# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Angeles Monge' _publ_contact_author_email AMONGE@ICMM.CSIC.ES _publ_section_title ; 3D scandium and yttrium arenedisulfonate MOF materials as high thermally stable bifunctional heterogeneous catalysts ; loop_ _publ_author_name 'Angeles Monge' 'Marta Iglesias' 'Josefina Perles' 'Natalia Snejko' # Attachment 'sulfcif.txt' data_sc14 _database_code_depnum_ccdc_archive 'CCDC 623276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 O10 S2 Sc2' _chemical_formula_sum 'C10 H10 O10 S2 Sc2' _chemical_formula_weight 444.22 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 5.8209(4) _cell_length_b 10.0529(8) _cell_length_c 24.9876(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1462.20(19) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1600 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 24.15 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.6313 _exptl_absorpt_correction_T_max 0.7858 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9875 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.49 _reflns_number_total 1515 _reflns_number_gt 1122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0436P)^2^+0.4095P] 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 1515 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_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_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 O2 O 0.2123(5) -0.1596(3) 0.34187(11) 0.0299(8) Uani 1 1 d . . . Sc1 Sc 0.20313(13) 0.19427(8) 0.28039(3) 0.0148(2) Uani 1 1 d . . . S2 S 0.05660(19) -0.06348(11) 0.36621(4) 0.0180(3) Uani 1 1 d . . . O1 O 0.1033(5) 0.0711(3) 0.34681(11) 0.0286(8) Uani 1 1 d . . . O3 O -0.1807(5) -0.0994(3) 0.36143(12) 0.0361(9) Uani 1 1 d . . . O4 O 0.0090(5) 0.0916(3) 0.22570(13) 0.0269(8) Uani 1 1 d . . . O5 O -0.1040(4) 0.3000(3) 0.27392(10) 0.0189(7) Uani 1 1 d . . . C1 C 0.1218(7) -0.0622(4) 0.43520(15) 0.0135(9) Uani 1 1 d . . . C2 C 0.3079(7) -0.1318(4) 0.45215(16) 0.0204(9) Uani 1 1 d . . . H2 H 0.4036 -0.1730 0.4274 0.024 Uiso 1 1 calc R . . C5 C -0.2156(7) 0.0829(4) 0.45628(16) 0.0198(10) Uani 1 1 d . . . H5 H -0.2460 0.0942 0.4200 0.024 Uiso 1 1 calc R . . C4 C -0.0261(7) 0.0058(4) 0.47208(15) 0.0135(9) Uani 1 1 d . . . C3 C 0.3559(7) -0.1416(4) 0.50697(17) 0.0227(10) Uani 1 1 d . . . H3 H 0.4845 -0.1885 0.5184 0.027 Uiso 1 1 calc R . . H5O H -0.1703 0.3031 0.3014 0.050 Uiso 1 1 d . . . H4 H 0.0124 0.0171 0.2100 0.050 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 O2 0.0397(19) 0.0323(18) 0.0177(16) -0.0120(14) 0.0020(14) 0.0059(16) Sc1 0.0147(4) 0.0191(4) 0.0108(4) 0.0001(4) -0.0005(3) 0.0001(4) S2 0.0212(6) 0.0248(6) 0.0079(5) -0.0037(5) 0.0021(5) -0.0027(5) O1 0.041(2) 0.0300(19) 0.0149(15) 0.0092(14) 0.0072(14) 0.0010(15) O3 0.0207(19) 0.065(2) 