# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #===================================================== _audit_creation_date 2011-04-30 _audit_creation_method 'WinGX routine CIF_UPDATE' #===================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Leone Spiccia' _publ_contact_author_address ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_contact_author_email leone.spiccia@monash.edu _publ_contact_author_phone +61-3-9905-4526 _publ_contact_author_fax +61-3-9905-4597 loop_ _publ_author_name _publ_author_address A.J.Fischmann ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; L.Spiccia ; School of Chemistry, Monash University, PO Box 23, VIC 3800, Australia ; _publ_contact_letter ; ; _publ_requested_category ? _publ_section_title ; Sodium thiosulfonate salts: molecular and supramolecular structural features and solution radiolytic properties ; data_1 _database_code_depnum_ccdc_archive 'CCDC 823756' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Sodium p-toluenethiosulfonate' _chemical_formula_sum 'C7 H7 Na O2 S2' _chemical_formula_weight 210.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 7.2976(5) _cell_length_b 9.6537(7) _cell_length_c 12.7994(10) _cell_angle_alpha 90 _cell_angle_beta 94.058(4) _cell_angle_gamma 90 _cell_volume 899.44(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 84 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS, (Sheldrick 1996)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method 'Thin Slice Phi/Omega Scans' _diffrn_standards_number 316 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_unetI/netI 0.0206 _diffrn_reflns_number 8368 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 30.58 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 1456 _reflns_number_gt 1405 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Apex II (Bruker, 2005)' _computing_cell_refinement 'Apex II (Bruker, 2005)' _computing_data_reduction 'Apex II (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0158P)^2^+1.5496P] 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_number_reflns 1456 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.24 _refine_ls_restrained_S_all 1.24 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.495 _refine_diff_density_min -0.34 _refine_diff_density_rms 0.063 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' 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 S1 S 0.01864(7) 0 0.17940(5) 0.01739(13) Uani 1 2 d S . . S2 S -0.23700(7) 0 0.12343(4) 0.01214(11) Uani 1 2 d S . . Na1 Na -0.5 -0.27992(9) 0 0.01575(18) Uani 1 2 d S . . O1 O -0.27838(15) -0.12708(12) 0.06394(9) 0.0184(2) Uani 1 1 d . . . C5 C -0.7833(4) 0 0.4576(2) 0.0420(8) Uani 1 2 d S . . H5A H -0.8067 0.0953 0.4794 0.063 Uiso 0.5 1 calc PR . . H5B H -0.7409 -0.0551 0.5189 0.063 Uiso 0.5 1 calc PR . . H5C H -0.8968 -0.0402 0.4252 0.063 Uiso 0.5 1 calc PR . . C1 C -0.3865(3) 0 0.22618(16) 0.0140(4) Uani 1 2 d S . . C2 C -0.4470(2) -0.12510(17) 0.26500(13) 0.0190(3) Uani 1 1 d . . . H2 H -0.4028 -0.2104 0.2395 0.023 Uiso 1 1 calc R . . C3 C -0.5726(2) -0.1239(2) 0.34146(13) 0.0258(4) Uani 1 1 d . . . H3 H -0.6146 -0.2092 0.3681 0.031 Uiso 1 1 calc R . . C4 C -0.6383(3) 0 0.37977(19) 0.0269(5) Uani 1 2 d S . . 