# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 1145/143 data_[N(CH3)4]2[Co(H2O)4V12O28] _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H32 Co N2 O32 V12' _chemical_formula_weight 1338.57 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Co' 'Co' 0.3494 0.9721 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6510(6) _cell_length_b 10.7485(10) _cell_length_c 13.4022(13) _cell_angle_alpha 83.003(2) _cell_angle_beta 85.739(2) _cell_angle_gamma 83.971(2) _cell_volume 943.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_method ? _exptl_crystal_F_000 653 _exptl_absorpt_coefficient_mu 3.348 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5593 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.1178 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.24 _reflns_number_total 3894 _reflns_number_observed 2575 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0834P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3894 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_obs 0.0668 _refine_ls_wR_factor_all 0.1741 _refine_ls_wR_factor_obs 0.1419 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.035 _refine_ls_restrained_S_all 1.021 _refine_ls_restrained_S_obs 1.035 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.5000 0.0170(4) Uani 1 d S . V1 V 0.2778(2) 0.06044(14) 0.89624(11) 0.0146(4) Uani 1 d . . V2 V -0.5254(2) 0.30443(14) 0.76130(11) 0.0136(4) Uani 1 d . . V3 V 0.2742(2) 0.29610(13) 0.56631(11) 0.0120(3) Uani 1 d . . V4 V 0.2451(2) 0.60868(14) 0.46316(11) 0.0129(4) Uani 1 d . . V5 V -0.2521(2) 0.18086(14) 0.91371(11) 0.0141(4) Uani 1 d . . V6 V -0.0050(2) 0.18880(14) 0.71766(11) 0.0131(4) Uani 1 d . . O1 O 0.2437(9) 0.4503(6) 0.4758(4) 0.0191(14) Uani 1 d . . O2 O -0.0228(8) 0.3160(6) 0.5960(4) 0.0168(13) Uani 1 d . . O3 O -0.4676(8) 0.3451(6) 0.6102(4) 0.0169(13) Uani 1 d . . O4 O -0.2419(8) 0.2675(6) 0.7786(4) 0.0174(13) Uani 1 d . . O5 O 0.0331(9) 0.1331(6) 0.8636(4) 0.0180(14) Uani 1 d . . O6 O 0.2462(9) 0.6552(6) 0.5732(5) 0.025(2) Uani 1 d . . O7 O 0.3342(9) 0.1814(6) 0.4990(5) 0.0186(14) Uani 1 d . . O8 O -0.2596(9) 0.0112(6) 0.9847(5) 0.0208(14) Uani 1 d . . O9 O -0.5391(8) 0.1762(6) 0.8836(5) 0.0192(14) Uani 1 d . . O10 O 0.3502(9) -0.0443(6) 0.8222(5) 0.027(2) Uani 1 d . . O11 O -0.0394(9) 0.0583(6) 0.6752(5) 0.0228(15) Uani 1 d . . O12 O -0.6093(10) 0.4337(6) 0.8029(5) 0.027(2) Uani 1 d . . O13 O -0.7347(8) 0.2280(6) 0.7054(4) 0.0164(13) Uani 1 d . . O14 O -0.2452(10) 0.2779(6) 0.9939(5) 0.027(2) Uani 1 d . . O15 O 0.4190(9) -0.0075(7) 0.3568(5) 0.028(2) Uani 1 d . . O16 O 0.2409(10) -0.0807(6) 