Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'A. F. Christiansen' 'H. Fjellvag' 'A. Kjekshus' 'B. Klewe' _publ_contact_author_name 'Dr Arne Kjekshus' _publ_contact_author_address ; Dr Arne Kjekshus Department of Chemistry University of Oslo PO Box 1033 Blindern N-0315 Oslo NORWAY ; data_MoO2SO4_(I) _database_code_CSD 158631 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'molybdenum oxide sulfate (mod I)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Mo O6 S' _chemical_formula_weight 224.00 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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.3359(3) _cell_length_b 12.29010(10) _cell_length_c 8.58920(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.4800(10) _cell_angle_gamma 90.00 _cell_volume 2691.76(5) _cell_formula_units_Z 24 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 3.323 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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_measurement_device_type 'Siemens SMART 1000 CCD diffractom.' _diffrn_measurement_method 'Sets of exposures each taken over 0.6\% \w rotation' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27317 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 39.34 _reflns_number_total 7699 _reflns_number_gt 6122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0400P)^2^+700.0000P] 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 0.00045(6) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7699 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1213 _refine_ls_R_factor_gt 0.1033 _refine_ls_wR_factor_ref 0.2800 _refine_ls_wR_factor_gt 0.2720 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 0.24227(3) 0.11726(6) 0.75929(10) 0.00877(15) Uani 1 1 d . . . Mo2 Mo 0.08416(3) -0.12598(6) 0.59735(9) 0.00673(14) Uani 1 1 d . . . Mo3 Mo 0.07853(3) 0.37835(6) 0.60909(10) 0.00792(15) Uani 1 1 d . . . S1 S 0.28637(8) -0.12846(17) 0.6810(3) 0.0063(3) Uani 1 1 d . . . S2 S 0.05551(8) 0.12537(17) 0.4742(2) 0.0054(3) Uani 1 1 d . . . S3 S 0.12193(9) 0.62721(17) 0.7421(3) 0.0065(3) Uani 1 1 d . . . O1 O 0.2224(4) 0.1316(9) 0.5626(13) 0.0246(18) Uiso 1 1 d . . . O2 O 0.1857(4) 0.0970(8) 0.8107(13) 0.0217(17) Uiso 1 1 d . . . O3 O 0.2662(3) -0.0400(7) 0.7676(11) 0.0164(14) Uiso 1 1 d . . . O4 O 0.2502(3) 0.2778(6) 0.8252(9) 0.0095(11) Uiso 1 1 d . . . O5 O 0.1753(4) 0.6563(8) 0.7401(11) 0.0183(15) Uiso 1 1 d . . . O6 O 0.2865(4) -0.0933(9) 0.5212(13) 0.0223(17) Uiso 1 1 d . . . O7 O 0.0592(3) 0.0322(6) 0.5879(9) 0.0090(10) Uiso 1 1 d . . . O8 O 0.1492(3) -0.1036(7) 0.6431(10) 