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 S1 0.0119(2) 0.0161(2) 0.0239(3) 0 -0.00052(19) 0 S2 0.0109(2) 0.0099(2) 0.0159(2) 0 0.00271(17) 0 Na1 0.0106(4) 0.0138(4) 0.0230(4) 0 0.0026(3) 0 O1 0.0158(5) 0.0173(5) 0.0223(6) -0.0073(4) 0.0035(4) -0.0036(4) C5 0.0200(12) 0.085(3) 0.0219(13) 0 0.0086(10) 0 C1 0.0117(9) 0.0155(9) 0.0148(9) 0 0.0020(7) 0 C2 0.0197(7) 0.0175(7) 0.0198(7) 0.0017(6) 0.0023(6) -0.0034(6) C3 0.0201(7) 0.0365(10) 0.0209(8) 0.0051(7) 0.0024(6) -0.0106(7) C4 0.0123(10) 0.0529(17) 0.0156(10) 0 0.0017(8) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 S2 1.9504(7) . ? S1 Na1 3.1242(7) 7_445 ? S1 Na1 3.1242(7) 3 ? S2 O1 1.4641(11) . ? S2 O1 1.4641(11) 6 ? S2 C1 1.767(2) . ? S2 Na1 3.2230(7) 3 ? S2 Na1 3.2230(7) 7_445 ? Na1 O1 2.2967(12) . ? Na1 O1 2.2967(12) 2_455 ? Na1 O1 2.4162(11) 8_445 ? Na1 O1 2.4162(11) 7_445 ? Na1 S1 3.1242(7) 7_445 ? Na1 S1 3.1242(7) 3_445 ? O1 Na1 2.4162(11) 7_445 ? C5 C4 1.504(3) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C1 C2 1.3896(18) 6 ? C1 C2 1.3896(18) . ? C2 C3 1.388(2) . ? C2 H2 0.95 . ? C3 C4 1.390(2) . ? C3 H3 0.95 . ? C4 C3 1.390(2) 6 ? 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 S1 Na1 74.889(18) . 7_445 ? S2 S1 Na1 74.889(18) . 3 ? Na1 S1 Na1 85.69(3) 7_445 3 ? O1 S2 O1 113.85(10) . 6 ? O1 S2 C1 105.75(6) . . ? O1 S2 C1 105.75(6) 6 . ? O1 S2 S1 110.35(5) . . ? O1 S2 S1 110.35(5) 6 . ? C1 S2 S1 110.59(7) . . ? O1 Na1 O1 100.06(7) . 2_455 ? O1 Na1 O1 134.89(5) . 8_445 ? O1 Na1 O1 76.80(4) 2_455 8_445 ? O1 Na1 O1 76.80(4) . 7_445 ? O1 Na1 O1 134.89(5) 2_455 7_445 ? O1 Na1 O1 136.38(7) 8_445 7_445 ? O1 Na1 S1 133.76(3) . 7_445 ? O1 Na1 S1 100.49(3) 2_455 7_445 ? O1 Na1 S1 90.13(4) 8_445 7_445 ? O1 Na1 S1 59.49(3) 7_445 7_445 ? O1 Na1 S1 100.49(3) . 3_445 ? O1 Na1 S1 133.76(3) 2_455 3_445 ? O1 Na1 S1 59.49(3) 8_445 3_445 ? O1 Na1 S1 90.13(4) 7_445 3_445 ? S1 Na1 S1 94.31(3) 7_445 3_445 ? S2 O1 Na1 146.90(7) . . ? S2 O1 Na1 109.88(6) . 7_445 ? Na1 O1 Na1 103.20(4) . 7_445 ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C1 C2 120.7(2) 6 . ? C2 C1 S2 119.63(10) 6 . ? C2 C1 S2 119.63(10) . . ? C3 C2 C1 119.14(17) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 121.16(17) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C3 118.7(2) 6 . ? C3 C4 C5 120.65(11) 6 . ? C3 C4 C5 120.65(11) . . ? # Attachment 'web_deposit_cif_file_1_LeoneSpiccia_1304241487.cif' data_mono1 _database_code_depnum_ccdc_archive 'CCDC 823757' #TrackingRef 'web_deposit_cif_file_1_LeoneSpiccia_1304241487.cif' _audit_creation_date 2011-05-01T00:56:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Sodium benzenethiosulfonate hemitrihydrate' _chemical_formula_sum 'C6 H8 Na O3.50 S2' _chemical_formula_weight 223.23 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 26.688(3) _cell_length_b 6.4934(8) _cell_length_c 11.1130(13) _cell_angle_alpha 90 _cell_angle_beta 103.873(7) _cell_angle_gamma 90 _cell_volume 1869.