Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Carola Schulzke' _publ_contact_author_address ; Institut fuer Anorganische Chemie University of Goettingen Tammannstr. 4 Goettingen D-37077 GERMANY ; _publ_contact_author_email CAROLA.SCHULZKE@CHEM.UNI-GOETTINGEN.DE _publ_section_title ; Structural, Electrochemical and Oxygen Atom Transfer Catalysis of a Molybdenum Selenoether Complex [Mo2O4(OC3H6SeC3H6O)2] and its Thioether Analogue [Mo2O4(OC3H6SC3H6O)2] ; loop_ _publ_author_name 'Carola Schulzke' 'Xiaoli Ma.' 'Mathias Noltemeyer' 'Hans-Georg Schmidt' # Attachment 'compound1.cif' data_schu5 _database_code_depnum_ccdc_archive 'CCDC 606461' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Mo2 O8 S2' _chemical_formula_weight 552.31 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 P2(1)/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 9.4886(7) _cell_length_b 8.7913(5) _cell_length_c 11.1434(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.044(6) _cell_angle_gamma 90.00 _cell_volume 878.67(11) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7271 _exptl_absorpt_correction_T_max 0.8482 _exptl_absorpt_process_details 'multirun sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 IPDS2 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12108 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 24.77 _reflns_number_total 1507 _reflns_number_gt 1394 _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^)+(0.0123P)^2^+5.2641P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1507 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.290 _refine_ls_restrained_S_all 1.290 _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 0.42368(4) 0.01043(5) 0.12323(4) 0.01276(15) Uani 1 1 d . . . S1 S 0.36836(13) -0.28811(14) 0.03123(11) 0.0151(3) Uani 1 1 d . . . O1 O 0.2144(4) 0.0028(4) 0.0813(3) 0.0179(7) Uani 1 1 d . . . O2 O 0.3907(4) 0.0522(4) -0.0815(3) 0.0133(7) Uani 1 1 d . . . O3 O 0.4595(4) 0.1984(4) 0.1585(3) 0.0184(8) Uani 1 1 d . . . O4 O 0.4793(4) -0.0769(4) 0.2677(3) 0.0188(8) Uani 1 1 d . . . C1 C 0.1215(6) -0.0967(6) 0.1255(5) 0.0187(11) Uani 1 1 d . . . H1A H 0.0245 -0.0460 0.1127 0.022 Uiso 1 1 calc R . . H1B H 0.1691 -0.1132 0.2178 0.022 Uiso 1 1 calc R . . C2 C 0.0933(6) -0.2499(6) 0.0597(5) 0.0197(11) Uani 1 1 d . . . H2A H 0.0110 -0.3013 0.0799 0.024 Uiso 1 1 calc R . . H2B H 0.0608 -0.2336 -0.0332 0.024 Uiso 1 1 calc R . . C3 C 0.2281(6) -0.3529(6) 0.0973(5) 0.0202(11) Uani 1 1 d . . . H3B H 0.1970 -0.4574 0.0671 0.024 Uiso 1 1 calc R . . H3C H 0.2714 -0.3559 0.1910 0.024 Uiso 1 1 calc R . . C4 C 0.5332(5) -0.3793(6) 0.1399(5) 0.0188(11) Uani 1 1 d . . . H4B H 0.5393 -0.3562 0.2285 0.023 Uiso 1 1 calc R . . H4C H 0.5242 -0.4909 0.1283 0.023 Uiso 1 1 calc R . . C5 C 0.6752(5) -0.3254(6) 0.1178(5) 0.0184(11) Uani 1 1 d . . . H5A H 0.7584 -0.3918 0.1667 0.022 Uiso 1 1 calc R . . H5B H 0.6631 -0.3385 0.0267 0.022 Uiso 1 1 calc R . . C6 C 0.2818(5) 0.1612(5) -0.1543(5) 0.0150(10) Uani 1 1 d . . . H6A H 0.1849 0.1399 -0.1423 0.018 Uiso 1 1 calc R . . H6B H 0.2686 0.1476 -0.2455 0.018 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0134(2) 0.0144(2) 0.0120(2) -0.00031(16) 0.00620(16) 0.00012(16) S1 0.0147(6) 0.0168(6) 0.0154(6) 0.0003(5) 0.0072(5) -0.0004(5) O1 0.0174(17) 0.0179(17) 0.0205(18) 0.0024(14) 0.0089(15) -0.0012(14) O2 0.0127(17) 0.0165(17) 0.0109(16) 0.0028(13) 