# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Mezei, Gellert' _publ_contact_author_email ? _publ_section_title ; Cation Effect on the Inorganic-Organic Layered Structure of Pyrazole-4-Sulfonate Networks and Inhibitory Effects on Copper Corrosion ; loop_ _publ_author_name G.Mezei I.Fernando K.Demadis N.Daskalakis # Attachment '- Gellert Mezei - CIF files.txt' data_rubidiumpyrazolesulfonate _database_code_depnum_ccdc_archive 'CCDC 742361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H3 N2 O3 Rb S' _chemical_formula_weight 232.60 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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 9.7332(4) _cell_length_b 9.7332(4) _cell_length_c 29.9414(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2836.5(2) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 29.18 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 7.223 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.1093 _exptl_absorpt_correction_T_max 0.1865 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 62644 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 29.30 _reflns_number_total 1942 _reflns_number_gt 1643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5000P] 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 0.0025(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1942 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Rb1 Rb 0.5000 0.7500 0.020401(13) 0.03479(17) Uani 1 2 d S . . Rb2 Rb 0.0000 0.7500 0.018678(13) 0.03726(17) Uani 1 2 d S . . S1 S 0.24397(7) 0.43184(6) 0.047693(19) 0.02950(19) Uani 1 1 d . . . O1 O 0.3457(4) 0.5078(3) 0.02315(8) 0.0778(10) Uani 1 1 d . . . O2 O 0.1059(3) 0.4782(3) 0.03964(10) 0.0758(10) Uani 1 1 d . . . O3 O 0.2575(2) 0.2862(2) 0.04012(6) 0.0396(5) Uani 1 1 d . . . N1 N 0.3809(3) 0.5033(3) 0.16973(8) 0.0498(7) Uani 1 1 d . . . N2 N 0.2444(3) 0.4966(3) 0.17538(8) 0.0365(5) Uani 1 1 d . . . C3 C 0.3997(3) 0.4836(3) 0.12655(8) 0.0416(7) Uani 1 1 d . . . H3 H 0.4853 0.4830 0.1127 0.050 Uiso 1 1 calc R . . C2 C 0.2754(2) 0.4638(2) 0.10411(7) 0.0245(4) Uani 1 1 d . . . C1 C 0.1771(3) 0.4731(3) 0.13707(9) 0.0314(5) Uani 1 1 d . . . H1 H 0.0826 0.4647 0.1335 0.038 Uiso 1 1 calc R . . H2 H 0.203(3) 0.515(3) 0.1989(12) 0.023(7) 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 Rb1 0.0343(2) 0.0290(2) 0.0411(3) 0.000 0.000 -0.00540(12) Rb2 0.0370(2) 0.0353(2) 0.0395(3) 0.000 0.000 -0.00544(13) S1 0.0460(4) 0.0223(3) 0.0202(3) 0.0010(2) -0.0037(2) -0.0026(2) O1 0.140(3) 0.0623(16) 0.0312(11) -0.0055(10) 0.0216(14) -0.0611(16) O2 0.0779(19) 0.0808(19) 0.0688(17) -0.0307(15) -0.0473(16) 0.0394(15) O3 0.0633(14) 0.0254(8) 0.0302(8) -0.0009(7) 0.0018(8) 0.0007(8) N1 0.0371(13) 0.084(2) 0.0279(11) -0.0083(11) -0.0057(10) 0.0028(12) N2 0.0392(11) 0.0485(13) 0.0218(12) -0.0005(9) 0.0048(9) 0.0027(9) C3 0.0269(13) 0.069(2) 0.0286(13) -0.0035(11) -0.0016(9) -0.0008(13) C2 0.0271(11) 0.0282(11) 0.0182(10) -0.0008(8) 0.0011(8) -0.0012(9) C1 0.0259(12) 0.0403(14) 0.0281(11) -0.0005(10) 0.0040(10) -0.0004(10) _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 Rb1 O1 2.796(2) 6_564 ? Rb1 O1 2.796(2) . ? Rb1 O3 2.996(2) 14 ? Rb1 O3 2.996(2) 9_665 ? Rb1 O1 3.202(3) 9_665 ? Rb1 O1 3.202(3) 14 ? Rb1 N1 3.213(3) 12_766 ? Rb1 N1 3.213(3) 15_565 ? Rb1 S1 3.6741(7) 14 ? Rb1 S1 3.6741(7) 9_665 ? Rb1 Rb2 4.8669(2) 1_655 ? Rb1 Rb1 5.0176(3) 9_665 ? Rb2 O2 2.908(3) 6_464 ? Rb2 O2 2.908(3) . ? Rb2 O2 3.007(3) 9_565 ? Rb2 O2 3.007(3) 14 ? Rb2 O3 3.083(2) 9_565 ? Rb2 O3 3.083(2) 14 ? Rb2 N1 3.290(3) 15_565 ? Rb2 N1 3.290(3) 12_666 ? Rb2 S1 3.5666(6) 9_565 ? Rb2 S1 3.5666(6) 14 ? Rb2 S1 3.9979(6) 6_464 ? Rb2 Rb1 4.8669(2) 1_455 ? S1 O1 1.438(3) . ? S1 O2 1.438(2) . ? S1 O3 1.442(2) . ? S1 C2 1.745(2) . ? S1 Rb2 3.5665(6) 9_565 ? S1 Rb1 3.6741(7) 9_665 ? O1 Rb1 3.202(3) 9_665 ? O2 Rb2 3.007(3) 9_565 ? O3 Rb1 2.996(2) 9_665 ? O3 Rb2 3.083(2) 9_565 ? N1 C3 1.320(3) . ? N1 N2 1.341(4) . ? N1 Rb1 3.213(3) 15_565 ? N1 Rb2 3.290(3) 15 ? N2 C1 1.341(4) . ? C3 C2 1.397(3) . ? C2 C1 1.377(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 Rb1 O1 176.62(10) 6_564 . ? O1 Rb1 O3 109.99(8) 6_564 14 ? O1 Rb1 O3 72.17(9) . 14 ? O1 Rb1 O3 72.17(9) 6_564 9_665 ? O1 Rb1 O3 109.99(8) . 