# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/402 data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Disodium salt of5-N-sulfinohydroxylamino-2-pyridinesulfonic acid ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C5H4N2O7S2.Na2.4H2O _chemical_formula_sum 'C5 H11.50 N2 Na2 O11 S2' _chemical_formula_weight 385.76 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' 'N' 'N' 0.0061 0.0033 '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' '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' _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 5.40230(10) _cell_length_b 11.5582(3) _cell_length_c 12.6662(3) _cell_angle_alpha 66.5210(10) _cell_angle_beta 79.9700(10) _cell_angle_gamma 88.0550(10) _cell_volume 713.77(3) _cell_formula_units_Z 2 _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 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 395 _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type ? _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 ? _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 10834 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 6.81 _diffrn_reflns_theta_max 33.14 _reflns_number_total 5016 _reflns_number_gt 4086 _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^)+(0.0480P)^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 5016 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.224 _refine_ls_shift/su_mean 0.009 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 1.09282(5) 0.92842(3) 0.33957(3) 0.01230(7) Uani 1 1 d . . . S2 S 0.91061(5) 0.42364(3) 0.19359(3) 0.01157(7) Uani 1 1 d . . . Na1 Na 0.5000 0.5000 0.0000 0.01576(15) Uani 1 2 d S . . Na2 Na 0.5000 0.0000 0.5000 0.01689(15) Uani 1 2 d S . . Na3 Na -0.34818(10) 0.14238(5) 0.19776(5) 0.01987(12) Uani 1 1 d . . . O1 O 1.27618(19) 1.00191(9) 0.23582(9) 0.0214(2) Uani 1 1 d . . . O2 O 1.19564(18) 0.89037(9) 0.44942(9) 0.01891(19) Uani 1 1 d . . . O3 O 0.84689(17) 0.98676(9) 0.34662(9) 0.01752(18) Uani 1 1 d . . . O4 O 0.72780(17) 0.35338(9) 0.41087(8) 0.01666(18) Uani 1 1 d . . . H4 H 0.774(4) 0.285(2) 0.4492(17) 0.025(5) Uiso 1 1 d . . . O5 O 1.10814(17) 0.51306(9) 0.11064(8) 0.01703(18) Uani 1 1 d . . . O6 O 0.95203(17) 0.29090(9) 0.21145(9) 0.01743(18) Uani 1 1 d . . . O7 O 0.65367(16) 0.46069(10) 0.17707(8) 0.01809(19) Uani 1 1 d . . . O8 O 1.6205(3) 0.87280(18) 0.08141(16) 0.0457(4) Uani 1 1 d . . . H8A H 1.521(6) 0.834(3) 0.158(3) 0.066(8) Uiso 1 1 d . . . H8B H 1.525(5) 0.890(3) 0.062(2) 0.034(8) Uiso 1 1 d . . . O9 O 0.38604(19) 0.19271(10) 