H7B H 1.4341 1.0301 0.0731 0.176 Uiso 1 1 calc R . . H7C H 1.3322 1.1033 0.1054 0.176 Uiso 1 1 calc R . . H7D H 1.3637 1.1013 0.0095 0.176 Uiso 1 1 calc R . . C8 C 1.2435(11) 0.8305(11) -0.0163(8) 0.131(5) Uani 1 1 d . . . H8B H 1.3288 0.8116 -0.0005 0.197 Uiso 1 1 calc R . . H8C H 1.2410 0.8487 -0.0749 0.197 Uiso 1 1 calc R . . H8D H 1.1650 0.7584 -0.0092 0.197 Uiso 1 1 calc R . . C9 C 0.8081(14) 0.6542(13) 0.0933(8) 0.115(4) Uani 1 1 d . . . H9A H 0.8548 0.7324 0.0678 0.138 Uiso 1 1 calc R . . C10 C 0.5635(12) 0.7213(13) 0.5037(7) 0.132(5) Uani 1 1 d . . . H10A H 0.5104 0.7457 0.4586 0.198 Uiso 1 1 calc R . . H10B H 0.5688 0.7755 0.5551 0.198 Uiso 1 1 calc R . . H10C H 0.5186 0.6341 0.5131 0.198 Uiso 1 1 calc R . . C11 C 1.1303(12) 0.9064(11) 0.4248(8) 0.131(5) Uani 1 1 d . . . H11A H 1.0660 0.9248 0.4623 0.197 Uiso 1 1 calc R . . H11B H 1.1605 0.9751 0.3896 0.197 Uiso 1 1 calc R . . H11C H 1.2100 0.8972 0.4581 0.197 Uiso 1 1 calc R . . C12 C 0.7953(11) 0.7020(12) 0.5457(7) 0.126(5) Uani 1 1 d . . . H12A H 0.8873 0.7152 0.5275 0.189 Uiso 1 1 calc R . . H12B H 0.7562 0.6141 0.5555 0.189 Uiso 1 1 calc R . . H12C H 0.8011 0.7555 0.5976 0.189 Uiso 1 1 calc R . . C13 C 0.8181(14) 0.3732(11) 0.3994(9) 0.147(5) Uani 1 1 d . . . H13A H 0.8548 0.3059 0.4154 0.220 Uiso 1 1 calc R . . H13B H 0.7177 0.3422 0.3926 0.220 Uiso 1 1 calc R . . H13C H 0.8482 0.4436 0.4431 0.220 Uiso 1 1 calc R . . C14 C 0.8675(16) 0.4140(12) 0.3218(10) 0.139(5) Uani 1 1 d . . . H14A H 0.9659 0.4597 0.3406 0.167 Uiso 1 1 calc R . . C15 C 0.6017(11) 0.9919(10) 0.3269(10) 0.157(6) Uani 1 1 d . . . H15A H 0.6456 0.9966 0.3837 0.235 Uiso 1 1 calc R . . H15B H 0.5137 1.0092 0.3298 0.235 Uiso 1 1 calc R . . H15C H 0.6613 1.0539 0.2954 0.235 Uiso 1 1 calc R . . C16 C 0.4344(14) 0.3371(13) 0.2353(11) 0.182(7) Uani 1 1 d . . . H16A H 0.3401 0.2818 0.2333 0.272 Uiso 1 1 calc R . . H16B H 0.4884 0.3247 0.2848 0.272 Uiso 1 1 calc R . . H16C H 0.4752 0.3175 0.1848 0.272 Uiso 1 1 calc R . . C17 C 0.881(2) 0.3369(12) 0.2556(10) 0.214(9) Uani 1 1 d . . . H17A H 0.9147 0.2703 0.2764 0.321 Uiso 1 1 calc R . . H17B H 0.9468 0.3852 0.2200 0.321 Uiso 1 1 calc R . . H17C H 0.7920 0.2997 0.2230 0.321 Uiso 1 1 calc R . . C18 C 0.4337(14) 0.4598(13) 0.2393(15) 0.204(10) Uani 1 1 d . . . C19 C 0.910(2) 0.5885(17) 0.0870(9) 0.228(10) Uani 1 1 d . . . H19A H 0.9104 0.5577 0.0285 0.342 Uiso 1 1 calc R . . H19B H 0.8886 0.5176 0.1211 0.342 Uiso 1 1 calc R . . H19C H 1.0012 0.6459 0.1072 0.342 Uiso 1 1 calc R . . C20 C 0.3196(13) 0.4916(13) 0.2279(12) 0.204(9) Uani 1 1 d . . . H20A H 0.2401 0.4172 0.2274 0.305 Uiso 1 1 calc R . . H20B H 0.3170 0.5274 0.1743 0.305 Uiso 1 1 calc R . . H20C H 0.3175 0.5536 0.2734 0.305 Uiso 1 1 calc R . . C21 C 0.6840(19) 0.619(2) 0.0466(10) 0.280(14) Uani 1 1 d . . . H21A H 0.6340 0.6789 0.0608 0.421 Uiso 1 1 calc R . . H21B H 0.6308 0.5354 0.0584 0.421 Uiso 1 1 calc R . . H21C H 0.6982 0.6186 -0.0130 0.421 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 0.0552(2) 0.0474(2) 0.0555(2) 0.01071(16) 0.01221(16) 0.01973(16) Mo1 0.0440(4) 0.0472(4) 0.0517(4) 0.0115(3) 0.0084(3) 0.0202(3) Mo2 0.0405(3) 0.0469(4) 0.0542(5) 0.0135(3) 0.0087(3) 0.0182(3) O1 0.046(3) 0.046(3) 0.055(3) 0.011(2) 0.014(2) 0.018(2) O2 0.044(3) 0.051(3) 0.058(3) 0.010(3) 0.003(2) 0.019(2) O3 0.041(3) 0.058(3) 0.049(3) 0.023(3) 0.009(2) 0.020(2) O4 0.050(3) 0.074(4) 0.058(3) 0.025(3) 0.019(2) 0.042(3) O5 0.044(3) 0.060(3) 0.054(3) 0.019(3) 0.010(2) 0.024(2) O6 0.075(4) 0.062(4) 0.046(3) 0.000(3) 0.010(3) 0.033(3) O7 0.082(4) 0.063(4) 0.051(3) 0.003(3) 0.009(3) 0.032(3) O8 0.065(3) 0.042(3) 0.085(4) 0.006(3) 0.011(3) 0.010(3) O9 0.072(3) 0.057(4) 0.061(4) 0.017(3) 0.009(3) 0.015(3) O10 0.113(5) 0.057(4) 0.093(5) 0.026(3) 0.032(4) 0.051(4) O11 0.071(4) 0.083(5) 0.080(5) 0.012(4) 0.014(3) 0.016(4) C1 0.064(6) 0.099(8) 0.077(7) 0.029(6) 0.002(5) 0.036(6) C2 0.051(5) 0.092(7) 0.118(9) 0.044(6) 0.034(5) 0.045(5) C3 0.053(5) 0.108(8) 0.091(7) 0.014(6) 0.012(5) 0.051(6) C4 0.105(8) 0.089(8) 0.057(7) -0.010(6) 0.008(6) 0.017(7) C5 0.079(7) 0.180(12) 0.128(10) 0.059(9) 0.038(7) 0.082(8) C6 0.069(7) 0.261(17) 0.135(11) 0.117(11) 0.019(7) 0.074(9) C7 0.042(5) 0.129(10) 0.170(12) -0.024(9) -0.021(7) 0.026(6) C8 0.120(9) 0.138(11) 0.180(13) 0.004(9) 0.008(9) 0.110(9) C9 0.116(10) 0.121(10) 0.096(10) -0.038(8) -0.010(8) 0.033(9) C10 0.125(10) 0.220(15) 0.071(8) -0.002(8) 0.019(7) 0.084(10) C11 0.122(9) 0.114(10) 0.147(12) -0.033(9) -0.067(9) 0.045(8) C12 0.106(8) 0.186(14) 0.066(8) 0.000(8) 0.003(7) 0.019(9) C13 0.177(12) 0.112(10) 0.179(14) 0.067(10) 0.029(11) 0.070(10) C14 0.196(13) 0.091(9) 0.179(15) 0.070(10) 0.087(12) 0.090(10) C15 0.113(9) 0.080(8) 0.315(19) 0.038(10) 0.097(11) 0.065(8) C16 0.115(10) 0.102(12) 0.28(2) -0.034(13) 0.010(12) -0.025(9) C17 0.38(3) 0.104(11) 0.235(19) 0.063(11) 0.149(18) 0.148(15) C18 0.071(8) 0.068(9) 0.46(3) 0.001(14) 0.012(13) 0.013(8) C19 0.38(3) 0.28(2) 0.129(13) -0.003(13) 0.084(15) 0.25(2) C20 0.086(9) 0.112(12) 0.39(3) -0.049(14) 0.078(13) 0.008(9) C21 0.178(17) 0.46(4) 0.116(14) -0.098(18) -0.001(13) 0.00(2) _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 O11 1.847(6) . ? Ta1 O10 1.859(5) . ? Ta1 O9 1.873(5) . ? Ta1 O6 2.002(5) . ? Ta1 O2 2.133(5) . ? Ta1 O1 2.136(4) . ? Ta1 Mo1 3.1746(8) . ? Mo1 O7 1.680(5) . ? Mo1 O5 1.923(4) . ? Mo1 O3 1.923(4) . ? Mo1 O1 2.078(4) . ? Mo1 O2 2.099(4) . ? Mo1 O6 2.443(5) . ? Mo1 Mo2 2.5836(9) . ? Mo2 O8 1.673(5) . ? Mo2 O5 1.909(4) . ? Mo2 O3 1.926(4) . ? Mo2 O4 2.067(5) . ? Mo2 O4 2.085(5) 2_775 ? O1 C2 1.450(8) . ? O2 C1 1.448(8) . ? O4 C3 1.474(8) . ? O4 Mo2 2.085(5) 2_775 ? O6 C9 1.404(12) . ? O9 C4 1.421(10) . ? O10 C14 1.426(11) . ? O11 C18 1.397(13) . ? C1 C5 1.471(12) . ? C1 C11 1.484(13) . ? C2 C15 1.485(13) . ? C2 C6 1.529(13) . ? C3 C7 1.405(12) . ? C3 C8 1.458(13) . ? C4 C12 1.457(12) . ? C4 C10 1.478(13) . ? C9 C21 1.337(17) . ? C9 C19 1.426(16) . ? C13 C14 1.407(15) . ? C14 C17 1.337(16) . ? C16 C18 1.350(16) . ? C18 C20 1.297(16) . ? 