# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1353 data_paper8/09442J loop_ _publ_contact_author_name _publ_contact_author_address 'Dr. Marc Fourmigu\'e' ;Institut des Mat\'eriaux de Nantes (IMN) UMR 6502 CNRS-Universit\'e de Nantes BP 32229, 2, rue de la Houssini\`ere 44322 Nantes cedex 03, France ; _publ_contact_author_email fourmigue@cnrs-imn.fr _publ_contact_author_fax '33 (0)2 40 37 39 95' _publ_contact_author_phone '33 (0)2 40 37 39 15' _publ_contact_letter ; Please find enclosed, in CIF format, the supplementary materials for the three structures included in a paper ref 8/09442J accepted for publication in J. Chem. Soc. Dalton Trans, entitled: "Relative Basicities of Oxygen Atoms of the Linquist Polooxometalate, [Mo6O19]2-, and their Recognition by Hydroxyl Groups in Radical Cation Salts Based on the Functionalized pi-donors, Me3TTT(CH2OH), EDT-TTF(CH2OH)2 and TTF(CH2OH)4. by A. Dolbecq, A. Guirauden, M. Fourmigue, K. Boubekeur, P. Batail, M.-M. Rohmer, M. Benard, C. Coulon, M. Salle and P. Blanchard. This file replaces the one sent with the original version of the manuscript and should be the one used for deposition. With best regards, Marc Fourmigue ; ####################Material relevant to Me3TTF(CH2OH)######################## data_adohabs _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '(Me~3~TTF-CH~2~OH)~2~ Mo~6~O~19~' _chemical_formula_moiety '(C10H12OS4)2 Mo6O19' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H24 Mo6 O21 S8' _chemical_formula_weight 1432.51 _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 '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' 'S' 'S' 0.1246 0.1234 '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 7.8304(13) _cell_length_b 11.288(2) _cell_length_c 11.375(2) _cell_angle_alpha 109.08(2) _cell_angle_beta 95.29(2) _cell_angle_gamma 103.41(2) _cell_volume 908.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2. _cell_measurement_theta_max 26.8 _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.617 _exptl_crystal_density_method ? _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 2.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.793 _exptl_absorpt_process_details ; Empirical absorption correction based on measurments of equivalent reflections was performed with XPREP (Siemens-SHELXTL Version 5) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 2\%' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9813 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3642 _reflns_number_observed 3204 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'EXPOSE [Stoe IPDS]' _computing_cell_refinement 'SELECT [Stoe IPDS]' _computing_data_reduction 'INTEGRATE [Stoe IPDS]' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP [Johnson, 1976]' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.0425P)^2^+1.3641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3638 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_obs 0.0260 _refine_ls_wR_factor_all 0.0797 _refine_ls_wR_factor_obs 0.0669 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.169 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max -0.164 _refine_ls_shift/esd_mean 0.008 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 Mo1 Mo 0.12208(5) 0.91622(3) 0.82317(3) 0.01632(9) Uani 1 d . . Mo2 Mo -0.17895(5) 0.79364(3) 0.96479(3) 0.01579(9) Uani 1 d . . Mo3 Mo 0.22320(5) 0.96614(3) 1.12526(3) 0.01894(9) Uani 1 d . . O12 O -0.0511(4) 0.7629(2) 0.8290(2) 0.0203(6) Uani 1 d . . O31 O 0.2747(4) 0.9026(3) 0.9546(3) 0.0238(6) Uani 1 d . . O21 O 0.2349(4) 1.0979(2) 0.8799(2) 0.0227(6) Uani 1 d . . O13 O -0.0893(4) 0.9559(2) 0.7551(2) 0.0217(6) Uani 1 d . . O23 O -0.3266(4) 0.8607(3) 0.8761(2) 0.0205(6) Uani 1 d . . O32 O 0.0375(4) 0.8052(2) 1.0734(2) 0.0232(6) Uani 1 d . . O1 O 0.2002(4) 0.8533(3) 0.6903(2) 0.0264(7) Uani 1 d . . O2 O -0.3072(4) 0.6432(2) 0.9439(2) 0.0238(6) Uani 1 d . . O3 O 0.3835(5) 0.9422(3) 1.2164(3) 0.0324(7) Uani 1 d . . O19 O 0.0000 1.0000 1.0000 0.0130(7) Uani 1 d S . S1 S 0.52224(13) 0.74487(8) 0.55997(8) 0.0169(2) Uani 1 d . . S2 S 0.34015(13) 0.53153(8) 0.32489(7) 0.0150(2) Uani 1 d . . S3 S 0.30121(13) 0.59674(8) 0.71842(8) 0.0173(2) Uani 1 d . . S4 S 0.12373(13) 0.37814(8) 0.48750(8) 0.0155(2) Uani 1 d . . C1 C 0.3702(5) 0.5940(3) 0.4873(3) 0.0139(7) Uani 1 d . . C2 C 0.2751(5) 0.5298(3) 0.5567(3) 0.0151(7) Uani 1 d . . C3 C 0.5659(5) 0.7686(3) 0.4202(3) 0.0180(8) Uani 1 d . . C4 C 0.4835(6) 0.6685(3) 0.3111(3) 0.0184(8) Uani 1 d . . C5 C 0.1445(5) 0.4701(4) 0.7345(3) 0.0183(8) Uani 1 d . . C6 C 0.0632(5) 0.3662(4) 0.6275(3) 0.0187(8) Uani 1 d . . C7 C 0.6899(6) 0.8977(4) 0.4359(4) 0.0282(9) Uani 1 d . . C8 C 0.5014(7) 0.6637(4) 0.1798(4) 0.0299(10) Uani 1 d . . C9 C 0.1065(7) 0.4867(4) 0.8660(4) 0.0289(10) Uani 1 d . . C10 C -0.0716(6) 