# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name R.G.Raptis G.Mezei _publ_contact_author_name 'Dr Raphael G. Raptis' _publ_contact_author_address ; University of Puerto Rico P.O.Box 23346 San Juan Puerto Rico 00931-3346 UNITED STATES OF AMERICA ; _publ_contact_author_email RAPHAEL@ADAM.UPRR.PR _publ_section_title ; Pyrazole-4-sulphonate networks of alkali and alkaline-earth metals. Effect of cation size, charge, H-bonding and aromatic interactions on the three-dimensional supramolecular architecture ; data_4-SO3-pzH2 _database_code_CSD 201504 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H4 N2 O3 S' _chemical_formula_weight 148.14 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z+1/2' 'y, -x, z+1/2' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z-1/2' '-y, x, -z-1/2' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 10.8630(11) _cell_length_b 10.8630(11) _cell_length_c 9.1947(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1085.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 4250 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 23.23 _reflns_number_total 417 _reflns_number_gt 395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0425P)^2^+0.5675P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.047(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 417 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.23972(6) 0.52436(6) 1.0000 0.0256(3) Uani 1 2 d S . . O2 O 0.16815(11) 0.54506(11) 0.86886(13) 0.0338(5) Uani 1 1 d . . . O1 O 0.30581(18) 0.40989(17) 1.0000 0.0385(6) Uani 1 2 d S . . N1 N 0.48162(15) 0.78213(14) 0.92686(19) 0.0352(5) Uani 1 1 d . . . H1N H 0.5257 0.8291 0.8725 0.042 Uiso 1 1 calc R . . C2 C 0.3506(2) 0.6422(2) 1.0000 0.0274(6) Uani 1 2 d S . . C1 C 0.40279(17) 0.69827(17) 0.8802(2) 0.0320(5) Uani 1 1 d . . . H1C H 0.3855 0.6802 0.7834 0.038 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 S1 0.0254(4) 0.0265(5) 0.0249(5) 0.000 0.000 0.0007(2) O2 0.0332(7) 0.0416(8) 0.0266(8) -0.0044(5) -0.0037(6) 0.0020(5) O1 0.0368(11) 0.0282(11) 0.0505(12) 0.000 0.000 0.0041(8) N1 0.0347(10) 0.0320(9) 0.0389(10) 0.0048(8) 0.0045(7) -0.0044(7) C2 0.0276(13) 0.0283(13) 0.0264(12) 0.000 0.000 0.0033(11) C1 0.0340(10) 0.0336(10) 0.0283(9) -0.0002(8) 0.0004(8) -0.0014(8) _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 1.436(2) . ? S1 O2 1.4522(13) . ? S1 O2 1.4522(13) 10_557 ? S1 C2 1.758(3) . ? N1 C1 1.322(2) . ? N1 N1 1.345(4) 10_557 ? C2 C1 1.381(2) 10_557 ? C2 C1 1.381(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 O1 S1 O2 113.69(7) . . ? O1 S1 O2 113.69(7) . 10_557 ? O2 S1 O2 112.26(11) . 10_557 ? O1 S1 C2 106.74(11) . . ? O2 S1 C2 104.72(7) . . ? O2 S1 C2 104.72(7) 10_557 . ? C1 N1 N1 108.96(11) . 10_557 ? C1 C2 C1 105.9(2) 10_557 . ? C1 C2 S1 127.05(11) 10_557 . ? C1 C2 S1 127.05(11) . . ? N1 C1 C2 108.09(18) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.277 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.048 data_Na(4-SO3-pzH).2H2O _database_code_CSD 201505 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H7 N2 Na O5 S' _chemical_formula_weight 206.16 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' N N 0.0061 0.0033 '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' _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 9.979(3) _cell_length_b 7.848(3) _cell_length_c 20.583(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1612.0(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 6373 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 23.30 _reflns_number_total 1163 _reflns_number_gt 1101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0488P)^2^+1.2070P] 