data_ncet _publ_requested_journal J.Am.Chem.Soc. _publ_contact_author_name 'Daniel, Charles' _publ_contact_author_address ;Institut f\"ur Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_author_email charles.daniel@web.de _publ_contact_author_phone '+49 30 838-52446' _publ_contact_author_fax '+49 30 838-53310' loop_ _publ_author_name _publ_author_address 'Daniel, Charles' ;Institut f\"ur Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Germany ; 'Hartl, Hans' ;Institut f\"ur Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Germany ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m6-oxo-dodeca-\m-ethoxo-hexakis(oxovanadium) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 O19 V6' _chemical_formula_weight 958.36 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.338(4) _cell_length_b 17.760(8) _cell_length_c 11.002(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.408(8) _cell_angle_gamma 90.00 _cell_volume 1937.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 933 _cell_measurement_theta_min 5.996 _cell_measurement_theta_max 55.125 _exptl_crystal_description rhombohedron _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745824 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'ccd area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time '20 sec / frame' _diffrn_standards_decay_% ? _diffrn_reflns_number 19107 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.58 _reflns_number_total 4489 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0648P)^2^+1.7656P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4489 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.155 _refine_ls_shift/su_mean 0.042 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 C311 C 0.6145(2) 0.08199(14) 0.8602(2) 0.0231(5) Uani 1 1 d . . . H1A H 0.5592 0.0545 0.9031 0.028 Uiso 1 1 calc R . . H1B H 0.6030 0.0591 0.7778 0.028 Uiso 1 1 calc R . . C121 C 0.8194(3) -0.01243(15) 0.6189(2) 0.0246(5) Uani 1 1 d . . . H2A H 0.8268 -0.0644 0.5945 0.030 Uiso 1 1 calc R . . H2B H 0.8902 0.0162 0.5982 0.030 Uiso 1 1 calc R . . C231 C 1.1024(3) -0.10791(15) 0.7043(2) 0.0240(5) Uani 1 1 d . . . H4A H 1.1111 -0.0644 0.6539 0.029 Uiso 1 1 calc R . . H4B H 1.0263 -0.1374 0.6557 0.029 Uiso 1 1 calc R . . C131 C 1.1405(3) 0.13772(14) 0.7723(2) 0.0220(5) Uani 1 1 d . . . H5A H 1.2367 0.1359 0.8133 0.026 Uiso 1 1 calc R . . H5B H 1.1054 0.1837 0.7984 0.026 Uiso 1 1 calc R . . C211 C 0.9323(3) 0.22448(14) 1.0175(3) 0.0278(6) Uani 1 1 d . . . H6A H 0.9450 0.2309 1.1077 0.033 Uiso 1 1 calc R . . H6B H 0.8361 