0.2436(4) 0.6202(4) 0.0288(9) Uani 1 d . . O7A O 0.8436(28) 0.9234(18) 0.5012(17) 0.032(4) Uiso 0.17 d P . O7B O 0.6114(32) 0.9827(21) 0.4506(19) 0.042(5) Uiso 0.17 d P . O8 O 0.3716(19) 0.6732(12) 0.1223(12) 0.058(3) Uiso 0.34 d P . O9 O 0.1970(16) 0.6021(11) 0.9463(10) 0.045(3) Uiso 0.34 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0199(2) 0.01228(14) 0.01384(15) 0.00197(11) 0.00958(12) 0.00035(12) Mo2 0.0196(2) 0.00933(14) 0.01379(14) 0.00251(10) 0.00637(11) -0.00359(12) Mo3 0.0191(2) 0.0172(2) 0.0176(2) 0.00469(12) -0.00082(12) 0.00328(13) O12 0.028(2) 0.0107(11) 0.0166(12) 0.0013(9) 0.0091(11) -0.0012(11) O31 0.022(2) 0.0224(13) 0.0253(13) 0.0040(11) 0.0060(11) 0.0088(12) O21 0.028(2) 0.0141(12) 0.0188(12) 0.0021(10) 0.0131(11) -0.0055(11) O13 0.029(2) 0.0182(12) 0.0126(11) 0.0035(10) 0.0028(10) 0.0000(11) O23 0.014(2) 0.0195(12) 0.0202(12) 0.0042(10) -0.0008(10) -0.0035(10) O32 0.032(2) 0.0134(12) 0.0231(13) 0.0095(10) 0.0009(11) 0.0010(11) O1 0.032(2) 0.0172(13) 0.0220(13) -0.0008(10) 0.0149(12) -0.0007(12) O2 0.034(2) 0.0136(12) 0.0166(12) 0.0035(10) 0.0078(11) -0.0049(11) O3 0.031(2) 0.0273(15) 0.035(2) 0.0096(12) -0.0061(13) 0.0086(13) O19 0.013(2) 0.012(2) 0.0112(15) 0.0029(12) 0.0035(13) -0.0005(13) S1 0.0158(5) 0.0124(4) 0.0162(4) 0.0015(3) 0.0037(3) -0.0031(3) S2 0.0155(5) 0.0135(4) 0.0126(4) 0.0039(3) 0.0038(3) -0.0017(3) S3 0.0211(5) 0.0156(4) 0.0133(4) 0.0043(3) 0.0049(3) 0.0022(3) S4 0.0153(5) 0.0131(4) 0.0158(4) 0.0051(3) 0.0042(3) -0.0009(3) C1 0.012(2) 0.014(2) 0.0140(15) 0.0039(12) 0.0036(13) 0.0022(13) C2 0.016(2) 0.014(2) 0.016(2) 0.0050(13) 0.0053(13) 0.0052(14) C3 0.016(2) 0.016(2) 0.020(2) 0.0074(13) 0.0055(14) -0.0008(14) C4 0.018(2) 0.017(2) 0.021(2) 0.0103(14) 0.0071(14) -0.0002(15) C5 0.020(2) 0.020(2) 0.019(2) 0.0112(14) 0.0087(14) 0.005(2) C6 0.018(2) 0.021(2) 0.021(2) 0.0124(14) 0.0061(14) 0.0047(15) C7 0.025(3) 0.017(2) 0.037(2) 0.011(2) 0.006(2) -0.006(2) C8 0.039(3) 0.030(2) 0.018(2) 0.013(2) 0.008(2) -0.001(2) C9 0.037(3) 0.037(2) 0.019(2) 0.014(2) 0.013(2) 0.011(2) C10 0.025(3) 0.025(2) 0.041(2) 0.020(2) 0.013(2) 0.001(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 Mo1 O1 1.683(3) . ? Mo1 O21 1.896(3) . ? Mo1 O31 1.896(3) . ? Mo1 O12 1.960(3) . ? Mo1 O13 1.969(3) . ? Mo1 O19 2.3205(6) . ? Mo2 O2 1.688(3) . ? Mo2 O12 1.899(3) . ? Mo2 O23 1.901(3) . ? Mo2 O21 1.946(3) 2_577 ? Mo2 O32 1.955(3) . ? Mo2 O19 2.3071(6) . ? Mo3 O3 1.680(3) . ? Mo3 O13 1.906(3) 2_577 ? Mo3 O32 1.918(3) . ? Mo3 O23 1.941(3) 2_577 ? Mo3 O31 1.953(3) . ? Mo3 O19 2.3319(6) . ? O21 Mo2 1.946(3) 2_577 ? O13 Mo3 1.906(3) 2_577 ? O23 Mo3 1.941(3) 2_577 ? O19 Mo2 2.3071(7) 2_577 ? O19 Mo1 2.3205(6) 2_577 ? O19 Mo3 2.3319(6) 2_577 ? S1 C1 1.720(4) . ? S1 C3 1.747(4) . ? S2 C1 1.720(3) . ? S2 C4 1.749(4) . ? S3 C2 1.716(3) . ? S3 C5 1.727(4) . ? S4 C2 1.721(4) . ? S4 C6 1.740(4) . ? C1 C2 1.391(5) . ? C3 C4 1.352(5) . ? C3 C7 1.497(5) . ? C4 C8 1.498(5) . ? C5 C6 1.357(5) . ? C5 C9 1.512(5) . ? C6 C10 1.506(5) . ? C7 O7B 1.23(2) . ? C7 O7A 1.27(2) . ? C8 O8 1.203(14) . ? C9 O9 1.308(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 O1 Mo1 O21 104.29(13) . . ? O1 Mo1 O31 105.40(14) . . ? O21 Mo1 O31 89.92(13) . . ? O1 Mo1 O12 102.45(12) . . ? O21 Mo1 O12 152.96(11) . . ? O31 Mo1 O12 86.84(13) . . ? O1 Mo1 O13 101.19(14) . . ? O21 Mo1 O13 86.32(13) . . ? O31 Mo1 O13 153.24(11) . . ? O12 Mo1 O13 84.64(12) . . ? O1 Mo1 O19 177.06(11) . . ? O21 Mo1 O19 76.86(8) . . ? O31 Mo1 O19 77.22(8) . . ? O12 Mo1 O19 76.24(7) . . ? O13 Mo1 O19 76.12(7) . . ? O2 Mo2 O12 103.35(12) . . ? O2 Mo2 O23 104.12(14) . . ? O12 Mo2 O23 88.96(12) . . ? O2 Mo2 O21 102.61(12) . 2_577 ? O12 Mo2 O21 153.89(11) . 2_577 ? O23 Mo2 O21 87.37(12) . 2_577 ? O2 Mo2 O32 101.74(13) . . ? O12 Mo2 O32 87.20(12) . . ? O23 Mo2 O32 154.05(11) . . ? O21 Mo2 O32 84.92(13) 2_577 . ? O2 Mo2 O19 178.13(9) . . ? O12 Mo2 O19 77.71(8) . . ? O23 Mo2 O19 77.38(8) . . ? O21 Mo2 O19 76.26(8) 2_577 . ? O32 Mo2 O19 76.73(8) . . ? O3 Mo3 O13 102.61(14) . 2_577 ? O3 Mo3 O32 103.23(14) . . ? O13 Mo3 O32 88.71(12) 2_577 . ? O3 Mo3 O23 103.94(14) . 2_577 ? O13 Mo3 O23 87.04(12) 2_577 2_577 ? O32 Mo3 O23 152.78(12) . 2_577 ? O3 Mo3 O31 104.49(14) . . ? O13 Mo3 O31 152.88(12) 2_577 . ? O32 Mo3 O31 86.01(12) . . ? O23 Mo3 O31 85.63(12) 2_577 . ? O3 Mo3 O19 179.60(12) . . ? O13 Mo3 O19 76.99(8) 2_577 . ? O32 Mo3 O19 76.80(9) . . ? O23 Mo3 O19 76.04(8) 2_577 . ? O31 Mo3 O19 75.90(9) . . ? Mo2 O12 Mo1 116.03(12) . . ? Mo1 O31 Mo3 117.09(14) . . ? Mo1 O21 Mo2 116.77(13) . 2_577 ? Mo3 O13 Mo1 116.60(12) 2_577 . ? Mo2 O23 Mo3 116.79(13) . 2_577 ? Mo3 O32 Mo2 116.19(13) . . ? Mo2 O19 Mo2 180.0 2_577 . ? Mo2 O19 Mo1 90.02(2) 2_577 2_577 ? Mo2 O19 Mo1 89.98(2) . 2_577 ? Mo2 O19 Mo1 89.98(2) 2_577 . ? Mo2 O19 Mo1 90.02(2) . . ? Mo1 O19 Mo1 180.0 2_577 . ? Mo2 O19 Mo3 90.28(2) 2_577 2_577 ? Mo2 O19 Mo3 89.72(2) . 