9_665 ? O3 Rb1 O3 105.59(8) 14 9_665 ? O1 Rb1 O1 114.87(12) 6_564 9_665 ? O1 Rb1 O1 66.64(11) . 9_665 ? O3 Rb1 O1 102.44(7) 14 9_665 ? O3 Rb1 O1 44.93(6) 9_665 9_665 ? O1 Rb1 O1 66.64(11) 6_564 14 ? O1 Rb1 O1 114.87(12) . 14 ? O3 Rb1 O1 44.93(6) 14 14 ? O3 Rb1 O1 102.44(7) 9_665 14 ? O1 Rb1 O1 131.93(10) 9_665 14 ? O1 Rb1 N1 83.46(8) 6_564 12_766 ? O1 Rb1 N1 94.65(9) . 12_766 ? O3 Rb1 N1 165.59(6) 14 12_766 ? O3 Rb1 N1 72.92(6) 9_665 12_766 ? O1 Rb1 N1 66.04(8) 9_665 12_766 ? O1 Rb1 N1 149.37(6) 14 12_766 ? O1 Rb1 N1 94.65(9) 6_564 15_565 ? O1 Rb1 N1 83.46(8) . 15_565 ? O3 Rb1 N1 72.92(6) 14 15_565 ? O3 Rb1 N1 165.59(6) 9_665 15_565 ? O1 Rb1 N1 149.37(6) 9_665 15_565 ? O1 Rb1 N1 66.04(8) 14 15_565 ? N1 Rb1 N1 112.17(10) 12_766 15_565 ? O1 Rb1 S1 88.55(7) 6_564 14 ? O1 Rb1 S1 93.33(8) . 14 ? O3 Rb1 S1 22.11(4) 14 14 ? O3 Rb1 S1 104.79(4) 9_665 14 ? O1 Rb1 S1 118.01(6) 9_665 14 ? O1 Rb1 S1 22.83(4) 14 14 ? N1 Rb1 S1 172.01(5) 12_766 14 ? N1 Rb1 S1 68.22(5) 15_565 14 ? O1 Rb1 S1 93.33(8) 6_564 9_665 ? O1 Rb1 S1 88.55(7) . 9_665 ? O3 Rb1 S1 104.79(4) 14 9_665 ? O3 Rb1 S1 22.11(4) 9_665 9_665 ? O1 Rb1 S1 22.83(4) 9_665 9_665 ? O1 Rb1 S1 118.01(6) 14 9_665 ? N1 Rb1 S1 68.22(5) 12_766 9_665 ? N1 Rb1 S1 172.01(5) 15_565 9_665 ? S1 Rb1 S1 112.59(2) 14 9_665 ? O1 Rb1 Rb2 57.53(8) 6_564 1_655 ? O1 Rb1 Rb2 122.51(8) . 1_655 ? O3 Rb1 Rb2 141.38(4) 14 1_655 ? O3 Rb1 Rb2 37.43(4) 9_665 1_655 ? O1 Rb1 Rb2 61.75(6) 9_665 1_655 ? O1 Rb1 Rb2 117.69(6) 14 1_655 ? N1 Rb1 Rb2 42.15(5) 12_766 1_655 ? N1 Rb1 Rb2 138.87(5) 15_565 1_655 ? S1 Rb1 Rb2 132.247(12) 14 1_655 ? S1 Rb1 Rb2 46.835(10) 9_665 1_655 ? O1 Rb1 Rb1 145.56(8) 6_564 9_665 ? O1 Rb1 Rb1 35.86(7) . 9_665 ? O3 Rb1 Rb1 88.10(4) 14 9_665 ? O3 Rb1 Rb1 74.86(4) 9_665 9_665 ? O1 Rb1 Rb1 30.77(5) 9_665 9_665 ? O1 Rb1 Rb1 131.37(4) 14 9_665 ? N1 Rb1 Rb1 77.64(5) 12_766 9_665 ? N1 Rb1 Rb1 119.06(5) 15_565 9_665 ? S1 Rb1 Rb1 109.397(12) 14 9_665 ? S1 Rb1 Rb1 52.963(10) 9_665 9_665 ? Rb2 Rb1 Rb1 89.852(2) 1_655 9_665 ? O2 Rb2 O2 155.07(11) 6_464 . ? O2 Rb2 O2 132.51(10) 6_464 9_565 ? O2 Rb2 O2 64.84(8) . 9_565 ? O2 Rb2 O2 64.84(8) 6_464 14 ? O2 Rb2 O2 132.52(10) . 14 ? O2 Rb2 O2 109.02(14) 9_565 14 ? O2 Rb2 O3 86.50(8) 6_464 9_565 ? O2 Rb2 O3 107.91(6) . 9_565 ? O2 Rb2 O3 46.01(6) 9_565 9_565 ? O2 Rb2 O3 91.81(8) 14 9_565 ? O2 Rb2 O3 107.91(6) 6_464 14 ? O2 Rb2 O3 86.50(8) . 14 ? O2 Rb2 O3 91.81(8) 9_565 14 ? O2 Rb2 O3 46.01(6) 14 14 ? O3 Rb2 O3 110.36(7) 9_565 14 ? O2 Rb2 N1 79.88(8) 6_464 15_565 ? O2 Rb2 N1 86.21(7) . 15_565 ? O2 Rb2 N1 147.40(7) 9_565 15_565 ? O2 Rb2 N1 78.95(8) 14 15_565 ? O3 Rb2 N1 165.84(6) 9_565 15_565 ? O3 Rb2 N1 70.77(6) 14 15_565 ? O2 Rb2 N1 86.21(7) 6_464 12_666 ? O2 Rb2 N1 79.87(8) . 12_666 ? O2 Rb2 N1 78.95(8) 9_565 12_666 ? O2 Rb2 N1 147.40(7) 14 12_666 ? O3 Rb2 N1 70.77(6) 9_565 12_666 ? O3 Rb2 N1 165.84(6) 14 12_666 ? N1 Rb2 N1 111.81(9) 15_565 12_666 ? O2 Rb2 S1 109.62(7) 6_464 9_565 ? O2 Rb2 S1 84.54(5) . 9_565 ? O2 Rb2 S1 23.34(5) 9_565 9_565 ? O2 Rb2 S1 105.74(7) 14 9_565 ? O3 Rb2 S1 23.63(4) 9_565 9_565 ? O3 Rb2 S1 106.25(4) 14 9_565 ? N1 Rb2 S1 170.45(5) 15_565 9_565 ? N1 Rb2 S1 68.81(5) 12_666 9_565 ? O2 Rb2 S1 84.54(5) 6_464 14 ? O2 Rb2 S1 109.62(7) . 14 ? O2 Rb2 S1 105.74(7) 9_565 14 ? O2 Rb2 S1 23.34(5) 14 14 ? O3 Rb2 S1 106.25(4) 9_565 14 ? O3 Rb2 S1 23.63(4) 14 14 ? N1 Rb2 S1 68.81(5) 15_565 14 ? N1 Rb2 S1 170.45(5) 12_666 14 ? S1 Rb2 S1 112.28(2) 9_565 14 ? O2 Rb2 S1 15.81(6) 6_464 6_464 ? O2 Rb2 S1 150.27(7) . 6_464 ? O2 Rb2 S1 119.65(5) 9_565 6_464 ? O2 Rb2 S1 75.97(5) 14 6_464 ? O3 Rb2 S1 74.32(4) 9_565 6_464 ? O3 Rb2 S1 121.23(4) 14 6_464 ? N1 Rb2 S1 92.89(5) 15_565 6_464 ? N1 Rb2 S1 72.90(5) 12_666 6_464 ? S1 Rb2 S1 96.314(16) 9_565 6_464 ? S1 Rb2 S1 97.594(12) 14 6_464 ? O2 Rb2 Rb1 69.10(7) 6_464 1_455 ? O2 Rb2 Rb1 110.62(7) . 1_455 ? O2 Rb2 Rb1 70.33(6) 9_565 1_455 ? O2 Rb2 Rb1 110.42(5) 14 1_455 ? O3 Rb2 Rb1 36.21(4) 9_565 1_455 ? O3 Rb2 Rb1 144.98(4) 14 1_455 ? N1 Rb2 Rb1 138.03(5) 15_565 1_455 ? N1 Rb2 Rb1 40.94(5) 12_666 1_455 ? S1 Rb2 Rb1 48.711(11) 9_565 1_455 ? S1 Rb2 Rb1 132.197(12) 14 1_455 ? S1 Rb2 Rb1 53.399(9) 6_464 1_455 ? O1 S1 O2 113.3(2) . . ? O1 S1 O3 111.26(15) . . ? O2 S1 O3 111.56(15) . . ? O1 S1 C2 106.40(13) . . ? O2 S1 C2 105.69(14) . . ? O3 S1 C2 108.17(11) . . ? O1 S1 Rb2 115.40(12) . 