0.2219 0.9763 0.033 Uiso 1 1 calc R . . C232 C 1.2287(3) -0.15474(17) 0.7293(3) 0.0353(7) Uani 1 1 d . . . H9A H 1.3048 -0.1251 0.7743 0.053 Uiso 1 1 calc R . . H9B H 1.2413 -0.1711 0.6502 0.053 Uiso 1 1 calc R . . H9C H 1.2206 -0.1979 0.7792 0.053 Uiso 1 1 calc R . . C122 C 0.6839(3) 0.0185(2) 0.5456(3) 0.0399(7) Uani 1 1 d . . . H10A H 0.6138 -0.0093 0.5671 0.060 Uiso 1 1 calc R . . H10B H 0.6736 0.0139 0.4565 0.060 Uiso 1 1 calc R . . H10C H 0.6782 0.0706 0.5668 0.060 Uiso 1 1 calc R . . C312 C 0.5689(3) 0.16279(16) 0.8432(3) 0.0360(7) Uani 1 1 d . . . H8A H 0.5808 0.1856 0.9248 0.054 Uiso 1 1 calc R . . H8B H 0.4754 0.1647 0.7961 0.054 Uiso 1 1 calc R . . H8C H 0.6215 0.1896 0.7981 0.054 Uiso 1 1 calc R . . C212 C 0.9896(4) 0.28974(18) 0.9683(4) 0.0541(10) Uani 1 1 d . . . H11A H 1.0840 0.2937 1.0116 0.081 Uiso 1 1 calc R . . H11B H 0.9444 0.3348 0.9820 0.081 Uiso 1 1 calc R . . H11C H 0.9779 0.2833 0.8792 0.081 Uiso 1 1 calc R . . C132 C 1.1156(5) 0.13787(19) 0.6318(3) 0.0523(10) Uani 1 1 d . . . H12A H 1.1497 0.0921 0.6061 0.078 Uiso 1 1 calc R . . H12B H 1.1607 0.1801 0.6076 0.078 Uiso 1 1 calc R . . H12C H 1.0205 0.1415 0.5914 0.078 Uiso 1 1 calc R . . C321 C 0.6298(2) -0.10827(14) 0.8822(2) 0.0222(5) Uani 1 1 d . . . H32A H 0.6045 -0.0985 0.7918 0.027 Uiso 1 1 calc R . . H32B H 0.5674 -0.0814 0.9179 0.027 Uiso 1 1 calc R . . C322 C 0.6201(3) -0.19133(15) 0.9047(3) 0.0304(6) Uani 1 1 d . . . H32C H 0.6829 -0.2179 0.8706 0.046 Uiso 1 1 calc R . . H32D H 0.5302 -0.2084 0.8638 0.046 Uiso 1 1 calc R . . H32E H 0.6411 -0.2008 0.9941 0.046 Uiso 1 1 calc R . . V1 V 0.89901(4) 0.08900(2) 0.84702(4) 0.01615(13) Uani 1 1 d . . . V2 V 0.90876(4) -0.09351(2) 0.86410(4) 0.01595(13) Uani 1 1 d . . . V3 V 0.81100(4) 0.001407(19) 1.07218(4) 0.01497(13) Uani 1 1 d . . . O23 O 1.07675(17) -0.08296(9) 0.82019(15) 0.0180(3) Uani 1 1 d . . . O12 O 0.83683(18) -0.00852(9) 0.75365(16) 0.0179(4) Uani 1 1 d . . . O32 O 0.76543(16) -0.08079(9) 0.93927(16) 0.0172(3) Uani 1 1 d . . . O13 O 1.07629(17) 0.07402(10) 0.81052(16) 0.0180(3) Uani 1 1 d . . . O21 O 0.99494(16) 0.15493(10) 0.99602(14) 0.0183(4) Uani 1 1 d . . . O31 O 0.75393(16) 0.07701(10) 0.93300(16) 0.0179(3) Uani 1 1 d . . . O2 O 0.84693(18) -0.15763(10) 0.76343(17) 0.0227(4) Uani 1 1 d . . . O123 O 1.0000 0.0000 1.0000 0.0150(5) Uani 1 2 d S . . O3 O 0.68088(19) 0.00072(9) 1.12392(19) 0.0221(4) Uani 1 1 d . . . O1 O 0.83296(18) 0.15012(10) 0.74093(17) 0.0239(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 C311 0.0160(11) 0.0273(12) 0.0267(12) 0.0039(10) 