0.0151(13) Uiso 1 1 d . . . O9 O 0.0851(3) -0.2821(6) 0.6737(9) 0.0114(12) Uiso 1 1 d . . . O10 O 0.0726(4) -0.1458(8) 0.3984(12) 0.0199(16) Uiso 1 1 d . . . O11 O 0.0813(3) -0.0977(6) 0.8493(9) 0.0116(12) Uiso 1 1 d . . . O12 O -0.0012(3) -0.1575(6) 0.5865(9) 0.0108(11) Uiso 1 1 d . . . O13 O 0.0207(4) 0.3965(8) 0.4753(12) 0.0217(17) Uiso 1 1 d . . . O14 O 0.0617(4) 0.3717(8) 0.7866(12) 0.0195(15) Uiso 1 1 d . . . O15 O 0.1044(3) 0.5341(7) 0.6309(10) 0.0145(13) Uiso 1 1 d . . . O16 O 0.0857(3) 0.2165(6) 0.5696(9) 0.0094(11) Uiso 1 1 d . . . O17 O 0.3383(4) -0.1595(8) 0.7768(12) 0.0200(16) Uiso 1 1 d . . . O18 O 0.1171(4) 0.4000(8) 0.3996(12) 0.0211(17) 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 Mo1 0.0085(3) 0.0056(3) 0.0122(3) -0.0028(2) 0.0027(2) -0.0002(2) Mo2 0.0089(3) 0.0051(3) 0.0071(3) 0.0009(2) 0.0037(2) 0.0007(2) Mo3 0.0074(3) 0.0049(3) 0.0113(3) -0.0021(2) 0.0022(2) -0.0003(2) S1 0.0071(7) 0.0042(7) 0.0068(7) -0.0004(6) 0.0000(6) -0.0007(6) S2 0.0064(7) 0.0047(7) 0.0040(7) 0.0003(5) -0.0008(6) -0.0001(6) S3 0.0078(7) 0.0053(7) 0.0069(7) -0.0006(6) 0.0027(6) 0.0003(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 Mo1 O1 1.648(11) . ? Mo1 O2 1.675(10) . ? Mo1 O3 2.028(9) . ? Mo1 O4 2.048(7) . ? Mo1 O5 2.222(9) 4_546 ? Mo1 O6 2.279(11) 6_556 ? Mo2 O10 1.677(10) . ? Mo2 O8 1.680(9) . ? Mo2 O9 2.026(8) . ? Mo2 O7 2.048(7) . ? Mo2 O11 2.212(8) . ? Mo2 O12 2.261(8) . ? Mo3 O13 1.677(10) . ? Mo3 O14 1.693(10) . ? Mo3 O15 2.024(8) . ? Mo3 O16 2.034(7) . ? Mo3 O17 2.214(10) 4_556 ? Mo3 O18 2.292(10) . ? S1 O6 1.440(11) . ? S1 O17 1.459(10) . ? S1 O3 1.489(9) . ? S1 O4 1.495(8) 4_546 ? S2 O11 1.445(8) 6 ? S2 O12 1.449(8) 5_556 ? S2 O7 1.492(7) . ? S2 O16 1.494(8) . ? S3 O18 1.430(11) 6_566 ? S3 O5 1.455(10) . ? S3 O15 1.488(9) . ? S3 O9 1.498(8) 1_565 ? O4 S1 1.495(8) 4_556 ? O5 Mo1 2.222(9) 4_556 ? O6 Mo1 2.279(11) 6 ? O9 S3 1.497(8) 1_545 ? O11 S2 1.445(8) 6_556 ? O12 S2 1.449(8) 5_556 ? O17 Mo3 2.214(10) 4_546 ? O18 S3 1.430(10) 6_565 ? 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 O2 102.2(5) . . ? O1 Mo1 O3 98.9(5) . . ? O2 Mo1 O3 97.9(4) . . ? O1 Mo1 O4 99.5(4) . . ? O2 Mo1 O4 96.1(4) . . ? O3 Mo1 O4 153.9(3) . . ? O1 Mo1 O5 92.2(5) . 4_546 ? O2 Mo1 O5 164.7(4) . 4_546 ? O3 Mo1 O5 84.9(3) . 4_546 ? O4 Mo1 O5 76.0(3) . 4_546 ? O1 Mo1 O6 168.1(5) . 6_556 ? O2 Mo1 O6 89.4(4) . 6_556 ? O3 Mo1 O6 76.4(4) . 6_556 ? O4 Mo1 O6 81.9(3) . 