9_565 ? O2 S1 Rb2 55.95(11) . 9_565 ? O3 S1 Rb2 59.01(8) . 9_565 ? C2 S1 Rb2 138.14(8) . 9_565 ? O1 S1 Rb1 59.81(13) . 9_665 ? O2 S1 Rb1 133.78(11) . 9_665 ? O3 S1 Rb1 51.47(8) . 9_665 ? C2 S1 Rb1 120.28(8) . 9_665 ? Rb2 S1 Rb1 84.454(13) 9_565 9_665 ? S1 O1 Rb1 144.94(15) . . ? S1 O1 Rb1 97.36(13) . 9_665 ? Rb1 O1 Rb1 113.36(11) . 9_665 ? S1 O2 Rb2 130.77(19) . . ? S1 O2 Rb2 100.71(12) . 9_565 ? Rb2 O2 Rb2 115.16(8) . 9_565 ? S1 O3 Rb1 106.42(10) . 9_665 ? S1 O3 Rb2 97.36(9) . 9_565 ? Rb1 O3 Rb2 106.36(6) 9_665 9_565 ? C3 N1 N2 104.7(2) . . ? C3 N1 Rb1 127.2(2) . 15_565 ? N2 N1 Rb1 108.86(18) . 15_565 ? C3 N1 Rb2 113.1(2) . 15 ? N2 N1 Rb2 104.00(18) . 15 ? Rb1 N1 Rb2 96.91(6) 15_565 15 ? C1 N2 N1 112.6(2) . . ? N1 C3 C2 111.8(3) . . ? C1 C2 C3 104.4(2) . . ? C1 C2 S1 125.69(19) . . ? C3 C2 S1 129.95(19) . . ? N2 C1 C2 106.5(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.457 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.070 #===END data_cesiumpyrazolesulfonate _database_code_depnum_ccdc_archive 'CCDC 742362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H3 Cs N2 O3 S' _chemical_formula_weight 280.04 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' Cs Cs -0.3680 2.1192 '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 8.8211(14) _cell_length_b 8.1086(13) _cell_length_c 9.8888(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.560(3) _cell_angle_gamma 90.00 _cell_volume 707.05(19) _cell_formula_units_Z 4 _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 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 5.479 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1942 _exptl_absorpt_correction_T_max 0.3057 _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 3733 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1247 _reflns_number_gt 1140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.3526P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1247 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0490 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Cs1 Cs 0.09255(2) 0.83128(3) 0.685726(19) 0.03423(10) Uani 1 1 d . . . S1 S 0.21616(9) 0.32742(9) 0.55619(8) 0.02827(18) Uani 1 1 d . . . O1 O 0.2025(2) 0.4565(3) 0.6584(2) 0.0389(6) Uani 1 1 d . . . O2 O 0.1099(3) 0.1939(3) 0.5786(2) 0.0365(5) Uani 1 1 d . . . O3 O 0.2099(3) 0.3910(3) 0.4196(2) 0.0437(6) Uani 1 1 d . . . N1 N 0.6491(3) 0.1925(4) 0.5641(3) 0.0451(8) Uani 1 1 d . . . N2 N 0.5874(3) 0.0953(4) 0.6574(3) 0.0389(7) Uani 1 1 d . . . H2 H 0.6381 0.0229 0.7033 0.047 Uiso 1 1 calc R . . C1 C 0.4390(4) 0.1222(5) 0.6720(3) 0.0385(8) Uani 1 1 d . . . H1 H 0.3760 0.0694 0.7322 0.046 Uiso 1 1 calc R . . C2 C 0.3978(3) 0.2423(4) 0.5813(3) 0.0298(7) Uani 1 1 d . . . C3 C 0.5331(4) 0.2815(5) 0.5172(4) 0.0444(9) Uani 1 1 d . . . H3 H 0.5406 0.3607 0.4497 0.053 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 Cs1 0.03280(14) 0.03302(15) 0.03690(15) 0.00140(8) 0.00134(9) -0.00030(8) S1 0.0246(4) 0.0299(4) 0.0302(4) -0.0008(3) -0.0013(3) -0.0013(3) O1 0.0336(11) 0.0352(13) 0.0478(14) -0.0116(11) -0.0014(10) 0.0009(10) O2 0.0304(12) 0.0338(13) 0.0452(14) -0.0007(10) -0.0002(10) -0.0070(10) O3 0.0378(13) 0.0552(16) 0.0379(14) 0.0140(12) -0.0008(10) 0.0028(12) N1 0.0334(16) 0.049(2) 0.0534(19) 0.0086(15) 0.0053(14) 0.0044(13) N2 0.0306(15) 0.0405(18) 0.0453(16) 0.0076(14) -0.0034(12) 0.0033(12) C1 0.0302(17) 0.044(2) 0.0412(19) 0.0073(16) 0.0007(14) -0.0013(15) C2 0.0297(16) 0.0298(17) 0.0299(16) -0.0024(14) -0.0007(13) 0.0001(14) C3 0.0329(19) 0.050(2) 0.051(2) 0.0138(18) 0.0079(16) 0.0047(16) _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 Cs1 O2 3.130(2) 1_565 ? Cs1 O2 3.132(2) 3_566 ? Cs1 O2 3.176(2) 2_556 ? Cs1 O1 3.204(2) . ? Cs1 O1 3.225(2) 2_556 ? Cs1 O3 3.361(3) 3_566 ? Cs1 O3 3.370(2) 4_576 ? Cs1 N1 3.412(3) 3_666 ? Cs1 N1 3.503(3) 2_656 ? Cs1 N2 3.715(3) 2_656 ? Cs1 S1 3.7827(9) 2_556 ? Cs1 S1 3.8000(9) 3_566 ? S1 O3 1.446(2) . ? S1 O2 1.453(2) . ? S1 O1 1.462(2) . ? S1 C2 1.756(3) . ? S1 Cs1 3.7827(9) 2_546 ? S1 Cs1 3.8000(9) 3_566 ? O1 Cs1 3.225(2) 2_546 ? O2 Cs1 3.130(2) 1_545 ? O2 Cs1 3.132(2) 3_566 ? O2 Cs1 3.176(2) 2_546 ? O3 Cs1 3.361(3) 3_566 ? O3 Cs1 3.370(2) 4_575 ? N1 C3 1.325(5) . ? N1 N2 1.341(4) . ? N1 Cs1 3.412(3) 3_666 ? N1 Cs1 3.503(3) 2_646 ? N2 C1 1.339(4) . ? N2 Cs1 3.715(3) 2_646 ? C1 C2 1.366(5) . ? C1 Cs1 3.866(3) 1_545 ? C2 C3 1.404(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 O2 Cs1 O2 79.09(6) 1_565 3_566 ? O2 Cs1 O2 127.69(6) 1_565 2_556 ? O2 Cs1 O2 105.68(6) 3_566 2_556 ? O2 Cs1 O1 147.64(6) 1_565 . ? O2 Cs1 O1 91.99(6) 3_566 . ? O2 Cs1 O1 84.65(6) 2_556 . ? O2 Cs1 O1 85.04(6) 1_565 2_556 ? O2 Cs1 O1 88.30(6) 3_566 2_556 ? O2 Cs1 O1 44.15(6) 2_556 2_556 ? O1 Cs1 O1 126.09(6) . 