0.0227(18) -0.0189(16) 0.0005(14) -0.0139(17) O4 0.0190(16) 0.0263(17) 0.0352(19) -0.0157(14) -0.0064(13) 0.0071(14) O5 0.0162(14) 0.0260(16) 0.0146(15) -0.0038(13) -0.0004(12) 0.0024(13) C1 0.018(2) 0.015(2) 0.0081(19) 0.0003(18) 0.0013(16) -0.0032(18) C2 0.024(2) 0.021(2) 0.016(2) -0.0027(19) 0.0060(19) 0.002(2) C5 0.025(2) 0.023(2) 0.011(2) 0.0000(18) -0.0011(18) 0.002(2) C4 0.016(2) 0.016(2) 0.008(2) 0.0014(17) 0.0017(16) -0.0034(17) C3 0.021(2) 0.029(2) 0.018(2) 0.0028(19) -0.0032(19) 0.006(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 O2 S2 1.458(3) . ? O2 Sc1 2.182(3) 8_655 ? Sc1 O4 2.052(3) . ? Sc1 O5 2.057(3) 6_656 ? Sc1 O4 2.063(3) 6_656 ? Sc1 O5 2.086(3) . ? Sc1 O1 2.151(3) . ? Sc1 O2 2.182(3) 8_665 ? Sc1 Sc1 3.2829(7) 6_556 ? Sc1 Sc1 3.2829(7) 6_656 ? S2 O3 1.433(3) . ? S2 O1 1.462(3) . ? S2 C1 1.765(4) . ? O4 Sc1 2.063(3) 6_556 ? O4 H4 0.8459 . ? O5 Sc1 2.057(3) 6_556 ? O5 H5O 0.7885 . ? C1 C2 1.358(6) . ? C1 C4 1.434(6) . ? C2 C3 1.402(5) . ? C2 H2 0.9300 . ? C5 C3 1.363(6) 5_556 ? C5 C4 1.405(5) . ? C5 H5 0.9300 . ? C4 C4 1.433(8) 5_556 ? C3 C5 1.363(6) 5_556 ? C3 H3 0.9300 . ? 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 S2 O2 Sc1 151.7(2) . 8_655 ? O4 Sc1 O5 96.95(12) . 6_656 ? O4 Sc1 O4 100.05(11) . 6_656 ? O5 Sc1 O4 74.86(11) 6_656 6_656 ? O4 Sc1 O5 74.48(11) . . ? O5 Sc1 O5 98.83(11) 6_656 . ? O4 Sc1 O5 171.30(12) 6_656 . ? O4 Sc1 O1 94.33(13) . . ? O5 Sc1 O1 162.55(12) 6_656 . ? O4 Sc1 O1 90.12(12) 6_656 . ? O5 Sc1 O1 96.98(12) . . ? O4 Sc1 O2 158.72(12) . 8_665 ? O5 Sc1 O2 89.63(11) 6_656 8_665 ? O4 Sc1 O2 101.19(13) 6_656 8_665 ? O5 Sc1 O2 84.54(11) . 8_665 ? O1 Sc1 O2 84.57(12) . 8_665 ? O4 Sc1 Sc1 37.21(8) . 6_556 ? O5 Sc1 Sc1 100.29(8) 6_656 6_556 ? O4 Sc1 Sc1 136.95(10) 6_656 6_556 ? O5 Sc1 Sc1 37.28(7) . 6_556 ? O1 Sc1 Sc1 96.75(9) . 6_556 ? O2 Sc1 Sc1 121.71(9) 8_665 6_556 ? O4 Sc1 Sc1 100.38(9) . 6_656 ? O5 Sc1 Sc1 37.90(8) 6_656 6_656 ? O4 Sc1 Sc1 36.96(8) 6_656 6_656 ? O5 Sc1 Sc1 136.38(8) . 6_656 ? O1 Sc1 Sc1 126.62(9) . 6_656 ? O2 Sc1 Sc1 97.22(9) 8_665 6_656 ? Sc1 Sc1 Sc1 124.89(5) 6_556 6_656 ? O3 S2 O2 113.44(19) . . ? O3 S2 O1 112.6(2) . . ? O2 S2 O1 111.04(18) . . ? O3 S2 C1 106.89(19) . . ? O2 S2 C1 106.19(19) . . ? O1 S2 C1 106.06(18) . . ? S2 O1 Sc1 146.98(19) . . ? Sc1 O4 Sc1 105.83(12) . 6_556 ? Sc1 O4 H4 137.8 . . ? Sc1 O4 H4 115.4 6_556 . ? Sc1 O5 Sc1 104.82(12) 6_556 . ? Sc1 O5 H5O 109.1 6_556 . ? Sc1 O5 H5O 111.9 . . ? C2 C1 C4 121.6(4) . . ? C2 C1 S2 118.2(3) . . ? C4 C1 S2 120.1(3) . . ? C1 C2 C3 120.0(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C3 C5 C4 121.3(4) 5_556 . ? C3 C5 H5 119.3 5_556 . ? C4 C5 H5 119.3 . . ? C5 C4 C4 119.0(5) . 5_556 ? C5 C4 C1 123.6(4) . . ? C4 C4 C1 117.4(5) 5_556 . ? C5 C3 C2 120.6(4) 5_556 . ? C5 C3 H3 119.7 5_556 . ? C2 C3 H3 119.