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 1163 _refine_ls_number_parameters 113 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 S1 S 0.45291(5) 0.05603(7) 0.38549(3) 0.0255(2) Uani 1 1 d . . . Na1 Na 0.16154(8) -0.08326(11) 0.47939(4) 0.0313(3) Uani 1 1 d . . . O1 O 0.36491(16) -0.0545(2) 0.42171(8) 0.0367(4) Uani 1 1 d . . . O3 O 0.58926(16) -0.0106(3) 0.38212(7) 0.0404(5) Uani 1 1 d . . . O5 O 0.00666(17) 0.1151(2) 0.43370(8) 0.0349(4) Uani 1 1 d D . . O4 O 0.22474(15) 0.1827(2) 0.53694(8) 0.0354(4) Uani 1 1 d D . . C2 C 0.3944(2) 0.0526(3) 0.30567(10) 0.0260(5) Uani 1 1 d . . . C1 C 0.2823(2) -0.0280(3) 0.28302(11) 0.0354(6) Uani 1 1 d . . . H1 H 0.2209 -0.0902 0.3074 0.042 Uiso 1 1 calc R . . O2 O 0.45081(18) 0.2311(2) 0.40650(9) 0.0481(5) Uani 1 1 d . . . N2 N 0.2783(2) 0.0000(3) 0.21898(10) 0.0435(6) Uani 1 1 d . . . H2 H 0.2165 -0.0391 0.1940 0.052 Uiso 1 1 calc R . . N1 N 0.3809(2) 0.0957(3) 0.19775(9) 0.0440(6) Uani 1 1 d . . . C3 C 0.4514(2) 0.1278(3) 0.25073(11) 0.0361(6) Uani 1 1 d . . . H3 H 0.5294 0.1926 0.2513 0.043 Uiso 1 1 calc R . . H4A H 0.1637 0.2157 0.5600 0.056(9) Uiso 1 1 d RD . . H5A H 0.0535 0.2040 0.4316 0.063(10) Uiso 1 1 d RD . . H4B H 0.2790 0.1480 0.5620 0.072(11) Uiso 1 1 d RD . . H5B H -0.0366 0.1102 0.3985 0.060(10) Uiso 1 1 d RD . . 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 0.0233(3) 0.0288(4) 0.0243(3) 0.0003(2) 0.0023(2) -0.0006(2) Na1 0.0291(5) 0.0322(5) 0.0327(5) 0.0015(4) 0.0039(4) 0.0012(4) O1 0.0307(8) 0.0435(10) 0.0358(9) 0.0089(7) 0.0096(7) -0.0017(7) O3 0.0234(9) 0.0664(12) 0.0314(9) 0.0097(8) 0.0017(7) 0.0074(9) O5 0.0381(9) 0.0345(9) 0.0322(9) 0.0041(7) -0.0055(7) -0.0024(8) O4 0.0294(9) 0.0422(10) 0.0346(9) 0.0017(7) -0.0012(8) 0.0045(7) C2 0.0249(12) 0.0237(11) 0.0293(12) 0.0003(9) -0.0004(9) 0.0034(9) C1 0.0287(13) 0.0415(14) 0.0359(13) 0.0005(11) -0.0016(10) -0.0042(11) O2 0.0666(12) 0.0363(10) 0.0413(11) -0.0122(8) 0.0026(9) -0.0055(9) N2 0.0323(12) 0.0624(15) 0.0357(11) -0.0062(11) -0.0093(9) -0.0030(11) N1 0.0393(12) 0.0619(14) 0.0309(12) 0.0060(10) -0.0016(9) 0.0030(11) C3 0.0302(13) 0.0447(14) 0.0334(13) 0.0065(11) 0.0012(10) -0.0010(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 S1 O2 1.4407(19) . ? S1 O1 1.4418(16) . ? S1 O3 1.4593(18) . ? S1 C2 1.744(2) . ? Na1 O1 2.3620(18) . ? Na1 O2 2.373(2) 8_655 ? Na1 O5 2.3866(19) . ? Na1 O4 2.4627(19) 8_655 ? Na1 O5 2.4658(19) 5_556 ? Na1 O4 2.482(2) . ? Na1 Na1 3.5809(19) 5_556 ? O5 Na1 2.4658(19) 5_556 ? O4 Na1 2.4627(19) 8_665 ? C2 C1 1.366(3) . ? C2 C3 1.397(3) . ? C1 N2 1.337(3) . ? O2 Na1 2.373(2) 8_665 ? N2 N1 1.343(3) . ? N1 C3 1.322(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 O2 S1 O1 114.18(10) . . ? O2 S1 O3 111.69(12) . . ? O1 S1 O3 112.15(11) . . ? O2 S1 C2 107.02(11) . . ? O1 S1 C2 105.89(10) . . ? O3 S1 C2 105.18(10) . . ? O1 Na1 O2 98.45(7) . 8_655 ? O1 Na1 O5 107.22(7) . . ? O2 Na1 O5 81.10(7) 8_655 . ? O1 Na1 O4 85.25(6) . 8_655 ? O2 Na1 O4 93.67(7) 8_655 8_655 ? O5 Na1 O4 167.00(7) . 8_655 ? O1 Na1 O5 163.58(7) . 5_556 ? O2 Na1 O5 94.29(7) 8_655 5_556 ? O5 Na1 O5 84.90(6) . 5_556 ? O4 Na1 O5 83.64(6) 8_655 5_556 ? O1 Na1 O4 86.62(6) . . ? O2 Na1 O4 159.78(7) 8_655 . ? O5 Na1 O4 78.70(6) . . ? O4 Na1 O4 106.30(6) 8_655 . ? O5 Na1 O4 84.94(6) 5_556 . ? O1 Na1 Na1 149.07(6) . 5_556 ? O2 Na1 Na1 87.04(6) 8_655 5_556 ? O5 Na1 Na1 43.30(4) . 5_556 ? O4 Na1 Na1 124.97(6) 8_655 5_556 ? O5 Na1 Na1 41.59(4) 5_556 5_556 ? O4 Na1 Na1 78.97(5) . 5_556 ? S1 O1 Na1 147.22(11) . . ? Na1 O5 Na1 95.10(6) . 5_556 ? Na1 O4 Na1 120.98(7) 8_665 . ? C1 C2 C3 104.6(2) . . ? C1 C2 S1 127.06(18) . . ? C3 C2 S1 128.30(17) . . ? N2 C1 C2 106.6(2) . . ? S1 O2 Na1 141.46(12) . 