0.0067(9) 0.0028(9) C121 0.0251(13) 0.0321(13) 0.0157(11) -0.0010(9) 0.0044(10) 0.0035(10) C231 0.0252(13) 0.0293(13) 0.0201(11) -0.0057(9) 0.0109(9) 0.0015(10) C131 0.0254(13) 0.0207(11) 0.0221(11) 0.0027(9) 0.0105(10) -0.0031(9) C211 0.0314(14) 0.0158(11) 0.0379(14) -0.0048(10) 0.0126(11) 0.0021(10) C232 0.0349(16) 0.0334(15) 0.0425(16) -0.0112(12) 0.0187(13) 0.0041(12) C122 0.0353(17) 0.0532(18) 0.0230(13) -0.0005(13) -0.0052(12) 0.0121(15) C312 0.0233(14) 0.0326(15) 0.0529(18) 0.0146(13) 0.0121(13) 0.0085(11) C212 0.085(3) 0.0170(14) 0.075(2) 0.0045(15) 0.047(2) 0.0055(15) C132 0.099(3) 0.0387(17) 0.0293(15) -0.0027(13) 0.0349(18) -0.0214(19) C321 0.0149(11) 0.0236(12) 0.0274(12) -0.0063(10) 0.0049(9) -0.0036(9) C322 0.0275(14) 0.0238(13) 0.0423(15) -0.0064(11) 0.0136(12) -0.0081(10) V1 0.0175(2) 0.0152(2) 0.0169(2) 0.00159(13) 0.00679(15) 0.00074(14) V2 0.0170(2) 0.0148(2) 0.0172(2) -0.00367(13) 0.00673(15) -0.00194(14) V3 0.0157(2) 0.0148(2) 0.0160(2) -0.00143(12) 0.00715(16) -0.00067(13) O23 0.0203(9) 0.0190(8) 0.0169(8) -0.0049(6) 0.0089(6) -0.0018(6) O12 0.0194(8) 0.0211(8) 0.0132(8) -0.0015(6) 0.0045(6) 0.0001(6) O32 0.0148(8) 0.0172(8) 0.0205(8) -0.0043(6) 0.0063(6) -0.0044(6) O13 0.0195(8) 0.0175(8) 0.0186(8) 0.0020(6) 0.0083(6) -0.0010(7) O21 0.0218(9) 0.0129(8) 0.0224(9) -0.0016(5) 0.0099(7) 0.0008(6) O31 0.0153(8) 0.0181(8) 0.0204(8) 0.0019(6) 0.0049(6) 0.0024(6) O2 0.0235(9) 0.0220(9) 0.0243(8) -0.0082(7) 0.0091(7) -0.0048(7) O123 0.0175(12) 0.0139(11) 0.0150(11) -0.0013(7) 0.0068(9) -0.0017(8) O3 0.0197(9) 0.0246(9) 0.0254(9) -0.0025(6) 0.0120(7) -0.0016(6) O1 0.0260(9) 0.0231(9) 0.0242(9) 0.0069(7) 0.0098(7) 0.0028(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 C311 O31 1.441(3) . ? C311 C312 1.505(4) . ? C121 O12 1.444(3) . ? C121 C122 1.508(4) . ? C231 O23 1.444(3) . ? C231 C232 1.507(4) . ? C131 O13 1.433(3) . ? C131 C132 1.493(4) . ? C211 O21 1.445(3) . ? C211 C212 1.473(4) . ? C321 O32 1.449(3) . ? C321 C322 1.504(4) . ? V1 O1 1.5990(18) . ? V1 O31 1.9978(19) . ? V1 O13 2.0016(19) . ? V1 O12 2.0236(18) . ? V1 O21 2.0306(17) . ? V1 O123 2.3299(8) . ? V2 O2 1.5913(17) . ? V2 O32 1.9035(18) . ? V2 O21 1.9194(17) 3_757 ? V2 O23 1.9386(19) . ? V2 O12 1.9487(18) . ? V2 O123 2.2553(7) . ? V3 O3 1.602(2) . ? V3 O13 1.9920(18) 3_757 ? V3 O31 1.9964(18) . ? V3 O23 2.0175(18) 3_757 ? V3 O32 2.0254(18) . ? V3 O123 2.3077(9) . ? O23 V3 2.0175(18) 3_757 ? O13 V3 1.9920(18) 3_757 ? O21 V2 1.9194(17) 3_757 ? O123 V2 2.2553(7) 3_757 ? O123 V3 2.3077(9) 3_757 ? O123 V1 2.3299(7) 3_757 ? 