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.415 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.094 #============================================================================== data_sc26ndsj _database_code_depnum_ccdc_archive 'CCDC 623277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 O10 S2 Sc2' _chemical_formula_sum 'C10 H10 O10 S2 Sc2' _chemical_formula_weight 444.22 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' Sc Sc 0.2519 0.3716 '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 5.2459(7) _cell_length_b 10.8963(14) _cell_length_c 13.2466(17) _cell_angle_alpha 86.026(2) _cell_angle_beta 81.604(2) _cell_angle_gamma 85.685(2) _cell_volume 745.64(17) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2393 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.93 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7893 _exptl_absorpt_correction_T_max 0.8859 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3686 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0999 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 23.50 _reflns_number_total 1954 _reflns_number_gt 1007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The restraints present in the CIF file are the fixed O-H distances in the coordinated water molecule. 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^)+(0.1972P)^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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.001(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1954 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.2926 _refine_ls_wR_factor_gt 0.2494 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.002 _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 Sc1 Sc 1.4021(3) 0.63263(14) 0.44381(11) 0.0350(7) Uani 1 1 d . . . Sc2 Sc 1.0771(3) 0.86535(14) 0.55651(12) 0.0360(7) Uani 1 1 d . . . S1 S 0.9668(4) 0.6863(2) 0.27352(16) 0.0360(7) Uani 1 1 d . . . S2 S 0.5084(4) 0.8147(2) 0.72809(16) 0.0371(8) Uani 1 1 d . . . O1 O 1.2184(11) 0.6463(6) 0.3042(4) 0.0447(16) Uani 1 1 d . . . O2 O 0.7585(12) 0.6332(6) 0.3441(5) 0.0469(17) Uani 1 1 d . . . O3 O 0.9302(13) 0.8176(6) 0.2569(5) 0.0523(18) Uani 1 1 d . . . O4 O 0.7139(12) 0.8737(6) 0.6610(5) 0.0480(17) Uani 1 1 d . . . O5 O 0.5596(13) 0.6841(6) 0.7478(5) 0.0522(18) Uani 1 1 d . . . O6 O 1.2562(11) 0.8432(6) 0.6922(4) 0.0472(17) Uani 1 1 d . . . O7 O 1.4208(11) 0.8171(5) 0.4677(4) 0.0378(14) Uani 1 1 d . . . H7O H 1.5551 0.8672 0.4436 0.045 Uiso 1 1 calc R . . O8 O 1.0545(11) 0.6814(5) 0.5300(4) 0.0398(15) Uani 1 1 d . . . H8O H 0.9178 0.6319 0.5521 0.048 Uiso 1 1 calc R . . O9 O 1.4068(11) 0.4409(5) 0.4349(4) 0.0376(15) Uani 1 1 d . . . H9 H 1.3392 0.3981 0.3877 0.045 Uiso 1 1 calc R . . O10 O 1.1093(11) 1.0554(5) 0.5629(4) 0.0370(14) Uani 1 1 d . . . H10O