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 O11 Ta1 O10 99.1(3) . . ? O11 Ta1 O9 96.0(2) . . ? O10 Ta1 O9 95.8(2) . . ? O11 Ta1 O6 94.6(2) . . ? O10 Ta1 O6 98.7(2) . . ? O9 Ta1 O6 160.4(2) . . ? O11 Ta1 O2 164.7(2) . . ? O10 Ta1 O2 94.3(2) . . ? O9 Ta1 O2 89.8(2) . . ? O6 Ta1 O2 76.0(2) . . ? O11 Ta1 O1 95.7(2) . . ? O10 Ta1 O1 164.4(2) . . ? O9 Ta1 O1 87.5(2) . . ? O6 Ta1 O1 75.13(18) . . ? O2 Ta1 O1 70.35(17) . . ? O11 Ta1 Mo1 123.87(18) . . ? O10 Ta1 Mo1 124.95(18) . . ? O9 Ta1 Mo1 110.29(16) . . ? O6 Ta1 Mo1 50.31(15) . . ? O2 Ta1 Mo1 40.98(12) . . ? O1 Ta1 Mo1 40.43(11) . . ? O7 Mo1 O5 107.3(2) . . ? O7 Mo1 O3 107.6(2) . . ? O5 Mo1 O3 91.72(18) . . ? O7 Mo1 O1 98.9(2) . . ? O5 Mo1 O1 91.50(18) . . ? O3 Mo1 O1 151.0(2) . . ? O7 Mo1 O2 96.8(2) . . ? O5 Mo1 O2 152.8(2) . . ? O3 Mo1 O2 92.77(17) . . ? O1 Mo1 O2 72.16(17) . . ? O7 Mo1 O6 161.5(2) . . ? O5 Mo1 O6 86.02(19) . . ? O3 Mo1 O6 84.15(19) . . ? O1 Mo1 O6 67.34(18) . . ? O2 Mo1 O6 67.80(18) . . ? O7 Mo1 Mo2 100.89(18) . . ? O5 Mo1 Mo2 47.38(13) . . ? O3 Mo1 Mo2 47.89(12) . . ? O1 Mo1 Mo2 138.13(13) . . ? O2 Mo1 Mo2 140.16(13) . . ? O6 Mo1 Mo2 97.54(12) . . ? O7 Mo1 Ta1 122.48(18) . . ? O5 Mo1 Ta1 112.12(14) . . ? O3 Mo1 Ta1 111.21(14) . . ? O1 Mo1 Ta1 41.81(12) . . ? O2 Mo1 Ta1 41.81(12) . . ? O6 Mo1 Ta1 39.08(12) . . ? Mo2 Mo1 Ta1 136.62(3) . . ? O8 Mo2 O5 111.3(2) . . ? O8 Mo2 O3 109.1(2) . . ? O5 Mo2 O3 92.07(18) . . ? O8 Mo2 O4 108.3(2) . . ? O5 Mo2 O4 138.5(2) . . ? O3 Mo2 O4 86.48(18) . . ? O8 Mo2 O4 103.9(2) . 2_775 ? O5 Mo2 O4 87.15(18) . 2_775 ? O3 Mo2 O4 144.8(2) . 2_775 ? O4 Mo2 O4 71.54(18) . 2_775 ? O8 Mo2 Mo1 105.13(18) . . ? O5 Mo2 Mo1 47.83(13) . . ? O3 Mo2 Mo1 47.80(13) . . ? O4 Mo2 Mo1 130.29(13) . . ? O4 Mo2 Mo1 132.91(13) 2_775 . ? C2 O1 Mo1 131.7(4) . . ? C2 O1 Ta1 127.8(5) . . ? Mo1 O1 Ta1 97.76(17) . . ? C1 O2 Mo1 132.1(5) . . ? C1 O2 Ta1 128.4(5) . . ? Mo1 O2 Ta1 97.20(18) . . ? Mo1 O3 Mo2 84.31(17) . . ? C3 O4 Mo2 123.4(5) . . ? C3 O4 Mo2 128.1(5) . 2_775 ? Mo2 O4 Mo2 108.46(18) . 2_775 ? Mo2 O5 Mo1 84.79(17) . . ? C9 O6 Ta1 139.8(7) . . ? C9 O6 Mo1 129.5(7) . . ? Ta1 O6 Mo1 90.61(19) . . ? C4 O9 Ta1 146.7(6) . . ? C14 O10 Ta1 165.8(7) . . ? C18 O11 Ta1 155.9(10) . . ? O2 C1 C5 111.4(8) . . ? O2 C1 C11 110.1(8) . . ? C5 C1 C11 111.8(9) . . ? O1 C2 C15 109.8(8) . . ? O1 C2 C6 109.7(8) . . ? C15 C2 C6 115.4(9) . . ? C7 C3 C8 123.7(8) . . ? C7 C3 O4 111.8(8) . . ? C8 C3 O4 110.3(8) . . ? O9 C4 C12 109.2(9) . . ? O9 C4 C10 109.8(8) . . ? C12 C4 C10 113.1(9) . . ? C21 C9 O6 113.9(12) . . ? C21 C9 C19 124.3(15) . . ? O6 C9 C19 112.9(11) . . ? C17 C14 C13 124.9(13) . . ? C17 C14 O10 112.7(13) . . ? C13 C14 O10 112.0(11) . . ? C20 C18 C16 122.7(14) . . ? C20 C18 O11 118.3(13) . . ? C16 C18 O11 118.3(12) . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 0.899 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.143 #=END data_mo3ta2m _audit_creation_method SHELXL-97 _chemical_name_systematic trimolybdenumditantalumoctaoxodecaisopropoxide _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H70 Mo3 O18 Ta2' _chemical_formula_sum 'C30 H70 Mo3 O18 Ta2' _chemical_formula_weight 1368.58 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.8123(11) _cell_length_b 18.5541(11) _cell_length_c 29.0517(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10140.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '999 with I>10sigma(I) ' _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 28.43 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5328 _exptl_absorpt_coefficient_mu 5.079 _exptl_absorpt_correction_type 'Bruker SADABS ' _exptl_absorpt_correction_T_min 0.1063 _exptl_absorpt_correction_T_max 0.1856 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' SMART CCD 1K ' _diffrn_measurement_method ' Bruker SMART ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47702 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.43 _reflns_number_total 11928 _reflns_number_gt 5189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART ' _computing_cell_refinement ' Bruker SMART ' _computing_data_reduction 'Bruker SAINTPLUS ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.3 ' _computing_publication_material 'SHELXTL 5.3' _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^)+(0.0777P)^2^+0.0000P] 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 11928 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 3.460 _refine_ls_shift/su_mean 0.278 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 0.60234(2) 0.73936(3) 