2_577 ? Mo1 O19 Mo3 89.77(2) 2_577 2_577 ? Mo1 O19 Mo3 90.23(2) . 2_577 ? Mo2 O19 Mo3 89.72(2) 2_577 . ? Mo2 O19 Mo3 90.28(2) . . ? Mo1 O19 Mo3 90.23(2) 2_577 . ? Mo1 O19 Mo3 89.77(2) . . ? Mo3 O19 Mo3 180.0 2_577 . ? C1 S1 C3 95.7(2) . . ? C1 S2 C4 95.5(2) . . ? C2 S3 C5 95.9(2) . . ? C2 S4 C6 95.9(2) . . ? C2 C1 S2 122.9(3) . . ? C2 C1 S1 121.4(3) . . ? S2 C1 S1 115.6(2) . . ? C1 C2 S3 122.1(3) . . ? C1 C2 S4 122.7(3) . . ? S3 C2 S4 115.2(2) . . ? C4 C3 C7 127.9(3) . . ? C4 C3 S1 116.3(3) . . ? C7 C3 S1 115.8(3) . . ? C3 C4 C8 126.5(4) . . ? C3 C4 S2 116.7(3) . . ? C8 C4 S2 116.8(3) . . ? C6 C5 C9 125.9(4) . . ? C6 C5 S3 117.1(3) . . ? C9 C5 S3 117.1(3) . . ? C5 C6 C10 125.9(3) . . ? C5 C6 S4 115.9(3) . . ? C10 C6 S4 118.2(3) . . ? O7B C7 O7A 120.3(14) . . ? O7B C7 C3 111.8(12) . . ? O7A C7 C3 114.7(9) . . ? O8 C8 C4 113.6(8) . . ? O9 C9 C5 110.5(6) . . ? _refine_diff_density_max 1.281 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.144 #=END #########################Material relevant to EDT-TTF(CH2OH)2################# data_adoh2 _audit_creation_method SHELXL _chemical_name_systematic ; Bis[3,4-(ethylenedithio)-3'-4'-bis(hydroxymethyl)-tetrathiafulvalene] nonadecaoxohexamolybdate(VI) ; _chemical_name_common ? _chemical_formula_moiety '(C10 H10 O2 S6)2 Mo6 O19' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H20 Mo6 O23 S12' _chemical_formula_weight 1588.72 _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 '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' 'S' 'S' 0.1246 0.1234 '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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.654(2) _cell_length_b 11.5411(8) _cell_length_c 17.1100(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.342(9) _cell_angle_gamma 90.00 _cell_volume 3998.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.8 _exptl_crystal_description 'plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.639 _exptl_crystal_density_method ? _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 2.538 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'FACEIT (Stoe IPDS)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 1.1\%' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34134 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.87 _reflns_number_total 8121 _reflns_number_observed 6918 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS)' _computing_cell_refinement 'SELECT (Stoe IPDS)' _computing_data_reduction 'INTEGRATE (Stoe IPDS)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0176P)^2^+82.1288P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8120 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_obs 0.0637 _refine_ls_wR_factor_all 0.1335 _refine_ls_wR_factor_obs 0.1292 _refine_ls_goodness_of_fit_all 1.292 _refine_ls_goodness_of_fit_obs 1.376 _refine_ls_restrained_S_all 1.306 _refine_ls_restrained_S_obs 1.376 _refine_ls_shift/esd_max 0.012 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.21131(4) 0.22599(7) 0.37916(5) 0.0150(2) Uani 1 d . . Mo2 Mo 0.18353(4) 0.10658(6) 0.20232(5) 0.0134(2) Uani 1 d . . Mo3 Mo 0.32973(4) 0.08795(7) 0.31631(5) 0.0170(2) Uani 1 d . . Mo4 Mo 0.33490(4) 0.37137(7) 0.33266(5) 0.0176(2) Uani 1 d . . Mo5 Mo 0.30526(4) 0.25253(7) 0.15491(5) 0.0145(2) Uani 1 d . . Mo6 Mo 0.18727(4) 0.39036(6) 0.21895(5) 0.0126(2) Uani 1 d . . O1 O 0.1743(4) 0.2157(6) 0.4579(5) 0.026(2) Uani 1 d . . O2 O 0.1287(3) 0.0096(5) 0.1533(5) 0.021(2) Uani 1 d . . O3 O 0.3830(4) -0.0193(7) 0.3514(5) 0.028(2) Uani 1 d . . O4 O 0.3895(3) 0.4685(7) 0.3806(5) 0.028(2) Uani 1 d . . O5 O 0.3440(3) 0.2624(6) 0.0775(4) 0.022(2) Uani 1 d . . O6 O 0.1336(3) 0.4961(5) 0.1804(4) 0.0190(15) Uani 1 d . . O12 O 0.1592(3) 0.1187(6) 0.3030(4) 0.0166(14) Uani 1 d . . O13 O 0.2774(3) 0.1070(6) 0.3965(4) 0.0179(14) Uani 1 d . . O14 O 0.2778(3) 0.3389(6) 0.4089(4) 0.0171(14) Uani 1 d . . O16 O 0.1600(3) 0.3459(5) 0.3147(4) 0.0147(13) Uani 1 d . . O19 O 0.2588(3) 0.2395(5) 0.2672(4) 0.0086(11) Uani 1 d . . O23 O 0.2567(3) 0.0090(5) 0.2540(4) 0.0192(15) Uani 1 d . . O25 O 0.2391(3) 0.1396(5) 0.1244(4) 0.0168(14) Uani 1 d . . O26 O 0.1405(3) 0.2506(5) 0.1723(4) 0.0126(13) Uani 1 d . . O34 O 0.3764(3) 0.2272(6) 0.3619(4) 0.0178(14) Uani 1 d . . O35 O 0.3572(3) 0.1316(6) 0.2190(4) 0.0173(14) Uani 1 d . . O45 O 0.3586(3) 0.3599(6) 0.2314(4) 0.0192(15) Uani 1 d . . O46 O 0.2601(3) 0.4687(5) 0.2803(4) 0.0179(14) Uani 1 d . . O56 O 0.2401(3) 0.3703(5) 0.1375(4) 0.0157(14) Uani 1 d . . S1A S 0.31477(12) -0.2770(2) 0.1756(2) 0.0202(5) Uani 1 d . . S2A S 0.32313(11) -0.4499(2) 0.0534(2) 0.0159(5) Uani 1 d . . S3A S 0.16958(10) -0.2184(2) 0.09653(15) 0.0141(5) Uani 1 d . . S4A S 0.15978(11) -0.4210(2) -0.00692(15) 0.0144(5) Uani 1 d . . S5A S 0.03328(11) -0.1392(2) 