H 1.1886 1.0952 0.6086 0.044 Uiso 1 1 calc R . . C1 C 0.9537(17) 0.6229(8) 0.1559(7) 0.040(2) Uani 1 1 d . . . C2 C 0.7463(17) 0.6704(9) 0.1000(7) 0.047(2) Uani 1 1 d . . . H2 H 0.6285 0.7327 0.1256 0.056 Uiso 1 1 calc R . . C3 C 0.7261(18) 0.6227(9) 0.0097(8) 0.056(3) Uani 1 1 d . . . H3A H 0.5967 0.6539 -0.0279 0.067 Uiso 1 1 calc R . . C4 C 0.9019(17) 0.5256(9) -0.0272(7) 0.045(2) Uani 1 1 d . . . C5 C 1.1188(19) 0.5282(9) 0.1213(7) 0.049(3) Uani 1 1 d . . . H5 H 1.2478 0.4976 0.1592 0.058 Uiso 1 1 calc R . . C6 C 0.4704(17) 0.8823(8) 0.8467(7) 0.040(2) Uani 1 1 d . . . C7 C 0.2641(16) 0.8461(8) 0.9221(7) 0.044(2) Uani 1 1 d . . . H7 H 0.1534 0.7889 0.9076 0.053 Uiso 1 1 calc R . . C8 C 0.2279(17) 0.8948(9) 1.0153(7) 0.045(2) Uani 1 1 d . . . H8 H 0.0908 0.8718 1.0640 0.053 Uiso 1 1 calc R . . C9 C 0.6015(18) 1.0191(8) 0.9612(7) 0.043(2) Uani 1 1 d . . . C10 C 0.6363(17) 0.9677(8) 0.8652(7) 0.046(2) Uani 1 1 d . . . H10 H 0.7695 0.9911 0.8148 0.055 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 Sc1 0.0341(12) 0.0341(11) 0.0370(11) -0.0042(8) -0.0063(8) 0.0004(8) Sc2 0.0338(12) 0.0364(11) 0.0387(11) -0.0055(8) -0.0074(8) -0.0014(8) S1 0.0331(14) 0.0400(14) 0.0357(13) -0.0052(10) -0.0065(10) -0.0031(10) S2 0.0362(14) 0.0406(14) 0.0352(13) -0.0045(10) -0.0068(10) -0.0018(10) O1 0.034(4) 0.061(4) 0.041(4) -0.004(3) -0.011(3) -0.006(3) O2 0.041(4) 0.054(4) 0.045(4) -0.009(3) -0.002(3) -0.005(3) O3 0.067(5) 0.044(4) 0.047(4) -0.009(3) -0.009(3) -0.001(3) O4 0.041(4) 0.063(4) 0.042(4) -0.012(3) -0.005(3) -0.007(3) O5 0.074(5) 0.037(4) 0.048(4) -0.009(3) -0.019(3) 0.005(3) O6 0.036(4) 0.067(5) 0.040(4) -0.004(3) -0.012(3) 0.000(3) O7 0.034(3) 0.031(3) 0.048(4) -0.001(3) -0.002(3) -0.005(3) O8 0.036(4) 0.037(3) 0.043(3) -0.004(3) 0.002(3) -0.003(3) O9 0.040(4) 0.037(3) 0.036(3) -0.004(3) -0.005(3) -0.005(3) O10 0.035(3) 0.034(3) 0.043(3) -0.007(3) -0.009(3) 0.001(3) C1 0.042(5) 0.039(5) 0.040(5) -0.006(4) -0.010(4) -0.007(4) C2 0.039(6) 0.046(6) 0.057(6) -0.017(5) -0.003(4) -0.006(4) C3 0.049(7) 0.053(6) 0.070(7) -0.009(5) -0.023(5) 0.002(5) C4 0.039(6) 0.053(6) 0.046(6) -0.017(5) -0.011(4) -0.006(4) C5 0.048(6) 0.042(6) 0.056(6) 0.004(5) -0.011(5) 0.001(5) C6 0.041(5) 0.040(5) 0.040(5) -0.005(4) -0.011(4) 0.006(4) C7 0.027(5) 0.048(6) 0.060(6) -0.010(5) -0.010(4) -0.006(4) C8 0.039(5) 0.056(6) 0.041(5) 0.001(5) -0.008(4) -0.014(4) C9 0.045(6) 0.040(5) 0.046(5) -0.008(4) -0.009(4) 0.005(4) C10 0.039(5) 0.045(6) 0.056(6) -0.009(5) -0.006(4) -0.008(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 Sc1 O8 2.060(6) . ? Sc1 O7 2.068(6) . ? Sc1 O9 2.097(6) 2_866 ? Sc1 O9 2.099(6) . ? Sc1 O2 2.126(6) 1_655 ? Sc1 O1 2.198(6) . ? Sc1 Sc2 3.271(2) . ? Sc1 Sc1 3.321(3) 2_866 ? Sc2 O7 2.058(6) . ? Sc2 O8 2.074(6) . ? Sc2 O10 2.083(5) 2_776 ? Sc2 O10 