0.234298(15) 0.08061(16) Uani 1 1 d . . . Ta2 Ta 0.71532(2) 0.87377(2) 0.019606(15) 0.08071(16) Uani 1 1 d . . . Mo1 Mo 0.56295(4) 0.86223(5) 0.07049(3) 0.0715(2) Uani 1 1 d . . . Mo2 Mo 0.52188(4) 0.81252(5) 0.14877(3) 0.0696(2) Uani 1 1 d . . . Mo3 Mo 0.7101(4) 0.7552(5) 0.1248(2) 0.084(3) Uani 0.412(13) 1 d P . . Mo3A Mo 0.72864(16) 0.7921(3) 0.13971(14) 0.0802(11) Uani 0.588(13) 1 d P . . O1 O 0.5698(3) 0.8998(3) 0.13166(19) 0.0701(16) Uani 1 1 d . . . O2 O 0.5494(3) 0.7661(3) 0.0934(2) 0.0773(17) Uani 1 1 d . . . O3 O 0.6361(3) 0.9390(3) 0.0498(2) 0.0757(17) Uani 1 1 d . . . O4 O 0.6160(4) 0.8206(4) 0.0136(2) 0.0843(19) Uani 1 1 d . . . O5 O 0.5461(3) 0.8344(4) 0.2174(2) 0.0784(17) Uani 1 1 d . . . O6 O 0.6492(3) 0.7718(4) 0.1735(2) 0.086(2) Uani 1 1 d . . . O7 O 0.5255(3) 0.7145(3) 0.1840(2) 0.0777(18) Uani 1 1 d . . . O8 O 0.6451(4) 0.6504(4) 0.2312(3) 0.107(2) Uani 1 1 d . . . O9 O 0.4338(3) 0.8265(4) 0.1471(2) 0.096(2) Uani 1 1 d . . . O10 O 0.7017(4) 0.8280(3) 0.0838(2) 0.085(2) Uani 1 1 d . . . O11 O 0.6687(4) 0.7879(5) 0.2696(3) 0.117(3) Uani 1 1 d . . . O12 O 0.4858(4) 0.8896(4) 0.0476(3) 0.103(2) Uani 1 1 d . . . O13 O 0.7897(4) 0.9295(5) 0.0399(3) 0.111(3) Uani 1 1 d . . . O14 O 0.7019(4) 0.9202(4) -0.0364(3) 0.114(3) Uani 1 1 d . . . O15 O 0.5374(4) 0.7184(4) 0.2805(3) 0.103(2) Uani 1 1 d . . . O16 O 0.7636(5) 0.7939(4) -0.0023(3) 0.108(3) Uani 1 1 d . . . O17 O 0.7746(17) 0.7190(18) 0.1317(11) 0.169(17) Uani 0.588(13) 1 d P . . O18 O 0.7827(12) 0.8502(15) 0.1678(7) 0.170(10) Uani 0.588(13) 1 d P . . O17A O 0.7031(13) 0.6733(10) 0.1031(9) 0.122(9) Uani 0.412(13) 1 d P . . O18A O 0.7935(17) 0.765(4) 0.150(2) 0.20(3) Uani 0.412(13) 1 d P . . C1 C 0.6452(6) 1.0142(5) 0.0628(4) 0.090(3) Uani 1 1 d . . . C2 C 0.4990(7) 0.6445(7) 0.1740(5) 0.116(4) Uani 1 1 d . . . C3 C 0.6808(7) 1.0193(7) 0.1095(5) 0.118(4) Uani 1 1 d . . . C4 C 0.5688(7) 1.0487(6) 0.0621(4) 0.119(4) Uani 1 1 d . . . C5 C 0.6022(10) 0.7588(8) -0.0135(6) 0.134(6) Uani 1 1 d . . . C6 C 0.5455(9) 0.8994(9) 0.2440(5) 0.133(5) Uani 1 1 d . . . C7 C 0.5278(12) 0.6129(9) 0.1312(6) 0.192(9) Uani 1 1 d . . . C8 C 0.4705(9) 0.7155(10) 0.3043(7) 0.161(7) Uani 1 1 d . . . C9 C 0.8107(13) 0.7440(10) -0.0207(9) 0.194(10) Uani 1 1 d . . . C10 C 0.4174(8) 0.6493(10) 0.1717(7) 0.175(8) Uani 1 1 d . . . C11 C 0.6009(11) 0.9490(10) 0.2311(6) 0.175(7) Uani 1 1 d . . . C13 C 0.8503(15) 0.7688(14) -0.0568(9) 0.273(17) Uani 1 1 d . . . C14 C 0.8521(12) 0.9688(14) 0.0562(9) 0.201(9) Uani 1 1 d . . . C15 C 0.6248(15) 0.6911(11) 0.0086(8) 0.234(12) Uani 1 1 d . . . C16 C 0.4744(13) 0.7566(15) 0.3472(8) 0.253(13) Uani 1 1 d . . . C17 C 0.4488(14) 0.6439(15) 0.3127(9) 0.256(13) Uani 1 1 d . . . C18 C 0.8328(16) 0.6950(16) 0.0074(11) 0.300(17) Uani 1 1 d . . . C19 C 0.7287(15) 0.8076(16) 0.2988(11) 0.245(12) Uani 1 1 d . . . C20 C 0.8900(15) 0.986(2) 0.0152(13) 0.35(2) Uani 1 1 d . . . C21 C 0.8943(15) 0.9182(16) 0.0834(13) 0.32(2) Uani 1 1 d . . . C24 C 0.530(2) 0.7605(15) -0.0269(12) 0.33(2) Uani 1 1 d . . . C22 C 0.4746(14) 0.9321(15) 0.2369(10) 0.308(18) Uani 1 1 d . . . C29 C 0.7824(15) 0.821(3) 0.2798(14) 0.40(4) Uani 1 1 d . . . C30 C 0.702(3) 0.832(3) 0.3433(12) 0.45(3) Uani 1 1 d . . . C23 C 0.657(2) 0.993(2) -0.0734(11) 0.285(15) Uiso 1 1 d . . . C27 C 0.729(3) 0.995(2) -0.0857(18) 0.42(2) Uiso 1 1 d . . . C28 C 0.6350(18) 0.936(2) -0.0880(12) 0.311(17) Uiso 1 1 d . . . C12 C 0.7006(15) 0.5920(16) 0.2178(9) 0.227(10) Uiso 1 1 d . . . C25 C 0.750(2) 0.601(2) 0.2498(17) 0.40(2) Uiso 1 1 d . . . C26 C 0.6723(19) 0.525(2) 0.2188(11) 0.324(16) Uiso 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 Ta1 0.0699(3) 0.0984(4) 0.0735(3) 0.0125(2) 0.0071(2) 0.0005(2) Ta2 0.0873(3) 0.0749(3) 0.0799(3) 0.0108(2) 0.0206(2) 0.0095(2) Mo1 0.0668(5) 0.0778(6) 0.0698(5) 0.0028(4) -0.0037(4) 0.0052(4) Mo2 0.0542(4) 0.0782(6) 0.0765(5) 0.0005(4) 0.0021(4) -0.0010(4) Mo3 0.060(2) 0.105(5) 0.087(3) 0.032(3) 0.0158(19) 0.024(3) Mo3A 0.0586(12) 0.101(3) 0.0808(15) 0.0175(16) 0.0014(10) -0.0027(14) O1 0.062(4) 0.073(4) 0.075(4) 0.000(3) 0.005(3) 0.004(3) O2 0.077(4) 0.075(4) 0.080(4) -0.002(3) -0.004(3) -0.001(3) O3 0.078(4) 0.068(4) 0.081(4) 0.007(3) 0.016(3) 0.009(3) O4 0.095(5) 0.084(5) 0.075(4) -0.011(4) 0.008(3) 0.001(4) O5 0.079(4) 0.084(5) 0.073(4) -0.006(4) 0.011(3) -0.003(4) O6 0.069(4) 0.110(5) 0.079(4) 0.005(4) 0.017(3) -0.009(4) O7 0.068(4) 0.076(4) 0.089(4) 0.004(3) 0.008(3) -0.009(3) O8 0.096(5) 0.111(6) 0.116(6) 0.022(5) 0.015(4) 0.028(5) O9 0.055(4) 0.121(6) 0.111(5) 0.004(4) 0.001(4) 0.003(4) O10 0.092(5) 0.085(5) 0.078(4) 0.021(4) 0.009(3) 0.007(4) O11 0.089(5) 0.169(8) 0.092(5) 0.014(5) -0.010(4) -0.033(5) O12 0.083(5) 0.122(6) 0.105(5) 0.008(5) -0.029(4) 0.012(4) O13 0.084(5) 0.119(7) 0.129(7) 0.006(5) 0.020(5) -0.025(5) O14 0.133(7) 0.107(6) 0.103(5) 0.037(5) 0.036(5) 0.021(5) O15 0.084(5) 0.133(7) 0.091(5) 0.018(5) 0.026(4) 0.009(5) O16 0.124(6) 0.094(5) 0.105(5) 0.007(4) 0.049(5) 0.039(5) O17 0.18(4) 0.18(3) 0.14(2) 0.073(18) 0.06(2) 0.12(3) O18 0.164(19) 0.22(2) 0.130(14) 0.035(15) -0.030(12) -0.117(18) O17A 0.131(19) 0.078(14) 0.16(2) 0.044(13) 0.063(16) 0.052(13) O18A 0.044(12) 0.34(9) 0.21(6) 0.15(6) -0.01(2) 0.02(3) C1 0.112(9) 0.053(6) 0.105(8) -0.005(6) 0.012(7) 0.015(6) C2 