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 96 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method 'Thin Slice Phi/Omega Scans' _diffrn_standards_number 316 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_unetI/netI 0.045 _diffrn_reflns_number 8493 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 29.9 _diffrn_reflns_theta_full 29.9 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 2632 _reflns_number_gt 2343 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Apex II (Bruker, 2005)' _computing_cell_refinement 'Apex II (Bruker, 2005)' _computing_data_reduction 'Apex II (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0127P)^2^+3.3114P] 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_number_reflns 2632 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.16 _refine_ls_restrained_S_all 1.16 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.429 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' 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 S1 S 0.38558(2) 0.32458(7) 0.21132(4) 0.01434(12) Uani 1 1 d . . . Na1 Na 0.51082(3) -0.23947(12) 0.43765(7) 0.01366(18) Uani 1 1 d . . . O1 O 0.43254(5) -0.0437(2) 0.14959(12) 0.0167(3) Uani 1 1 d . . . C1 C 0.35996(7) -0.1076(3) 0.26486(17) 0.0122(4) Uani 1 1 d . . . S2 S 0.413828(18) 0.04457(7) 0.25152(4) 0.01110(11) Uani 1 1 d . . . O2 O 0.45070(5) 0.0386(2) 0.37305(12) 0.0139(3) Uani 1 1 d . . . C2 C 0.34792(8) -0.1251(3) 0.37970(18) 0.0153(4) Uani 1 1 d . . . H2 H 0.3693(9) -0.064(4) 0.450(2) 0.016(6) Uiso 1 1 d . . . C3 C 0.30443(8) -0.2374(3) 0.3893(2) 0.0184(4) Uani 1 1 d . . . H3 H 0.2963(9) -0.250(4) 0.469(2) 0.026(7) Uiso 1 1 d . . . C4 C 0.27359(9) -0.3289(3) 0.2836(2) 0.0203(5) Uani 1 1 d . . . H4 H 0.2440(10) -0.404(4) 0.290(2) 0.028(7) Uiso 1 1 d . . . C5 C 0.28670(8) -0.3136(3) 0.17006(19) 0.0191(5) Uani 1 1 d . . . H5 H 0.2664(9) -0.385(4) 0.098(2) 0.028(7) Uiso 1 1 d . . . C6 C 0.32999(8) -0.2033(3) 0.15943(18) 0.0155(4) Uani 1 1 d . . . H6 H 0.3401(8) -0.194(3) 0.086(2) 0.014(6) Uiso 1 1 d . . . O1W O 0.44060(6) -0.4613(2) 0.47744(14) 0.0164(3) Uani 1 1 d . . . H1W H 0.4235(12) -0.412(5) 0.524(3) 0.048(10) Uiso 1 1 d . . . O2W O 0.5 -0.4418(3) 0.25 0.0158(4) Uani 1 2 d S . . H2W H 0.4216(11) -0.503(4) 0.413(3) 0.034(8) Uiso 1 1 d . . . H3W H 0.4747(10) -0.525(4) 0.237(3) 0.042(9) 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 S1 0.0161(3) 0.0118(2) 0.0144(2) 0.00158(16) 0.00212(18) 0.00131(18) Na1 0.0150(4) 0.0118(4) 0.0138(4) 0.0007(3) 0.0028(3) 0.0000(3) O1 0.0157(7) 0.0221(8) 0.0139(6) -0.0036(5) 0.0065(6) 0.0032(6) C1 0.0118(9) 0.0103(8) 0.0140(9) 0.0009(6) 0.0022(7) 