8_665 ? C1 N2 N1 112.9(2) . . ? C3 N1 N2 104.12(19) . . ? N1 C3 C2 111.7(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.280 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.078 data_K(4-SO3-pzH).H2O _database_code_CSD 201506 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H5 K N2 O4 S' _chemical_formula_weight 204.25 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' K K 0.2009 0.2494 '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 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 8.1743(12) _cell_length_b 8.9723(13) _cell_length_c 19.912(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1460.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 5775 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1047 _reflns_number_gt 864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.1150P)^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 1047 _refine_ls_number_parameters 108 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _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 C1 C 0.0710(5) 0.3290(5) 0.4829(2) 0.0299(10) Uani 1 1 d . . . H1 H -0.0203 0.2679 0.4785 0.036 Uiso 1 1 calc R . . C2 C 0.1581(4) 0.3945(4) 0.4317(2) 0.0189(9) Uani 1 1 d . . . C3 C 0.2815(5) 0.4764(5) 0.4640(2) 0.0286(10) Uani 1 1 d . . . H3 H 0.3588 0.5344 0.4418 0.034 Uiso 1 1 calc R . . H1O H 0.128(5) 0.422(4) 0.1163(17) 0.039(14) Uiso 1 1 d D . . H2O H 0.015(4) 0.393(8) 0.159(3) 0.10(3) Uiso 1 1 d D . . K1 K 0.25773(10) 0.13997(10) 0.22742(5) 0.0251(4) Uani 1 1 d . . . N1 N 0.2733(4) 0.4604(5) 0.53049(17) 0.0369(10) Uani 1 1 d . . . N2 N 0.1422(4) 0.3699(4) 0.53981(19) 0.0343(10) Uani 1 1 d . . . H2 H 0.1087 0.3418 0.5788 0.041 Uiso 1 1 calc R . . O1 O 0.2737(3) 0.3919(3) 0.31255(15) 0.0278(8) Uani 1 1 d . . . O2 O 0.0292(3) 0.2501(3) 0.33470(14) 0.0365(8) Uani 1 1 d . . . O3 O 0.0186(3) 0.5196(3) 0.33028(13) 0.0338(8) Uani 1 1 d . . . O4 O 0.1093(4) 0.3697(4) 0.14922(18) 0.0400(9) Uani 1 1 d D . . S1 S 0.11498(11) 0.38837(11) 0.34587(5) 0.0203(4) Uani 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 C1 0.033(2) 0.028(2) 0.029(2) 0.0008(19) 0.0002(18) -0.004(2) C2 0.0169(19) 0.019(2) 0.021(2) -0.0017(15) -0.0043(17) 0.0016(14) C3 0.023(2) 0.033(3) 0.029(2) -0.0035(19) 0.0005(17) -0.0009(18) K1 0.0193(7) 0.0299(7) 0.0261(7) 0.0003(3) -0.0008(3) -0.0025(4) N1 0.032(2) 0.047(3) 0.031(2) -0.0062(18) -0.0073(16) 0.0027(18) N2 0.035(2) 0.047(3) 0.021(2) 0.0036(16) 0.0025(16) 0.0010(17) O1 0.0207(15) 0.0405(19) 0.0221(16) -0.0006(12) 0.0018(12) 0.0028(11) O2 0.0361(17) 0.0396(18) 0.0337(17) -0.0093(13) -0.0064(13) -0.0138(15) O3 0.0323(17) 0.0406(18) 0.0285(16) 0.0066(13) -0.0033(13) 0.0152(14) O4 0.028(2) 0.056(2) 0.037(2) 0.0138(16) 0.0079(15) 0.0042(15) S1 0.0159(7) 0.0253(7) 0.0196(7) -0.0018(4) -0.0029(4) 0.0011(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 C1 N2 1.326(6) . ? C1 C2 1.375(6) . ? C2 C3 1.403(5) . ? C2 S1 1.746(4) . ? C3 N1 1.334(5) . ? K1 O2 2.726(3) 6_656 ? K1 O3 2.755(3) 3_545 ? K1 O1 2.810(3) 8_655 ? K1 O1 2.828(3) . ? K1 O4 2.854(4) . ? K1 O3 2.950(3) 8_655 ? K1 O2 3.005(3) . ? K1 O4 3.080(4) 8_655 ? K1 S1 3.4267(13) 8_655 ? K1 S1 3.4484(13) . ? K1 K1 4.1849(7) 6_656 ? K1 K1 4.1849(7) 6_556 ? N1 N2 1.358(5) . ? O1 S1 1.458(3) . ? O1 K1 2.810(3) 8_665 ? O2 S1 1.442(3) . ? O2 K1 2.726(3) 6_556 ? O3 S1 1.450(3) . ? O3 K1 2.755(3) 3 ? O3 K1 2.950(3) 8_665 ? O4 K1 3.080(4) 8_665 ? S1 K1 3.4267(13) 8_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 106.7(4) . . ? C1 C2 C3 104.9(4) . . ? C1 C2 S1 127.4(3) . . ? C3 C2 S1 127.6(3) . . ? N1 C3 C2 111.2(4) . . ? O2 K1 O3 128.35(10) 6_656 3_545 ? O2 K1 O1 129.45(9) 6_656 8_655 ? O3 K1 O1 82.30(9) 3_545 8_655 ? O2 K1 O1 86.82(9) 6_656 . ? O3 K1 O1 126.95(9) 3_545 . ? O1 K1 O1 106.01(10) 8_655 . ? O2 K1 O4 80.60(10) 6_656 . ? O3 K1 O4 72.96(10) 3_545 . ? O1 K1 O4 149.59(9) 8_655 . ? O1 K1 O4 76.68(10) . . ? O2 K1 O3 86.75(8) 6_656 8_655 ? O3 K1 O3 130.86(11) 3_545 8_655 ? O1 K1 O3 49.29(8) 8_655 8_655 ? O1 K1 O3 81.24(8) . 