0.109(10) 0.092(9) 0.146(12) -0.016(8) -0.004(8) -0.026(8) C3 0.119(10) 0.122(11) 0.114(10) -0.005(8) -0.008(8) -0.026(8) C4 0.142(11) 0.091(8) 0.123(10) 0.009(7) 0.001(8) 0.051(8) C5 0.146(14) 0.093(11) 0.164(15) -0.043(10) -0.026(11) -0.004(10) C6 0.112(11) 0.119(12) 0.167(14) -0.045(10) 0.010(10) -0.008(10) C7 0.32(3) 0.121(12) 0.135(13) -0.053(10) 0.070(14) -0.069(14) C8 0.124(12) 0.177(16) 0.184(18) -0.043(14) 0.066(12) -0.038(11) C9 0.23(2) 0.137(15) 0.22(2) 0.040(14) 0.112(19) 0.077(15) C10 0.104(11) 0.165(15) 0.26(2) 0.021(14) -0.057(13) -0.043(11) C11 0.22(2) 0.166(16) 0.140(14) -0.005(11) -0.010(13) -0.050(15) C13 0.29(3) 0.31(3) 0.22(3) 0.07(2) 0.17(3) 0.14(2) C14 0.145(19) 0.23(3) 0.23(3) 0.017(19) 0.039(19) -0.016(17) C15 0.33(3) 0.121(15) 0.25(2) -0.074(16) 0.12(2) -0.044(18) C16 0.24(3) 0.34(3) 0.185(19) -0.13(2) 0.081(18) -0.06(2) C17 0.26(3) 0.25(3) 0.26(3) -0.01(2) 0.10(2) -0.12(2) C18 0.27(3) 0.27(3) 0.36(4) 0.15(3) 0.14(3) 0.13(3) C19 0.17(2) 0.35(3) 0.22(3) -0.07(2) -0.03(2) -0.09(2) C20 0.20(3) 0.47(6) 0.39(5) 0.09(4) 0.05(3) -0.17(3) C21 0.25(3) 0.22(3) 0.48(5) -0.01(3) -0.20(3) -0.01(2) C24 0.34(4) 0.25(3) 0.40(5) -0.18(3) -0.13(4) -0.02(3) C22 0.23(3) 0.28(3) 0.42(4) -0.19(3) 0.00(3) 0.11(2) C29 0.13(2) 0.72(10) 0.34(5) 0.21(5) -0.06(2) -0.16(4) C30 0.47(7) 0.68(9) 0.19(3) -0.11(4) -0.09(4) -0.14(6) _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 O8 1.839(8) . ? Ta1 O11 1.850(8) . ? Ta1 O15 1.855(7) . ? Ta1 O6 2.065(6) . ? Ta1 O7 2.106(6) . ? Ta1 O5 2.113(7) . ? Ta1 Mo2 3.2106(10) . ? Ta2 O13 1.836(8) . ? Ta2 O16 1.851(7) . ? Ta2 O14 1.859(7) . ? Ta2 O10 2.065(6) . ? Ta2 O3 2.110(6) . ? Ta2 O4 2.120(7) . ? Ta2 Mo1 3.2323(10) . ? Mo1 O12 1.675(7) . ? Mo1 O1 1.913(6) . ? Mo1 O2 1.921(6) . ? Mo1 O3 2.071(6) . ? Mo1 O4 2.080(6) . ? Mo1 Mo2 2.5728(12) . ? Mo2 O9 1.679(6) . ? Mo2 O2 1.896(6) . ? Mo2 O1 1.919(6) . ? Mo2 O7 2.089(6) . ? Mo2 O5 2.086(6) . ? Mo3 Mo3A 0.882(6) . ? Mo3 O17 1.40(3) . ? Mo3 O17A 1.65(2) . ? Mo3 O18A 1.74(4) . ? Mo3 O10 1.808(7) . ? Mo3 O6 1.845(7) . ? Mo3A O18A 1.36(3) . ? Mo3A O17 1.63(2) . ? Mo3A O18 1.691(18) . ? Mo3A O6 1.827(6) . ? Mo3A O10 1.827(7) . ? Mo3A O17A 2.49(2) . ? O3 C1 1.456(11) . ? O4 C5 1.415(15) . ? O5 C6 1.433(15) . ? O7 C2 1.419(13) . ? O8 C12 1.55(3) . ? O11 C19 1.46(2) . ? O13 C14 1.46(2) . ? O14 C23 1.92(3) . ? O15 C8 1.438(15) . ? O16 C9 1.389(18) . ? O17 O18A 1.07(6) . ? O17 O17A 1.79(4) . ? O18 O18A 1.68(6) . ? C1 C3 1.515(16) . ? C1 C4 1.574(15) . ? C2 C7 1.479(19) . ? C2 C10 1.539(18) . ? C5 C24 1.42(3) . ? C5 C15 1.47(3) . ? C6 C11 1.44(2) . ? C6 C22 1.48(3) . ? C8 C17 1.41(3) . ? C8 C16 1.46(2) . ? C9 C18 1.29(3) . ? C9 C13 1.37(2) . ? C14 C20 1.42(3) . ? C14 C21 1.46(3) . ? C19 C29 1.18(3) . ? C19 C30 1.46(4) . ? C23 C28 1.20(4) . ? C23 C27 1.41(5) . ? C12 C25 1.33(5) . ? C12 C26 1.35(4) . ? 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 O8 Ta1 O11 99.7(4) . . ? O8 Ta1 O15 97.8(3) . . ? O11 Ta1 O15 98.4(4) . . ? O8 Ta1 O6 91.9(3) . . ? O11 Ta1 O6 92.5(3) . . ? O15 Ta1 O6 163.9(3) . . ? O8 Ta1 O7 94.0(3) . . ? O11 Ta1 O7 162.7(3) . . ? O15 Ta1 O7 90.2(3) . . ? O6 Ta1 O7 76.3(2) . . ? O8 Ta1 O5 163.0(3) . . ? O11 Ta1 O5 93.5(3) . . ? O15 Ta1 O5 90.7(3) . . ? O6 Ta1 O5 76.8(3) . . ? O7 Ta1 O5 71.3(2) . . ? O8 Ta1 Mo2 123.2(3) . . ? O11 Ta1 Mo2 122.8(3) . . ? O15 Ta1 Mo2 109.7(2) . . ? O6 Ta1 Mo2 54.23(19) . . ? O7 Ta1 Mo2 39.87(17) . . ? O5 Ta1 Mo2 39.82(17) . . ? O13 Ta2 O16 100.8(4) . . ? O13 Ta2 O14 97.1(4) . . ? O16 Ta2 O14 97.8(3) . . ? O13 Ta2 O10 92.1(3) . . ? O16 Ta2 O10 92.4(3) . . ? O14 Ta2 O10 164.7(3) . . ? O13 Ta2 O3 94.7(3) . . ? O16 Ta2 O3 161.5(3) . . ? O14 Ta2 O3 90.1(3) . . ? O10 Ta2 O3 76.9(2) . . ? O13 Ta2 O4 163.7(3) . . ? O16 Ta2 O4 91.8(3) . . ? O14 Ta2 O4 91.4(3) . . ? O10 Ta2 O4 76.9(3) . . ? O3 Ta2 O4 71.3(2) . . ? O13 Ta2 Mo1 124.5(3) . . ? O16 Ta2 Mo1 122.7(3) . . ? O14 Ta2 Mo1 108.1(2) . . ? O10 Ta2 Mo1 56.62(19) . . ? O3 Ta2 Mo1 38.92(17) . . ? O4 Ta2 Mo1 39.23(17) . . ? O12 Mo1 O1 108.4(3) . . ? O12 Mo1 O2 107.7(3) . . ? O1 Mo1 O2 91.5(3) . . ? O12 Mo1 O3 104.6(3) . . ? O1 Mo1 O3 88.5(2) . . ? O2 Mo1 O3 145.9(3) . . ? O12 Mo1 O4 102.3(3) . . ? O1 Mo1 O4 147.3(3) . . ? O2 Mo1 O4 89.7(3) . . ? O3 Mo1 O4 72.9(3) . . ? O12 Mo1 Mo2 101.5(3) . . ? O1 Mo1 Mo2 47.93(18) . . ? O2 Mo1 Mo2 47.21(19) . . ? O3 Mo1 Mo2 134.67(18) . . ? O4 Mo1 Mo2 135.50(19) . . ? O12 Mo1 Ta2 124.6(3) . . ? O1 Mo1 Ta2 109.96(17) . . ? O2 Mo1 Ta2 109.75(19) . . ? O3 Mo1 Ta2 39.82(16) . . ? O4 Mo1 Ta2 40.14(19) . . ? Mo2 Mo1 Ta2 133.97(4) . . ? O9 Mo2 O2 108.4(3) . . ? O9 Mo2 O1 109.0(3) . . ? O2 Mo2 O1 92.1(3) . . ? O9 Mo2 O7 100.4(3) . . ? O2 Mo2 O7 90.6(3) . . ? O1 Mo2 O7 147.9(3) . . ? O9 Mo2 O5 102.3(3) . . ? O2 Mo2 O5 147.1(3) . . ? O1 Mo2 O5 88.9(2) . . ? O7 Mo2 O5 72.1(3) . . ? O9 Mo2 Mo1 102.5(2) . . ? O2 Mo2 Mo1 48.04(19) . . ? O1 Mo2 Mo1 47.74(17) . . ? O7 Mo2 Mo1 137.38(18) . . ? O5 Mo2 Mo1 135.25(18) . . ? O9 Mo2 Ta1 123.6(2) . . ? O2 Mo2 Ta1 109.61(19) . . ? O1 Mo2 Ta1 109.64(17) . . ? O7 Mo2 Ta1 40.27(18) . . ? O5 Mo2 Ta1 40.45(18) . . ? Mo1 Mo2 Ta1 133.96(3) . . ? Mo3A Mo3 O17 87.7(16) . . ? Mo3A Mo3 O17A 159.0(9) . . ? O17 Mo3 O17A 71.4(15) . . ? Mo3A Mo3 O18A 50(2) . . ? O17 Mo3 O18A 38(2) . . ? O17A Mo3 O18A 109(2) . . ? Mo3A Mo3 O10 