2_556 ? O2 Cs1 O3 116.40(6) 1_565 3_566 ? O2 Cs1 O3 43.68(6) 3_566 3_566 ? O2 Cs1 O3 65.28(6) 2_556 3_566 ? O1 Cs1 O3 72.82(6) . 3_566 ? O1 Cs1 O3 70.91(6) 2_556 3_566 ? O2 Cs1 O3 65.65(6) 1_565 4_576 ? O2 Cs1 O3 140.68(6) 3_566 4_576 ? O2 Cs1 O3 84.22(6) 2_556 4_576 ? O1 Cs1 O3 127.14(6) . 4_576 ? O1 Cs1 O3 72.44(6) 2_556 4_576 ? O3 Cs1 O3 142.86(3) 3_566 4_576 ? O2 Cs1 N1 76.61(7) 1_565 3_666 ? O2 Cs1 N1 76.64(7) 3_566 3_666 ? O2 Cs1 N1 155.70(6) 2_556 3_666 ? O1 Cs1 N1 71.06(7) . 3_666 ? O1 Cs1 N1 158.08(6) 2_556 3_666 ? O3 Cs1 N1 106.59(7) 3_566 3_666 ? O3 Cs1 N1 109.63(7) 4_576 3_666 ? O2 Cs1 N1 120.24(7) 1_565 2_656 ? O2 Cs1 N1 156.02(6) 3_566 2_656 ? O2 Cs1 N1 74.76(7) 2_556 2_656 ? O1 Cs1 N1 64.06(6) . 2_656 ? O1 Cs1 N1 106.34(6) 2_556 2_656 ? O3 Cs1 N1 122.83(7) 3_566 2_656 ? O3 Cs1 N1 63.15(7) 4_576 2_656 ? N1 Cs1 N1 93.36(7) 3_666 2_656 ? O2 Cs1 N2 125.56(6) 1_565 2_656 ? O2 Cs1 N2 136.43(6) 3_566 2_656 ? O2 Cs1 N2 87.08(6) 2_556 2_656 ? O1 Cs1 N2 47.02(6) . 2_656 ? O1 Cs1 N2 125.21(6) 2_556 2_656 ? O3 Cs1 N2 116.15(7) 3_566 2_656 ? O3 Cs1 N2 80.91(6) 4_576 2_656 ? N1 Cs1 N2 76.01(7) 3_666 2_656 ? N1 Cs1 N2 21.15(7) 2_656 2_656 ? O2 Cs1 S1 106.19(4) 1_565 2_556 ? O2 Cs1 S1 99.09(5) 3_566 2_556 ? O2 Cs1 S1 21.96(4) 2_556 2_556 ? O1 Cs1 S1 105.92(4) . 2_556 ? O1 Cs1 S1 22.31(4) 2_556 2_556 ? O3 Cs1 S1 67.96(4) 3_566 2_556 ? O3 Cs1 S1 75.86(4) 4_576 2_556 ? N1 Cs1 S1 174.50(6) 3_666 2_556 ? N1 Cs1 S1 89.27(5) 2_656 2_556 ? N2 Cs1 S1 105.48(5) 2_656 2_556 ? O2 Cs1 S1 98.39(4) 1_565 3_566 ? O2 Cs1 S1 21.56(4) 3_566 3_566 ? O2 Cs1 S1 86.30(5) 2_556 3_566 ? O1 Cs1 S1 80.73(4) . 3_566 ? O1 Cs1 S1 80.43(4) 2_556 3_566 ? O3 Cs1 S1 22.22(4) 3_566 3_566 ? O3 Cs1 S1 149.27(4) 4_576 3_566 ? N1 Cs1 S1 90.37(6) 3_666 3_566 ? N1 Cs1 S1 141.00(5) 2_656 3_566 ? N2 Cs1 S1 127.72(5) 2_656 3_566 ? S1 Cs1 S1 84.56(2) 2_556 3_566 ? O3 S1 O2 113.58(15) . . ? O3 S1 O1 112.87(15) . . ? O2 S1 O1 111.24(14) . . ? O3 S1 C2 106.51(14) . . ? O2 S1 C2 105.98(14) . . ? O1 S1 C2 106.01(14) . . ? O3 S1 Cs1 128.13(10) . 2_546 ? O2 S1 Cs1 54.83(9) . 2_546 ? O1 S1 Cs1 56.86(9) . 2_546 ? C2 S1 Cs1 125.36(10) . 2_546 ? O3 S1 Cs1 61.56(10) . 3_566 ? O2 S1 Cs1 52.39(10) . 3_566 ? O1 S1 Cs1 127.32(10) . 3_566 ? C2 S1 Cs1 126.27(10) . 3_566 ? Cs1 S1 Cs1 84.88(2) 2_546 3_566 ? S1 O1 Cs1 140.21(13) . . ? S1 O1 Cs1 100.83(11) . 2_546 ? Cs1 O1 Cs1 90.47(6) . 2_546 ? S1 O2 Cs1 142.13(13) . 1_545 ? S1 O2 Cs1 106.05(12) . 3_566 ? Cs1 O2 Cs1 100.91(6) 1_545 3_566 ? S1 O2 Cs1 103.21(11) . 2_546 ? Cs1 O2 Cs1 92.73(6) 1_545 2_546 ? Cs1 O2 Cs1 108.41(7) 3_566 2_546 ? S1 O3 Cs1 96.21(12) . 3_566 ? S1 O3 Cs1 151.98(15) . 4_575 ? Cs1 O3 Cs1 85.38(5) 3_566 4_575 ? C3 N1 N2 103.7(3) . . ? C3 N1 Cs1 107.6(2) . 3_666 ? N2 N1 Cs1 139.2(2) . 3_666 ? C3 N1 Cs1 123.6(3) . 2_646 ? N2 N1 Cs1 88.3(2) . 2_646 ? Cs1 N1 Cs1 95.45(8) 3_666 2_646 ? C1 N2 N1 113.2(3) . . ? C1 N2 Cs1 127.2(2) . 2_646 ? N1 N2 Cs1 70.52(18) . 2_646 ? N2 C1 C2 106.8(3) . . ? N2 C1 Cs1 132.9(2) . 1_545 ? C2 C1 Cs1 105.2(2) . 1_545 ? C1 C2 C3 104.1(3) . . ? C1 C2 S1 126.8(2) . . ? C3 C2 S1 129.1(3) . . ? N1 C3 C2 112.1(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.347 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.107 #===END data_magnesiumpyrazolesulfonate _database_code_depnum_ccdc_archive 'CCDC 742363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Mg N4 O12 S2' _chemical_formula_weight 426.67 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' Mg Mg 0.0486 0.0363 '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 7.0543(7) _cell_length_b 7.7307(8) _cell_length_c 8.6389(9) _cell_angle_alpha 72.572(2) _cell_angle_beta 74.370(2) _cell_angle_gamma 76.045(2) _cell_volume 