0.0038(13) 0.0028(13) O3 0.0202(18) 0.0188(18) 0.0189(18) -0.0008(14) 0.0099(15) 0.0023(14) O4 0.0197(19) 0.0236(18) 0.0139(17) 0.0008(14) 0.0066(15) 0.0003(15) C1 0.016(3) 0.022(3) 0.022(3) 0.001(2) 0.011(2) -0.003(2) C2 0.016(3) 0.023(3) 0.022(3) 0.002(2) 0.009(2) -0.003(2) C3 0.022(3) 0.020(3) 0.023(3) 0.002(2) 0.013(2) -0.003(2) C4 0.018(3) 0.019(3) 0.019(3) 0.002(2) 0.006(2) 0.002(2) C5 0.015(2) 0.019(3) 0.020(3) 0.001(2) 0.004(2) 0.003(2) C6 0.014(2) 0.017(2) 0.015(2) 0.0050(19) 0.0058(19) 0.004(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 O4 1.704(3) . ? Mo1 O3 1.707(3) . ? Mo1 O1 1.887(3) . ? Mo1 O2 2.039(3) 3_655 ? Mo1 O2 2.229(3) . ? Mo1 S1 2.8042(13) . ? S1 C3 1.810(5) . ? S1 C4 1.822(5) . ? O1 C1 1.439(6) . ? O2 C6 1.448(5) . ? O2 Mo1 2.039(3) 3_655 ? C1 C2 1.514(7) . ? C2 C3 1.510(7) . ? C4 C5 1.523(7) . ? C5 C6 1.519(7) 3_655 ? C6 C5 1.519(7) 3_655 ? 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 O4 Mo1 O3 104.00(17) . . ? O4 Mo1 O1 101.22(15) . . ? O3 Mo1 O1 101.89(15) . . ? O4 Mo1 O2 93.98(14) . 3_655 ? O3 Mo1 O2 101.06(15) . 3_655 ? O1 Mo1 O2 148.38(14) . 3_655 ? O4 Mo1 O2 159.61(14) . . ? O3 Mo1 O2 91.53(14) . . ? O1 Mo1 O2 88.14(13) . . ? O2 Mo1 O2 69.77(14) 3_655 . ? O4 Mo1 S1 83.51(12) . . ? O3 Mo1 S1 171.76(12) . . ? O1 Mo1 S1 79.62(11) . . ? O2 Mo1 S1 74.71(10) 3_655 . ? O2 Mo1 S1 80.39(9) . . ? C3 S1 C4 100.2(2) . . ? C3 S1 Mo1 102.74(17) . . ? C4 S1 Mo1 98.69(17) . . ? C1 O1 Mo1 130.5(3) . . ? C6 O2 Mo1 124.2(3) . 3_655 ? C6 O2 Mo1 121.2(3) . . ? Mo1 O2 Mo1 110.23(14) 3_655 . ? O1 C1 C2 113.9(4) . . ? C3 C2 C1 113.5(4) . . ? C2 C3 S1 111.5(3) . . ? C5 C4 S1 111.6(3) . . ? C6 C5 C4 115.2(4) 3_655 . ? O2 C6 C5 113.5(4) . 3_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.77 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.442 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.119 data_schu19 _database_code_depnum_ccdc_archive 'CCDC 606462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Mo2 O8 Se2' _chemical_formula_weight 646.11 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' Se Se -0.0929 2.2259 '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 P2(1)/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 9.5298(14) _cell_length_b 8.8814(14) _cell_length_c 11.2161(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.874(2) _cell_angle_gamma 90.00 _cell_volume 898.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 5.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4067 _exptl_absorpt_correction_T_max 0.7711 _exptl_absorpt_process_details 'multirun sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17947 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.14 _reflns_number_total 1783 _reflns_number_gt 1775 _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^)+(0.0180P)^2^+1.3000P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1783 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0179 _refine_ls_wR_factor_ref 0.0432 _refine_ls_wR_factor_gt 0.0431 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _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 0.42046(2) 0.01049(2) 0.120551(18) 0.00851(7) Uani 1 1 d . . . Se1 Se 0.36101(2) -0.29054(3) 0.02021(2) 0.01048(7) Uani 1 1 d . . . O1 O 0.21231(19) 0.00227(18) 0.08020(16) 0.0127(4) Uani 1 1 d . . . C1 C 0.1207(3) -0.0912(3) 0.1287(2) 0.0118(5) Uani 1 1 d . . . H1A H 0.0270 -0.0371 0.1197 0.014 Uiso 1 1 calc R . . H1B H 0.1718 -0.1077 0.2197 0.014 Uiso 1 1 calc R . . O2 O 0.39234(17) 0.05170(18) -0.08083(15) 0.0097(3) Uani 1 1 d . . . C2 C 0.0838(3) -0.2435(3) 0.0639(2) 0.0129(5) Uani 1 1 d . . . H2A H 0.0493 -0.2282 -0.0285 0.015 Uiso 1 1 calc R . . H2B H 0.0013 -0.2896 0.0867 0.015 Uiso 1 1 calc R . . O3 O 0.45664(19) 0.19700(19) 0.15392(16) 0.0135(3) Uani 1 1 d . . . C3 C 0.2148(3) -0.3519(3) 0.0991(2) 0.0149(5) Uani 1 1 d . . . H3B H 0.1794 -0.4548 0.0713 0.018 Uiso 1 1 calc R . . H3C H 0.2617 -0.3534 0.1918 0.018 Uiso 1 1 calc R . . O4 O 0.47559(18) -0.0763(2) 0.26395(15) 0.0139(3) Uani 1 1 d . . . C4 C 0.5386(3) -0.3784(3) 0.1432(2) 0.0131(5) Uani 1 1 d . . . H4B H 0.5412 -0.3512 0.2295 0.016 Uiso 1 1 calc R . . H4C H 0.5339 -0.4896 0.1359 0.016 Uiso 1 1 calc R . . C5 C 0.6792(3) -0.3222(3) 0.1212(2) 0.0136(5) Uani 1 1 d . . . H5A H 0.6685 -0.3364 0.0311 0.016 Uiso 1 1 calc R . . H5B H 0.7634 -0.3852 0.1710 0.016 Uiso 1 1 calc R . . C6 C 0.7169(3) -0.1577(3) 0.1555(2) 0.0118(5) Uani 1 1 d . . . H6A H 0.7275 -0.1431 0.2455 0.014 Uiso 1 1 calc R . . H6B H 0.8139 -0.1347 0.1450 0.014 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00935(11) 0.00848(11) 0.00831(11) -0.00055(7) 0.00370(8) -0.00021(7) Se1 0.01058(12) 0.00998(13) 0.01144(12) -0.00040(8) 0.00436(9) -0.00022(8) O1 0.0115(8) 0.0133(9) 0.0144(9) 0.0013(6) 0.0059(7) -0.0002(6) C1 0.0116(11) 0.0119(12) 0.0141(11) 0.0006(9) 0.0070(9) -0.0023(9) O2 0.0090(8) 0.0094(8) 0.0108(8) 0.0020(6) 0.0034(6) 0.0008(6) C2 0.0102(11) 0.0155(12) 0.0144(12) 0.0001(9) 0.0061(9) -0.0009(9) O3 0.0154(8) 0.0120(8) 0.0143(8) -0.0014(7) 0.0065(7) -0.0011(7) C3 0.0146(12) 0.0128(12) 0.0197(12) 0.0037(10) 0.0088(10) -0.0009(9) O4 0.0159(8) 0.0150(9) 0.0119(8) 0.0007(7) 0.0062(7) -0.0006(7) C4 0.0133(11) 0.0093(11) 0.0151(11) 0.0024(9) 0.0023(9) 0.0018(9) C5 0.0125(11) 0.0127(12) 0.0142(11) 0.0018(9) 0.0025(9) 0.0032(9) C6 0.0083(11) 0.0138(12) 0.0125(11) 0.0029(9) 0.0022(9) 0.0022(9) _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 O4 1.7058(17) . ? Mo1 O3 1.7086(17) . ? Mo1 O1 1.8879(17) . ? Mo1 O2 2.0495(16) 3_655 ? Mo1 O2 2.2172(16) . ? Mo1 Se1 2.8850(5) . ? Se1 C3 1.954(2) . ? Se1 C4 1.966(2) . ? O1 C1 1.433(3) . ? C1 C2 1.522(3) . ? O2 C6 1.452(3) 3_655 ? O2 Mo1 2.0495(16) 3_655 ? C2 C3 1.524(3) . ? C4 C5 1.523(3) . ? C5 C6 1.524(3) . ? C6 O2 1.452(3) 3_655 ? 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 O4 Mo1 O3 104.63(8) . . ? O4 Mo1 O1 100.82(8) . . ? O3 Mo1 O1 102.23(8) . . ? O4 Mo1 O2 93.38(7) . 3_655 ? O3 Mo1 O2 100.41(7) . 3_655 ? O1 Mo1 O2 149.14(7) . 3_655 ? O4 Mo1 O2 159.06(7) . . ? O3 Mo1 O2 90.71(7) . . ? O1 Mo1 O2 89.47(7) . . ? O2 Mo1 O2 69.50(7) 3_655 . ? O4 Mo1 Se1 84.89(6) . . ? O3 Mo1 Se1 169.78(6) . . ? O1 Mo1 Se1 79.17(5) . . ? O2 Mo1 Se1 74.95(5) 3_655 . ? O2 Mo1 Se1 79.15(4) . . ? C3 Se1 C4 98.59(10) . . ? C3 Se1 Mo1 99.23(8) . . ? C4 Se1 Mo1 94.50(7) . . ? C1 O1 Mo1 130.79(14) . . ? O1 C1 C2 114.15(19) . . ? C6 O2 Mo1 124.17(13) 3_655 3_655 ? C6 O2 Mo1 121.50(13) 3_655 . ? Mo1 O2 Mo1 110.50(7) 3_655 . ? C1 C2 C3 113.2(2) . . ? C2 C3 Se1 110.56(16) . . ? C5 C4 Se1 111.03(16) . . ? C4 C5 C6 115.0(2) . . ? O2 C6 C5 114.15(18) 3_655 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.14 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.659 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.087