77.2(5) . . ? O17 Mo3 O10 121.8(15) . . ? O17A Mo3 O10 115.4(9) . . ? O18A Mo3 O10 106.2(18) . . ? Mo3A Mo3 O6 74.9(5) . . ? O17 Mo3 O6 120.5(14) . . ? O17A Mo3 O6 113.4(8) . . ? O18A Mo3 O6 102.6(19) . . ? O10 Mo3 O6 109.0(4) . . ? Mo3 Mo3A O18A 100(3) . . ? Mo3 Mo3A O17 59.5(13) . . ? O18A Mo3A O17 41(3) . . ? Mo3 Mo3A O18 165.8(11) . . ? O18A Mo3A O18 66(3) . . ? O17 Mo3A O18 106.4(14) . . ? Mo3 Mo3A O6 77.3(4) . . ? O18A Mo3A O6 123(2) . . ? O17 Mo3A O6 109.9(13) . . ? O18 Mo3A O6 111.3(8) . . ? Mo3 Mo3A O10 74.7(4) . . ? O18A Mo3A O10 126(2) . . ? O17 Mo3A O10 108.9(12) . . ? O18 Mo3A O10 111.3(7) . . ? O6 Mo3A O10 109.0(3) . . ? Mo3 Mo3A O17A 13.7(6) . . ? O18A Mo3A O17A 87(3) . . ? O17 Mo3A O17A 45.9(13) . . ? O18 Mo3A O17A 152.2(11) . . ? O6 Mo3A O17A 83.6(5) . . ? O10 Mo3A O17A 83.7(6) . . ? Mo1 O1 Mo2 84.3(2) . . ? Mo2 O2 Mo1 84.7(3) . . ? C1 O3 Mo1 131.4(6) . . ? C1 O3 Ta2 125.1(6) . . ? Mo1 O3 Ta2 101.3(3) . . ? C5 O4 Mo1 130.9(9) . . ? C5 O4 Ta2 125.8(8) . . ? Mo1 O4 Ta2 100.6(3) . . ? C6 O5 Mo2 132.6(8) . . ? C6 O5 Ta1 125.6(8) . . ? Mo2 O5 Ta1 99.7(3) . . ? Mo3A O6 Mo3 27.8(2) . . ? Mo3A O6 Ta1 150.3(4) . . ? Mo3 O6 Ta1 150.7(4) . . ? C2 O7 Mo2 133.1(7) . . ? C2 O7 Ta1 125.7(7) . . ? Mo2 O7 Ta1 99.9(3) . . ? C12 O8 Ta1 158.8(12) . . ? Mo3 O10 Mo3A 28.1(2) . . ? Mo3 O10 Ta2 153.1(4) . . ? Mo3A O10 Ta2 156.7(4) . . ? C19 O11 Ta1 165.2(14) . . ? C14 O13 Ta2 175.7(12) . . ? Ta2 O14 C23 151.1(11) . . ? C8 O15 Ta1 158.9(10) . . ? C9 O16 Ta2 168.4(11) . . ? O18A O17 Mo3 89(3) . . ? O18A O17 Mo3A 56(3) . . ? Mo3 O17 Mo3A 32.8(6) . . ? O18A O17 O17A 149(3) . . ? Mo3 O17 O17A 60.7(14) . . ? Mo3A O17 O17A 93.6(15) . . ? Mo3A O18 O18A 47.5(12) . . ? Mo3 O17A O17 47.8(10) . . ? Mo3 O17A Mo3A 7.3(4) . . ? O17 O17A Mo3A 40.6(8) . . ? O17 O18A Mo3A 83(3) . . ? O17 O18A O18 150(4) . . ? Mo3A O18A O18 67(2) . . ? O17 O18A Mo3 54(2) . . ? Mo3A O18A Mo3 29.9(10) . . ? O18 O18A Mo3 97(2) . . ? O3 C1 C3 110.1(9) . . ? O3 C1 C4 106.2(9) . . ? C3 C1 C4 113.0(10) . . ? O7 C2 C7 114.0(11) . . ? O7 C2 C10 107.8(12) . . ? C7 C2 C10 110.6(15) . . ? O4 C5 C24 108.1(15) . . ? O4 C5 C15 113.3(15) . . ? C24 C5 C15 115(2) . . ? O5 C6 C11 113.1(13) . . ? O5 C6 C22 106.1(14) . . ? C11 C6 C22 111(2) . . ? C17 C8 O15 111.8(16) . . ? C17 C8 C16 111(2) . . ? O15 C8 C16 110.3(15) . . ? C18 C9 C13 123(2) . . ? C18 C9 O16 116(2) . . ? C13 C9 O16 114.7(17) . . ? C20 C14 O13 104(2) . . ? C20 C14 C21 109(3) . . ? O13 C14 C21 107(2) . . ? C29 C19 O11 116(3) . . ? C29 C19 C30 131(4) . . ? O11 C19 C30 109(3) . . ? C28 C23 C27 106(4) . . ? C28 C23 O14 75(3) . . ? C27 C23 O14 75(3) . . ? C25 C12 C26 112(4) . . ? C25 C12 O8 102(3) . . ? C26 C12 O8 112(3) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.966 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.123 #=END data_mowopp1m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ' molybdenum-tungsten oxoisopropoxide ' _chemical_melting_point ? _chemical_formula_moiety 'C36 H84 Mo4.96 O22 W1.04' _chemical_formula_sum 'C36 H84 Mo4.96 O22 W1.04' _chemical_formula_weight 1536.10 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.00(2) _cell_length_b 11.44(2) _cell_length_c 13.29(3) _cell_angle_alpha 98.95(4) _cell_angle_beta 91.64(4) _cell_angle_gamma 106.15(4) _cell_volume 1439(5) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used '999 with I>10sigma(I) ' _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour ' orange brown ' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 761 _exptl_absorpt_coefficient_mu 3.184 _exptl_absorpt_correction_type ' Bruker SADABS' _exptl_absorpt_correction_T_min 0.2510 _exptl_absorpt_correction_T_max 0.6466 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K ' _diffrn_measurement_method ' Bruker SMART ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4138 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.1113 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3526 _reflns_number_gt 1761 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Bruker SMART ' _computing_cell_refinement ' Bruker SMART ' _computing_data_reduction ' Bruker SAINTPLUS ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' SHELXTL 5.3 ' _computing_publication_material ' SHELXTL 5.3 ' _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^)+(0.0938P)^2^+0.0000P] 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 3526 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.131 _refine_ls_shift/su_mean 0.001 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 W1 W 0.28901(12) 0.88826(9) 0.20964(7) 0.0657(6) Uani 0.517(3) 1 d P . . Mo3 Mo 0.28901(12) 0.88826(9) 0.20964(7) 0.0657(6) Uani 0.48 1 d P . . Mo1 Mo 0.01889(16) 0.48851(13) 0.37465(9) 0.0545(6) Uani 1 1 d . . . Mo2 Mo 0.11257(16) 0.60420(13) 0.22779(9) 0.0585(6) Uani 1 1 d . . . O1 O 0.1165(12) 0.4853(9) 0.5124(6) 0.063(3) Uani 1 1 d . . . O2 O 0.3084(10) 0.7124(9) 0.1969(6) 0.055(3) Uani 1 1 d . . . O3 O 0.0825(11) 0.7514(9) 0.1698(7) 0.061(3) Uani 1 1 d . . . O4 O -0.0471(10) 0.6002(9) 0.3071(6) 0.056(3) Uani 1 1 d . . . O5 O 0.2066(11) 0.5501(9) 0.3339(6) 0.058(3) Uani 1 1 d . . . O6 O 0.2196(12) 0.8542(11) 0.3384(8) 0.074(4) Uani 1 1 d . . . O7 O 0.2185(14) 1.0200(10) 0.2133(8) 0.088(4) Uani 1 1 d . . . O8 O 0.4528(13) 0.9566(11) 