426.22(8) _cell_formula_units_Z 1 _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 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 222 _exptl_absorpt_coefficient_mu 0.417 _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 2057 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1225 _reflns_number_gt 1101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.1834P] 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 SHELXL _refine_ls_extinction_coef 0.131(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1225 _refine_ls_number_parameters 122 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.061 _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 Mg1 Mg 0.5000 0.0000 0.5000 0.0252(3) Uani 1 2 d S . . S1 S 0.24716(8) 0.72559(7) 0.17948(7) 0.0255(3) Uani 1 1 d . . . O1 O 0.1630(3) 0.9138(2) 0.1899(2) 0.0418(5) Uani 1 1 d . . . O2 O 0.3877(3) 0.7149(3) 0.0250(2) 0.0493(5) Uani 1 1 d . . . O3 O 0.3345(3) 0.6179(2) 0.3204(2) 0.0401(5) Uani 1 1 d . . . O4 O 0.4275(3) 0.2666(2) 0.5254(2) 0.0336(4) Uani 1 1 d D . . O5 O 0.4113(3) 0.0889(2) 0.2759(2) 0.0380(5) Uani 1 1 d D . . O6 O 0.2191(3) -0.0522(2) 0.6183(2) 0.0403(5) Uani 1 1 d D . . N1 N -0.1485(3) 0.4115(3) 0.2583(3) 0.0375(6) Uani 1 1 d . . . N2 N -0.2119(3) 0.5612(3) 0.1444(3) 0.0339(5) Uani 1 1 d . . . H2 H -0.3139 0.5717 0.1037 0.041 Uiso 1 1 calc R . . C1 C -0.1000(4) 0.6910(3) 0.1016(3) 0.0319(6) Uani 1 1 d . . . H1 H -0.1184 0.8052 0.0265 0.038 Uiso 1 1 calc R . . C2 C 0.0488(3) 0.6222(3) 0.1910(3) 0.0255(5) Uani 1 1 d . . . C3 C 0.0109(3) 0.4490(3) 0.2865(3) 0.0329(6) Uani 1 1 d . . . H3 H 0.0874 0.3700 0.3605 0.039 Uiso 1 1 calc R . . H4B H 0.3922 0.3621 0.4631 0.056(10) Uiso 1 1 d RD . . H5A H 0.3363 0.0446 0.2466 0.072(11) Uiso 1 1 d RD . . H4A H 0.4859 0.3012 0.5778 0.060(10) Uiso 1 1 d RD . . H5B H 0.4817 0.1306 0.1863 0.048(9) Uiso 1 1 d RD . . H6A H 0.2060 -0.1588 0.6558 0.057(10) Uiso 1 1 d RD . . H6B H 0.1227 0.0046 0.6661 0.074(12) 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 Mg1 0.0265(6) 0.0211(6) 0.0290(6) -0.0055(5) -0.0058(5) -0.0074(4) S1 0.0232(4) 0.0237(4) 0.0299(4) -0.0033(3) -0.0074(2) -0.0067(2) O1 0.0378(10) 0.0248(10) 0.0683(13) -0.0119(8) -0.0208(9) -0.0046(7) O2 0.0397(11) 0.0645(13) 0.0424(11) -0.0110(9) 0.0047(9) -0.0247(9) O3 0.0416(11) 0.0321(10) 0.0502(11) 0.0029(8) -0.0264(9) -0.0111(8) O4 0.0417(10) 0.0220(9) 0.0408(10) -0.0072(8) -0.0167(8) -0.0043(7) O5 0.0438(11) 0.0432(11) 0.0305(10) -0.0008(8) -0.0125(9) -0.0197(9) O6 0.0294(10) 0.0302(10) 0.0566(12) -0.0114(9) 0.0033(8) -0.0099(8) N1 0.0361(12) 0.0340(12) 0.0448(13) -0.0069(10) -0.0092(10) -0.0137(10) N2 0.0246(11) 0.0428(13) 0.0402(12) -0.0135(10) -0.0105(9) -0.0088(9) C1 0.0304(13) 0.0304(13) 0.0338(13) -0.0052(11) -0.0068(11) -0.0069(11) C2 0.0212(12) 0.0265(12) 0.0290(12) -0.0073(10) -0.0056(9) -0.0037(9) C3 0.0313(14) 0.0293(13) 0.0380(14) -0.0014(11) -0.0117(11) -0.0091(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 Mg1 O6 2.0452(17) . ? Mg1 O6 2.0452(17) 2_656 ? Mg1 O4 2.0641(16) . ? Mg1 O4 2.0641(16) 2_656 ? Mg1 O5 2.0643(16) . ? Mg1 O5 2.0643(16) 2_656 ? S1 O2 1.444(2) . ? S1 O3 1.4507(17) . ? S1 O1 1.4529(18) . ? S1 C2 1.738(2) . ? N1 C3 1.325(3) . ? N1 N2 1.346(3) . ? N2 C1 1.330(3) . ? C1 C2 1.379(3) . ? C2 C3 1.392(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 O6 Mg1 O6 180.00(5) . 2_656 ? O6 Mg1 O4 92.49(7) . . ? O6 Mg1 O4 87.51(7) 2_656 . ? O6 Mg1 O4 87.51(7) . 2_656 ? O6 Mg1 O4 92.49(7) 2_656 2_656 ? O4 Mg1 O4 180.000(1) . 2_656 ? O6 Mg1 O5 89.71(7) . . ? O6 Mg1 O5 90.29(7) 2_656 . ? O4 Mg1 O5 90.07(7) . . ? O4 Mg1 O5 89.93(7) 2_656 . ? O6 Mg1 O5 90.29(7) . 2_656 ? O6 Mg1 O5 89.71(7) 2_656 2_656 ? O4 Mg1 O5 89.93(7) . 2_656 ? O4 Mg1 O5 90.07(7) 2_656 2_656 ? O5 Mg1 O5 180.00(11) . 2_656 ? O2 S1 O3 110.99(11) . . ? O2 S1 O1 112.88(12) . . ? O3 S1 O1 112.42(11) . . ? O2 S1 C2 107.89(11) . . ? O3 S1 C2 105.45(10) . . ? O1 S1 C2 106.73(10) . . ? C3 N1 N2 104.71(19) . . ? C1 N2 N1 112.9(2) . . ? N2 C1 C2 106.2(2) . . ? C1 C2 C3 105.1(2) . . ? C1 C2 S1 127.31(19) . . ? C3 C2 S1 127.54(18) . . ? N1 C3 C2 111.1(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.261 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.056 #===END data_strontiumpyrazolesulfonate _database_code_depnum_ccdc_archive 'CCDC 742364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 N4 O6 S2 Sr' _chemical_formula_weight 381.