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 O31 C311 C312 110.9(2) . . ? O12 C121 C122 111.0(2) . . ? O23 C231 C232 112.0(2) . . ? O13 C131 C132 110.3(2) . . ? O21 C211 C212 111.5(2) . . ? O32 C321 C322 111.1(2) . . ? O1 V1 O31 101.25(9) . . ? O1 V1 O13 99.80(9) . . ? O31 V1 O13 158.94(7) . . ? O1 V1 O12 101.62(9) . . ? O31 V1 O12 88.61(8) . . ? O13 V1 O12 87.82(8) . . ? O1 V1 O21 102.03(9) . . ? O31 V1 O21 86.56(7) . . ? O13 V1 O21 88.43(7) . . ? O12 V1 O21 156.35(7) . . ? O1 V1 O123 178.61(7) . . ? O31 V1 O123 80.14(5) . . ? O13 V1 O123 78.81(5) . . ? O12 V1 O123 78.43(6) . . ? O21 V1 O123 77.94(6) . . ? O2 V2 O32 100.28(9) . . ? O2 V2 O21 99.60(9) . 3_757 ? O32 V2 O21 90.58(7) . 3_757 ? O2 V2 O23 96.18(8) . . ? O32 V2 O23 163.52(7) . . ? O21 V2 O23 87.51(7) 3_757 . ? O2 V2 O12 96.47(9) . . ? O32 V2 O12 88.41(8) . . ? O21 V2 O12 163.82(7) 3_757 . ? O23 V2 O12 88.89(8) . . ? O2 V2 O123 177.37(7) . . ? O32 V2 O123 81.70(5) . . ? O21 V2 O123 82.06(6) 3_757 . ? O23 V2 O123 81.82(5) . . ? O12 V2 O123 81.81(6) . . ? O3 V3 O13 99.26(9) . 3_757 ? O3 V3 O31 100.48(9) . . ? O13 V3 O31 160.26(8) 3_757 . ? O3 V3 O23 101.45(8) . 3_757 ? O13 V3 O23 88.18(8) 3_757 3_757 ? O31 V3 O23 87.92(8) . 3_757 ? O3 V3 O32 101.75(8) . . ? O13 V3 O32 87.55(8) 3_757 . ? O31 V3 O32 88.44(9) . . ? O23 V3 O32 156.80(7) 3_757 . ? O3 V3 O123 178.76(7) . . ? O13 V3 O123 79.54(6) 3_757 . ? O31 V3 O123 80.72(5) . . ? O23 V3 O123 78.89(5) 3_757 . ? O32 V3 O123 77.91(5) . . ? C231 O23 V2 126.27(15) . . ? C231 O23 V3 121.34(15) . 3_757 ? V2 O23 V3 109.29(8) . 3_757 ? C121 O12 V2 121.21(14) . . ? C121 O12 V1 119.48(15) . . ? V2 O12 V1 109.62(9) . . ? C321 O32 V2 123.26(14) . . ? C321 O32 V3 123.69(14) . . ? V2 O32 V3 110.39(8) . . ? C131 O13 V3 119.11(15) . 3_757 ? C131 O13 V1 118.67(15) . . ? V3 O13 V1 111.13(8) 3_757 . ? C211 O21 V2 120.63(15) . 3_757 ? C211 O21 V1 119.06(15) . . ? V2 O21 V1 110.12(9) 3_757 . ? C311 O31 V3 120.04(15) . . ? C311 O31 V1 119.81(15) . . ? V3 O31 V1 109.65(8) . . ? V2 O123 V2 180.000(13) 3_757 . ? V2 O123 V3 90.00(2) 3_757 3_757 ? V2 O123 V3 90.00(2) . 3_757 ? V2 O123 V3 90.00(2) 3_757 . ? V2 O123 V3 90.00(2) . . ? V3 O123 V3 180.0 3_757 . ? V2 O123 V1 89.86(4) 3_757 . ? V2 O123 V1 90.14(4) . . ? V3 O123 V1 90.51(3) 3_757 . ? V3 O123 V1 89.49(3) . . ? V2 O123 V1 90.14(3) 3_757 3_757 ? V2 O123 V1 89.86(3) . 3_757 ? V3 O123 V1 89.49(3) 3_757 3_757 ? V3 O123 V1 90.51(3) . 3_757 ? V1 O123 V1 180.0 . 3_757 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.450 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.155