0.04376(15) 0.0141(5) Uani 1 d . . S6A S 0.01582(11) -0.3881(2) -0.07416(15) 0.0153(5) Uani 1 d . . O1A1 O 0.4338(6) -0.2182(11) 0.2795(8) 0.027(3) Uiso 0.60 d P . O1A2 O 0.4965(9) -0.2649(16) 0.2393(12) 0.028(4) Uiso 0.40 d P . O2A O 0.4505(4) -0.5366(7) 0.0413(6) 0.042(2) Uani 1 d . . C1A C 0.4436(6) -0.3157(12) 0.2527(9) 0.046(4) Uani 1 d . . C2A C 0.4510(5) -0.4998(11) 0.1198(8) 0.036(3) Uani 1 d . . H2A1 H 0.4913(5) -0.4569(11) 0.1393(8) 0.043 Uiso 1 calc R . H2A2 H 0.4510(5) -0.5672(11) 0.1536(8) 0.043 Uiso 1 calc R . C3A C 0.3898(5) -0.3453(10) 0.1812(7) 0.029(3) Uani 1 d . . C4A C 0.3933(5) -0.4254(9) 0.1260(7) 0.024(2) Uani 1 d . . C5A C 0.2744(4) -0.3534(8) 0.0934(6) 0.016(2) Uani 1 d . . C6A C 0.2089(5) -0.3350(7) 0.0613(6) 0.014(2) Uani 1 d . . C7A C 0.0922(4) -0.2444(7) 0.0365(5) 0.009(2) Uiso 1 d . . C8A C 0.0887(4) -0.3379(8) -0.0117(6) 0.014(2) Uani 1 d . . C9A C -0.0420(4) -0.1978(7) -0.0151(6) 0.014(2) Uani 1 d . . H9A1 H -0.0791(4) -0.1709(7) 0.0070(6) 0.017 Uiso 1 calc R . H9A2 H -0.0474(4) -0.1680(7) -0.0690(6) 0.017 Uiso 1 calc R . C10A C -0.0433(4) -0.3301(8) -0.0183(6) 0.013(2) Uani 1 d . . H10A H -0.0873(4) -0.3557(8) -0.0429(6) 0.015 Uiso 1 calc R . H10B H -0.0334(4) -0.3604(8) 0.0356(6) 0.015 Uiso 1 calc R . S1B S 0.31851(11) -0.0529(2) 0.0388(2) 0.0164(5) Uani 1 d . . S2B S 0.35825(11) -0.2355(2) -0.06067(15) 0.0158(5) Uani 1 d . . S3B S 0.17228(10) -0.0567(2) -0.07131(15) 0.0129(5) Uani 1 d . . S4B S 0.20729(10) -0.2612(2) -0.15382(14) 0.0142(4) Uani 1 d . . S5B S 0.03387(11) -0.0463(2) -0.1603(2) 0.0175(5) Uani 1 d . . S6B S 0.07676(11) -0.3001(2) -0.2526(2) 0.0177(5) Uani 1 d . . O1B1 O 0.4473(7) -0.0402(12) 0.1907(10) 0.024(3) Uiso 0.50 d P . O1B2 O 0.4425(7) 0.0762(13) 0.1238(10) 0.026(3) Uiso 0.50 d P . O2B O 0.4993(4) -0.2503(7) -0.0587(5) 0.031(2) Uani 1 d . . C1B C 0.4461(6) -0.0215(16) 0.1201(10) 0.056(5) Uani 1 d . . C2B C 0.4883(5) -0.2184(10) 0.0152(7) 0.025(2) Uani 1 d . . H2B1 H 0.5198(5) -0.1590(10) 0.0375(7) 0.030 Uiso 1 calc R . H2B2 H 0.4953(5) -0.2849(10) 0.0506(7) 0.030 Uiso 1 calc R . C3B C 0.4017(4) -0.0888(9) 0.0564(6) 0.021(2) Uani 1 d . . C4B C 0.4194(4) -0.1732(9) 0.0105(6) 0.017(2) Uani 1 d . . C5B C 0.2957(4) -0.1503(7) -0.0387(6) 0.010(2) Uani 1 d . . C6B C 0.2314(4) -0.1554(7) -0.0821(6) 0.014(2) Uani 1 d . . C7B C 0.1097(4) -0.1183(7) -0.1418(6) 0.013(2) Uani 1 d . . C8B C 0.1251(4) -0.2132(7) -0.1809(6) 0.014(2) Uani 1 d . . C9B C 0.0021(5) -0.0971(8) -0.2596(6) 0.019(2) Uani 1 d . . H9B1 H -0.0412(5) -0.0636(8) -0.2784(6) 0.022 Uiso 1 calc R . H9B2 H 0.0308(5) -0.0705(8) -0.2945(6) 0.022 Uiso 1 calc R . C10B C -0.0033(4) -0.2288(8) -0.2650(6) 0.016(2) Uani 1 d . . H10C H -0.0296(4) -0.2499(8) -0.3164(6) 0.019 Uiso 1 calc R . H10D H -0.0261(4) -0.2566(8) -0.2242(6) 0.019 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 Mo1 0.0134(4) 0.0198(4) 0.0133(5) 0.0012(3) 0.0063(3) 0.0023(3) Mo2 0.0096(4) 0.0083(3) 0.0211(5) -0.0024(3) -0.0001(3) -0.0016(3) Mo3 0.0117(4) 0.0204(4) 0.0181(5) 0.0038(3) 0.0011(3) 0.0086(3) Mo4 0.0105(4) 0.0219(4) 0.0199(5) -0.0093(3) 0.0016(3) -0.0060(3) Mo5 0.0184(4) 0.0140(4) 0.0133(5) -0.0009(3) 0.0087(3) -0.0011(3) Mo6 0.0128(4) 0.0078(3) 0.0164(5) -0.0003(3) 0.0008(3) 0.0021(3) O1 0.025(4) 0.030(4) 0.025(5) 0.003(3) 0.012(3) -0.003(3) O2 0.015(3) 0.011(3) 0.035(5) -0.006(3) 0.001(3) 0.000(3) O3 0.021(4) 0.032(4) 0.029(5) 0.007(3) 0.001(3) 0.014(3) O4 0.017(4) 0.034(4) 0.032(5) -0.015(3) 0.005(3) -0.008(3) O5 0.023(3) 0.025(4) 0.021(4) 0.001(3) 0.014(3) 0.000(3) O6 0.017(3) 0.011(3) 0.030(5) 0.000(3) 0.008(3) 0.007(2) O12 0.010(3) 0.021(3) 0.021(4) 0.006(3) 0.008(3) -0.002(2) O13 0.010(3) 0.029(4) 0.016(4) 0.008(3) 0.005(3) 0.007(3) O14 0.011(3) 0.023(3) 0.016(4) -0.006(3) -0.001(3) 0.001(3) O16 0.012(3) 0.015(3) 0.016(4) -0.005(3) 0.000(3) 0.003(2) O19 0.008(3) 0.007(3) 0.009(3) -0.001(2) 0.000(2) -0.001(2) O23 0.016(3) 0.015(3) 0.025(4) 0.004(3) 0.002(3) 0.006(3) O25 0.025(4) 0.011(3) 0.014(4) -0.005(2) 0.002(3) 0.000(3) O26 0.013(3) 0.010(3) 0.012(4) -0.003(2) -0.004(2) 0.001(2) O34 0.011(3) 0.029(4) 0.011(4) -0.002(3) -0.004(3) 0.002(3) O35 0.016(3) 0.018(3) 0.021(4) 0.000(3) 0.008(3) 0.005(3) O45 0.012(3) 0.020(3) 0.026(4) -0.008(3) 0.007(3) -0.009(3) O46 0.016(3) 0.014(3) 0.023(4) -0.006(3) 0.003(3) -0.006(3) O56 0.022(3) 0.014(3) 0.011(4) 0.004(2) 0.004(3) 0.000(3) S1A 0.0177(11) 0.0289(13) 0.0134(14) -0.0027(10) 0.0019(9) -0.0031(9) S2A 0.0119(10) 0.0148(10) 0.0209(14) 0.0021(9) 0.0028(9) 0.0049(8) S3A 0.0098(10) 0.0171(10) 0.0145(13) -0.0058(8) 0.0000(8) -0.0003(8) S4A 0.0136(10) 0.0110(10) 0.0187(14) -0.0037(8) 0.0033(9) -0.0001(8) S5A 0.0121(10) 0.0130(10) 0.0157(13) -0.0049(8) -0.0013(8) 0.0031(8) S6A 0.0177(11) 0.0148(10) 0.0128(13) -0.0031(8) 0.0012(9) -0.0029(8) O2A 0.033(5) 0.036(5) 0.058(7) 0.011(4) 