0.0015(7) S2 0.0103(2) 0.0121(2) 0.0105(2) -0.00004(16) 0.00183(17) 0.00118(17) O2 0.0122(7) 0.0159(7) 0.0120(6) 0.0003(5) 0.0000(5) 0.0004(5) C2 0.0135(10) 0.0164(10) 0.0149(9) 0.0008(7) 0.0015(8) 0.0015(8) C3 0.0169(10) 0.0175(10) 0.0214(10) 0.0027(8) 0.0062(8) 0.0000(8) C4 0.0155(11) 0.0159(10) 0.0285(11) 0.0025(8) 0.0031(9) -0.0031(8) C5 0.0188(11) 0.0145(10) 0.0214(10) -0.0020(7) -0.0006(9) -0.0023(8) C6 0.0179(11) 0.0131(9) 0.0141(9) -0.0016(7) 0.0014(8) -0.0002(8) O1W 0.0176(8) 0.0181(7) 0.0132(7) -0.0004(6) 0.0030(6) 0.0026(6) O2W 0.0164(11) 0.0151(10) 0.0155(9) 0 0.0034(8) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 S1 S2 1.9780(7) . ? Na1 O1 2.3547(17) 2_655 ? Na1 O1W 2.4001(17) 5_646 ? Na1 O2 2.4077(16) . ? Na1 O2W 2.4227(14) . ? Na1 O2 2.4791(15) 5_656 ? Na1 O1W 2.4859(18) . ? O1 S2 1.4601(15) . ? O1 Na1 2.3547(17) 2_655 ? C1 C2 1.393(3) . ? C1 C6 1.396(2) . ? C1 S2 1.780(2) . ? S2 O2 1.4685(13) . ? O2 Na1 2.4791(15) 5_656 ? C2 C3 1.396(3) . ? C2 H2 0.94(2) . ? C3 C4 1.395(3) . ? C3 H3 0.96(2) . ? C4 C5 1.392(3) . ? C4 H4 0.94(3) . ? C5 C6 1.388(3) . ? C5 H5 0.97(2) . ? C6 H6 0.92(2) . ? O1W Na1 2.4001(17) 5_646 ? O1W H1W 0.83(3) . ? O1W H2W 0.82(3) . ? O2W Na1 2.4227(14) 2_655 ? O2W H3W 0.85(3) . ? 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 Na1 O1W 105.03(6) 2_655 5_646 ? O1 Na1 O2 85.42(6) 2_655 . ? O1W Na1 O2 169.38(6) 5_646 . ? O1 Na1 O2W 83.93(5) 2_655 . ? O1W Na1 O2W 80.85(6) 5_646 . ? O2 Na1 O2W 102.51(5) . . ? O1 Na1 O2 83.63(5) 2_655 5_656 ? O1W Na1 O2 91.00(5) 5_646 5_656 ? O2 Na1 O2 88.24(5) . 5_656 ? O2W Na1 O2 162.82(5) . 5_656 ? O1 Na1 O1W 166.38(6) 2_655 . ? O1W Na1 O1W 79.64(6) 5_646 . ? O2 Na1 O1W 90.61(6) . . ? O2W Na1 O1W 84.23(5) . . ? O2 Na1 O1W 109.31(6) 5_656 . ? S2 O1 Na1 154.69(9) . 2_655 ? C2 C1 C6 121.40(19) . . ? C2 C1 S2 119.32(14) . . ? C6 C1 S2 119.27(16) . . ? O1 S2 O2 115.13(8) . . ? O1 S2 C1 106.26(9) . . ? O2 S2 C1 106.57(8) . . ? O1 S2 S1 111.60(7) . . ? O2 S2 S1 111.54(6) . . ? C1 S2 S1 104.92(7) . . ? S2 O2 Na1 123.08(8) . . ? S2 O2 Na1 144.72(9) . 5_656 ? Na1 O2 Na1 91.76(5) . 5_656 ? C1 C2 C3 119.37(18) . . ? C1 C2 H2 120.3(14) . . ? C3 C2 H2 120.3(14) . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 121.2(15) . . ? C2 C3 H3 119.3(15) . . ? C5 C4 C3 120.5(2) . . ? C5 C4 H4 120.1(15) . . ? C3 C4 H4 119.5(15) . . ? C6 C5 C4 120.63(19) . . ? C6 C5 H5 118.9(15) . . ? C4 C5 H5 120.4(15) . . ? C5 C6 C1 118.6(2) . . ? C5 C6 H6 122.3(14) . . ? C1 C6 H6 119.0(14) . . ? Na1 O1W Na1 100.36(6) 5_646 . ? Na1 O1W H1W 113(2) 5_646 . ? Na1 O1W H1W 116(2) . . ? Na1 O1W H2W 104(2) 5_646 . ? Na1 O1W H2W 112(2) . . ? H1W O1W H2W 111(3) . . ? Na1 O2W Na1 114.32(9) . 2_655 ? Na1 O2W H3W 115(2) . . ? Na1 O2W H3W 106(2) 2_655 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W S1 0.83(3) 2.59(3) 3.3955(18) 165(3) 6_556 O1W H2W S1 0.82(3) 2.48(3) 3.2792(16) 165(3) 1_545 O2W H3W S1 0.85(3) 2.53(3) 3.3439(11) 163(3) 1_545