8_655 ? O4 K1 O3 155.04(10) . 8_655 ? O2 K1 O2 135.19(11) 6_656 . ? O3 K1 O2 85.16(8) 3_545 . ? O1 K1 O2 76.98(9) 8_655 . ? O1 K1 O2 48.69(8) . . ? O4 K1 O2 83.46(9) . . ? O3 K1 O2 90.69(9) 8_655 . ? O2 K1 O4 76.63(9) 6_656 8_655 ? O3 K1 O4 76.69(9) 3_545 8_655 ? O1 K1 O4 73.35(9) 8_655 8_655 ? O1 K1 O4 156.33(9) . 8_655 ? O4 K1 O4 116.28(13) . 8_655 ? O3 K1 O4 81.03(9) 8_655 8_655 ? O2 K1 O4 146.89(9) . 8_655 ? O2 K1 S1 107.69(7) 6_656 8_655 ? O3 K1 S1 106.13(7) 3_545 8_655 ? O1 K1 S1 24.58(6) 8_655 8_655 ? O1 K1 S1 95.73(6) . 8_655 ? O4 K1 S1 168.65(8) . 8_655 ? O3 K1 S1 24.88(6) 8_655 8_655 ? O2 K1 S1 85.19(6) . 8_655 ? O4 K1 S1 73.87(7) 8_655 8_655 ? O2 K1 S1 110.58(7) 6_656 . ? O3 K1 S1 105.14(7) 3_545 . ? O1 K1 S1 93.92(7) 8_655 . ? O1 K1 S1 24.39(6) . . ? O4 K1 S1 76.27(8) . . ? O3 K1 S1 88.36(6) 8_655 . ? O2 K1 S1 24.61(6) . . ? O4 K1 S1 166.91(7) 8_655 . ? S1 K1 S1 93.31(3) 8_655 . ? O2 K1 K1 45.77(6) 6_656 6_656 ? O3 K1 K1 152.93(7) 3_545 6_656 ? O1 K1 K1 87.69(6) 8_655 6_656 ? O1 K1 K1 79.98(6) . 6_656 ? O4 K1 K1 122.17(7) . 6_656 ? O3 K1 K1 41.03(5) 8_655 6_656 ? O2 K1 K1 117.02(6) . 6_656 ? O4 K1 K1 76.35(7) 8_655 6_656 ? S1 K1 K1 63.61(3) 8_655 6_656 ? S1 K1 K1 100.57(3) . 6_656 ? O2 K1 K1 153.20(7) 6_656 6_556 ? O3 K1 K1 44.66(6) 3_545 6_556 ? O1 K1 K1 77.35(6) 8_655 6_556 ? O1 K1 K1 85.20(6) . 6_556 ? O4 K1 K1 72.67(7) . 6_556 ? O3 K1 K1 117.13(6) 8_655 6_556 ? O2 K1 K1 40.55(5) . 6_556 ? O4 K1 K1 116.95(7) 8_655 6_556 ? S1 K1 K1 98.55(3) 8_655 6_556 ? S1 K1 K1 61.48(3) . 6_556 ? K1 K1 K1 155.18(5) 6_656 6_556 ? C3 N1 N2 103.9(3) . . ? C1 N2 N1 113.3(4) . . ? S1 O1 K1 102.14(13) . 8_665 ? S1 O1 K1 102.37(15) . . ? K1 O1 K1 105.50(10) 8_665 . ? S1 O2 K1 141.04(18) . 6_556 ? S1 O2 K1 95.18(14) . . ? K1 O2 K1 93.68(8) 6_556 . ? S1 O3 K1 148.52(18) . 3 ? S1 O3 K1 96.28(13) . 8_665 ? K1 O3 K1 94.31(8) 3 8_665 ? K1 O4 K1 98.21(11) . 8_665 ? O2 S1 O3 113.67(19) . . ? O2 S1 O1 112.41(17) . . ? O3 S1 O1 111.62(17) . . ? O2 S1 C2 106.04(17) . . ? O3 S1 C2 107.08(17) . . ? O1 S1 C2 105.37(18) . . ? O2 S1 K1 127.45(12) . 8_665 ? O3 S1 K1 58.85(12) . 8_665 ? O1 S1 K1 53.28(11) . 8_665 ? C2 S1 K1 126.28(13) . 8_665 ? O2 S1 K1 60.20(12) . . ? O3 S1 K1 124.20(12) . . ? O1 S1 K1 53.24(12) . . ? C2 S1 K1 128.42(13) . . ? K1 S1 K1 81.50(3) 8_665 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.302 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.162 data_Ca(4-SO3-pzH)2.3H2O _database_code_CSD 201507 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H12 Ca N4 O9 S2' _chemical_formula_weight 388.40 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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 5.9972(6) _cell_length_b 9.2102(9) _cell_length_c 12.9567(13) _cell_angle_alpha 76.536(2) _cell_angle_beta 89.264(2) _cell_angle_gamma 79.057(2) _cell_volume 682.98(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 3005 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1965 _reflns_number_gt 1833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0665P)^2^+0.3929P] 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 1965 _refine_ls_number_parameters 205 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _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 Ca1 Ca 0.17844(8) 0.06194(5) 0.69860(4) 0.01917(19) Uani 1 1 d . . . S1 S 