0.35306(9) 0.01897(19) Uani 1 1 d . . . H9A H 0.256(5) 0.209(2) 0.334(2) 0.044(6) Uiso 1 1 d . . . H9B H 0.424(5) 0.260(3) 0.349(2) 0.044(6) Uiso 1 1 d . . . O10 O 0.40784(19) 0.27930(10) 0.05821(9) 0.01993(19) Uani 1 1 d . . . H10A H 0.394(4) 0.241(2) 0.011(2) 0.036(5) Uiso 1 1 d . . . H10B H 0.273(5) 0.274(2) 0.094(2) 0.048(7) Uiso 1 1 d . . . N1 N 1.2261(2) 0.73337(11) 0.28039(11) 0.0185(2) Uani 1 1 d . . . N2 N 0.94670(19) 0.42317(10) 0.32780(9) 0.01283(19) Uani 1 1 d . . . C2 C 1.0293(2) 0.78101(11) 0.32985(11) 0.0125(2) Uani 1 1 d . . . C3 C 0.7927(2) 0.71948(12) 0.37841(12) 0.0161(2) Uani 1 1 d . . . H3 H 0.654(4) 0.7599(18) 0.4138(17) 0.026(5) Uiso 1 1 d . . . C4 C 0.7582(2) 0.59967(12) 0.37787(11) 0.0158(2) Uani 1 1 d . . . H4 H 0.598(4) 0.5536(19) 0.4105(18) 0.030(5) Uiso 1 1 d . . . C5 C 0.9610(2) 0.54795(11) 0.32864(11) 0.0124(2) Uani 1 1 d . . . C6 C 1.1919(2) 0.61802(13) 0.28033(13) 0.0180(2) Uani 1 1 d . . . H6 H 1.338(4) 0.5871(19) 0.2413(18) 0.032(5) Uiso 1 1 d . . . O11A O -0.0999(5) 0.2008(3) 0.0000(2) 0.0363(6) Uani 0.50 1 d P . . O11B O -0.0875(12) 0.0884(6) 0.0701(6) 0.0329(12) Uani 0.25 1 d P . . O11C O -0.1637(10) 0.0972(5) 0.0267(5) 0.0251(10) Uani 0.25 1 d P . . H11A H -0.060(9) 0.119(5) 0.011(4) 0.097(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 S1 0.01312(12) 0.00987(13) 0.01553(14) -0.00595(10) -0.00455(10) 0.00077(9) S2 0.01070(12) 0.01254(14) 0.01380(14) -0.00740(10) -0.00296(9) 0.00093(9) Na1 0.0147(3) 0.0173(4) 0.0142(3) -0.0048(3) -0.0033(3) 0.0002(3) Na2 0.0191(3) 0.0147(3) 0.0192(4) -0.0079(3) -0.0065(3) 0.0006(3) Na3 0.0204(2) 0.0164(3) 0.0219(3) -0.0050(2) -0.0075(2) -0.0003(2) O1 0.0230(4) 0.0167(5) 0.0228(5) -0.0077(4) 0.0016(4) -0.0057(4) O2 0.0250(4) 0.0139(4) 0.0217(5) -0.0073(3) -0.0132(4) 0.0017(4) O3 0.0168(4) 0.0148(4) 0.0237(5) -0.0095(4) -0.0067(3) 0.0051(3) O4 0.0194(4) 0.0120(4) 0.0151(4) -0.0028(3) -0.0001(3) -0.0019(3) O5 0.0166(4) 0.0176(4) 0.0164(4) -0.0077(3) 0.0012(3) -0.0024(3) O6 0.0176(4) 0.0148(4) 0.0239(5) -0.0123(4) -0.0027(3) 0.0004(3) O7 0.0130(4) 0.0259(5) 0.0193(5) -0.0118(4) -0.0069(3) 0.0047(3) O8 0.0339(8) 0.0679(11) 0.0450(9) -0.0371(8) 0.0036(7) 0.0019(7) O9 0.0170(4) 0.0137(5) 0.0268(5) -0.0076(4) -0.0066(4) 0.0005(4) O10 0.0180(4) 0.0189(5) 0.0208(5) -0.0065(4) -0.0012(4) -0.0009(4) N1 0.0132(4) 0.0186(5) 0.0286(6) -0.0153(5) -0.0019(4) 0.0001(4) N2 0.0153(4) 0.0112(5) 0.0130(5) -0.0055(4) -0.0028(4) -0.0010(4) C2 0.0130(5) 0.0117(5) 0.0152(5) -0.0073(4) -0.0037(4) 0.0007(4) C3 0.0136(5) 0.0149(6) 