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Sr Sr -1.5307 3.2498 '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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 6.027(2) _cell_length_b 7.243(3) _cell_length_c 14.186(5) _cell_angle_alpha 92.491(8) _cell_angle_beta 101.383(7) _cell_angle_gamma 97.471(7) _cell_volume 600.4(4) _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 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 4.867 _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_reflns_number 2757 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 23.31 _reflns_number_total 1719 _reflns_number_gt 1622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0742P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1719 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Sr1 Sr 0.17727(4) 0.77032(4) 0.481410(19) 0.01520(14) Uani 1 1 d . . . S1 S 0.61661(13) 0.82697(11) 0.32572(5) 0.0183(2) Uani 1 1 d . . . S2 S -0.24255(13) 0.71342(11) 0.60449(5) 0.0143(3) Uani 0.984(3) 1 d P . . O1 O 0.4020(4) 0.7486(3) 0.34954(16) 0.0286(6) Uani 1 1 d . . . O2 O 0.8053(4) 0.7244(3) 0.35862(16) 0.0273(6) Uani 1 1 d . . . O3 O 0.6741(4) 1.0258(3) 0.35370(16) 0.0284(6) Uani 1 1 d . . . O4 O -0.1796(4) 0.8966(3) 0.57026(15) 0.0253(5) Uani 1 1 d . . . O5 O -0.1029(3) 0.5823(3) 0.57170(14) 0.0185(5) Uani 1 1 d . . . O6 O -0.4851(4) 0.6514(3) 0.58119(15) 0.0227(5) Uani 1 1 d . . . N1 N 0.6326(6) 0.8031(5) 0.0485(2) 0.0439(9) Uani 1 1 d . . . N2 N 0.4138(6) 0.7353(5) 0.0486(2) 0.0405(8) Uani 1 1 d . . . H2 H 0.3134 0.6982 -0.0030 0.049 Uiso 1 1 calc R . . N3 N 0.0347(5) 0.6843(5) 0.8786(2) 0.0379(8) Uani 1 1 d . . . N4 N -0.1613(5) 0.7576(4) 0.8823(2) 0.0349(8) Uani 1 1 d . . . H4 H -0.2026 0.7857 0.9352 0.042 Uiso 1 1 calc R . . C1 C 0.3688(6) 0.7314(5) 0.1371(2) 0.0297(8) Uani 1 1 d . . . H1 H 0.2295 0.6891 0.1532 0.036 Uiso 1 1 calc R . . C2 C 0.5683(6) 0.8020(5) 0.1992(2) 0.0213(7) Uani 1 1 d . . . C3 C 0.7259(6) 0.8439(6) 0.1416(3) 0.0349(9) Uani 1 1 d . . . H3 H 0.8779 0.8943 0.1649 0.042 Uiso 1 1 calc R . . C4 C -0.2811(6) 0.7810(5) 0.7958(2) 0.0274(8) Uani 1 1 d . . . H4A H -0.4202 0.8269 0.7825 0.033 Uiso 1 1 calc R . . C5 C -0.1613(5) 0.7245(5) 0.7300(2) 0.0204(7) Uani 1 1 d . . . C6 C 0.0328(6) 0.6653(5) 0.7848(2) 0.0294(8) Uani 1 1 d . . . H6 H 0.1461 0.6186 0.7588 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 Sr1 0.01460(19) 0.0156(2) 0.0155(2) 0.00079(12) 0.00328(12) 0.00222(12) S1 0.0181(4) 0.0242(5) 0.0122(4) -0.0008(3) 0.0021(3) 0.0046(3) S2 0.0154(5) 0.0151(5) 0.0124(5) 0.0004(3) 0.0024(3) 0.0032(3) O1 0.0247(13) 0.0384(15) 0.0250(13) 0.0034(10) 0.0109(10) 0.0035(11) O2 0.0240(13) 0.0342(14) 0.0223(13) -0.0009(10) -0.0023(10) 0.0114(11) O3 0.0336(13) 0.0255(13) 0.0243(13) -0.0044(10) 0.0024(10) 0.0053(11) O4 0.0353(14) 0.0200(13) 0.0209(12) 0.0030(9) 0.0061(10) 0.0037(10) O5 0.0203(11) 0.0188(12) 0.0173(11) -0.0003(9) 0.0045(9) 0.0052(9) O6 0.0171(12) 0.0261(13) 0.0248(13) -0.0004(9) 0.0026(9) 0.0056(10) N1 0.047(2) 0.064(2) 0.0209(18) -0.0005(16) 0.0086(15) 0.0052(18) N2 0.0405(19) 0.057(2) 0.0183(17) -0.0044(15) -0.0047(14) 0.0054(16) N3 0.0375(19) 0.054(2) 0.0197(17) 0.0039(15) -0.0014(14) 0.0072(16) N4 0.0440(19) 0.046(2) 0.0157(16) -0.0027(14) 0.0103(14) 0.0064(16) C1 0.0221(19) 0.044(2) 0.0212(19) 0.0001(16) 0.0017(15) 0.0041(17) C2 0.0240(18) 0.0244(18) 0.0157(17) -0.0009(13) 0.0039(14) 0.0047(14) C3 0.029(2) 0.049(3) 0.027(2) -0.0004(17) 0.0090(16) 0.0014(18) C4 0.0272(19) 0.036(2) 0.0210(19) 0.0014(15) 0.0068(15) 0.0084(16) C5 0.0242(18) 0.0228(18) 0.0128(17) 0.0001(13) 0.0022(14) 0.0005(14) C6 0.0258(19) 0.043(2) 0.0191(19) 0.0010(16) 0.0018(15) 0.0070(17) _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 Sr1 O6 2.512(2) 1_655 ? Sr1 O2 2.527(2) 1_455 ? Sr1 O1 2.528(2) . ? Sr1 O4 2.550(2) 2_576 ? Sr1 O5 2.587(2) 2_566 ? Sr1 O5 2.599(2) . ? Sr1 O3 2.642(2) 2_676 ? Sr1 O4 2.921(2) . ? Sr1 S2 3.6706(15) 1_655 ? Sr1 Sr1 4.2491(14) 2_576 ? Sr1 Sr1 4.3159(15) 2_566 ? Sr1 Sr1 4.7067(15) 2_676 ? S1 O2 1.450(2) . ? S1 