6_556 ? O5 Mo1 O6 76.6(4) 4_546 6_556 ? O10 Mo2 O8 100.2(4) . . ? O10 Mo2 O9 100.2(4) . . ? O8 Mo2 O9 98.6(4) . . ? O10 Mo2 O7 97.1(4) . . ? O8 Mo2 O7 98.8(4) . . ? O9 Mo2 O7 152.9(3) . . ? O10 Mo2 O11 168.0(4) . . ? O8 Mo2 O11 91.6(4) . . ? O9 Mo2 O11 80.4(3) . . ? O7 Mo2 O11 78.5(3) . . ? O10 Mo2 O12 90.5(4) . . ? O8 Mo2 O12 169.2(4) . . ? O9 Mo2 O12 77.4(3) . . ? O7 Mo2 O12 81.6(3) . . ? O11 Mo2 O12 77.9(3) . . ? O13 Mo3 O14 103.1(5) . . ? O13 Mo3 O15 99.4(4) . . ? O14 Mo3 O15 96.9(4) . . ? O13 Mo3 O16 97.0(4) . . ? O14 Mo3 O16 99.2(4) . . ? O15 Mo3 O16 153.8(3) . . ? O13 Mo3 O17 163.6(4) . 4_556 ? O14 Mo3 O17 92.5(4) . 4_556 ? O15 Mo3 O17 83.4(4) . 4_556 ? O16 Mo3 O17 75.3(3) . 4_556 ? O13 Mo3 O18 87.2(4) . . ? O14 Mo3 O18 168.5(4) . . ? O15 Mo3 O18 76.0(4) . . ? O16 Mo3 O18 84.5(3) . . ? O17 Mo3 O18 77.8(4) 4_556 . ? O6 S1 O17 113.0(6) . . ? O6 S1 O3 110.1(6) . . ? O17 S1 O3 108.1(5) . . ? O6 S1 O4 110.6(5) . 4_546 ? O17 S1 O4 108.9(5) . 4_546 ? O3 S1 O4 105.9(5) . 4_546 ? O11 S2 O12 113.6(5) 6 5_556 ? O11 S2 O7 109.9(4) 6 . ? O12 S2 O7 109.9(4) 5_556 . ? O11 S2 O16 107.4(4) 6 . ? O12 S2 O16 109.6(4) 5_556 . ? O7 S2 O16 106.1(4) . . ? O18 S3 O5 112.6(6) 6_566 . ? O18 S3 O15 109.9(5) 6_566 . ? O5 S3 O15 109.2(5) . . ? O18 S3 O9 110.1(5) 6_566 1_565 ? O5 S3 O9 110.2(5) . 1_565 ? O15 S3 O9 104.7(5) . 1_565 ? S1 O3 Mo1 145.6(6) . . ? S1 O4 Mo1 135.4(5) 4_556 . ? S3 O5 Mo1 153.3(6) . 4_556 ? S1 O6 Mo1 141.2(6) . 6 ? S2 O7 Mo2 136.2(5) . . ? S3 O9 Mo2 141.8(5) 1_545 . ? S2 O11 Mo2 145.7(5) 6_556 . ? S2 O12 Mo2 148.2(5) 5_556 . ? S3 O15 Mo3 146.1(6) . . ? S2 O16 Mo3 140.0(5) . . ? S1 O17 Mo3 151.5(6) . 4_546 ? S3 O18 Mo3 151.3(6) 6_565 . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 39.34 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 9.705 _refine_diff_density_min -8.215 _refine_diff_density_rms 0.692 "#==END" data_MoO2SO4_(II) _database_code_CSD 158632 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'molybdenum oxide sulfate (mod II)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Mo O6 S' _chemical_formula_weight 224.00 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' '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.827(5) _cell_length_b 8.592(2) _cell_length_c 12.294(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2622.5(9) _cell_formula_units_Z 24 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 3.411 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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_measurement_device_type 'Siemens SMART 1000 CCD diffractom.' _diffrn_measurement_method 'Sets of exposures each taken over 0.6\% \w rotation' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31314 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 