0.014(4) 0.019(4) C1A 0.036(7) 0.050(8) 0.041(9) 0.023(6) -0.021(6) -0.024(6) C2A 0.013(5) 0.042(7) 0.052(9) 0.022(6) 0.005(5) 0.015(5) C3A 0.016(5) 0.033(6) 0.031(7) 0.013(5) -0.010(4) -0.006(4) C4A 0.011(4) 0.034(6) 0.028(7) 0.016(5) 0.006(4) 0.006(4) C5A 0.014(4) 0.012(4) 0.024(6) 0.002(4) 0.006(4) -0.003(3) C6A 0.021(5) 0.008(4) 0.013(5) -0.002(3) 0.005(4) -0.003(3) C8A 0.012(4) 0.014(4) 0.016(5) 0.003(3) -0.001(3) 0.003(3) C9A 0.009(4) 0.011(4) 0.020(6) 0.002(3) -0.002(3) -0.001(3) C10A 0.010(4) 0.018(4) 0.010(5) 0.005(3) 0.002(3) -0.003(3) S1B 0.0094(10) 0.0191(11) 0.0202(14) -0.0059(9) 0.0016(9) 0.0005(8) S2B 0.0129(10) 0.0188(11) 0.0162(14) 0.0015(9) 0.0043(9) 0.0056(8) S3B 0.0090(10) 0.0095(9) 0.0194(14) -0.0008(8) 0.0006(8) 0.0015(7) S4B 0.0115(10) 0.0162(10) 0.0152(13) -0.0036(9) 0.0033(8) 0.0029(8) S5B 0.0097(10) 0.0189(11) 0.0222(15) -0.0031(9) -0.0012(9) 0.0034(8) S6B 0.0128(10) 0.0219(11) 0.0175(14) -0.0065(9) 0.0005(9) -0.0006(9) O2B 0.025(4) 0.033(4) 0.039(5) 0.009(4) 0.018(4) 0.010(3) C1B 0.013(6) 0.098(12) 0.052(11) -0.050(9) -0.001(6) 0.001(6) C2B 0.009(4) 0.038(6) 0.028(7) 0.009(5) 0.000(4) 0.006(4) C3B 0.008(4) 0.036(6) 0.017(6) 0.000(4) 0.001(4) 0.000(4) C4B 0.006(4) 0.030(5) 0.017(6) 0.011(4) 0.003(3) 0.005(4) C5B 0.009(4) 0.008(4) 0.013(5) 0.002(3) -0.001(3) 0.003(3) C6B 0.015(4) 0.013(4) 0.013(5) 0.000(3) 0.003(4) -0.003(3) C7B 0.012(4) 0.013(4) 0.015(5) -0.002(3) 0.002(3) -0.004(3) C8B 0.013(4) 0.012(4) 0.017(6) 0.002(3) 0.004(4) 0.002(3) C9B 0.008(4) 0.025(5) 0.023(6) 0.008(4) 0.002(4) -0.003(4) C10B 0.007(4) 0.028(5) 0.014(6) 0.002(4) 0.003(3) -0.001(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 Mo1 O1 1.679(7) . ? Mo1 O14 1.889(6) . ? Mo1 O13 1.918(6) . ? Mo1 O16 1.949(6) . ? Mo1 O12 1.959(7) . ? Mo1 O19 2.323(6) . ? Mo2 O2 1.693(7) . ? Mo2 O12 1.891(7) . ? Mo2 O26 1.906(6) . ? Mo2 O23 1.951(6) . ? Mo2 O25 1.960(7) . ? Mo2 O19 2.307(6) . ? Mo3 O3 1.686(7) . ? Mo3 O23 1.900(7) . ? Mo3 O13 1.918(7) . ? Mo3 O35 1.928(7) . ? Mo3 O34 1.955(7) . ? Mo3 O19 2.329(6) . ? Mo4 O4 1.684(7) . ? Mo4 O34 1.893(7) . ? Mo4 O45 1.896(7) . ? Mo4 O14 1.959(7) . ? Mo4 O46 1.976(7) . ? Mo4 O19 2.313(6) . ? Mo5 O5 1.680(7) . ? Mo5 O25 1.887(6) . ? Mo5 O56 1.894(6) . ? Mo5 O35 1.959(7) . ? Mo5 O45 1.973(7) . ? Mo5 O19 2.315(6) . ? Mo6 O6 1.693(6) . ? Mo6 O46 1.887(6) . ? Mo6 O16 1.904(7) . ? Mo6 O56 1.946(7) . ? Mo6 O26 1.967(6) . ? Mo6 O19 2.328(6) . ? S1A C3A 1.724(11) . ? S1A C5A 1.729(10) . ? S2A C5A 1.731(10) . ? S2A C4A 1.738(11) . ? S3A C6A 1.740(9) . ? S3A C7A 1.747(8) . ? S4A C6A 1.706(9) . ? S4A C8A 1.742(9) . ? S5A C7A 1.741(8) . ? S5A C9A 1.808(9) . ? S6A C8A 1.763(9) . ? S6A C10A 1.820(9) . ? O1A1 C1A 1.25(2) . ? O1A1 O1A2 1.67(2) . ? O1A2 C1A 1.30(2) . ? O2A C2A 1.41(2) . ? C1A C3A 1.52(2) . ? C2A C4A 1.489(14) . ? C3A C4A 1.33(2) . ? C5A C6A 1.373(13) . ? C7A C8A 1.351(12) . ? C9A C10A 1.528(12) . ? S1B C5B 1.732(9) . ? S1B C3B 1.735(9) . ? S2B C5B 1.723(8) . ? S2B C4B 1.730(10) . ? S3B C6B 1.707(9) . ? S3B C7B 1.737(9) . ? S4B C6B 1.734(9) . ? S4B C8B 1.758(9) . ? S5B C7B 1.745(9) . ? S5B C9B 1.795(11) . ? S6B C8B 1.740(10) . ? S6B C10B 1.822(9) . ? O1B1 C1B 1.22(2) . ? O1B1 O1B2 1.76(2) . ? O1B2 C1B 1.13(2) . ? O2B C2B 1.379(14) . ? C1B C3B 1.50(2) . ? C2B C4B 1.503(12) . ? C3B C4B 1.346(15) . ? C5B C6B 1.389(12) . ? C7B C8B 1.354(12) . ? C9B C10B 1.525(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O14 104.7(3) . . ? O1 Mo1 O13 104.4(3) . . ? O14 Mo1 O13 89.7(3) . . ? O1 Mo1 O16 102.8(3) . . ? O14 Mo1 O16 87.0(3) . . ? O13 Mo1 O16 152.6(3) . . ? O1 Mo1 O12 102.2(3) . . ? O14 Mo1 O12 152.9(3) . . ? O13 Mo1 O12 86.1(3) . . ? O16 Mo1 O12 84.6(3) . . ? O1 Mo1 O19 177.9(3) . . ? O14 Mo1 O19 76.9(3) . . ? O13 Mo1 O19 76.8(2) . . ? O16 Mo1 O19 75.9(2) . . ? O12 Mo1 O19 76.1(2) . . ? O2 Mo2 O12 103.3(3) . . ? O2 Mo2 O26 102.2(3) . . ? O12 Mo2 O26 89.3(3) . . ? O2 Mo2 O23 103.0(3) . . ? O12 Mo2 O23 87.2(3) . . ? O26 Mo2 O23 154.6(3) . . ? O2 Mo2 O25 102.4(3) . . ? O12 Mo2 O25 154.3(3) . . ? O26 Mo2 O25 87.2(3) . . ? O23 Mo2 O25 85.2(3) . . ? O2 Mo2 O19 179.0(3) . . ? O12 Mo2 O19 77.7(2) . . ? O26 Mo2 O19 77.5(2) . . ? O23 Mo2 O19 77.1(2) . . ? O25 Mo2 O19 76.6(2) . . ? O3 Mo3 O23 103.8(3) . . ? O3 Mo3 O13 104.4(3) . . ? O23 Mo3 O13 87.7(3) . . ? O3 Mo3 O35 102.5(3) . . ? O23 Mo3 O35 88.7(3) . . ? O13 Mo3 O35 152.9(3) . . ? O3 Mo3 O34 103.0(3) . . ? O23 Mo3 O34 153.2(3) . . ? O13 Mo3 O34 85.6(3) . . ? O35 Mo3 O34 85.7(3) . . ? O3 Mo3 O19 178.2(3) . . ? O23 Mo3 O19 77.5(2) . . ? O13 Mo3 O19 76.7(2) . . ? O35 Mo3 O19 76.3(2) . . ? O34 Mo3 O19 75.6(2) . . ? O4 Mo4 O34 103.4(3) . . ? O4 Mo4 O45 102.9(3) . . ? O34 Mo4 O45 89.8(3) . . ? O4 Mo4 O14 103.6(3) . . ? O34 Mo4 O14 87.5(3) . . ? O45 Mo4 O14 153.2(3) . . ? O4 Mo4 O46 103.4(3) . . ? O34 Mo4 O46 153.1(3) . . ? O45 Mo4 O46 