2.099(6) . ? Sc2 O6 2.138(6) . ? Sc2 O4 2.185(6) . ? Sc2 Sc2 3.301(3) 2_776 ? S1 O3 1.435(7) . ? S1 O2 1.457(6) . ? S1 O1 1.464(6) . ? S1 C1 1.760(9) . ? S2 O5 1.441(6) . ? S2 O4 1.453(6) . ? S2 O6 1.474(6) 1_455 ? S2 C6 1.760(9) . ? O9 Sc1 2.097(6) 2_866 ? C3 C2 1.358(13) . ? C3 C4 1.415(13) . ? C7 C8 1.361(12) . ? C7 C6 1.420(12) . ? C2 C1 1.448(12) . ? C9 C10 1.407(12) . ? C9 C8 1.423(12) 2_677 ? C9 C9 1.433(18) 2_677 ? C4 C4 1.402(18) 2_765 ? C4 C5 1.435(13) 2_765 ? C1 C5 1.357(13) . ? C10 C6 1.378(12) . ? O6 S2 1.474(6) 1_655 ? C5 C4 1.435(13) 2_765 ? O10 Sc2 2.083(5) 2_776 ? C8 C9 1.423(12) 2_677 ? O2 Sc1 2.126(6) 1_455 ? 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 O8 Sc1 O7 75.3(2) . . ? O8 Sc1 O9 97.1(2) . 2_866 ? O7 Sc1 O9 97.7(2) . 2_866 ? O8 Sc1 O9 105.2(2) . . ? O7 Sc1 O9 173.1(2) . . ? O9 Sc1 O9 75.4(3) 2_866 . ? O8 Sc1 O2 164.8(3) . 1_655 ? O7 Sc1 O2 90.7(2) . 1_655 ? O9 Sc1 O2 90.6(2) 2_866 1_655 ? O9 Sc1 O2 89.4(2) . 1_655 ? O8 Sc1 O1 90.7(2) . . ? O7 Sc1 O1 100.8(2) . . ? O9 Sc1 O1 161.2(3) 2_866 . ? O9 Sc1 O1 86.1(2) . . ? O2 Sc1 O1 86.0(2) 1_655 . ? O8 Sc1 Sc2 37.85(17) . . ? O7 Sc1 Sc2 37.46(16) . . ? O9 Sc1 Sc2 98.64(17) 2_866 . ? O9 Sc1 Sc2 142.48(16) . . ? O2 Sc1 Sc2 128.03(19) 1_655 . ? O1 Sc1 Sc2 98.01(18) . . ? O8 Sc1 Sc1 104.13(18) . 2_866 ? O7 Sc1 Sc1 135.42(18) . 2_866 ? O9 Sc1 Sc1 37.70(16) 2_866 2_866 ? O9 Sc1 Sc1 37.66(15) . 2_866 ? O2 Sc1 Sc1 89.98(19) 1_655 2_866 ? O1 Sc1 Sc1 123.72(19) . 2_866 ? Sc2 Sc1 Sc1 126.60(8) . 2_866 ? O7 Sc2 O8 75.2(2) . . ? O7 Sc2 O10 96.2(2) . 2_776 ? O8 Sc2 O10 98.6(2) . 2_776 ? O7 Sc2 O10 100.5(2) . . ? O8 Sc2 O10 172.6(2) . . ? O10 Sc2 O10 75.8(3) 2_776 . ? O7 Sc2 O6 91.3(2) . . ? O8 Sc2 O6 99.4(3) . . ? O10 Sc2 O6 161.8(3) 2_776 . ? O10 Sc2 O6 86.6(2) . . ? O7 Sc2 O4 167.4(3) . . ? O8 Sc2 O4 93.5(2) . . ? O10 Sc2 O4 90.8(2) 2_776 . ? O10 Sc2 O4 91.3(2) . . ? O6 Sc2 O4 85.1(2) . . ? O7 Sc2 Sc1 37.66(16) . . ? O8 Sc2 Sc1 37.54(16) . . ? O10 Sc2 Sc1 100.07(17) 2_776 . ? O10 Sc2 Sc1 137.99(17) . . ? O6 Sc2 Sc1 95.99(19) . . ? O4 Sc2 Sc1 130.72(19) . . ? O7 Sc2 Sc2 100.61(17) . 2_776 ? O8 Sc2 Sc2 136.44(18) . 2_776 ? O10 Sc2 Sc2 38.05(16) 2_776 2_776 ? O10 Sc2 Sc2 37.70(15) . 2_776 ? O6 Sc2 Sc2 124.2(2) . 2_776 ? O4 Sc2 Sc2 91.32(19) . 2_776 ? Sc1 Sc2 Sc2 125.65(8) . 2_776 ? O3 S1 O2 113.2(4) . . ? O3 S1 O1 113.1(4) . . ? O2 S1 O1 110.9(4) . . ? O3 S1 C1 106.7(4) . . ? O2 S1 C1 105.0(4) . . ? O1 S1 C1 107.3(4) . . ? O5 S2 O4 114.0(4) . . ? O5 S2 O6 111.8(4) . 1_455 ? O4 S2 O6 111.6(4) . 1_455 ? O5 S2 C6 107.0(4) . . ? O4 S2 C6 108.0(4) . . ? O6 S2 C6 103.7(4) 1_455 . ? Sc2 O7 Sc1 104.9(2) . . ? Sc1 O9 Sc1 104.6(3) 2_866 . ? S2 O4 Sc2 151.5(4) . . ? Sc1 O8 Sc2 104.6(3) . . ? C2 C3 C4 120.0(9) . . ? C8 C7 C6 120.2(8) . . ? C3 C2 C1 119.1(9) . . ? C10 C9 C8 121.1(9) . 