30.51 _reflns_number_total 7894 _reflns_number_gt 7210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0050P)^2^+58.3000P] 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 0.00112(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(8) _refine_ls_number_reflns 7894 _refine_ls_number_parameters 254 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.145 _refine_ls_shift/su_mean 0.029 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 0.34609(3) 0.47767(9) 0.24970(6) 0.00397(14) Uani 1 1 d . . . Mo2 Mo 0.32840(3) -0.02210(11) -0.00947(7) 0.0114(2) Uani 1 1 d . . . Mo3 Mo 0.33853(3) 0.49739(10) 0.74471(7) 0.00747(17) Uani 1 1 d . . . Mo4 Mo 0.67824(3) -0.00006(11) -0.00905(6) 0.00631(17) Uani 1 1 d . . . Mo5 Mo 0.50789(2) -0.01655(9) -0.26109(7) 0.00522(16) Uani 1 1 d . . . Mo6 Mo 0.50482(3) 0.49095(11) -0.52023(7) 0.00874(18) Uani 1 1 d . . . S1 S 0.30956(8) 0.5960(3) 0.4967(2) 0.0088(4) Uani 1 1 d . . . S2 S 0.70603(7) 0.1369(2) -0.2627(2) 0.0048(4) Uani 1 1 d . . . S3 S 0.36705(7) 0.0929(2) -0.2614(2) 0.0042(4) Uani 1 1 d . . . S4 S 0.53663(7) 0.1163(3) -0.0114(2) 0.0066(4) Uani 1 1 d . . . S5 S 0.36796(8) 0.3668(3) 0.0025(2) 0.0074(4) Uani 1 1 d . . . S6 S 0.52303(8) 0.3801(3) -0.2727(2) 0.0074(4) Uani 1 1 d . . . O1 O 0.3831(2) 0.3184(8) 0.2688(5) 0.0102(12) Uiso 1 1 d . . . O2 O 0.2827(2) 0.4067(8) 0.2437(7) 0.0143(12) Uiso 1 1 d . . . O3 O 0.3460(2) 0.5582(7) 0.4042(5) 0.0036(10) Uiso 1 1 d . . . O4 O 0.3598(2) 0.4922(8) 0.0852(6) 0.0090(12) Uiso 1 1 d . . . O5 O 0.3155(3) 0.7140(9) 0.2045(6) 0.0165(14) Uiso 1 1 d . . . O6 O 0.4207(2) 0.6335(7) 0.2535(6) 0.0112(11) Uiso 1 1 d . . . O7 O 0.3951(3) -0.0515(10) 0.0049(7) 0.0272(17) Uiso 1 1 d . . . O8 O 0.3036(4) -0.1984(12) -0.0380(8) 0.035(2) Uiso 1 1 d . . . O9 O 0.3333(3) 0.0674(10) -0.1635(7) 0.0194(16) Uiso 1 1 d . . . O10 O 0.3056(2) -0.0202(8) 0.1510(5) 0.0074(11) Uiso 1 1 d . . . O11 O 0.3383(3) 0.2299(9) 0.0356(6) 0.0099(13) Uiso 1 1 d . . . O12 O 0.2535(3) 0.5865(9) 0.4609(6) 0.0174(14) Uiso 1 1 d . . . O13 O 0.3985(3) 0.5765(10) 0.7280(7) 0.0252(16) Uiso 1 1 d . . . O14 O 0.2996(3) 0.6549(10) 0.7670(7) 0.0245(16) Uiso 1 1 d . . . O15 O 0.3447(3) 0.4278(11) 0.9005(7) 0.0192(16) Uiso 1 1 d . . . O16 O 0.3205(2) 0.4772(8) 0.5826(5) 0.0057(11) Uiso 1 1 d . . . O17 O 0.2642(3) 0.3510(9) 0.7576(7) 0.0207(14) Uiso 1 1 d . . . O18 O 0.3688(3) 0.2556(8) 0.7118(6) 0.0124(12) Uiso 1 1 d . . . O19 O 0.7455(3) -0.0003(10) 0.0054(8) 0.0246(16) Uiso 1 1 d . . . O20 O 0.6635(3) -0.1855(9) -0.0386(7) 0.0180(15) Uiso 1 1 d . . . O21 O 0.6779(3) 0.0805(11) -0.1640(8) 