86.8(3) . . ? O14 Mo4 O46 83.8(3) . . ? O4 Mo4 O19 179.2(3) . . ? O34 Mo4 O19 77.2(2) . . ? O45 Mo4 O19 77.5(2) . . ? O14 Mo4 O19 75.9(2) . . ? O46 Mo4 O19 76.0(2) . . ? O5 Mo5 O25 105.1(3) . . ? O5 Mo5 O56 105.1(3) . . ? O25 Mo5 O56 89.9(3) . . ? O5 Mo5 O35 101.3(3) . . ? O25 Mo5 O35 87.1(3) . . ? O56 Mo5 O35 153.3(3) . . ? O5 Mo5 O45 100.9(3) . . ? O25 Mo5 O45 153.8(3) . . ? O56 Mo5 O45 86.6(3) . . ? O35 Mo5 O45 84.5(3) . . ? O5 Mo5 O19 176.1(3) . . ? O25 Mo5 O19 77.8(3) . . ? O56 Mo5 O19 77.3(2) . . ? O35 Mo5 O19 76.1(2) . . ? O45 Mo5 O19 76.1(2) . . ? O6 Mo6 O46 105.1(3) . . ? O6 Mo6 O16 104.3(3) . . ? O46 Mo6 O16 89.4(3) . . ? O6 Mo6 O56 102.9(3) . . ? O46 Mo6 O56 87.6(3) . . ? O16 Mo6 O56 152.4(3) . . ? O6 Mo6 O26 101.6(3) . . ? O46 Mo6 O26 153.2(3) . . ? O16 Mo6 O26 85.6(3) . . ? O56 Mo6 O26 84.9(3) . . ? O6 Mo6 O19 177.4(3) . . ? O46 Mo6 O19 77.3(2) . . ? O16 Mo6 O19 76.6(2) . . ? O56 Mo6 O19 76.0(2) . . ? O26 Mo6 O19 75.9(2) . . ? Mo2 O12 Mo1 116.3(3) . . ? Mo3 O13 Mo1 117.1(3) . . ? Mo1 O14 Mo4 117.0(3) . . ? Mo6 O16 Mo1 117.3(3) . . ? Mo2 O19 Mo4 179.5(2) . . ? Mo2 O19 Mo5 89.7(2) . . ? Mo4 O19 Mo5 90.4(2) . . ? Mo2 O19 Mo1 89.9(2) . . ? Mo4 O19 Mo1 90.1(2) . . ? Mo5 O19 Mo1 179.5(3) . . ? Mo2 O19 Mo6 90.3(2) . . ? Mo4 O19 Mo6 90.2(2) . . ? Mo5 O19 Mo6 89.7(2) . . ? Mo1 O19 Mo6 90.1(2) . . ? Mo2 O19 Mo3 89.5(2) . . ? Mo4 O19 Mo3 90.0(2) . . ? Mo5 O19 Mo3 90.8(2) . . ? Mo1 O19 Mo3 89.4(2) . . ? Mo6 O19 Mo3 179.4(3) . . ? Mo3 O23 Mo2 115.9(3) . . ? Mo5 O25 Mo2 115.8(3) . . ? Mo2 O26 Mo6 116.1(3) . . ? Mo4 O34 Mo3 117.1(3) . . ? Mo3 O35 Mo5 116.6(3) . . ? Mo4 O45 Mo5 116.0(3) . . ? Mo6 O46 Mo4 116.5(3) . . ? Mo5 O56 Mo6 117.0(3) . . ? C3A S1A C5A 95.5(5) . . ? C5A S2A C4A 94.6(5) . . ? C6A S3A C7A 95.6(4) . . ? C6A S4A C8A 95.4(4) . . ? C7A S5A C9A 103.7(4) . . ? C8A S6A C10A 98.1(4) . . ? C1A O1A1 O1A2 50.3(10) . . ? C1A O1A2 O1A1 47.6(10) . . ? O1A1 C1A O1A2 82.1(12) . . ? O1A1 C1A C3A 110.6(12) . . ? O1A2 C1A C3A 117.8(14) . . ? O2A C2A C4A 112.8(9) . . ? C4A C3A C1A 126.3(11) . . ? C4A C3A S1A 116.9(8) . . ? C1A C3A S1A 116.6(10) . . ? C3A C4A C2A 127.4(11) . . ? C3A C4A S2A 117.7(8) . . ? C2A C4A S2A 114.9(9) . . ? C6A C5A S1A 121.8(7) . . ? C6A C5A S2A 123.0(8) . . ? S1A C5A S2A 115.1(5) . . ? C5A C6A S4A 126.2(7) . . ? C5A C6A S3A 118.1(7) . . ? S4A C6A S3A 115.6(5) . . ? C8A C7A S5A 130.2(7) . . ? C8A C7A S3A 115.5(6) . . ? S5A C7A S3A 114.2(5) . . ? C7A C8A S4A 117.8(7) . . ? C7A C8A S6A 124.7(7) . . ? S4A C8A S6A 117.3(5) . . ? C10A C9A S5A 113.6(6) . . ? C9A C10A S6A 112.1(6) . . ? C5B S1B C3B 95.1(5) . . ? C5B S2B C4B 94.8(4) . . ? C6B S3B C7B 95.9(4) . . ? C6B S4B C8B 95.4(4) . . ? C7B S5B C9B 99.4(4) . . ? C8B S6B C10B 101.8(4) . . ? C1B O1B1 O1B2 39.9(10) . . ? C1B O1B2 O1B1 43.8(11) . . ? O1B2 C1B O1B1 96.3(14) . . ? O1B2 C1B C3B 121.3(16) . . ? O1B1 C1B C3B 121.2(16) . . ? O2B C2B C4B 111.6(9) . . ? C4B C3B C1B 127.0(9) . . ? C4B C3B S1B 116.5(8) . . ? C1B C3B S1B 116.5(8) . . ? C3B C4B C2B 125.7(10) . . ? C3B C4B S2B 117.8(7) . . ? C2B C4B S2B 116.5(8) . . ? C6B C5B S2B 122.6(7) . . ? C6B C5B S1B 121.6(7) . . ? S2B C5B S1B 115.8(5) . . ? C5B C6B S3B 122.9(7) . . ? C5B C6B S4B 121.3(7) . . ? S3B C6B S4B 115.7(5) . . ? C8B C7B S3B 117.3(7) . . ? C8B C7B S5B 125.8(7) . . ? S3B C7B S5B 116.7(5) . . ? C7B C8B S6B 131.0(7) . . ? C7B C8B S4B 115.7(7) . . ? S6B C8B S4B 113.3(5) . . ? C10B C9B S5B 113.0(7) . . ? C9B C10B S6B 112.9(6) . . ? _refine_diff_density_max 2.767 _refine_diff_density_min -1.525 _refine_diff_density_rms 0.210 #=END ############################Material relevant to TTF(CH2OH)4################## data_adoh4 _audit_creation_method SHELXL _chemical_name_systematic ; Bis[tetrakis-3,4,3',4'-(hydroxymethyl)tetrathiafulvalenium] nonadecaoxohexamolybdate(VI) ; _chemical_name_common '[TTF(CH~2~OH)~4~]^2^Mo~6~O~19~' _chemical_formula_moiety '(C10 H12 O4 S4)~2~, Mo6 O19' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H24 Mo6 O27 S8' _chemical_formula_weight 1528.51 _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 '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' 'S' 'S' 0.1246 0.1234 '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 8.668(2) _cell_length_b 10.862(2) _cell_length_c 11.478(2) _cell_angle_alpha 69.58(3) _cell_angle_beta 83.28(3) _cell_angle_gamma 77.00(3) _cell_volume 985.