0.5570(5) 0.030(2) Uani 1 d . . N1 N -0.1869(15) 0.6671(8) 0.8265(7) 0.035(2) Uani 1 d . . C1 C -0.0895(28) 0.7834(14) 0.8188(14) 0.104(7) Uani 1 d . . H11 H -0.1824(92) 0.8482(45) 0.8445(118) 0.205(32) Uiso 1 calc R . H12 H -0.0503(232) 0.8088(87) 0.7495(21) 0.205(32) Uiso 1 calc R . H13 H 0.0285(149) 0.7699(46) 0.8574(106) 0.205(32) Uiso 1 calc R . C2 C -0.3638(28) 0.6881(16) 0.7647(15) 0.105(7) Uani 1 d . . H21 H -0.4638(114) 0.7470(130) 0.7931(77) 0.205(32) Uiso 1 calc R . H22 H -0.4202(165) 0.6097(35) 0.7633(111) 0.205(32) Uiso 1 calc R . H23 H -0.3227(56) 0.7212(156) 0.6973(37) 0.205(32) Uiso 1 calc R . C3 C -0.0500(26) 0.5631(15) 0.7942(11) 0.131(9) Uani 1 d . . H31 H -0.1196(21) 0.4884(19) 0.8010(20) 0.205(32) Uiso 1 calc R . H32 H 0.0643(23) 0.5491(21) 0.8353(23) 0.205(32) Uiso 1 calc R . H33 H -0.0041(58) 0.5831(23) 0.7251(16) 0.205(32) Uiso 1 calc R . C4 C -0.2709(30) 0.6316(16) 0.9311(10) 0.147(10) Uani 1 d R . H41 H -0.1958(31) 0.5563(17) 0.9599(10) 0.205(32) Uiso 1 calc R . H42 H -0.4107(25) 0.6172(15) 0.9298(16) 0.205(32) Uiso 1 calc R . H43 H -0.2604(30) 0.6987(19) 0.9711(12) 0.205(32) Uiso 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 Co1 0.0107(9) 0.0183(9) 0.0216(10) -0.0022(7) -0.0006(7) -0.0003(7) V1 0.0046(7) 0.0201(8) 0.0173(8) 0.0053(6) -0.0008(6) -0.0009(6) V2 0.0047(7) 0.0177(8) 0.0169(8) 0.0026(6) -0.0011(6) 0.0004(6) V3 0.0049(7) 0.0132(8) 0.0169(8) 0.0018(6) -0.0010(5) 0.0001(5) V4 0.0043(7) 0.0167(8) 0.0162(8) 0.0046(6) -0.0013(5) -0.0015(6) V5 0.0053(7) 0.0218(9) 0.0145(8) 0.0014(6) -0.0019(6) -0.0009(6) V6 0.0056(7) 0.0159(8) 0.0169(8) 0.0037(6) -0.0019(6) -0.0020(6) O1 0.020(3) 0.021(3) 0.014(3) 0.005(3) -0.002(3) -0.002(3) O2 0.005(3) 0.021(3) 0.021(3) 0.009(3) -0.003(2) -0.002(2) O3 0.003(3) 0.025(4) 0.020(3) 0.009(3) -0.001(2) -0.002(2) O4 0.008(3) 0.025(3) 0.017(3) 0.005(3) -0.001(2) -0.001(2) O5 0.010(3) 0.026(4) 0.016(3) 0.009(3) -0.004(2) 0.000(3) O6 0.021(4) 0.035(4) 0.021(4) -0.005(3) -0.002(3) -0.007(3) O7 0.011(3) 0.020(3) 0.023(3) -0.002(3) 0.001(3) 0.004(3) O8 0.012(3) 0.026(4) 0.023(4) 0.010(3) -0.006(3) -0.004(3) O9 0.007(3) 0.027(4) 0.021(3) 0.008(3) -0.003(2) -0.003(3) O10 0.019(4) 0.030(4) 0.030(4) 0.004(3) 0.004(3) 0.001(3) O11 0.016(3) 0.026(4) 0.025(4) 0.000(3) -0.002(3) -0.002(3) O12 0.029(4) 0.020(4) 0.032(4) -0.008(3) 0.001(3) 0.008(3) O13 0.007(3) 0.028(4) 0.014(3) 0.003(3) -0.002(2) -0.007(3) O14 0.023(4) 0.036(4) 0.024(4) -0.010(3) -0.004(3) -0.002(3) O15 0.017(4) 0.046(5) 0.023(4) -0.005(3) -0.002(3) -0.002(3) O16 0.019(4) 0.028(4) 0.045(5) -0.011(3) 0.011(3) -0.005(3) N1 