0.0218(17) Uiso 1 1 d . . . O22 O 0.6616(3) -0.0123(11) 0.1515(8) 0.0240(18) Uiso 1 1 d . . . O23 O 0.3254(3) 0.7514(9) 0.5369(7) 0.0194(15) Uiso 1 1 d . . . O24 O 0.5903(3) 0.0540(11) -0.0245(8) 0.0299(18) Uiso 1 1 d . . . O25 O 0.5754(3) -0.0050(8) -0.2726(6) 0.0149(13) Uiso 1 1 d . . . O26 O 0.4981(3) -0.2032(9) -0.2269(6) 0.0148(14) Uiso 1 1 d . . . O27 O 0.4918(3) -0.0309(9) -0.4226(7) 0.0180(15) Uiso 1 1 d . . . O28 O 0.5037(2) 0.0845(7) -0.1099(5) 0.0020(10) Uiso 1 1 d . . . O29 O 0.4193(2) 0.0238(8) -0.2469(6) 0.0139(12) Uiso 1 1 d . . . O30 O 0.4997(2) 0.2355(8) -0.3136(6) 0.0082(13) Uiso 1 1 d . . . O31 O 0.4460(3) 0.3959(9) -0.5233(6) 0.0153(13) Uiso 1 1 d . . . O32 O 0.5501(3) 0.3501(9) -0.5394(6) 0.0147(13) Uiso 1 1 d . . . O33 O 0.5138(3) 0.5037(9) -0.3564(6) 0.0129(13) Uiso 1 1 d . . . O34 O 0.5066(3) 0.5723(9) -0.6753(7) 0.0146(14) Uiso 1 1 d . . . O35 O 0.5367(2) 0.2838(8) 0.0107(5) 0.0094(12) Uiso 1 1 d . . . O36 O 0.4257(2) 0.3326(8) -0.0099(6) 0.0126(12) 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 Mo1 0.0012(2) 0.0053(3) 0.0053(3) 0.0007(3) -0.0009(3) 0.0009(2) Mo2 0.0229(5) 0.0058(4) 0.0056(4) 0.0009(3) 0.0021(4) -0.0003(3) Mo3 0.0099(3) 0.0053(3) 0.0072(4) -0.0009(3) -0.0033(4) 0.0017(2) Mo4 0.0064(3) 0.0049(3) 0.0077(4) 0.0016(3) -0.0005(3) -0.0001(2) Mo5 0.0056(3) 0.0050(3) 0.0051(4) 0.0012(3) -0.0007(3) 0.0011(2) Mo6 0.0111(3) 0.0079(3) 0.0072(5) 0.0011(3) -0.0014(3) -0.0035(2) S1 0.0124(9) 0.0076(9) 0.0063(9) 0.0015(8) 0.0038(8) 0.0059(7) S2 0.0016(6) 0.0067(9) 0.0062(9) -0.0011(8) -0.0014(7) -0.0001(6) S3 0.0008(6) 0.0065(8) 0.0051(9) -0.0020(8) -0.0006(7) 0.0017(6) S4 0.0051(7) 0.0090(9) 0.0056(10) -0.0013(8) -0.0014(7) 0.0024(6) S5 0.0088(8) 0.0074(9) 0.0059(9) -0.0010(9) -0.0018(7) -0.0017(6) S6 0.0103(8) 0.0055(8) 0.0065(10) 0.0011(8) -0.0009(7) -0.0043(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 Mo1 O1 1.665(7) . ? Mo1 O2 1.689(6) . ? Mo1 O3 2.022(6) . ? Mo1 O4 2.055(7) . ? Mo1 O5 2.237(8) . ? Mo1 O6 2.285(6) . ? Mo2 O8 1.673(10) . ? Mo2 O7 1.685(9) . ? Mo2 O9 2.047(9) . ? Mo2 O10 2.053(7) . ? Mo2 O11 2.248(7) . ? Mo2 O12 2.267(7) 4_544 ? Mo3 O13 1.650(8) . ? Mo3 O14 1.686(8) . ? Mo3 O15 2.012(9) . ? Mo3 O16 2.050(6) . ? Mo3 O17 2.238(7) . ? Mo3 O18 2.247(7) . ? Mo4 O19 1.679(8) . ? Mo4 O20 1.675(8) . ? Mo4 O22 2.019(10) . ? Mo4 O21 2.026(10) . ? Mo4 O23 2.212(8) 2_664 ? Mo4 O24 2.240(9) . ? Mo5 O26 1.675(7) . ? Mo5 O25 1.685(6) . ? Mo5 O27 2.029(9) . ? Mo5 O28 2.055(7) . ? Mo5 O29 2.233(6) . ? Mo5 O30 2.269(7) . ? Mo6 O31 1.673(7) . ? Mo6 O32 1.669(7) . ? Mo6 O33 2.029(8) . ? Mo6 