0.07168(10) 0.76859(6) 0.55850(5) 0.0201(2) Uani 1 1 d . . . S2 S -0.14606(10) 0.23417(7) 0.88872(5) 0.0208(2) Uani 1 1 d . . . O1 O 0.0955(3) 0.80872(19) 0.44295(14) 0.0279(4) Uani 1 1 d . . . O2 O -0.1607(3) 0.7646(2) 0.58690(17) 0.0381(5) Uani 1 1 d . . . O3 O 0.1828(3) 0.8614(2) 0.60879(14) 0.0310(4) Uani 1 1 d . . . O4 O -0.1098(3) 0.2121(2) 0.78049(14) 0.0289(4) Uani 1 1 d . . . O5 O 0.0625(3) 0.2258(2) 0.94529(15) 0.0349(5) Uani 1 1 d . . . O6 O -0.2900(3) 0.1333(2) 0.94442(15) 0.0318(5) Uani 1 1 d . . . O7 O 0.0238(3) -0.1345(2) 0.82485(15) 0.0315(5) Uani 1 1 d D . . O8 O 0.4320(3) -0.0162(2) 0.85215(14) 0.0291(4) Uani 1 1 d D . . O9 O 0.5400(3) 0.0243(2) 0.62215(17) 0.0393(5) Uani 1 1 d . . . N1 N 0.2885(4) 0.3280(2) 0.65754(18) 0.0283(5) Uani 1 1 d . . . N2 N 0.4841(4) 0.3812(2) 0.64884(17) 0.0267(5) Uani 1 1 d . . . H2 H 0.6162 0.3238 0.6622 0.032 Uiso 1 1 calc R . . N3 N -0.5988(4) 0.6120(3) 0.86141(19) 0.0359(6) Uani 1 1 d . . . N4 N -0.4005(4) 0.6625(3) 0.8495(2) 0.0419(6) Uani 1 1 d . . . H4A H -0.3912 0.7569 0.8385 0.050 Uiso 1 1 calc R . . C1 C 0.4503(4) 0.5323(3) 0.6173(2) 0.0277(6) Uani 1 1 d . . . H1 H 0.5613 0.5920 0.6074 0.033 Uiso 1 1 calc R . . C2 C 0.2210(4) 0.5826(3) 0.60229(18) 0.0198(5) Uani 1 1 d . . . C3 C 0.1281(4) 0.4519(3) 0.6283(2) 0.0280(6) Uani 1 1 d . . . H3 H -0.0267 0.4514 0.6257 0.034 Uiso 1 1 calc R . . C4 C -0.2202(5) 0.5495(3) 0.8567(2) 0.0373(7) Uani 1 1 d . . . H4 H -0.0687 0.5589 0.8505 0.045 Uiso 1 1 calc R . . H8B H 0.5274 0.0295 0.8719 0.048(10) Uiso 1 1 d R . . H8A H 0.3778 -0.0487 0.9110 0.058(11) Uiso 1 1 d RD . . H7A H -0.0320 -0.1328 0.8858 0.059(11) Uiso 1 1 d R . . H9B H 0.6314 0.0841 0.6010 0.093(16) Uiso 1 1 d R . . H7B H 0.1112 -0.2151 0.8417 0.066(13) Uiso 1 1 d RD . . H9A H 0.6074 -0.0602 0.6156 0.064(12) Uiso 1 1 d R . . C5 C -0.3025(4) 0.4177(3) 0.8748(2) 0.0239(6) Uani 1 1 d . . . C6 C -0.5388(5) 0.4631(3) 0.8773(2) 0.0293(6) Uani 1 1 d . . . H6 H -0.6404 0.3966 0.8886 0.035 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 Ca1 0.0200(3) 0.0151(3) 0.0216(3) -0.0045(2) 0.0012(2) -0.0012(2) S1 0.0210(4) 0.0137(3) 0.0249(4) -0.0047(3) 0.0021(3) -0.0013(3) S2 0.0217(4) 0.0172(4) 0.0226(4) -0.0039(3) 0.0030(3) -0.0024(3) O1 0.0346(10) 0.0214(9) 0.0243(9) -0.0026(7) -0.0024(8) 0.0001(8) O2 0.0238(10) 0.0263(10) 0.0603(14) -0.0059(9) 0.0111(9) -0.0011(8) O3 0.0408(11) 0.0202(9) 0.0345(10) -0.0113(8) -0.0030(8) -0.0057(8) O4 0.0336(10) 0.0237(10) 0.0261(10) -0.0064(8) 0.0068(8) 0.0028(8) O5 0.0266(10) 0.0348(11) 0.0417(11) -0.0085(9) -0.0053(9) -0.0020(8) O6 0.0393(11) 0.0254(10) 0.0319(10) -0.0039(8) 0.0070(8) -0.0130(8) O7 0.0343(11) 0.0267(10) 0.0316(11) -0.0037(8) 0.0057(8) -0.0057(9) O8 0.0301(10) 0.0315(10) 0.0273(10) -0.0068(8) 0.0006(8) -0.0099(8) O9 0.0340(11) 0.0317(11) 0.0565(13) -0.0181(10) 0.0210(10) -0.0088(9) N1 0.0270(12) 0.0180(12) 0.0385(13) -0.0045(10) 0.0017(10) -0.0036(10) N2 0.0199(11) 0.0209(12) 0.0353(13) -0.0044(9) -0.0004(9) 0.0030(9) N3 0.0369(14) 0.0293(14) 0.0370(14) -0.0096(10) 0.0000(11) 0.0072(11) N4 0.0487(16) 0.0186(12) 0.0564(17) -0.0099(11) 0.0010(13) -0.0002(11) C1 0.0240(14) 0.0209(14) 0.0365(15) -0.0023(11) 0.0000(11) -0.0051(11) C2 0.0207(12) 0.0179(13) 0.0210(12) -0.0054(10) 0.0013(10) -0.0034(10) C3 0.0198(13) 0.0183(13) 0.0435(16) -0.0030(11) -0.0006(11) -0.0030(11) C4 0.0309(15) 0.0251(15) 0.0568(19) -0.0119(14) 0.0036(14) -0.0048(13) C5 0.0266(13) 0.0205(14) 0.0244(13) -0.0074(10) 0.0036(10) -0.0020(11) C6 0.0264(14) 0.0298(16) 0.0305(14) -0.0078(12) 0.0021(11) -0.0013(12) _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 Ca1 O9 2.3709(19) . ? Ca1 O3 2.3977(18) 1_545 ? Ca1 O4 2.3991(17) . ? Ca1 O8 2.4051(19) . ? Ca1 O1 2.4080(18) 2_566 ? Ca1 O7 2.4557(19) . ? Ca1 N1 2.593(2) . ? S1 O2 1.4418(19) . ? S1 O3 1.4442(19) . ? S1 O1 1.4681(18) . ? S1 C2 1.742(2) . ? S2 O5 1.4385(19) . ? S2 O6 1.4510(19) . ? S2 O4 1.4706(18) . ? S2 C5 1.741(2) . ? O1 Ca1 2.4080(18) 2_566 ? O3 Ca1 2.3977(18) 1_565 ? N1 C3 1.328(3) . ? N1 N2 1.348(3) . ? N2 C1 1.332(3) . ? N3 C6 1.318(4) . ? N3 N4 1.351(4) . ? N4 C4 1.338(4) . ? C1 C2 1.366(4) . ? C2 C3 1.391(4) . ? C4 C5 1.365(4) . ? C5 C6 1.402(4) . ? 