0.047(6) 0.020(5) 0.037(6) 0.000(4) -0.006(5) 0.001(4) C1 0.139(17) 0.057(10) 0.131(16) 0.019(10) -0.062(14) -0.072(11) C2 0.113(16) 0.069(12) 0.142(18) -0.013(12) -0.069(14) -0.007(11) C3 0.085(15) 0.095(16) 0.197(24) -0.031(16) 0.050(15) 0.040(12) C4 0.153(23) 0.235(29) 0.042(12) -0.015(14) 0.029(12) 0.011(19) _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 Co1 O15 2.045(6) 2_656 ? Co1 O15 2.045(6) . ? Co1 O16 2.064(7) 2_656 ? Co1 O16 2.064(7) . ? Co1 O7 2.136(6) 2_656 ? Co1 O7 2.136(6) . ? V1 O10 1.603(7) . ? V1 O8 1.687(6) 2_557 ? V1 O5 1.790(6) . ? V1 O9 1.815(6) 1_655 ? V2 O12 1.592(6) . ? V2 O4 1.911(6) . ? V2 O13 1.928(6) . ? V2 O9 2.012(6) . ? V2 O3 2.036(6) . ? V2 V5 2.937(2) . ? V2 V3 3.035(2) 1_455 ? V3 O7 1.615(6) . ? V3 O13 1.916(6) 1_655 ? V3 O1 1.933(6) . ? V3 O2 1.980(6) . ? V3 O3 1.997(6) 1_655 ? V3 V6 2.866(2) . ? V3 V2 3.035(2) 1_655 ? V4 O6 1.614(6) . ? V4 O1 1.691(6) . ? V4 O3 1.795(6) 2_566 ? V4 O2 1.799(6) 2_566 ? V5 O14 1.592(6) . ? V5 O4 1.932(6) . ? V5 O8 1.955(6) . ? V5 O9 1.987(6) . ? V5 O5 2.001(6) . ? V5 V6 2.991(2) . ? V6 O11 1.620(6) . ? V6 O13 1.880(6) 1_655 ? V6 O4 1.888(6) . ? V6 O2 1.998(6) . ? V6 O5 2.002(6) . ? O2 V4 1.799(6) 2_566 ? O3 V4 1.795(6) 2_566 ? O3 V3 1.997(6) 1_455 ? O8 V1 1.687(6) 2_557 ? O9 V1 1.815(6) 1_455 ? O13 V6 1.880(6) 1_455 ? O13 V3 1.916(6) 1_455 ? N1 C3 1.453(14) . ? N1 C1 1.457(15) . ? N1 C2 1.47(2) . ? N1 C4 1.49(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 O15 Co1 O15 180.0 2_656 . ? O15 Co1 O16 89.9(3) 2_656 2_656 ? O15 Co1 O16 90.1(3) . 2_656 ? O15 Co1 O16 90.1(3) 2_656 . ? O15 Co1 O16 89.9(3) . . ? O16 Co1 O16 180.0 2_656 . ? O15 Co1 O7 89.2(2) 2_656 2_656 ? O15 Co1 O7 90.8(2) . 2_656 ? O16 Co1 O7 89.1(2) 2_656 2_656 ? O16 Co1 O7 90.9(2) . 2_656 ? O15 Co1 O7 90.8(2) 2_656 . ? O15 Co1 O7 89.2(2) . . ? O16 Co1 O7 90.9(2) 2_656 . ? O16 Co1 O7 89.1(2) . . ? O7 Co1 O7 180.0 2_656 . ? O10 V1 O8 108.5(3) . 2_557 ? O10 V1 O5 108.8(3) . . ? O8 V1 O5 108.9(3) 2_557 . ? O10 V1 O9 109.1(3) . 1_655 ? O8 V1 O9 110.8(3) 2_557 1_655 ? O5 V1 O9 110.7(3) . 1_655 ? O12 V2 O4 111.1(3) . . ? O12 V2 O13 111.9(3) . . ? O4 V2 O13 136.9(3) . . ? O12 V2 O9 103.9(3) . . ? O4 V2 O9 81.1(2) . . ? O13 V2 O9 89.5(3) . . ? O12 V2 O3 106.5(3) . . ? O4 V2 O3 90.2(2) . . ? O13 V2 O3 77.1(2) . . ? O9 V2 O3 149.5(3) . . ? O12 V2 V5 104.0(2) . . ? O4 V2 V5 40.4(2) . . ? O13 V2 V5 126.0(2) . . ? O9 V2 V5 42.4(2) . . ? O3 V2 V5 129.1(2) . . ? O12 V2 V3 107.1(2) . 1_455 ? O4 V2 V3 124.8(2) . 1_455 ? O13 V2 V3 37.7(2) . 1_455 ? O9 V2 V3 125.8(2) . 1_455 ? O3 V2 V3 40.7(2) . 1_455 ? V5 V2 V3 148.84(7) . 