O34 2.031(8) . ? Mo6 O35 2.226(7) 2_664 ? Mo6 O36 2.299(6) 2_664 ? S1 O12 1.462(7) . ? S1 O23 1.477(8) . ? S1 O3 1.489(6) . ? S1 O16 1.493(7) . ? S2 O5 1.446(8) 2_664 ? S2 O17 1.470(7) 3_554 ? S2 O21 1.482(10) . ? S2 O10 1.487(7) 2_654 ? S3 O29 1.438(6) . ? S3 O18 1.437(7) 1_554 ? S3 O22 1.460(9) 2_654 ? S3 O9 1.483(9) . ? S4 O24 1.445(9) . ? S4 O35 1.465(7) . ? S4 O28 1.486(7) . ? S4 O27 1.493(8) 2_655 ? S5 O11 1.446(7) . ? S5 O15 1.477(9) 1_554 ? S5 O36 1.472(6) . ? S5 O4 1.495(7) . ? S6 O6 1.439(6) 2_664 ? S6 O30 1.461(7) . ? S6 O34 1.463(8) 2_665 ? S6 O33 1.496(8) . ? O5 S2 1.446(8) 2_665 ? O6 S6 1.439(6) 2_665 ? O10 S2 1.487(7) 2_655 ? O12 Mo2 2.267(7) 4 ? O15 S5 1.477(9) 1_556 ? O17 S2 1.470(7) 3_456 ? O18 S3 1.437(7) 1_556 ? O22 S3 1.460(9) 2_655 ? O23 Mo4 2.212(8) 2_665 ? O27 S4 1.493(8) 2_654 ? O34 S6 1.463(8) 2_664 ? O35 Mo6 2.226(7) 2_665 ? O36 Mo6 2.299(6) 2_665 ? 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 O2 102.9(3) . . ? O1 Mo1 O3 98.6(3) . . ? O2 Mo1 O3 99.4(3) . . ? O1 Mo1 O4 95.6(3) . . ? O2 Mo1 O4 97.7(3) . . ? O3 Mo1 O4 154.7(3) . . ? O1 Mo1 O5 165.4(3) . . ? O2 Mo1 O5 90.1(3) . . ? O3 Mo1 O5 85.5(3) . . ? O4 Mo1 O5 75.9(3) . . ? O1 Mo1 O6 91.8(3) . . ? O2 Mo1 O6 165.3(3) . . ? O3 Mo1 O6 77.4(2) . . ? O4 Mo1 O6 81.4(3) . . ? O5 Mo1 O6 75.4(2) . . ? O8 Mo2 O7 104.3(5) . . ? O8 Mo2 O9 99.7(4) . . ? O7 Mo2 O9 95.5(4) . . ? O8 Mo2 O10 96.2(4) . . ? O7 Mo2 O10 99.9(4) . . ? O9 Mo2 O10 154.5(3) . . ? O8 Mo2 O11 164.7(4) . . ? O7 Mo2 O11 90.6(3) . . ? O9 Mo2 O11 82.0(3) . . ? O10 Mo2 O11 77.6(3) . . ? O8 Mo2 O12 90.5(4) . 4_544 ? O7 Mo2 O12 163.8(4) . 4_544 ? O9 Mo2 O12 75.5(3) . 4_544 ? O10 Mo2 O12 84.5(3) . 4_544 ? O11 Mo2 O12 75.0(3) . 4_544 ? O13 Mo3 O14 102.0(4) . . ? O13 Mo3 O15 99.9(4) . . ? O14 Mo3 O15 97.3(4) . . ? O13 Mo3 O16 96.4(3) . . ? O14 Mo3 O16 95.8(3) . . ? O15 Mo3 O16 156.4(3) . . ? O13 Mo3 O17 169.8(4) . . ? O14 Mo3 O17 88.1(3) . . ? O15 Mo3 O17 80.1(3) . . ? O16 Mo3 O17 80.8(3) . . ? O13 Mo3 O18 93.2(3) . . ? O14 Mo3 O18 164.6(3) . . ? O15 Mo3 O18 82.6(3) . . ? O16 Mo3 O18 79.6(3) . . ? O17 Mo3 O18 76.6(3) . . ? O19 Mo4 O20 103.8(4) . . ? O19 Mo4 O22 95.8(4) . . ? O20 Mo4 O22 96.7(4) . . ? O19 Mo4 O21 96.0(4) . . ? O20 Mo4 O21 96.9(4) . . ? O22 Mo4 O21 159.3(4) . . ? O19 Mo4 O23 90.8(4) . 2_664 ? O20 Mo4 O23 164.9(3) . 2_664 ? O22 Mo4 O23 78.0(3) . 2_664 ? O21 Mo4 O23 84.8(3) . 