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 O9 Ca1 O3 73.92(7) . 1_545 ? O9 Ca1 O4 150.44(7) . . ? O3 Ca1 O4 134.43(7) 1_545 . ? O9 Ca1 O8 77.63(7) . . ? O3 Ca1 O8 112.06(6) 1_545 . ? O4 Ca1 O8 94.35(6) . . ? O9 Ca1 O1 107.50(7) . 2_566 ? O3 Ca1 O1 80.41(6) 1_545 2_566 ? O4 Ca1 O1 75.56(6) . 2_566 ? O8 Ca1 O1 167.53(6) . 2_566 ? O9 Ca1 O7 125.07(7) . . ? O3 Ca1 O7 74.91(6) 1_545 . ? O4 Ca1 O7 78.08(6) . . ? O8 Ca1 O7 73.81(6) . . ? O1 Ca1 O7 110.43(6) 2_566 . ? O9 Ca1 N1 75.59(7) . . ? O3 Ca1 N1 137.12(7) 1_545 . ? O4 Ca1 N1 75.97(7) . . ? O8 Ca1 N1 89.72(7) . . ? O1 Ca1 N1 80.81(7) 2_566 . ? O7 Ca1 N1 147.97(7) . . ? O2 S1 O3 115.35(12) . . ? O2 S1 O1 111.92(12) . . ? O3 S1 O1 110.66(11) . . ? O2 S1 C2 105.88(11) . . ? O3 S1 C2 106.23(11) . . ? O1 S1 C2 106.08(10) . . ? O5 S2 O6 114.19(12) . . ? O5 S2 O4 112.85(11) . . ? O6 S2 O4 109.99(11) . . ? O5 S2 C5 107.20(12) . . ? O6 S2 C5 105.77(12) . . ? O4 S2 C5 106.23(11) . . ? S1 O1 Ca1 131.10(10) . 2_566 ? S1 O3 Ca1 152.46(12) . 1_565 ? S2 O4 Ca1 134.86(11) . . ? C3 N1 N2 104.2(2) . . ? C3 N1 Ca1 119.67(17) . . ? N2 N1 Ca1 135.85(15) . . ? C1 N2 N1 112.7(2) . . ? C6 N3 N4 104.5(2) . . ? C4 N4 N3 112.6(2) . . ? N2 C1 C2 106.7(2) . . ? C1 C2 C3 105.1(2) . . ? C1 C2 S1 128.53(19) . . ? C3 C2 S1 126.37(19) . . ? N1 C3 C2 111.3(2) . . ? N4 C4 C5 106.5(3) . . ? C4 C5 C6 105.0(2) . . ? C4 C5 S2 127.0(2) . . ? C6 C5 S2 127.9(2) . . ? N3 C6 C5 111.3(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.297 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.084 data_Ba(4-SO3-pzH)2(H2O).H2O _database_code_CSD 201508 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Ba N4 O8 S2' _chemical_formula_weight 467.64 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3856(14) _cell_length_b 4.9098(6) _cell_length_c 24.348(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.702(2) _cell_angle_gamma 90.00 _cell_volume 1361.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 3.270 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2030 _exptl_absorpt_correction_T_max 0.2834 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5491 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1966 _reflns_number_gt 1779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART-NT V5.0' _computing_cell_refinement 'BRUKER SMART-NT V5.0' _computing_data_reduction 'BRUKER SAINT-NT V5/6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL-NT V5.1' _computing_publication_material 'BRUKER SHELXTL-NT V5.1' _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^)+(0.0434P)^2^+0.8279P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0097(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1966 _refine_ls_number_parameters 193 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.262 _refine_ls_shift/su_max 0.003 _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 Ba1 Ba -0.09784(2) -0.00316(4) 0.583315(9) 0.02068(17) Uani 1 1 d . . . S1 S 0.15277(8) 0.4218(2) 0.53527(4) 0.0190(3) Uani 1 1 d . . . S2 S 0.22628(9) 0.0633(2) 0.81777(4) 0.0211(3) Uani 1 1 d . . . O1 O 0.1211(2) 0.1342(6) 0.53127(11) 0.0275(7) Uani 1 1 d . . . O2 O 0.0747(3) 0.5635(6) 0.57265(13) 