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26.75 _exptl_crystal_description 'thin plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.574 _exptl_crystal_density_method ? _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 2.371 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACEIT, Stoe IDPS' _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.9910 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'area detector' _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'rotation, phi incr. 2\%' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10552 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.95 _reflns_number_total 3914 _reflns_number_observed 2948 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'EXPOSE [Stoe IPDS]' _computing_cell_refinement 'SELECT [Stoe IPDS]' _computing_data_reduction 'INTEGRATE [Stoe IPDS]' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP [Johnson, 1976]' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 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^)+(0.0129P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3912 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_obs 0.0247 _refine_ls_wR_factor_all 0.0446 _refine_ls_wR_factor_obs 0.0403 _refine_ls_goodness_of_fit_all 0.890 _refine_ls_goodness_of_fit_obs 0.962 _refine_ls_restrained_S_all 0.914 _refine_ls_restrained_S_obs 0.962 _refine_ls_shift/esd_max -0.002 _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 Mo1 Mo -0.07187(4) 0.17826(3) 0.82046(3) 0.00929(8) Uani 1 d . . Mo2 Mo -0.11950(4) 0.13283(3) 1.11995(3) 0.00876(8) Uani 1 d . . Mo3 Mo -0.23719(4) -0.06722(3) 1.00556(3) 0.00949(8) Uani 1 d . . O1 O -0.1379(4) 0.3120(2) 0.6956(3) 0.0173(7) Uani 1 d . . O2 O -0.2098(3) 0.2223(2) 1.2108(3) 0.0142(6) Uani 1 d . . O3 O -0.3991(3) -0.1312(2) 1.0128(3) 0.0170(7) Uani 1 d . . O13 O -0.2528(3) 0.0830(2) 0.8628(3) 0.0112(6) Uani 1 d . . O31 O 0.1179(3) 0.2086(2) 0.8536(3) 0.0129(6) Uani 1 d . . O12 O 0.0334(3) 0.0433(2) 0.7566(2) 0.0128(6) Uani 1 d . . O21 O -0.1732(3) 0.2474(2) 0.9563(2) 0.0095(6) Uani 1 d . . O32 O 0.0863(3) 0.1645(2) 1.0937(3) 0.0107(6) Uani 1 d . . O23 O -0.2854(3) 0.0369(2) 1.1107(3) 0.0113(6) Uani 1 d . . O19 O 0.0000 0.0000 1.0000 0.0061(8) Uani 1 d S . S1A S 0.21531(12) -0.13892(8) 0.47664(9) 0.0117(2) Uani 1 d . . S2A S 0.13987(12) 0.15188(8) 0.40620(10) 0.0134(2) Uani 1 d . . O4A O 0.5263(4) -0.2754(2) 0.4455(3) 0.0226(7) Uani 1 d . . H4A H 0.5336(4) -0.2792(2) 0.5173(3) 0.034 Uiso 1 calc R . O5A O 0.3894(4) 0.2930(2) 0.3222(3) 0.0206(7) Uani 1 d . . H5A H 0.4122(4) 0.3578(2) 0.2653(3) 0.031 Uiso 1 calc R . C1A C 0.0749(4) 0.0022(3) 0.4752(4) 0.0087(7) Uani 1 d . . C2A C 0.3629(5) -0.0541(3) 0.3951(4) 0.0123(8) Uani 1 d . . C3A C 0.3269(5) 0.0811(3) 0.3616(4) 0.0110(8) Uani 1 d . . C4A C 0.5142(5) -0.1398(3) 0.3646(4) 0.0152(9) Uani 1 d . . H4A1 H 0.5153(5) -0.1361(3) 0.2789(4) 0.018 Uiso 1 calc R . H4A2 H 0.6044(5) -0.1055(3) 0.3741(4) 0.018 Uiso 1 calc R . C5A C 0.4321(5) 0.1763(3) 0.2850(4) 0.0186(9) Uani 1 d . . H5A1 H 0.5426(5) 0.1352(3) 0.3003(4) 0.022 Uiso 1 calc R . H5A2 H 0.4158(5) 0.2001(3) 0.1971(4) 0.022 Uiso 1 calc R . S1B S 0.00177(12) 0.46839(8) 0.19676(9) 0.0098(2) Uani 1 d . . S2B S -0.25540(11) 0.55376(8) 0.02704(9) 0.0115(2) Uani 1 d . . O4B O -0.0547(4) 0.4175(3) 0.4444(3) 0.0223(7) Uani 1 d . . H4B H -0.0316(4) 0.4458(3) 0.4963(3) 0.033 Uiso 1 calc R . O5B O -0.5719(3) 0.5349(2) 0.1518(3) 0.0151(6) Uani 1 d . . H5B H -0.6469(3) 0.5928(2) 0.1182(3) 0.023 Uiso 1 calc R . C1B C -0.0554(5) 0.5057(3) 0.0480(3) 0.0092(8) Uani 1 d . . C2B C -0.1890(4) 0.5069(3) 0.2580(4) 0.0083(8) Uani 1 d . . C3B C -0.3081(5) 0.5470(3) 0.1792(4) 0.0097(8) Uani 1 d . . C4B C -0.2004(5) 0.4959(4) 0.3920(4) 0.0166(9) Uani 1 d . . H4B1 H -0.2181(5) 0.5842(4) 0.3998(4) 0.020 Uiso 1 calc R . H4B2 H -0.2878(5) 0.4532(4) 0.4347(4) 0.020 Uiso 1 calc R . C5B C -0.4803(5) 0.5903(3) 0.2097(4) 0.0111(8) Uani 1 d . . H5B1 H -0.5005(5) 0.5591(3) 0.2991(4) 0.013 Uiso 1 calc R . H5B2 H -0.5097(5) 0.6873(3) 0.1795(4) 0.013 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 Mo1 0.0128(2) 0.00629(13) 0.0064(2) 0.00083(11) -0.00170(13) -0.00121(12) Mo2 0.0107(2) 0.00763(14) 0.0083(2) -0.00384(12) 0.00156(13) -0.00158(12) Mo3 0.0072(2) 0.00843(13) 0.0133(2) -0.00321(12) -0.00014(14) -0.00327(12) O1 0.024(2) 0.0099(11) 0.012(2) 0.0020(10) -0.0051(12) 0.0015(11) O2 0.018(2) 0.0088(11) 0.017(2) -0.0068(10) 0.0033(12) -0.0019(10) O3 0.013(2) 0.0127(12) 0.028(2) -0.0089(11) 0.0003(13) -0.0047(11) O13 0.012(2) 0.0105(11) 0.012(2) -0.0046(10) -0.0045(11) 0.0003(10) O31 0.012(2) 0.0071(10) 0.017(2) -0.0004(10) 0.0014(11) -0.0033(10) O12 0.018(2) 0.0114(11) 0.007(2) -0.0018(10) -0.0021(11) -0.0005(10) O21 0.0099(15) 0.0052(10) 0.012(2) -0.0018(9) -0.0030(11) 0.0019(9) O32 0.0110(15) 0.0094(11) 0.015(2) -0.0075(10) -0.0005(11) -0.0026(10) O23 0.0080(15) 0.0103(11) 0.016(2) -0.0049(10) 0.0015(11) -0.0030(10) O19 0.008(2) 0.0041(14) 0.006(2) -0.0014(13) -0.0023(15) -0.0010(13) S1A 0.0113(5) 0.0078(4) 0.0147(6) -0.0030(3) 0.0012(4) -0.0015(3) S2A 0.0122(5) 0.0081(4) 0.0179(6) -0.0029(3) 0.0026(4) -0.0017(3) O4A 0.026(2) 0.0139(12) 0.025(2) -0.0069(11) 0.0002(14) 0.0012(11) O5A 0.026(2) 0.0106(11) 0.024(2) -0.0016(11) 0.0032(13) -0.0105(11) C1A 0.008(2) 0.0105(15) 