0.0217(6) -0.0105(5) -0.0001(4) -0.0001(4) C4 0.0140(5) 0.0148(6) 0.0188(6) -0.0077(4) -0.0007(4) -0.0012(4) C5 0.0136(5) 0.0123(5) 0.0137(5) -0.0063(4) -0.0055(4) 0.0011(4) C6 0.0125(5) 0.0190(6) 0.0280(7) -0.0157(5) -0.0021(5) 0.0001(4) O11A 0.0304(12) 0.0432(16) 0.0356(14) -0.0187(12) 0.0003(10) 0.0027(11) O11B 0.030(3) 0.037(3) 0.034(3) -0.022(3) 0.008(3) -0.009(2) O11C 0.024(2) 0.031(3) 0.019(2) -0.011(2) -0.001(2) 0.0077(19) _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 O1 1.4642(10) . ? S1 O3 1.4744(9) . ? S1 O2 1.4842(10) . ? S1 C2 1.8049(12) . ? S2 O5 1.4594(9) . ? S2 O7 1.4640(9) . ? S2 O6 1.4742(9) . ? S2 N2 1.7424(11) . ? Na1 O5 2.3625(9) 2_765 ? Na1 O5 2.3625(9) 1_455 ? Na1 O7 2.3952(9) . ? Na1 O7 2.3952(9) 2_665 ? Na1 O10 2.3996(10) 2_665 ? Na1 O10 2.3996(10) . ? Na1 Na3 4.0333(5) 2_565 ? Na1 Na3 4.0333(5) 1_655 ? Na1 H10B 2.64(2) . ? Na2 O9 2.4098(10) . ? Na2 O9 2.4098(10) 2_656 ? Na2 O2 2.4238(9) 2_766 ? Na2 O2 2.4238(9) 1_445 ? Na2 O3 2.5017(9) 2_666 ? Na2 O3 2.5018(9) 1_545 ? Na2 Na3 3.4662(6) 2_556 ? Na2 Na3 3.4662(6) 1_655 ? Na3 O11B 2.222(5) . ? Na3 O3 2.4005(10) 1_445 ? Na3 O10 2.4098(11) 1_455 ? Na3 O11A 2.464(3) . ? Na3 O11C 2.465(6) . ? Na3 O6 2.4761(11) 1_455 ? Na3 O9 2.4780(12) 1_455 ? Na3 O1 2.4991(11) 1_345 ? Na3 Na2 3.4662(6) 1_455 ? Na3 Na1 4.0333(5) 1_455 ? O1 Na3 2.4992(11) 1_765 ? O2 Na2 2.4238(9) 1_665 ? O3 Na3 2.4004(10) 1_665 ? O3 Na2 2.5018(9) 1_565 ? O4 N2 1.4530(13) . ? O4 H4 0.80(2) . ? O5 Na1 2.3625(9) 1_655 ? O6 Na3 2.4761(11) 1_655 ? O8 H8A 0.96(3) . ? O8 H8B 0.60(3) . ? O9 Na3 2.4780(12) 1_655 ? O9 H9A 0.78(3) . ? O9 H9B 0.79(3) . ? O10 Na3 2.4098(11) 1_655 ? O10 H10A 0.89(2) . ? O10 H10B 0.78(3) . ? N1 C6 1.3525(17) . ? N1 C2 1.3523(16) . ? N2 C5 1.4512(15) . ? C2 C3 1.3989(17) . ? C3 C4 1.4064(18) . ? C3 H3 1.002(19) . ? C4 C5 1.4002(17) . ? C4 H4 0.97(2) . ? C5 C6 1.4122(17) . ? C6 H6 0.99(2) . ? O11A O11C 1.154(7) . ? O11A O11B 1.256(8) . ? O11A H11A 0.93(5) . ? O11B O11C 0.716(7) . ? O11B H11A 0.68(5) . ? O11C H11A 0.59(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 S1 O3 114.04(6) . . ? O1 S1 O2 112.64(6) . . ? O3 S1 O2 112.38(6) . . ? O1 S1 C2 107.28(6) . . ? O3 S1 C2 105.37(5) . . ? O2 S1 C2 104.21(5) . . ? O5 S2 O7 114.99(6) . . ? O5 S2 O6 114.60(5) . . ? O7 S2 O6 112.78(6) . . ? O5 S2 N2 103.52(5) . . ? O7 S2 N2 107.17(5) . . ? O6 S2 N2 102.12(5) . . ? O5 Na1 O5 180.0 2_765 1_455 ? O5 Na1 O7 96.20(3) 2_765 . ? O5 Na1 O7 83.80(3) 1_455 . ? O5 Na1 O7 83.80(3) 2_765 2_665 ? O5 Na1 O7 96.20(3) 1_455 2_665 ? O7 Na1 O7 180.0 . 