0.0303(7) Uani 1 1 d . . . O3 O 0.1605(3) 0.5469(6) 0.48143(13) 0.0295(8) Uani 1 1 d . . . O4 O 0.1359(3) -0.0355(6) 0.85458(13) 0.0317(8) Uani 1 1 d . . . O5 O 0.3370(3) -0.0739(7) 0.82581(14) 0.0376(8) Uani 1 1 d . . . O6 O 0.2324(3) 0.3582(6) 0.82034(12) 0.0336(7) Uani 1 1 d . . . O7 O -0.3408(4) 0.0022(7) 0.56843(19) 0.0574(13) Uani 1 1 d . . . O8 O 0.4784(5) 0.0043(7) 0.2771(2) 0.0716(16) Uani 1 1 d D . . N1 N 0.4714(4) 0.6223(13) 0.5819(2) 0.0683(15) Uani 1 1 d . . . N2 N 0.4446(4) 0.4295(10) 0.61860(19) 0.0472(11) Uani 1 1 d . . . H2 H 0.4911 0.3805 0.6449 0.057 Uiso 1 1 calc R . . N3 N 0.0767(4) -0.0023(6) 0.67162(16) 0.0289(10) Uani 1 1 d . . . N4 N 0.1532(3) -0.2120(7) 0.67248(14) 0.0354(9) Uani 1 1 d . . . H4A H 0.1606 -0.3253 0.6458 0.042 Uiso 1 1 calc R . . C1 C 0.3391(4) 0.3219(10) 0.61028(19) 0.0371(11) Uani 1 1 d . . . H1 H 0.3034 0.1884 0.6314 0.044 Uiso 1 1 calc R . . C2 C 0.2926(4) 0.4464(9) 0.56418(18) 0.0259(10) Uani 1 1 d . . . C3 C 0.3783(4) 0.6356(13) 0.5487(2) 0.0589(17) Uani 1 1 d . . . H3 H 0.3709 0.7545 0.5191 0.071 Uiso 1 1 calc R . . H8A H 0.4827 0.1505 0.2615 0.07(2) Uiso 1 1 d RD . . H8B H 0.4234 0.0228 0.2979 0.08(3) Uiso 1 1 d RD . . C4 C 0.2160(4) -0.2256(9) 0.71895(17) 0.0316(11) Uani 1 1 d . . . H4 H 0.2733 -0.3540 0.7278 0.038 Uiso 1 1 calc R . . C5 C 0.1800(4) -0.0146(7) 0.75086(18) 0.0206(10) Uani 1 1 d . . . C6 C 0.0937(4) 0.1192(9) 0.71940(16) 0.0256(9) Uani 1 1 d . . . H6 H 0.0536 0.2739 0.7307 0.031 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 Ba1 0.0213(2) 0.0241(2) 0.0167(2) 0.00034(9) -0.00085(13) 0.00021(9) S1 0.0175(5) 0.0224(5) 0.0171(5) -0.0009(4) -0.0023(4) -0.0008(4) S2 0.0218(6) 0.0246(5) 0.0168(5) -0.0030(4) -0.0012(4) -0.0014(4) O1 0.0311(16) 0.0229(16) 0.0284(16) -0.0018(13) -0.0004(12) -0.0045(13) O2 0.0245(17) 0.0377(16) 0.0285(18) -0.0108(14) -0.0021(13) 0.0047(14) O3 0.0301(18) 0.0347(17) 0.0238(17) 0.0083(13) -0.0034(14) -0.0034(13) O4 0.037(2) 0.0347(19) 0.0234(17) 0.0027(12) 0.0074(14) -0.0037(13) O5 0.0288(18) 0.0474(19) 0.036(2) -0.0092(17) -0.0097(15) 0.0070(16) O6 0.050(2) 0.0236(16) 0.0268(17) -0.0039(13) 0.0013(14) -0.0053(14) O7 0.030(2) 0.081(4) 0.061(3) 0.0224(19) -0.003(2) -0.0050(16) O8 0.063(3) 0.046(3) 0.107(5) -0.004(2) 0.039(3) -0.0053(17) N1 0.034(3) 0.099(4) 0.072(4) 0.018(3) -0.021(2) -0.021(3) N2 0.035(3) 0.068(3) 0.039(3) 0.002(2) -0.016(2) 0.003(2) N3 0.031(2) 0.031(2) 0.024(2) -0.0008(14) -0.0040(18) 0.0031(15) N4 0.048(2) 0.035(2) 0.023(2) -0.0126(16) -0.0086(17) 0.0127(19) C1 0.031(3) 0.048(3) 0.032(3) 0.007(2) -0.007(2) 0.001(2) C2 0.020(2) 0.033(2) 0.025(2) -0.0020(19) -0.0033(18) -0.0003(19) C3 0.036(3) 0.079(4) 0.061(4) 0.026(3) -0.016(3) -0.023(3) C4 0.039(3) 0.035(3) 0.021(2) -0.0039(19) -0.0072(19) 0.011(2) C5 0.021(2) 0.022(2) 0.019(2) -0.0024(16) 0.0007(18) -0.0028(15) C6 0.026(2) 0.026(2) 0.024(2) -0.0014(19) -0.0012(18) 0.0023(18) _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 Ba1 O7 2.785(4) . ? Ba1 O4 2.786(3) 2_556 ? Ba1 O3 2.826(3) 3_566 ? Ba1 O1 2.872(3) 3_556 ? Ba1 O1 2.890(3) . ? Ba1 O6 2.899(3) 2_546 ? Ba1 O2 2.910(3) 1_545 ? Ba1 N3 2.910(4) . ? Ba1 O4 3.053(3) 2_546 ? Ba1 O3 3.177(3) 3_556 ? Ba1 S2 3.5434(11) 2_546 ? Ba1 S1 3.5930(11) 3_556 ? S1 O3 1.451(3) . ? S1 O2 1.457(3) . ? S1 O1 1.460(3) . ? S1 C2 1.737(4) . ? S1 Ba1 3.5930(10) 3_556 ? S2 O5 1.441(3) . ? S2 O6 1.451(3) . ? S2 O4 1.456(3) . ? S2 C5 1.748(4) . ? S2 Ba1 3.5434(11) 2_556 ? O1 Ba1 2.872(3) 3_556 ? O2 Ba1 2.910(3) 1_565 ? O3 Ba1 2.826(3) 3_566 ? O3 Ba1 3.177(3) 3_556 ? O4 Ba1 2.786(3) 2_546 ? O4 Ba1 3.053(3) 2_556 ? O6 Ba1 2.899(3) 2_556 ? N1 C3 1.327(7) . ? N1 N2 1.339(7) . ? N2 C1 1.326(6) . ? N3 C6 1.320(6) . ? N3 N4 1.348(5) . ? N4 C4 1.333(5) . ? C1 C2 1.378(6) . ? C2 C3 1.402(7) . ? C4 C5 1.361(6) . ? C5 C6 1.402(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 O7 Ba1 O4 84.38(11) . 