O1 1.452(2) . ? S1 O3 1.455(3) . ? S1 C2 1.757(3) . ? S2 O6 1.440(2) . ? S2 O4 1.462(2) . ? S2 O5 1.467(2) . ? S2 C5 1.747(3) . ? S2 Sr1 3.6706(15) 1_455 ? O2 Sr1 2.527(2) 1_655 ? O3 Sr1 2.642(2) 2_676 ? O4 Sr1 2.550(2) 2_576 ? O5 Sr1 2.587(2) 2_566 ? O6 Sr1 2.512(2) 1_455 ? N1 C3 1.333(5) . ? N1 N2 1.346(5) . ? N2 C1 1.337(4) . ? N3 C6 1.330(4) . ? N3 N4 1.365(4) . ? N4 C4 1.325(5) . ? C1 C2 1.366(5) . ? C2 C3 1.384(5) . ? C4 C5 1.367(5) . ? C5 C6 1.398(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 O6 Sr1 O2 152.36(8) 1_655 1_455 ? O6 Sr1 O1 83.22(8) 1_655 . ? O2 Sr1 O1 91.03(8) 1_455 . ? O6 Sr1 O4 124.27(8) 1_655 2_576 ? O2 Sr1 O4 81.08(8) 1_455 2_576 ? O1 Sr1 O4 81.27(8) . 2_576 ? O6 Sr1 O5 77.53(7) 1_655 2_566 ? O2 Sr1 O5 74.83(7) 1_455 2_566 ? O1 Sr1 O5 77.02(7) . 2_566 ? O4 Sr1 O5 147.01(7) 2_576 2_566 ? O6 Sr1 O5 91.67(7) 1_655 . ? O2 Sr1 O5 77.34(8) 1_455 . ? O1 Sr1 O5 144.25(8) . . ? O4 Sr1 O5 128.67(7) 2_576 . ? O5 Sr1 O5 67.35(7) 2_566 . ? O6 Sr1 O3 69.00(7) 1_655 2_676 ? O2 Sr1 O3 133.74(7) 1_455 2_676 ? O1 Sr1 O3 124.62(8) . 2_676 ? O4 Sr1 O3 77.13(8) 2_576 2_676 ? O5 Sr1 O3 135.83(7) 2_566 2_676 ? O5 Sr1 O3 85.29(7) . 2_676 ? O6 Sr1 O4 120.99(7) 1_655 . ? O2 Sr1 O4 71.00(7) 1_455 . ? O1 Sr1 O4 154.57(7) . . ? O4 Sr1 O4 78.33(7) 2_576 . ? O5 Sr1 O4 113.56(7) 2_566 . ? O5 Sr1 O4 50.70(6) . . ? O3 Sr1 O4 64.91(7) 2_676 . ? O6 Sr1 S2 16.19(5) 1_655 1_655 ? O2 Sr1 S2 160.52(5) 1_455 1_655 ? O1 Sr1 S2 74.48(6) . 1_655 ? O4 Sr1 S2 108.79(5) 2_576 1_655 ? O5 Sr1 S2 89.02(5) 2_566 1_655 ? O5 Sr1 S2 106.78(5) . 1_655 ? O3 Sr1 S2 65.69(5) 2_676 1_655 ? O4 Sr1 S2 126.68(5) . 1_655 ? O6 Sr1 Sr1 133.79(5) 1_655 2_576 ? O2 Sr1 Sr1 71.53(6) 1_455 2_576 ? O1 Sr1 Sr1 122.00(6) . 2_576 ? O4 Sr1 Sr1 42.32(5) 2_576 2_576 ? O5 Sr1 Sr1 141.11(5) 2_566 2_576 ? O5 Sr1 Sr1 86.54(5) . 2_576 ? O3 Sr1 Sr1 64.83(5) 2_676 2_576 ? O4 Sr1 Sr1 36.00(4) . 2_576 ? S2 Sr1 Sr1 127.16(2) 1_655 2_576 ? O6 Sr1 Sr1 83.57(6) 1_655 2_566 ? O2 Sr1 Sr1 73.21(6) 1_455 2_566 ? O1 Sr1 Sr1 110.74(6) . 2_566 ? O4 Sr1 Sr1 151.52(5) 2_576 2_566 ? O5 Sr1 Sr1 33.76(5) 2_566 2_566 ? O5 Sr1 Sr1 33.59(4) . 2_566 ? O3 Sr1 Sr1 112.36(6) 2_676 2_566 ? O4 Sr1 Sr1 81.85(5) . 2_566 ? S2 Sr1 Sr1 99.42(2) 1_655 2_566 ? Sr1 Sr1 Sr1 115.48(3) 2_576 2_566 ? O6 Sr1 Sr1 70.90(6) 1_655 2_676 ? O2 Sr1 Sr1 130.85(6) 1_455 2_676 ? O1 Sr1 Sr1 66.09(6) . 2_676 ? O4 Sr1 Sr1 53.86(5) 2_576 2_676 ? O5 Sr1 Sr1 133.36(5) 2_566 2_676 ? O5 Sr1 Sr1 144.57(5) . 2_676 ? O3 Sr1 Sr1 59.90(5) 2_676 2_676 ? O4 Sr1 Sr1 111.95(5) . 2_676 ? S2 Sr1 Sr1 55.03(3) 1_655 2_676 ? Sr1 Sr1 Sr1 84.43(3) 2_576 2_676 ? Sr1 Sr1 Sr1 154.449(14) 2_566 2_676 ? O2 S1 O1 114.31(15) . . ? O2 S1 O3 112.50(14) . . ? O1 S1 O3 112.15(14) . . ? O2 S1 C2 105.02(14) . . ? O1 S1 C2 104.97(15) . . ? O3 S1 C2 107.05(15) . . ? O6 S2 O4 112.95(14) . . ? O6 S2 O5 114.73(14) . . ? O4 S2 O5 108.80(13) . . ? O6 S2 C5 106.52(14) . . ? O4 S2 C5 109.40(14) . . ? O5 S2 C5 103.93(14) . . ? O6 S2 Sr1 29.11(9) . 1_455 ? O4 S2 Sr1 84.05(10) . 1_455 ? O5 S2 Sr1 125.08(9) . 1_455 ? C5 S2 Sr1 122.09(11) . 1_455 ? S1 O1 Sr1 140.53(14) . . ? S1 O2 Sr1 138.28(14) . 1_655 ? S1 O3 Sr1 135.20(13) . 2_676 ? S2 O4 Sr1 164.29(14) . 2_576 ? S2 O4 Sr1 93.24(10) . . ? Sr1 O4 Sr1 101.68(7) 2_576 . ? S2 O5 Sr1 133.76(12) . 2_566 ? S2 O5 Sr1 107.18(11) . . ? Sr1 O5 Sr1 112.65(7) 2_566 . ? S2 O6 Sr1 134.69(14) . 1_455 ? C3 N1 N2 103.8(3) . . ? C1 N2 N1 113.1(3) . . ? C6 N3 N4 103.7(3) . . ? C4 N4 N3 112.9(3) . . ? N2 C1 C2 106.2(3) . . ? C1 C2 C3 105.4(3) . . ? C1 C2 S1 127.2(3) . . ? C3 C2 S1 127.4(3) . . ? N1 C3 C2 111.6(3) . . ? N4 C4 C5 106.9(3) . . ? C4 C5 C6 105.1(3) . . ? C4 C5 S2 127.4(3) . . ? C6 C5 S2 127.3(3) . . ? N3 C6 C5 111.4(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.365 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.131 #===END data_copperpyrazolesulfonate _database_code_depnum_ccdc_archive 'CCDC 742365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Cu N4 O12 S2' _chemical_formula_weight 465.90 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' Cu Cu 0.3201 1.2651 '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 9.0315(10) _cell_length_b 13.2968(15) _cell_length_c 7.7103(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.747(2) _cell_angle_gamma 