2_677 ? C10 C9 C9 120.0(11) . 2_677 ? C8 C9 C9 118.8(11) 2_677 2_677 ? C4 C4 C3 122.2(11) 2_765 . ? C4 C4 C5 116.7(11) 2_765 2_765 ? C3 C4 C5 121.1(9) . 2_765 ? C5 C1 C2 120.7(9) . . ? C5 C1 S1 122.1(7) . . ? C2 C1 S1 117.1(7) . . ? C6 C10 C9 119.1(9) . . ? S2 O6 Sc2 142.2(4) 1_655 . ? C10 C6 C7 121.4(9) . . ? C10 C6 S2 120.7(7) . . ? C7 C6 S2 117.9(7) . . ? C1 C5 C4 121.3(9) . 2_765 ? Sc2 O10 Sc2 104.2(3) 2_776 . ? C7 C8 C9 120.4(9) . 2_677 ? S1 O2 Sc1 156.6(4) . 1_455 ? S1 O1 Sc1 138.1(4) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 1.547 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.176 #============================================================================== data_y1 _database_code_depnum_ccdc_archive 'CCDC 718897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H9 O8 S2 Y' _chemical_formula_sum 'C10 H9 O8 S2 Y' _chemical_formula_weight 410.20 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' Y Y -2.7962 3.5667 '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 7.6693(5) _cell_length_b 7.8627(5) _cell_length_c 21.0191(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.6070(10) _cell_angle_gamma 90.00 _cell_volume 1266.98(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4074 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.94 _exptl_crystal_description plane _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 4.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2411 _exptl_absorpt_correction_T_max 0.4364 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10900 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.93 _reflns_number_total 3090 _reflns_number_gt 2257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0272P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3090 _refine_ls_number_parameters 202 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 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 Y1 Y 0.83252(4) 0.33623(4) 0.008699(14) 0.01309(9) Uani 1 1 d . . . O1 O 0.7036(3) 0.5053(3) 0.08272(10) 0.0201(5) Uani 1 1 d . . . O2 O 0.6551(3) 0.8011(3) 0.05757(11) 0.0224(5) Uani 1 1 d . . . O3 O 0.5870(3) 0.3949(3) -0.06075(11) 0.0201(5) Uani 1 1 d . . . S1 S 0.58531(10) 0.65133(10) 0.08605(3) 0.01370(16) Uani 1 1 d . . . C1 C 0.5641(4) 0.6943(4) 0.16867(14) 0.0127(6) Uani 1 1 d . . . C2 C 0.6103(4) 0.8516(4) 0.18984(15) 0.0194(7) Uani 1 1 d . . . H2 H 0.6511 0.9322 0.1615 0.023 Uiso 1 1 calc R . . C3 C 0.5965(4) 0.8928(4) 0.25499(16) 0.0188(7) Uani 1 1 d . . . H3 H 0.6270 1.0010 0.2693 0.023 Uiso 1 1 calc R . . C4 C 0.5049(4) 0.5652(4) 0.21090(14) 0.0129(6) Uani 1 1 d . . . C5 C 0.4572(4) 0.3980(4) 0.19061(15) 0.0161(7) Uani 1 1 d . . . H5 H 0.4611 0.3704 0.1476 0.019 Uiso 1 1 calc R . . C6 C 1.0611(4) -0.0241(4) 0.18043(14) 0.0143(6) Uani 1 1 d . . . C7 C 1.1031(4) -0.1838(4) 