2_556 ? O7 Ba1 O3 71.13(10) . 3_566 ? O4 Ba1 O3 67.02(9) 2_556 3_566 ? O7 Ba1 O1 78.23(11) . 3_556 ? O4 Ba1 O1 134.32(9) 2_556 3_556 ? O3 Ba1 O1 67.42(9) 3_566 3_556 ? O7 Ba1 O1 143.25(11) . . ? O4 Ba1 O1 100.73(9) 2_556 . ? O3 Ba1 O1 77.49(9) 3_566 . ? O1 Ba1 O1 72.32(8) 3_556 . ? O7 Ba1 O6 64.76(11) . 2_546 ? O4 Ba1 O6 70.56(9) 2_556 2_546 ? O3 Ba1 O6 120.36(9) 3_566 2_546 ? O1 Ba1 O6 133.63(8) 3_556 2_546 ? O1 Ba1 O6 151.28(8) . 2_546 ? O7 Ba1 O2 131.75(10) . 1_545 ? O4 Ba1 O2 139.52(9) 2_556 1_545 ? O3 Ba1 O2 134.10(9) 3_566 1_545 ? O1 Ba1 O2 78.69(8) 3_556 1_545 ? O1 Ba1 O2 62.90(9) . 1_545 ? O6 Ba1 O2 105.35(9) 2_546 1_545 ? O7 Ba1 N3 139.85(12) . . ? O4 Ba1 N3 72.98(10) 2_556 . ? O3 Ba1 N3 125.20(9) 3_566 . ? O1 Ba1 N3 140.53(10) 3_556 . ? O1 Ba1 N3 74.84(10) . . ? O6 Ba1 N3 76.44(10) 2_546 . ? O2 Ba1 N3 67.11(9) 1_545 . ? O7 Ba1 O4 85.75(10) . 2_546 ? O4 Ba1 O4 114.38(11) 2_556 2_546 ? O3 Ba1 O4 156.73(10) 3_566 2_546 ? O1 Ba1 O4 106.10(8) 3_556 2_546 ? O1 Ba1 O4 123.05(8) . 2_546 ? O6 Ba1 O4 47.04(8) 2_546 2_546 ? O2 Ba1 O4 61.20(9) 1_545 2_546 ? N3 Ba1 O4 74.64(9) . 2_546 ? O7 Ba1 O3 74.15(10) . 3_556 ? O4 Ba1 O3 157.88(10) 2_556 3_556 ? O3 Ba1 O3 109.63(10) 3_566 3_556 ? O1 Ba1 O3 46.55(8) 3_556 3_556 ? O1 Ba1 O3 99.68(8) . 3_556 ? O6 Ba1 O3 94.96(8) 2_546 3_556 ? O2 Ba1 O3 59.27(8) 1_545 3_556 ? N3 Ba1 O3 120.99(8) . 3_556 ? O4 Ba1 O3 59.60(8) 2_546 3_556 ? O7 Ba1 S2 71.14(8) . 2_546 ? O4 Ba1 S2 93.32(7) 2_556 2_546 ? O3 Ba1 S2 138.77(7) 3_566 2_546 ? O1 Ba1 S2 119.45(6) 3_556 2_546 ? O1 Ba1 S2 143.47(6) . 2_546 ? O6 Ba1 S2 23.39(6) 2_546 2_546 ? O2 Ba1 S2 84.62(7) 1_545 2_546 ? N3 Ba1 S2 77.44(8) . 2_546 ? O4 Ba1 S2 24.06(6) 2_546 2_546 ? O3 Ba1 S2 74.96(6) 3_556 2_546 ? O7 Ba1 S1 74.81(9) . 3_556 ? O4 Ba1 S1 151.76(7) 2_556 3_556 ? O3 Ba1 S1 87.99(7) 3_566 3_556 ? O1 Ba1 S1 22.80(6) 3_556 3_556 ? O1 Ba1 S1 85.63(6) . 3_556 ? O6 Ba1 S1 115.30(6) 2_546 3_556 ? O2 Ba1 S1 67.73(6) 1_545 3_556 ? N3 Ba1 S1 134.84(7) . 3_556 ? O4 Ba1 S1 83.33(6) 2_546 3_556 ? O3 Ba1 S1 23.75(6) 3_556 3_556 ? S2 Ba1 S1 97.66(3) 2_546 3_556 ? O3 S1 O2 113.98(19) . . ? O3 S1 O1 111.50(18) . . ? O2 S1 O1 110.58(19) . . ? O3 S1 C2 105.8(2) . . ? O2 S1 C2 106.1(2) . . ? O1 S1 C2 108.56(19) . . ? O3 S1 Ba1 61.83(13) . 3_556 ? O2 S1 Ba1 132.36(13) . 3_556 ? O1 S1 Ba1 49.67(11) . 3_556 ? C2 S1 Ba1 121.00(15) . 3_556 ? O5 S2 O6 114.8(2) . . ? O5 S2 O4 112.6(2) . . ? O6 S2 O4 109.87(18) . . ? O5 S2 C5 106.1(2) . . ? O6 S2 C5 105.82(17) . . ? O4 S2 C5 107.1(2) . . ? O5 S2 Ba1 123.80(14) . 2_556 ? O6 S2 Ba1 52.50(12) . 2_556 ? O4 S2 Ba1 58.74(12) . 2_556 ? C5 S2 Ba1 130.00(14) . 2_556 ? S1 O1 Ba1 107.53(14) . 3_556 ? S1 O1 Ba1 114.20(15) . . ? Ba1 O1 Ba1 107.68(8) 3_556 . ? S1 O2 Ba1 145.35(19) . 1_565 ? S1 O3 Ba1 145.26(19) . 3_566 ? S1 O3 Ba1 94.42(14) . 3_556 ? Ba1 O3 Ba1 109.63(10) 3_566 3_556 ? S2 O4 Ba1 136.42(18) . 2_546 ? S2 O4 Ba1 97.20(13) . 2_556 ? Ba1 O4 Ba1 114.38(11) 2_546 2_556 ? S2 O6 Ba1 104.11(15) . 2_556 ? C3 N1 N2 104.8(4) . . ? C1 N2 N1 113.2(4) . . ? C6 N3 N4 104.1(4) . . ? C6 N3 Ba1 138.0(3) . . ? N4 N3 Ba1 116.4(2) . . ? C4 N4 N3 113.0(3) . . ? N2 C1 C2 106.6(4) . . ? C1 C2 C3 104.5(4) . . ? C1 C2 S1 129.8(4) . . ? C3 C2 S1 125.1(4) . . ? N1 C3 C2 110.9(5) . . ? N4 C4 C5 106.5(4) . . ? C4 C5 C6 105.0(4) . . ? C4 C5 S2 127.5(3) . . ? C6 C5 S2 127.4(3) . . ? N3 C6 C5 111.3(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.633 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.134