0.2524(8) 0.084(4) Uani 1 1 d . . . O9 O -0.0496(14) 0.3427(10) 0.3185(8) 0.085(4) Uani 1 1 d . . . O10 O 0.3176(12) 0.8737(10) 0.0729(8) 0.072(3) Uani 1 1 d . . . O11 O 0.0678(14) 0.4901(10) 0.1292(7) 0.085(4) Uani 1 1 d . . . C1 C 0.271(2) 0.9072(17) 0.4405(13) 0.090(7) Uani 1 1 d . . . H1A H 0.3732 0.9377 0.4421 0.108 Uiso 1 1 calc R . . C2 C -0.042(2) 0.7855(18) 0.1510(13) 0.074(6) Uani 1 1 d . . . H2A H -0.0201 0.8440 0.1031 0.088 Uiso 1 1 calc R . . C3 C 0.251(3) 0.820(2) -0.0284(15) 0.112(8) Uani 1 1 d . . . H3A H 0.1500 0.8004 -0.0211 0.134 Uiso 1 1 calc R . . C4 C 0.256(2) 0.465(2) 0.5257(15) 0.098(8) Uani 1 1 d . . . C5 C 0.438(2) 0.679(2) 0.1894(15) 0.095(7) Uani 1 1 d . . . H5A H 0.4958 0.7311 0.1457 0.114 Uiso 1 1 calc R . . C6 C 0.516(2) 0.706(2) 0.2926(18) 0.136(9) Uani 1 1 d . . . H6A H 0.5320 0.7920 0.3211 0.204 Uiso 1 1 calc R . . H6B H 0.6035 0.6883 0.2857 0.204 Uiso 1 1 calc R . . H6C H 0.4615 0.6560 0.3369 0.204 Uiso 1 1 calc R . . C7 C 0.279(3) 0.700(2) -0.0666(16) 0.151(11) Uani 1 1 d . . . H7A H 0.2359 0.6685 -0.1346 0.227 Uiso 1 1 calc R . . H7B H 0.2409 0.6419 -0.0226 0.227 Uiso 1 1 calc R . . H7C H 0.3777 0.7124 -0.0672 0.227 Uiso 1 1 calc R . . C8 C 0.241(2) 0.335(2) 0.5044(17) 0.142(10) Uani 1 1 d . . . H8B H 0.1799 0.2988 0.4437 0.213 Uiso 1 1 calc R . . H8C H 0.2014 0.2978 0.5608 0.213 Uiso 1 1 calc R . . H8D H 0.3304 0.3220 0.4945 0.213 Uiso 1 1 calc R . . C9 C -0.148(2) 0.6780(19) 0.0976(13) 0.092(7) Uani 1 1 d . . . H9B H -0.1109 0.6413 0.0392 0.137 Uiso 1 1 calc R . . H9C H -0.2274 0.7024 0.0756 0.137 Uiso 1 1 calc R . . H9D H -0.1771 0.6190 0.1425 0.137 Uiso 1 1 calc R . . C10 C -0.084(2) 0.8543(18) 0.2460(13) 0.115(8) Uani 1 1 d . . . H10A H -0.1655 0.8787 0.2289 0.173 Uiso 1 1 calc R . . H10B H -0.0092 0.9263 0.2728 0.173 Uiso 1 1 calc R . . H10C H -0.1054 0.8014 0.2963 0.173 Uiso 1 1 calc R . . C11 C 0.410(3) 0.548(2) 0.1394(19) 0.147(10) Uani 1 1 d . . . H11B H 0.3636 0.5360 0.0729 0.221 Uiso 1 1 calc R . . H11C H 0.3519 0.4950 0.1802 0.221 Uiso 1 1 calc R . . H11D H 0.4968 0.5278 0.1331 0.221 Uiso 1 1 calc R . . C12 C 0.230(4) 1.130(2) 0.188(3) 0.25(2) Uani 1 1 d . . . H12A H 0.2643 1.1117 0.1213 0.296 Uiso 1 1 calc R . . C13 C 0.281(3) 0.907(2) -0.1021(17) 0.146(10) Uani 1 1 d . . . H13A H 0.2331 0.8666 -0.1673 0.219 Uiso 1 1 calc R . . H13B H 0.3794 0.9334 -0.1088 0.219 Uiso 1 1 calc R . . H13C H 0.2491 0.9776 -0.0779 0.219 Uiso 1 1 calc R . . C14 C 0.238(4) 0.829(2) 0.5095(17) 0.26(2) Uani 1 1 d . . . H14A H 0.2590 0.8762 0.5774 0.390 Uiso 1 1 calc R . . H14B H 0.2923 0.7714 0.5002 0.390 Uiso 1 1 calc R . . H14C H 0.1408 0.7855 0.4995 0.390 Uiso 1 1 calc R . . C15 C 0.337(2) 0.545(2) 0.6154(18) 0.124(8) Uani 1 1 d . . . H15A H 0.3303 0.6272 0.6173 0.186 Uiso 1 1 calc R . . H15B H 0.4324 0.5447 0.6128 0.186 Uiso 1 1 calc R . . H15C H 0.3004 0.5146 0.6756 0.186 Uiso 1 1 calc R . . C16 C 0.367(4) 1.227(3) 0.236(3) 0.210(15) Uani 1 1 d . . . H16A H 0.3853 1.2973 0.2018 0.314 Uiso 1 1 calc R . . H16B H 0.4433 1.1913 0.2294 0.314 Uiso 1 1 calc R . . H16C H 0.3586 1.2536 0.3074 0.314 Uiso 1 1 calc R . . C17 C 0.132(4) 1.171(3) 0.156(2) 0.205(16) Uani 1 1 d . . . H17A H 0.1719 1.2499 0.1365 0.307 Uiso 1 1 calc R . . H17B H 0.0701 1.1788 0.2087 0.307 Uiso 1 1 calc R . . H17C H 0.0803 1.1139 0.0975 0.307 Uiso 1 1 calc R . . C18 C 0.221(4) 1.007(3) 0.4762(19) 0.26(2) Uani 1 1 d . . . H18A H 0.2645 1.0455 0.5429 0.383 Uiso 1 1 calc R . . H18B H 0.1216 0.9779 0.4799 0.383 Uiso 1 1 calc R . . H18C H 0.2415 1.0655 0.4304 0.383 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 W1 0.0532(12) 0.0758(10) 0.0682(7) 0.0207(5) 0.0099(5) 0.0133(8) Mo3 0.0532(12) 0.0758(10) 0.0682(7) 0.0207(5) 0.0099(5) 0.0133(8) Mo1 0.0436(14) 0.0696(13) 0.0530(8) 0.0171(7) 0.0099(6) 0.0166(10) Mo2 0.0481(14) 0.0801(13) 0.0497(8) 0.0160(7) 0.0099(7) 0.0189(11) O1 0.060(10) 0.095(8) 0.048(5) 0.032(5) 0.010(5) 0.030(8) O2 0.000(8) 0.105(9) 0.060(6) 0.012(5) 0.016(4) 0.016(7) O3 0.049(10) 0.076(8) 0.069(6) 0.021(5) 0.009(5) 0.031(7) O4 0.034(9) 0.085(8) 0.060(6) 0.034(5) 0.022(5) 0.021(7) O5 0.041(9) 0.075(8) 0.061(6) 0.015(5) 0.005(5) 0.020(7) O6 0.018(9) 0.128(11) 0.071(7) 0.015(6) 0.016(5) 0.013(8) O7 0.096(14) 0.040(8) 0.112(9) 0.017(6) 0.013(8) -0.006(8) O8 0.040(11) 0.092(10) 0.098(9) 0.005(6) -0.005(7) -0.012(8) O9 0.107(13) 0.078(9) 0.080(7) 0.037(6) 0.027(7) 0.028(9) O10 0.013(9) 0.094(10) 0.095(9) 0.020(6) 0.021(6) -0.011(7) O11 0.098(12) 0.102(10) 0.057(6) 0.008(6) 0.008(6) 0.035(9) C1 0.10(2) 0.084(15) 0.080(13) 0.023(11) 0.032(12) 0.015(15) C2 0.039(17) 0.093(16) 0.085(13) 0.024(11) -0.003(10) 0.010(15) C3 0.11(2) 0.16(2) 0.077(14) 0.016(14) 0.026(13) 0.048(19) C4 0.09(2) 0.15(2) 0.088(13) 0.043(13) 0.015(12) 0.077(18) C5 0.08(2) 0.102(18) 0.112(16) 0.022(12) 0.037(13) 0.033(16) C6 0.10(3) 0.17(2) 0.15(2) 0.068(17) 0.005(17) 0.045(19) C7 0.16(3) 0.21(3) 0.089(16) 0.038(16) 0.023(16) 0.06(2) C8 0.09(3) 0.18(3) 0.17(2) 0.001(17) 0.003(15) 0.08(2) C9 0.06(2) 0.131(19) 0.099(14) 0.035(12) 0.033(12) 0.047(17) C10 0.15(3) 0.122(18) 0.096(15) 0.024(12) 0.023(14) 0.064(18) C11 0.12(3) 0.13(2) 0.21(3) 0.057(19) 0.06(2) 0.05(2) C12 0.26(5) 0.041(16) 0.39(5) 0.06(2) -0.21(4) -0.03(2) C13 0.17(3) 0.15(2) 0.132(19) 0.072(16) 0.004(17) 