2_664 ? O19 Mo4 O24 168.1(4) . . ? O20 Mo4 O24 88.0(4) . . ? O22 Mo4 O24 83.9(3) . . ? O21 Mo4 O24 81.1(3) . . ? O23 Mo4 O24 77.4(3) 2_664 . ? O26 Mo5 O25 102.8(3) . . ? O26 Mo5 O27 99.2(3) . . ? O25 Mo5 O27 96.7(3) . . ? O26 Mo5 O28 99.8(3) . . ? O25 Mo5 O28 95.8(3) . . ? O27 Mo5 O28 154.3(3) . . ? O26 Mo5 O29 89.2(3) . . ? O25 Mo5 O29 167.7(3) . . ? O27 Mo5 O29 83.8(3) . . ? O28 Mo5 O29 79.3(2) . . ? O26 Mo5 O30 166.4(3) . . ? O25 Mo5 O30 90.5(3) . . ? O27 Mo5 O30 76.2(3) . . ? O28 Mo5 O30 81.3(3) . . ? O29 Mo5 O30 77.6(2) . . ? O31 Mo6 O32 103.3(3) . . ? O31 Mo6 O33 98.3(3) . . ? O32 Mo6 O33 96.0(3) . . ? O31 Mo6 O34 99.5(3) . . ? O32 Mo6 O34 95.9(3) . . ? O33 Mo6 O34 155.6(3) . . ? O31 Mo6 O35 91.4(3) . 2_664 ? O32 Mo6 O35 165.3(3) . 2_664 ? O33 Mo6 O35 80.5(3) . 2_664 ? O34 Mo6 O35 82.6(3) . 2_664 ? O31 Mo6 O36 167.8(3) . 2_664 ? O32 Mo6 O36 88.9(3) . 2_664 ? O33 Mo6 O36 80.0(3) . 2_664 ? O34 Mo6 O36 79.0(3) . 2_664 ? O35 Mo6 O36 76.4(2) 2_664 2_664 ? O12 S1 O23 113.8(4) . . ? O12 S1 O3 109.6(4) . . ? O23 S1 O3 106.9(4) . . ? O12 S1 O16 110.3(4) . . ? O23 S1 O16 109.5(4) . . ? O3 S1 O16 106.3(4) . . ? O5 S2 O17 110.4(4) 2_664 3_554 ? O5 S2 O21 110.1(5) 2_664 . ? O17 S2 O21 110.4(5) 3_554 . ? O5 S2 O10 109.1(4) 2_664 2_654 ? O17 S2 O10 111.1(4) 3_554 2_654 ? O21 S2 O10 105.8(5) . 2_654 ? O29 S3 O18 113.7(4) . 1_554 ? O29 S3 O22 109.5(5) . 2_654 ? O18 S3 O22 107.9(5) 1_554 2_654 ? O29 S3 O9 110.5(5) . . ? O18 S3 O9 110.3(5) 1_554 . ? O22 S3 O9 104.5(5) 2_654 . ? O24 S4 O35 112.5(5) . . ? O24 S4 O28 110.4(5) . . ? O35 S4 O28 109.4(4) . . ? O24 S4 O27 109.6(5) . 2_655 ? O35 S4 O27 110.4(4) . 2_655 ? O28 S4 O27 104.2(4) . 2_655 ? O11 S5 O15 109.2(5) . 1_554 ? O11 S5 O36 111.2(4) . . ? O15 S5 O36 111.4(5) 1_554 . ? O11 S5 O4 109.0(4) . . ? O15 S5 O4 105.6(5) 1_554 . ? O36 S5 O4 110.2(4) . . ? O6 S6 O30 113.2(4) 2_664 . ? O6 S6 O34 109.1(4) 2_664 2_665 ? O30 S6 O34 108.6(4) . 2_665 ? O6 S6 O33 111.1(4) 2_664 . ? O30 S6 O33 107.9(4) . . ? O34 S6 O33 106.7(4) 2_665 . ? S1 O3 Mo1 142.5(4) . . ? S5 O4 Mo1 130.4(4) . . ? S2 O5 Mo1 149.4(5) 2_665 . ? S6 O6 Mo1 137.3(4) 2_665 . ? S3 O9 Mo2 147.1(5) . . ? S2 O10 Mo2 137.2(4) 2_655 . ? S5 O11 Mo2 140.3(4) . . ? S1 O12 Mo2 145.9(5) . 4 ? S5 O15 Mo3 160.6(5) 1_556 . ? S1 O16 Mo3 132.0(4) . . ? S2 O17 Mo3 139.3(5) 3_456 . ? S3 O18 Mo3 148.0(4) 1_556 . ? S2 O21 Mo4 151.5(6) . . ? S3 O22 Mo4 147.3(6) 2_655 . ? S1 O23 Mo4 141.0(5) . 2_665 ? S4 O24 Mo4 165.1(6) . . ? S4 O27 Mo5 146.9(5) 2_654 . ? S4 O28 Mo5 141.9(4) . . ? S3 O29 Mo5 160.6(5) . . ? S6 O30 Mo5 132.7(4) . . ? S6 O33 Mo6 131.4(5) . . ? S6 O34 Mo6 148.6(5) 2_664 . ? S4 O35 Mo6 145.2(4) . 2_665 ? S5 O36 Mo6 127.2(4) . 2_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.396 _refine_diff_density_min -1.949 _refine_diff_density_rms 0.301