2_665 ? O5 Na1 O10 88.89(3) 2_765 2_665 ? O5 Na1 O10 91.11(3) 1_455 2_665 ? O7 Na1 O10 88.35(4) . 2_665 ? O7 Na1 O10 91.65(4) 2_665 2_665 ? O5 Na1 O10 91.11(3) 2_765 . ? O5 Na1 O10 88.89(3) 1_455 . ? O7 Na1 O10 91.65(4) . . ? O7 Na1 O10 88.35(4) 2_665 . ? O10 Na1 O10 180.0 2_665 . ? O5 Na1 Na3 98.63(2) 2_765 2_565 ? O5 Na1 Na3 81.37(2) 1_455 2_565 ? O7 Na1 Na3 118.32(3) . 2_565 ? O7 Na1 Na3 61.68(3) 2_665 2_565 ? O10 Na1 Na3 33.08(3) 2_665 2_565 ? O10 Na1 Na3 146.92(3) . 2_565 ? O5 Na1 Na3 81.37(2) 2_765 1_655 ? O5 Na1 Na3 98.63(2) 1_455 1_655 ? O7 Na1 Na3 61.68(3) . 1_655 ? O7 Na1 Na3 118.32(3) 2_665 1_655 ? O10 Na1 Na3 146.92(3) 2_665 1_655 ? O10 Na1 Na3 33.08(3) . 1_655 ? Na3 Na1 Na3 180.0 2_565 1_655 ? O5 Na1 H10B 108.1(6) 2_765 . ? O5 Na1 H10B 71.9(6) 1_455 . ? O7 Na1 H10B 90.7(6) . . ? O7 Na1 H10B 89.3(6) 2_665 . ? O10 Na1 H10B 163.0(6) 2_665 . ? O10 Na1 H10B 17.0(6) . . ? Na3 Na1 H10B 138.1(6) 2_565 . ? Na3 Na1 H10B 41.9(6) 1_655 . ? O9 Na2 O9 180.0 . 2_656 ? O9 Na2 O2 92.52(3) . 2_766 ? O9 Na2 O2 87.48(3) 2_656 2_766 ? O9 Na2 O2 87.48(3) . 1_445 ? O9 Na2 O2 92.52(3) 2_656 1_445 ? O2 Na2 O2 179.999(2) 2_766 1_445 ? O9 Na2 O3 92.44(3) . 2_666 ? O9 Na2 O3 87.56(3) 2_656 2_666 ? O2 Na2 O3 93.29(3) 2_766 2_666 ? O2 Na2 O3 86.71(3) 1_445 2_666 ? O9 Na2 O3 87.56(3) . 1_545 ? O9 Na2 O3 92.44(3) 2_656 1_545 ? O2 Na2 O3 86.71(3) 2_766 1_545 ? O2 Na2 O3 93.29(3) 1_445 1_545 ? O3 Na2 O3 180.0 2_666 1_545 ? O9 Na2 Na3 134.37(3) . 2_556 ? O9 Na2 Na3 45.63(3) 2_656 2_556 ? O2 Na2 Na3 80.35(3) 2_766 2_556 ? O2 Na2 Na3 99.65(3) 1_445 2_556 ? O3 Na2 Na3 43.83(2) 2_666 2_556 ? O3 Na2 Na3 136.17(2) 1_545 2_556 ? O9 Na2 Na3 45.64(3) . 1_655 ? O9 Na2 Na3 134.37(3) 2_656 1_655 ? O2 Na2 Na3 99.65(3) 2_766 1_655 ? O2 Na2 Na3 80.35(3) 1_445 1_655 ? O3 Na2 Na3 136.17(2) 2_666 1_655 ? O3 Na2 Na3 43.83(2) 1_545 1_655 ? Na3 Na2 Na3 180.0 2_556 1_655 ? O11B Na3 O3 86.7(2) . 1_445 ? O11B Na3 O10 95.6(2) . 1_455 ? O3 Na3 O10 172.35(4) 1_445 1_455 ? O11B Na3 O11A 30.5(2) . . ? O3 Na3 O11A 112.87(7) 1_445 . ? O10 Na3 O11A 71.57(7) 1_455 . ? O11B Na3 O11C 16.56(19) . . ? O3 Na3 O11C 100.57(14) 1_445 . ? O10 Na3 O11C 80.71(14) 1_455 . ? O11A Na3 O11C 27.08(15) . . ? O11B Na3 O6 96.09(17) . 1_455 ? O3 Na3 O6 83.81(4) 1_445 1_455 ? O10 Na3 O6 103.14(4) 1_455 1_455 ? O11A Na3 O6 83.58(7) . 1_455 ? O11C Na3 O6 106.43(15) . 1_455 ? O11B Na3 O9 174.8(2) . 1_455 ? O3 Na3 O9 88.32(4) 1_445 1_455 ? O10 Na3 O9 89.48(4) 1_455 1_455 ? O11A Na3 O9 152.82(8) . 1_455 ? O11C Na3 O9 168.26(15) . 1_455 ? O6 Na3 O9 81.97(4) 1_455 1_455 ? O11B Na3 O1 100.82(16) . 