0.04(2) C14 0.52(7) 0.083(19) 0.087(17) 0.023(13) 0.00(3) -0.06(3) C15 0.04(2) 0.14(2) 0.17(2) 0.033(17) -0.008(15) 0.002(15) C16 0.15(4) 0.18(3) 0.30(4) 0.05(3) 0.08(3) 0.04(3) C17 0.23(5) 0.21(3) 0.25(3) 0.12(3) 0.05(3) 0.15(3) C18 0.38(6) 0.28(4) 0.14(3) -0.08(3) -0.07(3) 0.23(4) _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 W1 O8 1.648(13) . ? W1 O7 1.828(12) . ? W1 O10 1.837(11) . ? W1 O6 1.920(11) . ? W1 O2 2.055(11) . ? W1 O3 2.208(12) . ? Mo1 O9 1.659(12) . ? Mo1 O4 1.915(9) . ? Mo1 O5 1.938(11) . ? Mo1 O1 2.061(9) . ? Mo1 O1 2.093(10) 2_566 ? Mo1 Mo2 2.580(4) . ? Mo2 O11 1.652(10) . ? Mo2 O4 1.933(9) . ? Mo2 O5 1.943(9) . ? Mo2 O3 2.047(9) . ? Mo2 O2 2.096(11) . ? O1 C4 1.49(2) . ? O1 Mo1 2.093(10) 2_566 ? O2 C5 1.45(2) . ? O3 C2 1.436(19) . ? O6 C1 1.416(19) . ? O7 C12 1.33(2) . ? O10 C3 1.45(2) . ? C1 C14 1.36(2) . ? C1 C18 1.39(3) . ? C2 C9 1.45(2) . ? C2 C10 1.51(2) . ? C3 C13 1.48(3) . ? C3 C7 1.49(3) . ? C4 C8 1.43(3) . ? C4 C15 1.45(3) . ? C5 C11 1.49(3) . ? C5 C6 1.50(3) . ? C12 C17 1.29(4) . ? C12 C16 1.56(4) . ? 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 O8 W1 O7 101.8(6) . . ? O8 W1 O10 96.9(5) . . ? O7 W1 O10 95.2(5) . . ? O8 W1 O6 96.9(5) . . ? O7 W1 O6 92.6(5) . . ? O10 W1 O6 162.3(5) . . ? O8 W1 O2 94.6(5) . . ? O7 W1 O2 163.4(5) . . ? O10 W1 O2 85.4(4) . . ? O6 W1 O2 82.7(4) . . ? O8 W1 O3 163.3(5) . . ? O7 W1 O3 93.4(5) . . ? O10 W1 O3 88.5(4) . . ? O6 W1 O3 75.2(4) . . ? O2 W1 O3 70.0(4) . . ? O9 Mo1 O4 111.9(5) . . ? O9 Mo1 O5 109.6(5) . . ? O4 Mo1 O5 92.3(4) . . ? O9 Mo1 O1 107.0(5) . . ? O4 Mo1 O1 139.5(4) . . ? O5 Mo1 O1 84.9(4) . . ? O9 Mo1 O1 104.0(5) . 2_566 ? O4 Mo1 O1 87.1(4) . 2_566 ? O5 Mo1 O1 143.9(4) . 2_566 ? O1 Mo1 O1 72.8(5) . 2_566 ? O9 Mo1 Mo2 104.5(4) . . ? O4 Mo1 Mo2 48.2(3) . . ? O5 Mo1 Mo2 48.4(3) . . ? O1 Mo1 Mo2 130.3(3) . . ? O1 Mo1 Mo2 133.5(3) 2_566 . ? O11 Mo2 O4 108.9(6) . . ? O11 Mo2 O5 107.9(5) . . ? O4 Mo2 O5 91.6(4) . . ? O11 Mo2 O3 103.4(5) . . ? O4 Mo2 O3 89.6(4) . . ? O5 Mo2 O3 146.4(4) . . ? O11 Mo2 O2 104.2(5) . . ? O4 Mo2 O2 145.2(4) . . ? O5 Mo2 O2 88.1(4) . . ? O3 Mo2 O2 72.5(4) . . ? O11 Mo2 Mo1 100.9(4) . . ? O4 Mo2 Mo1 47.6(3) . . ? O5 Mo2 Mo1 48.2(3) . . ? O3 Mo2 Mo1 136.0(3) . . ? O2 Mo2 Mo1 134.8(2) . . ? C4 O1 Mo1 125.1(9) . . ? C4 O1 Mo1 127.7(9) . 2_566 ? Mo1 O1 Mo1 107.2(5) . 2_566 ? C5 O2 W1 125.8(11) . . ? C5 O2 Mo2 128.4(11) . . ? W1 O2 Mo2 104.7(4) . . ? C2 O3 Mo2 130.9(11) . . ? C2 O3 W1 122.9(11) . . ? Mo2 O3 W1 101.1(4) . . ? Mo1 O4 Mo2 84.2(4) . . ? Mo1 O5 Mo2 83.3(4) . . ? C1 O6 W1 132.1(12) . . ? C12 O7 W1 148(2) . . ? C3 O10 W1 143.6(13) . . ? C14 C1 C18 106(2) . . ? C14 C1 O6 115.2(19) . . ? C18 C1 O6 111.5(18) . . ? O3 C2 C9 108.8(15) . . ? O3 C2 C10 112.5(14) . . ? C9 C2 C10 116.3(18) . . ? O10 C3 C13 113(2) . . ? O10 C3 C7 111.6(18) . . ? C13 C3 C7 113.0(19) . . ? C8 C4 C15 122.4(17) . . ? C8 C4 O1 109(2) . . ? C15 C4 O1 111.6(17) . . ? O2 C5 C11 110.3(18) . . ? O2 C5 C6 110.5(16) . . ? C11 C5 C6 112.6(18) . . ? C17 C12 O7 128(3) . . ? C17 C12 C16 117(3) . . ? O7 C12 C16 112(2) . . ? _diffrn_measured_fraction_theta_max 0.695 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.695 _refine_diff_density_max 1.215 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.167 #=END data_motan2m _audit_creation_method SHELXL-97 _chemical_name_systematic ditantalumdimethoxooctaisopropoxide _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H62 O10 Ta2' _chemical_formula_sum 'C26 H62 O10 Ta2' _chemical_formula_weight 896.66 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' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.137(2) _cell_length_b 9.865(2) _cell_length_c 12.474(3) _cell_angle_alpha 111.551(4) _cell_angle_beta 98.789(4) _cell_angle_gamma 104.757(4) _cell_volume 972.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ' 999 with I>2sigma(I) ' _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 24.99 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 444 _exptl_absorpt_coefficient_mu 5.662 _exptl_absorpt_correction_type 'Bruker SADABS ' _exptl_absorpt_correction_T_min 0.1468 _exptl_absorpt_correction_T_max 0.4839 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD 1K ' _diffrn_measurement_method 'Bruker SMART ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4752 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3347 _reflns_number_gt 2081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART ' _computing_cell_refinement 'Bruker SMART ' _computing_data_reduction ' Bruker SAINTPLUS ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' Bruker SHELXTL 5.3 ' _computing_publication_material 'Bruker SHELXTL 5.3 ' _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^)+(0.0420P)^2^+0.0000P] 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 3347 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 0.798 _refine_ls_restrained_S_all 0.798 _refine_ls_shift/su_max 1.993 _refine_ls_shift/su_mean 0.089 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 0.50048(5) 0.07115(4) 0.14980(3) 0.06673(17) Uani 1 1 d . . . O1 O 0.6069(6) -0.0454(6) 0.0231(4) 0.0601(14) Uani 1 1 d . . . O2 O 0.3464(8) -0.1106(8) 0.1183(5) 0.094(2) Uani 1 1 d . . . O3 O 0.6467(7) 0.2528(9) 0.1778(5) 0.098(2) Uani 1 1 d . . . O4 