0.007(2) -0.0036(13) 0.0000(15) -0.0010(13) C2A 0.014(2) 0.012(2) 0.010(2) -0.0049(14) 0.001(2) -0.0006(14) C3A 0.007(2) 0.017(2) 0.009(2) -0.0052(14) 0.0015(15) -0.0022(14) C4A 0.011(2) 0.017(2) 0.018(3) -0.008(2) 0.002(2) 0.0001(14) C5A 0.023(3) 0.015(2) 0.020(3) -0.008(2) 0.008(2) -0.010(2) S1B 0.0100(5) 0.0107(4) 0.0078(5) -0.0032(3) -0.0008(4) 0.0001(3) S2B 0.0097(5) 0.0142(4) 0.0101(6) -0.0049(3) -0.0011(4) 0.0003(3) O4B 0.020(2) 0.0297(14) 0.015(2) -0.0066(12) -0.0032(12) -0.0004(12) O5B 0.012(2) 0.0136(11) 0.020(2) -0.0057(10) -0.0054(12) -0.0003(10) C1B 0.014(2) 0.0038(14) 0.011(2) -0.0020(13) -0.003(2) -0.0021(13) C2B 0.011(2) 0.0047(14) 0.009(2) -0.0019(12) 0.0010(15) -0.0018(13) C3B 0.015(2) 0.0067(14) 0.008(2) -0.0040(13) 0.002(2) -0.0022(13) C4B 0.015(2) 0.021(2) 0.012(2) -0.006(2) 0.001(2) 0.000(2) C5B 0.009(2) 0.011(2) 0.016(2) -0.0058(14) 0.000(2) -0.0026(14) _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 O1 1.690(3) . ? Mo1 O31 1.854(3) . ? Mo1 O12 1.873(3) . ? Mo1 O21 1.991(3) . ? Mo1 O13 1.992(3) . ? Mo1 O19 2.3146(10) . ? Mo2 O2 1.679(3) . ? Mo2 O32 1.863(3) . ? Mo2 O21 1.899(3) . ? Mo2 O12 1.985(2) 2_557 ? Mo2 O23 1.988(3) . ? Mo2 O19 2.3303(8) . ? Mo3 O3 1.683(3) . ? Mo3 O13 1.858(2) . ? Mo3 O23 1.879(3) . ? Mo3 O31 1.996(3) 2_557 ? Mo3 O32 1.999(3) 2_557 ? Mo3 O19 2.3187(6) . ? O31 Mo3 1.996(3) 2_557 ? O12 Mo2 1.985(2) 2_557 ? O32 Mo3 1.999(3) 2_557 ? O19 Mo1 2.3146(10) 2_557 ? O19 Mo3 2.3187(6) 2_557 ? O19 Mo2 2.3302(8) 2_557 ? S1A C1A 1.726(3) . ? S1A C2A 1.735(4) . ? S2A C1A 1.731(3) . ? S2A C3A 1.732(4) . ? O4A C4A 1.429(4) . ? O5A C5A 1.434(4) . ? C1A C1A 1.360(7) 2_556 ? C2A C3A 1.352(5) . ? C2A C4A 1.510(5) . ? C3A C5A 1.509(5) . ? S1B C1B 1.717(4) . ? S1B C2B 1.740(4) . ? S2B C1B 1.715(4) . ? S2B C3B 1.733(4) . ? O4B C4B 1.420(5) . ? O5B C5B 1.432(5) . ? C1B C1B 1.395(8) 2_565 ? C2B C3B 1.347(5) . ? C2B C4B 1.494(6) . ? C3B C5B 1.499(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O31 104.55(12) . . ? O1 Mo1 O12 105.68(13) . . ? O31 Mo1 O12 91.90(12) . . ? O1 Mo1 O21 99.71(12) . . ? O31 Mo1 O21 87.69(12) . . ? O12 Mo1 O21 153.85(10) . . ? O1 Mo1 O13 101.76(12) . . ? O31 Mo1 O13 153.08(11) . . ? O12 Mo1 O13 86.37(11) . . ? O21 Mo1 O13 82.38(10) . . ? O1 Mo1 O19 175.41(10) . . ? O31 Mo1 O19 77.83(8) . . ? O12 Mo1 O19 78.01(8) . . ? O21 Mo1 O19 76.35(7) . . ? O13 Mo1 O19 75.53(8) . . ? O2 Mo2 O32 104.38(12) . . ? O2 Mo2 O21 104.08(12) . . ? O32 Mo2 O21 91.69(11) . . ? O2 Mo2 O12 102.48(12) . 2_557 ? O32 Mo2 O12 87.26(11) . 2_557 ? O21 Mo2 O12 152.81(11) . 2_557 ? O2 Mo2 O23 102.29(12) . . ? O32 Mo2 O23 152.90(11) . . ? O21 Mo2 O23 86.39(11) . . ? O12 Mo2 O23 82.41(11) 2_557 . ? O2 Mo2 O19 177.20(8) . . ? O32 Mo2 O19 77.65(8) . . ? O21 Mo2 O19 77.67(8) . . ? O12 Mo2 O19 75.57(8) 2_557 . ? O23 Mo2 O19 75.54(8) . . ? O3 Mo3 O13 106.00(13) . . ? O3 Mo3 O23 105.68(13) . . ? O13 Mo3 O23 92.64(11) . . ? O3 Mo3 O31 100.60(12) . 2_557 ? O13 Mo3 O31 152.63(11) . 2_557 ? O23 Mo3 O31 86.23(11) . 2_557 ? O3 Mo3 O32 100.62(12) . 2_557 ? O13 Mo3 O32 86.91(11) . 2_557 ? O23 Mo3 O32 152.72(11) . 2_557 ? O31 Mo3 O32 81.93(11) 2_557 2_557 ? O3 Mo3 O19 174.46(8) . . ? O13 Mo3 O19 77.90(9) . . ? O23 Mo3 O19 77.80(8) . . ? O31 Mo3 O19 75.13(8) 2_557 . ? O32 Mo3 O19 75.44(7) 2_557 . ? Mo3 O13 Mo1 116.57(13) . . ? Mo1 O31 Mo3 116.60(12) . 2_557 ? Mo1 O12 Mo2 116.52(14) . 2_557 ? Mo2 O21 Mo1 115.32(11) . . ? Mo2 O32 Mo3 116.81(12) . 2_557 ? Mo3 O23 Mo2 116.26(14) . . ? Mo1 O19 Mo1 180.0 . 2_557 ? Mo1 O19 Mo3 89.98(3) . . ? Mo1 O19 Mo3 90.02(3) 2_557 . ? Mo1 O19 Mo3 90.02(3) . 2_557 ? Mo1 O19 Mo3 89.98(3) 2_557 2_557 ? Mo3 O19 Mo3 180.0 . 2_557 ? Mo1 O19 Mo2 89.90(3) . 2_557 ? Mo1 O19 Mo2 90.10(3) 2_557 2_557 ? Mo3 O19 Mo2 90.10(2) . 2_557 ? Mo3 O19 Mo2 89.90(3) 2_557 2_557 ? Mo1 O19 Mo2 90.10(3) . . ? Mo1 O19 Mo2 89.90(3) 2_557 . ? Mo3 O19 Mo2 89.90(3) . . ? Mo3 O19 Mo2 90.10(3) 2_557 . ? Mo2 O19 Mo2 179.998(2) 2_557 . ? C1A S1A C2A 96.0(2) . . ? C1A S2A C3A 95.8(2) . . ? C1A C1A S1A 123.3(3) 2_556 . ? C1A C1A S2A 122.0(3) 2_556 . ? S1A C1A S2A 114.7(2) . . ? C3A C2A C4A 127.5(3) . . ? C3A C2A S1A 116.5(3) . . ? C4A C2A S1A 116.0(2) . . ? C2A C3A C5A 126.1(4) . . ? C2A C3A S2A 117.0(3) . . ? C5A C3A S2A 116.9(3) . . ? O4A C4A C2A 110.2(3) . . ? O5A C5A C3A 106.7(3) . . ? C1B S1B C2B 95.2(2) . . ? C1B S2B C3B 95.6(2) . . ? C1B C1B S2B 122.8(4) 2_565 . ? C1B C1B S1B 121.4(4) 2_565 . ? S2B C1B S1B 115.8(2) . . ? C3B C2B C4B 127.6(4) . . ? C3B C2B S1B 116.9(3) . . ? C4B C2B S1B 115.5(3) . . ? C2B C3B C5B 126.2(4) . . ? C2B C3B S2B 116.5(3) . . ? C5B C3B S2B 117.2(3) . . ? O4B C4B C2B 107.2(3) . . ? O5B C5B C3B 108.7(3) . . ? _refine_diff_density_max 0.567 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.126 ###############################################################################