0.20201(15) 0.0191(7) Uani 1 1 d . . . H7 H 1.1378 -0.2670 0.1736 0.023 Uiso 1 1 calc R . . C8 C 1.0936(4) -0.2216(4) 0.26718(15) 0.0190(7) Uani 1 1 d . . . H8 H 1.1226 -0.3301 0.2816 0.023 Uiso 1 1 calc R . . C9 C 1.0066(4) 0.1069(4) 0.22318(15) 0.0137(6) Uani 1 1 d . . . C10 C 0.9614(4) 0.2749(4) 0.20315(15) 0.0166(7) Uani 1 1 d . . . H10 H 0.9717 0.3045 0.1606 0.020 Uiso 1 1 calc R . . S2 S 1.09522(10) 0.01998(9) 0.09865(4) 0.01400(17) Uani 1 1 d . . . O4 O 0.9399(3) 0.1060(3) 0.07332(10) 0.0173(5) Uani 1 1 d . . . O5 O 1.2511(3) 0.1213(3) 0.09559(11) 0.0251(6) Uani 1 1 d . . . O6 O 0.8865(3) 0.1480(3) -0.06947(10) 0.0245(5) Uani 1 1 d . . . O7 O 1.0880(3) 0.4363(3) 0.04563(12) 0.0216(5) Uani 1 1 d . . . H7O H 1.167(6) 0.382(6) 0.074(2) 0.056(14) Uiso 1 1 d . . . O8 O 0.6077(3) 0.1539(3) 0.04476(13) 0.0265(6) Uani 1 1 d D . . H8A H 0.627(6) 0.059(3) 0.054(2) 0.050(15) Uiso 1 1 d D . . H8B H 0.508(3) 0.165(7) 0.037(3) 0.09(2) Uiso 1 1 d 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 Y1 0.01460(15) 0.01077(14) 0.01396(15) -0.00037(13) 0.00145(10) 0.00049(13) O1 0.0229(12) 0.0216(12) 0.0160(12) 0.0011(10) 0.0053(9) 0.0080(10) O2 0.0310(14) 0.0164(12) 0.0202(12) 0.0032(9) 0.0067(10) -0.0041(10) O3 0.0170(12) 0.0244(12) 0.0185(12) 0.0019(9) -0.0053(9) -0.0012(10) S1 0.0156(4) 0.0132(4) 0.0123(4) 0.0005(3) 0.0016(3) 0.0005(3) C1 0.0137(15) 0.0134(16) 0.0110(15) -0.0004(11) 0.0016(12) 0.0017(11) C2 0.0237(18) 0.0170(17) 0.0176(16) 0.0033(14) 0.0036(13) 0.0001(14) C3 0.0236(19) 0.0127(15) 0.0202(17) -0.0028(13) -0.0012(14) -0.0038(13) C4 0.0134(16) 0.0103(15) 0.0150(16) 0.0001(12) -0.0005(12) 0.0000(12) C5 0.0203(17) 0.0141(15) 0.0138(16) -0.0039(12) 0.0006(13) -0.0008(12) C6 0.0164(16) 0.0154(15) 0.0111(15) 0.0011(12) 0.0009(12) 0.0014(12) C7 0.0241(18) 0.0146(17) 0.0184(16) -0.0031(13) 0.0000(13) 0.0069(14) C8 0.0215(18) 0.0137(16) 0.0217(18) 0.0049(13) -0.0011(14) 0.0041(13) C9 0.0130(16) 0.0128(15) 0.0151(16) 0.0018(12) -0.0003(13) 0.0001(11) C10 0.0229(18) 0.0131(15) 0.0138(16) 0.0029(12) -0.0008(13) -0.0001(13) S2 0.0177(4) 0.0131(4) 0.0113(4) -0.0001(3) 0.0014(3) 0.0024(3) O4 0.0185(12) 0.0160(11) 0.0172(11) 0.0033(9) -0.0046(9) 0.0024(9) O5 0.0179(13) 0.0333(14) 0.0244(13) 0.0035(10) 0.0039(10) -0.0068(10) O6 0.0414(15) 0.0176(12) 0.0145(11) -0.0039(10) 0.0016(10) 0.0082(11) O7 0.0195(12) 0.0209(12) 0.0241(13) 0.0093(10) -0.0048(10) -0.0048(10) O8 0.0181(14) 0.0186(13) 0.0425(16) 0.0064(12) -0.0021(12) -0.0002(11) _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 Y1 O7 2.217(2) 3_765 ? Y1 O7 2.231(2) . ? Y1 O6 2.258(2) . ? Y1 O1 2.291(2) . ? Y1 O8 2.382(3) . ? Y1 O3 2.395(2) . ? Y1 O4 2.396(2) . ? Y1 Y1 3.6631(6) 3_765 ? O1 S1 1.466(2) . ? O2 S1 1.432(2) . ? O3 S1 1.457(2) 3_665 ? S1 O3 1.457(2) 3_665 ? S1 C1 1.781(3) . ? C1 C2 