O 0.3769(8) 0.1831(8) 0.2259(6) 0.113(2) Uani 1 1 d . . . O5 O 0.6292(8) 0.0543(8) 0.2714(6) 0.104(2) Uani 1 1 d . . . C1 C 0.7518(14) -0.0638(17) 0.0504(10) 0.152(6) Uani 1 1 d . . . H1A H 0.8251 0.0306 0.1139 0.228 Uiso 1 1 calc R . . H1B H 0.7904 -0.0888 -0.0193 0.228 Uiso 1 1 calc R . . H1C H 0.7399 -0.1461 0.0756 0.228 Uiso 1 1 calc R . . C3 C 0.737(2) 0.089(3) 0.3656(16) 0.232(10) Uani 1 1 d . . . H3 H 0.8210 0.1617 0.3533 0.278 Uiso 1 1 calc R . . C4 C 0.243(2) -0.220(2) 0.135(2) 0.198(8) Uani 1 1 d . . . H4 H 0.2540 -0.1463 0.2169 0.238 Uiso 1 1 calc R . . C5 C 0.724(2) 0.410(2) 0.208(2) 0.221(9) Uani 1 1 d . . . H5 H 0.7833 0.3921 0.1485 0.265 Uiso 1 1 calc R . . C51 C 0.849(2) 0.496(2) 0.3033(18) 0.244(11) Uani 1 1 d . . . H51A H 0.8202 0.4999 0.3748 0.367 Uiso 1 1 calc R . . H51B H 0.8869 0.5991 0.3085 0.367 Uiso 1 1 calc R . . H51C H 0.9308 0.4511 0.2945 0.367 Uiso 1 1 calc R . . C21 C 0.212(2) 0.330(2) 0.2568(18) 0.236(10) Uani 1 1 d . . . H21A H 0.1975 0.3050 0.1731 0.354 Uiso 1 1 calc R . . H21B H 0.2629 0.4397 0.3026 0.354 Uiso 1 1 calc R . . H21C H 0.1116 0.2986 0.2717 0.354 Uiso 1 1 calc R . . C52 C 0.633(3) 0.482(2) 0.159(2) 0.252(11) Uani 1 1 d . . . H52A H 0.6286 0.4510 0.0758 0.378 Uiso 1 1 calc R . . H52B H 0.6804 0.5927 0.2013 0.378 Uiso 1 1 calc R . . H52C H 0.5279 0.4515 0.1670 0.378 Uiso 1 1 calc R . . C41 C 0.0837(19) -0.2332(19) 0.0986(19) 0.229(9) Uani 1 1 d . . . H41A H 0.0335 -0.2397 0.1596 0.344 Uiso 1 1 calc R . . H41B H 0.0312 -0.3250 0.0253 0.344 Uiso 1 1 calc R . . H41C H 0.0784 -0.1442 0.0859 0.344 Uiso 1 1 calc R . . C42 C 0.284(3) -0.319(2) 0.176(2) 0.257(11) Uani 1 1 d . . . H42A H 0.3793 -0.3309 0.1568 0.385 Uiso 1 1 calc R . . H42B H 0.2016 -0.4176 0.1386 0.385 Uiso 1 1 calc R . . H42C H 0.3011 -0.2777 0.2613 0.385 Uiso 1 1 calc R . . C2 C 0.302(3) 0.256(3) 0.2890(17) 0.243(11) Uani 1 1 d . . . H2 H 0.3935 0.3509 0.3264 0.292 Uiso 1 1 calc R . . C31 C 0.817(3) -0.008(3) 0.3790(19) 0.271(12) Uani 1 1 d . . . H31A H 0.7452 -0.0979 0.3785 0.406 Uiso 1 1 calc R . . H31B H 0.8980 0.0461 0.4537 0.406 Uiso 1 1 calc R . . H31C H 0.8641 -0.0382 0.3142 0.406 Uiso 1 1 calc R . . C22 C 0.306(3) 0.248(2) 0.4049(17) 0.265(11) Uani 1 1 d . . . H22A H 0.3087 0.1482 0.3974 0.398 Uiso 1 1 calc R . . H22B H 0.2146 0.2634 0.4286 0.398 Uiso 1 1 calc R . . H22C H 0.3990 0.3271 0.4643 0.398 Uiso 1 1 calc R . . C32 C 0.723(3) 0.197(3) 0.4745(16) 0.311(15) Uani 1 1 d . . . H32A H 0.7181 0.2886 0.4659 0.466 Uiso 1 1 calc R . . H32B H 0.8125 0.2237 0.5391 0.466 Uiso 1 1 calc R . . H32C H 0.6287 0.1505 0.4915 0.466 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 0.0769(3) 0.0749(3) 0.0517(2) 0.02389(19) 0.02188(17) 0.0329(2) O1 0.062(3) 0.076(4) 0.057(3) 0.033(3) 0.013(3) 0.040(3) O2 0.103(5) 0.111(5) 0.092(5) 0.061(4) 0.045(4) 0.035(4) O3 0.090(5) 0.101(5) 0.075(4) 0.014(4) 0.012(4) 0.030(4) O4 0.127(6) 0.139(6) 0.080(5) 0.019(5) 0.054(4) 0.083(5) O5 0.106(5) 0.142(6) 0.068(5) 0.039(5) 0.014(4) 0.060(5) C1 0.152(11) 0.265(16) 0.084(8) 0.069(10) 0.031(8) 0.153(12) C3 0.23(2) 0.35(3) 0.119(15) 0.056(18) 0.009(14) 0.19(2) C4 0.134(14) 0.181(16) 0.34(3) 0.166(18) 0.072(16) 0.062(13) C5 0.178(18) 0.169(18) 0.28(3) 0.10(2) 0.009(17) 0.036(16) C51 0.186(17) 0.161(17) 0.22(2) -0.017(15) -0.011(15) -0.027(14) C21 0.28(2) 0.233(19) 0.30(3) 0.116(18) 0.135(19) 0.204(18) C52 0.30(3) 0.177(17) 0.38(3) 0.18(2) 0.14(2) 0.128(18) C41 0.137(13) 0.195(17) 0.36(3) 0.118(18) 0.092(16) 0.053(13) C42 0.32(3) 0.190(17) 0.33(3) 0.20(2) 0.07(2) 0.070(17) C2 0.42(3) 0.33(3) 0.160(17) 0.142(18) 0.19(2) 0.28(3) C31 0.30(3) 0.42(3) 0.26(2) 0.23(3) 0.080(19) 0.24(3) C22 0.43(3) 0.29(2) 0.183(19) 0.099(18) 0.21(2) 0.23(2) C32 0.30(3) 0.44(4) 0.086(13) 0.000(18) 0.026(15) 0.15(3) _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 O3 1.815(8) . ? Ta1 O2 1.838(7) . ? Ta1 O5 1.857(7) . ? Ta1 O4 1.895(6) . ? Ta1 O1 2.114(5) . ? Ta1 O1 2.122(5) 2_655 ? O1 C1 1.390(10) . ? O1 Ta1 2.122(5) 2_655 ? O2 C4 1.344(16) . ? O3 C5 1.405(19) . ? O4 C2 1.269(16) . ? O5 C3 1.282(16) . ? C3 C31 1.39(2) . ? C3 C32 1.43(2) . ? C4 C42 1.360(19) . ? C4 C41 1.412(18) . ? C5 C51 1.34(2) . ? C5 C52 1.43(2) . ? C21 C2 1.33(2) . ? C2 C22 1.47(2) . ? 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 O3 Ta1 O2 177.7(3) . . ? O3 Ta1 O5 90.4(3) . . ? O2 Ta1 O5 91.8(3) . . ? O3 Ta1 O4 89.3(3) . . ? O2 Ta1 O4 89.4(3) . . ? O5 Ta1 O4 105.1(3) . . ? O3 Ta1 O1 88.6(2) . . ? O2 Ta1 O1 92.1(2) . . ? O5 Ta1 O1 91.1(2) . . ? O4 Ta1 O1 163.7(2) . . ? O3 Ta1 O1 90.6(2) . 2_655 ? O2 Ta1 O1 87.6(2) . 2_655 ? O5 Ta1 O1 160.8(2) . 2_655 ? O4 Ta1 O1 94.1(3) . 2_655 ? O1 Ta1 O1 69.8(2) . 2_655 ? C1 O1 Ta1 125.3(6) . . ? C1 O1 Ta1 122.2(6) . 2_655 ? Ta1 O1 Ta1 110.2(2) . 2_655 ? C4 O2 Ta1 160.7(10) . . ? C5 O3 Ta1 163.0(10) . . ? C2 O4 Ta1 172.5(11) . . ? C3 O5 Ta1 161.6(13) . . ? O5 C3 C31 124(2) . . ? O5 C3 C32 114.9(17) . . ? C31 C3 C32 115.3(18) . . ? O2 C4 C42 123.4(16) . . ? O2 C4 C41 115.0(15) . . ? C42 C4 C41 121.4(17) . . ? C51 C5 O3 122(2) . . ? C51 C5 C52 120(2) . . ? O3 C5 C52 115.1(17) . . ? O4 C2 C21 126.1(17) . . ? O4 C2 C22 116.0(17) . . ? C21 C2 C22 117.8(16) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.079 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.118