90.00 _cell_volume 871.48(17) _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 blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 478 _exptl_absorpt_coefficient_mu 1.559 _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 3709 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1252 _reflns_number_gt 1180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.3861P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1252 _refine_ls_number_parameters 121 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Cu1 Cu 0.5000 0.5000 0.0000 0.02472(17) Uani 1 2 d S . . S1 S 0.28292(6) 0.09072(4) 0.03222(7) 0.02409(18) Uani 1 1 d . . . O1 O 0.2403(2) 0.04705(13) -0.1514(2) 0.0374(4) Uani 1 1 d . . . O2 O 0.3699(2) 0.01986(12) 0.1726(2) 0.0356(4) Uani 1 1 d . . . O3 O 0.14845(19) 0.13461(12) 0.0665(2) 0.0389(4) Uani 1 1 d . . . O4 O 0.30405(18) 0.52269(12) 0.0527(2) 0.0289(4) Uani 1 1 d D . . O5 O 0.03962(19) 0.44578(14) 0.8255(2) 0.0414(4) Uani 1 1 d D . . O6 O 0.8938(3) 0.2857(2) 0.9712(5) 0.0992(10) Uani 1 1 d D . . N1 N 0.4881(2) 0.35052(14) 0.0309(2) 0.0264(4) Uani 1 1 d . . . N2 N 0.5987(2) 0.28560(14) 0.0180(3) 0.0306(4) Uani 1 1 d . . . H2 H 0.6875 0.3036 0.0095 0.037 Uiso 1 1 calc R . . C1 C 0.5540(3) 0.19047(17) 0.0199(3) 0.0322(5) Uani 1 1 d . . . H1 H 0.6114 0.1335 0.0127 0.039 Uiso 1 1 calc R . . C2 C 0.4067(2) 0.19250(15) 0.0347(3) 0.0252(5) Uani 1 1 d . . . C3 C 0.3707(3) 0.29334(16) 0.0419(3) 0.0274(5) Uani 1 1 d . . . H3 H 0.2777 0.3176 0.0528 0.033 Uiso 1 1 calc R . . H4B H 0.2229 0.5027 -0.0188 0.035(8) Uiso 1 1 d RD . . H4A H 0.3074 0.5070 0.1528 0.028(7) Uiso 1 1 d RD . . H5A H -0.0368 0.4824 0.7755 0.056(10) Uiso 1 1 d RD . . H5B H 0.0662 0.4249 0.7442 0.061(10) Uiso 1 1 d RD . . H6A H 0.9288 0.3274 0.9220 0.079(12) Uiso 1 1 d RD . . H6B H 0.9402 0.2334 0.9806 0.111(16) 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 Cu1 0.0251(3) 0.0164(2) 0.0349(3) 0.00110(14) 0.01317(18) -0.00050(13) S1 0.0269(3) 0.0193(3) 0.0274(3) -0.0003(2) 0.0108(2) -0.0024(2) O1 0.0393(10) 0.0427(10) 0.0317(9) -0.0092(8) 0.0139(7) -0.0140(8) O2 0.0427(10) 0.0234(8) 0.0375(9) 0.0063(7) 0.0095(8) 0.0000(7) O3 0.0370(9) 0.0318(9) 0.0572(11) 0.0044(8) 0.0281(8) 0.0024(7) O4 0.0292(9) 0.0279(8) 0.0318(9) 0.0020(7) 0.0130(7) -0.0010(7) O5 0.0310(10) 0.0564(12) 0.0377(9) 0.0011(9) 0.0126(8) 0.0095(8) O6 0.0656(16) 0.0665(16) 0.194(3) 0.0554(19) 0.0818(19) 0.0287(14) N1 0.0281(10) 0.0189(10) 0.0333(10) 0.0002(8) 0.0119(8) 0.0007(8) N2 0.0258(10) 0.0237(10) 0.0456(11) 0.0010(9) 0.0164(9) -0.0003(8) C1 0.0326(13) 0.0196(12) 0.0471(14) 0.0008(10) 0.0170(10) 0.0023(10) C2 0.0287(12) 0.0194(12) 0.0273(11) 0.0011(9) 0.0093(9) -0.0022(9) C3 0.0272(12) 0.0232(12) 0.0339(12) 0.0012(10) 0.0130(10) 0.0017(10) _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 Cu1 O4 1.9681(15) . ? Cu1 O4 1.9681(15) 3_665 ? Cu1 N1 2.0091(19) 3_665 ? Cu1 N1 2.0091(19) . ? Cu1 O2 2.4124(16) 2_655 ? Cu1 O2 2.4124(16) 4_565 ? S1 O2 1.4496(16) . ? S1 O3 1.4499(17) . ? S1 O1 1.4563(16) . ? S1 C2 1.751(2) . ? O2 Cu1 2.4124(16) 2_645 ? N1 C3 1.330(3) . ? N1 N2 1.349(3) . ? N2 C1 1.329(3) . ? C1 C2 1.374(3) . ? C2 C3 1.385(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 O4 Cu1 O4 180.00(9) . 3_665 ? O4 Cu1 N1 87.75(7) . 3_665 ? O4 Cu1 N1 92.25(7) 3_665 3_665 ? O4 Cu1 N1 92.25(7) . . ? O4 Cu1 N1 87.75(7) 3_665 . ? N1 Cu1 N1 180.0 3_665 . ? O4 Cu1 O2 85.48(6) . 2_655 ? O4 Cu1 O2 94.52(6) 3_665 2_655 ? N1 Cu1 O2 89.38(6) 3_665 2_655 ? N1 Cu1 O2 90.62(6) . 2_655 ? O4 Cu1 O2 94.52(6) . 4_565 ? O4 Cu1 O2 85.48(6) 3_665 4_565 ? N1 Cu1 O2 90.62(6) 3_665 4_565 ? N1 Cu1 O2 89.38(6) . 4_565 ? O2 Cu1 O2 180.0 2_655 4_565 ? O2 S1 O3 113.68(10) . . ? O2 S1 O1 111.41(10) . . ? O3 S1 O1 112.02(10) . . ? O2 S1 C2 108.14(10) . . ? O3 S1 C2 104.94(10) . . ? O1 S1 C2 106.07(9) . . ? S1 O2 Cu1 143.31(10) . 2_645 ? C3 N1 N2 105.36(17) . . ? C3 N1 Cu1 130.45(15) . . ? N2 N1 Cu1 123.60(14) . . ? C1 N2 N1 111.87(19) . . ? N2 C1 C2 106.78(19) . . ? C1 C2 C3 105.60(18) . . ? C1 C2 S1 128.06(16) . . ? C3 C2 S1 126.25(17) . . ? N1 C3 C2 110.38(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.331 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.058