1_345 ? O3 Na3 O1 93.69(4) 1_445 1_345 ? O10 Na3 O1 78.72(4) 1_455 1_345 ? O11A Na3 O1 112.92(7) . 1_345 ? O11C Na3 O1 90.81(15) . 1_345 ? O6 Na3 O1 162.75(4) 1_455 1_345 ? O9 Na3 O1 80.89(4) 1_455 1_345 ? O11B Na3 Na2 131.5(2) . 1_455 ? O3 Na3 Na2 46.20(2) 1_445 1_455 ? O10 Na3 Na2 129.51(3) 1_455 1_455 ? O11A Na3 Na2 158.92(7) . 1_455 ? O11C Na3 Na2 141.61(13) . 1_455 ? O6 Na3 Na2 90.46(3) 1_455 1_455 ? O9 Na3 Na2 44.05(3) 1_455 1_455 ? O1 Na3 Na2 75.79(3) 1_345 1_455 ? O11B Na3 Na1 102.19(19) . 1_455 ? O3 Na3 Na1 153.35(3) 1_445 1_455 ? O10 Na3 Na1 32.93(3) 1_455 1_455 ? O11A Na3 Na1 71.78(7) . 1_455 ? O11C Na3 Na1 93.27(13) . 1_455 ? O6 Na3 Na1 70.40(3) 1_455 1_455 ? O9 Na3 Na1 81.71(3) 1_455 1_455 ? O1 Na3 Na1 108.89(3) 1_345 1_455 ? Na2 Na3 Na1 125.059(16) 1_455 1_455 ? S1 O1 Na3 134.73(6) . 1_765 ? S1 O2 Na2 129.69(6) . 1_665 ? S1 O3 Na3 130.89(6) . 1_665 ? S1 O3 Na2 138.56(6) . 1_565 ? Na3 O3 Na2 89.97(3) 1_665 1_565 ? N2 O4 H4 106.8(14) . . ? S2 O5 Na1 136.06(6) . 1_655 ? S2 O6 Na3 126.74(5) . 1_655 ? S2 O7 Na1 123.49(5) . . ? H8A O8 H8B 88(3) . . ? Na2 O9 Na3 90.32(4) . 1_655 ? Na2 O9 H9A 127.6(18) . . ? Na3 O9 H9A 106.1(17) 1_655 . ? Na2 O9 H9B 121.9(18) . . ? Na3 O9 H9B 111.1(17) 1_655 . ? H9A O9 H9B 98(2) . . ? Na1 O10 Na3 113.99(4) . 1_655 ? Na1 O10 H10A 126.4(14) . . ? Na3 O10 H10A 105.1(14) 1_655 . ? Na1 O10 H10B 99.0(18) . . ? Na3 O10 H10B 104.9(19) 1_655 . ? H10A O10 H10B 105(2) . . ? C6 N1 C2 117.57(11) . . ? C5 N2 O4 109.11(9) . . ? C5 N2 S2 114.15(8) . . ? O4 N2 S2 105.92(7) . . ? N1 C2 C3 124.02(11) . . ? N1 C2 S1 115.80(9) . . ? C3 C2 S1 120.07(9) . . ? C2 C3 C4 118.12(11) . . ? C2 C3 H3 120.1(11) . . ? C4 C3 H3 121.8(11) . . ? C5 C4 C3 118.68(11) . . ? C5 C4 H4 120.3(12) . . ? C3 C4 H4 121.0(12) . . ? C4 C5 C6 119.08(11) . . ? C4 C5 N2 122.75(11) . . ? C6 C5 N2 118.15(10) . . ? N1 C6 C5 122.52(11) . . ? N1 C6 H6 115.5(12) . . ? C5 C6 H6 121.9(12) . . ? O11C O11A O11B 34.3(3) . . ? O11C O11A Na3 76.5(3) . . ? O11B O11A Na3 64.0(3) . . ? O11C O11A H11A 30(3) . . ? O11B O11A H11A 32(3) . . ? Na3 O11A H11A 95(3) . . ? O11C O11B O11A 65.1(7) . . ? O11C O11B Na3 101.3(7) . . ? O11A O11B Na3 85.5(3) . . ? O11C O11B H11A 50(4) . . ? O11A O11B H11A 46(4) . . ? Na3 O11B H11A 129(4) . . ? O11B O11C O11A 80.7(8) . . ? O11B O11C Na3 62.1(7) . . ? O11A O11C Na3 76.4(3) . . ? O11B O11C H11A 62(5) . . ? O11A O11C H11A 53(5) . . ? Na3 O11C H11A 108(5) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.506 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.071