1_455 ? O7 V3 O13 108.2(3) . 1_655 ? O7 V3 O1 107.9(3) . . ? O13 V3 O1 143.9(3) 1_655 . ? O7 V3 O2 109.8(3) . . ? O13 V3 O2 81.0(2) 1_655 . ? O1 V3 O2 87.8(2) . . ? O7 V3 O3 106.9(3) . 1_655 ? O13 V3 O3 78.3(2) 1_655 1_655 ? O1 V3 O3 90.4(2) . 1_655 ? O2 V3 O3 141.9(3) . 1_655 ? O7 V3 V6 101.9(2) . . ? O13 V3 V6 40.5(2) 1_655 . ? O1 V3 V6 130.2(2) . . ? O2 V3 V6 44.2(2) . . ? O3 V3 V6 118.0(2) 1_655 . ? O7 V3 V2 120.9(2) . 1_655 ? O13 V3 V2 38.0(2) 1_655 1_655 ? O1 V3 V2 117.5(2) . 1_655 ? O2 V3 V2 107.8(2) . 1_655 ? O3 V3 V2 41.7(2) 1_655 1_655 ? V6 V3 V2 76.44(5) . 1_655 ? O6 V4 O1 109.2(3) . . ? O6 V4 O3 108.5(3) . 2_566 ? O1 V4 O3 110.4(3) . 2_566 ? O6 V4 O2 108.4(3) . 2_566 ? O1 V4 O2 110.7(3) . 2_566 ? O3 V4 O2 109.6(3) 2_566 2_566 ? O14 V5 O4 110.3(3) . . ? O14 V5 O8 109.0(3) . . ? O4 V5 O8 140.6(3) . . ? O14 V5 O9 108.3(3) . . ? O4 V5 O9 81.2(2) . . ? O8 V5 O9 88.3(3) . . ? O14 V5 O5 107.7(3) . . ? O4 V5 O5 77.7(2) . . ? O8 V5 O5 89.0(2) . . ? O9 V5 O5 142.7(3) . . ? O14 V5 V2 106.5(2) . . ? O4 V5 V2 39.9(2) . . ? O8 V5 V2 126.9(2) . . ? O9 V5 V2 43.1(2) . . ? O5 V5 V2 116.0(2) . . ? O14 V5 V6 124.2(3) . . ? O4 V5 V6 37.9(2) . . ? O8 V5 V6 113.5(2) . . ? O9 V5 V6 107.3(2) . . ? O5 V5 V6 41.7(2) . . ? V2 V5 V6 74.38(5) . . ? O11 V6 O13 114.4(3) . 1_655 ? O11 V6 O4 113.6(3) . . ? O13 V6 O4 131.8(3) 1_655 . ? O11 V6 O2 103.6(3) . . ? O13 V6 O2 81.5(2) 1_655 . ? O4 V6 O2 91.1(2) . . ? O11 V6 O5 102.3(3) . . ? O13 V6 O5 87.7(2) 1_655 . ? O4 V6 O5 78.7(2) . . ? O2 V6 O5 154.1(3) . . ? O11 V6 V3 102.0(2) . . ? O13 V6 V3 41.5(2) 1_655 . ? O4 V6 V3 128.6(2) . . ? O2 V6 V3 43.7(2) . . ? O5 V6 V3 129.1(2) . . ? O11 V6 V5 104.0(2) . . ? O13 V6 V5 122.3(2) 1_655 . ? O4 V6 V5 39.0(2) . . ? O2 V6 V5 129.6(2) . . ? O5 V6 V5 41.6(2) . . ? V3 V6 V5 153.87(7) . . ? V4 O1 V3 145.9(4) . . ? V4 O2 V3 138.5(3) 2_566 . ? V4 O2 V6 128.7(3) 2_566 . ? V3 O2 V6 92.2(2) . . ? V4 O3 V3 130.1(3) 2_566 1_455 ? V4 O3 V2 131.9(3) 2_566 . ? V3 O3 V2 97.6(2) 1_455 . ? V6 O4 V2 141.2(3) . . ? V6 O4 V5 103.1(3) . . ? V2 O4 V5 99.7(3) . . ? V1 O5 V5 146.0(3) . . ? V1 O5 V6 117.2(3) . . ? V5 O5 V6 96.7(2) . . ? V3 O7 Co1 142.8(4) . . ? V1 O8 V5 139.2(4) 2_557 . ? V1 O9 V5 137.2(3) 1_455 . ? V1 O9 V2 120.7(3) 1_455 . ? V5 O9 V2 94.5(3) . . ? V6 O13 V3 98.0(3) 1_455 1_455 ? V6 O13 V2 147.2(3) 1_455 . ? V3 O13 V2 104.3(3) 1_455 . ? C3 N1 C1 112.2(14) . . ? C3 N1 C2 109.8(12) . . ? C1 N1 C2 108.9(11) . . ? C3 N1 C4 109.4(11) . . ? C1 N1 C4 111.4(13) . . ? C2 N1 C4 105.0(14) . . ? _refine_diff_density_max 1.006 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.230