1.358(4) . ? C1 C4 1.431(4) . ? C2 C3 1.414(5) . ? C2 H2 0.9300 . ? C3 C10 1.361(4) 2_655 ? C3 H3 0.9300 . ? C4 C5 1.426(4) . ? C4 C9 1.429(4) 2_655 ? C5 C8 1.358(4) 2_655 ? C5 H5 0.9300 . ? C6 C7 1.371(4) . ? C6 C9 1.436(4) . ? C6 S2 1.780(3) . ? C7 C8 1.405(4) . ? C7 H7 0.9300 . ? C8 C5 1.358(4) 2_645 ? C8 H8 0.9300 . ? C9 C10 1.426(4) . ? C9 C4 1.429(4) 2_645 ? C10 C3 1.361(4) 2_645 ? C10 H10 0.9300 . ? S2 O5 1.440(2) . ? S2 O4 1.457(2) . ? S2 O6 1.465(2) 3_755 ? O6 S2 1.465(2) 3_755 ? O7 Y1 2.217(2) 3_765 ? O7 H7O 0.94(5) . ? O8 H8A 0.784(19) . ? O8 H8B 0.78(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Y1 O7 69.09(10) 3_765 . ? O7 Y1 O6 95.47(9) 3_765 . ? O7 Y1 O6 107.89(9) . . ? O7 Y1 O1 90.67(9) 3_765 . ? O7 Y1 O1 87.17(9) . . ? O6 Y1 O1 164.92(9) . . ? O7 Y1 O8 149.47(9) 3_765 . ? O7 Y1 O8 137.56(9) . . ? O6 Y1 O8 89.21(9) . . ? O1 Y1 O8 78.65(9) . . ? O7 Y1 O3 75.73(8) 3_765 . ? O7 Y1 O3 144.31(8) . . ? O6 Y1 O3 80.78(8) . . ? O1 Y1 O3 87.44(8) . . ? O8 Y1 O3 75.30(9) . . ? O7 Y1 O4 143.78(8) 3_765 . ? O7 Y1 O4 77.55(8) . . ? O6 Y1 O4 81.38(8) . . ? O1 Y1 O4 101.62(8) . . ? O8 Y1 O4 66.75(8) . . ? O3 Y1 O4 138.01(8) . . ? O7 Y1 Y1 34.67(6) 3_765 3_765 ? O7 Y1 Y1 34.42(6) . 3_765 ? O6 Y1 Y1 104.17(6) . 3_765 ? O1 Y1 Y1 88.68(6) . 3_765 ? O8 Y1 Y1 166.08(7) . 3_765 ? O3 Y1 Y1 110.20(6) . 3_765 ? O4 Y1 Y1 110.91(5) . 3_765 ? S1 O1 Y1 139.99(13) . . ? S1 O3 Y1 149.79(14) 3_665 . ? O2 S1 O3 113.50(14) . 3_665 ? O2 S1 O1 112.63(14) . . ? O3 S1 O1 110.09(14) 3_665 . ? O2 S1 C1 107.28(14) . . ? O3 S1 C1 107.26(14) 3_665 . ? O1 S1 C1 105.58(13) . . ? C2 C1 C4 121.8(3) . . ? C2 C1 S1 117.5(2) . . ? C4 C1 S1 120.6(2) . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C10 C3 C2 120.3(3) 2_655 . ? C10 C3 H3 119.9 2_655 . ? C2 C3 H3 119.9 . . ? C5 C4 C9 118.6(3) . 2_655 ? C5 C4 C1 123.5(3) . . ? C9 C4 C1 117.9(3) 2_655 . ? C8 C5 C4 121.2(3) 2_655 . ? C8 C5 H5 119.4 2_655 . ? C4 C5 H5 119.4 . . ? C7 C6 C9 121.3(3) . . ? C7 C6 S2 117.3(2) . . ? C9 C6 S2 121.2(2) . . ? C6 C7 C8 119.9(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C5 C8 C7 120.9(3) 2_645 . ? C5 C8 H8 119.5 2_645 . ? C7 C8 H8 119.5 . . ? C10 C9 C4 118.5(3) . 2_645 ? C10 C9 C6 123.5(3) . . ? C4 C9 C6 118.0(3) 2_645 . ? C3 C10 C9 121.4(3) 2_645 . ? C3 C10 H10 119.3 2_645 . ? C9 C10 H10 119.3 . . ? O5 S2 O4 113.46(14) . . ? O5 S2 O6 113.01(15) . 3_755 ? O4 S2 O6 110.63(14) . 3_755 ? O5 S2 C6 107.19(14) . . ? O4 S2 C6 107.60(14) . . ? O6 S2 C6 104.32(14) 3_755 . ? S2 O4 Y1 145.33(14) . . ? S2 O6 Y1 156.55(15) 3_755 . ? Y1 O7 Y1 110.91(10) 3_765 . ? Y1 O7 H7O 121(3) 3_765 . ? Y1 O7 H7O 127(3) . . ? Y1 O8 H8A 121(4) . . ? Y1 O8 H8B 125(4) . . ? H8A O8 H8B 109(5) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.568 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.125