# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email marc.fourmigue@univ-rennes1.fr _publ_contact_author_name 'Marc Fourmigue' _publ_author_name 'Marc Fourmigue' data_import1 _database_code_depnum_ccdc_archive 'CCDC 848302' #TrackingRef '- (S2O4)C=O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Marc Fourmigue' _chemical_melting_point ? _chemical_formula_moiety 'C13 H20 O5 S4' _chemical_formula_sum 'C13 H20 O5 S4' _chemical_formula_weight 384.53 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 8.2045(16) _cell_length_b 11.888(2) _cell_length_c 17.949(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.79(3) _cell_angle_gamma 90.00 _cell_volume 1725.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3083 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.945 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.8357028 # #-------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16204 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3937 _reflns_number_gt 2726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0249P)^2^+0.7544P] 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 3937 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.23116(8) -0.01062(5) 0.06377(4) 0.04611(16) Uani 1 1 d . . . S2 S 0.49124(7) 0.16025(5) 0.04782(3) 0.04124(15) Uani 1 1 d . . . S3 S 0.31089(8) 0.32306(5) 0.15917(3) 0.04517(16) Uani 1 1 d . . . S4 S 0.08262(8) 0.12587(5) 0.17136(4) 0.04522(16) Uani 1 1 d . . . O1 O -0.0245(2) -0.07570(15) 0.12417(12) 0.0614(5) Uani 1 1 d . . . O2 O 0.3035(2) 0.37393(14) -0.11794(9) 0.0472(4) Uani 1 1 d . . . O3 O 0.2261(2) 0.57528(14) -0.03249(9) 0.0465(4) Uani 1 1 d . . . O4 O 0.2513(2) 0.71088(14) 0.11037(9) 0.0465(4) Uani 1 1 d . . . O5 O 0.2520(2) 0.54101(13) 0.22909(9) 0.0451(4) Uani 1 1 d . . . C1 C 0.0757(3) -0.0026(2) 0.12002(14) 0.0437(5) Uani 1 1 d . . . C2 C 0.3172(3) 0.12246(18) 0.08696(11) 0.0340(5) Uani 1 1 d . . . C3 C 0.4014(3) 0.2147(2) -0.04448(12) 0.0416(5) Uani 1 1 d . . . H3A H 0.4767 0.2005 -0.0796 0.050 Uiso 1 1 calc R . . H3B H 0.2992 0.1749 -0.0627 0.050 Uiso 1 1 calc R . . C4 C 0.3664(3) 0.3384(2) -0.04285(12) 0.0444(5) Uani 1 1 d . . . H4A H 0.2860 0.3533 -0.0102 0.053 Uiso 1 1 calc R . . H4B H 0.4670 0.3792 -0.0234 0.053 Uiso 1 1 calc R . . C5 C 0.3375(3) 0.4884(2) -0.13276(14) 0.0515(6) Uani 1 1 d . . . H5A H 0.3419 0.4965 -0.1862 0.062 Uiso 1 1 calc R . . H5B H 0.4458 0.5076 -0.1049 0.062 Uiso 1 1 calc R . . C6 C 0.2142(3) 0.5699(2) -0.11229(13) 0.0505(6) Uani 1 1 d . . . H6A H 0.2344 0.6439 -0.1317 0.061 Uiso 1 1 calc R . . H6B H 0.1036 0.5466 -0.1350 0.061 Uiso 1 1 calc R . . C7 C 0.1092(3) 0.6504(2) -0.01003(14) 0.0501(6) Uani 1 1 d . . . H7A H -0.0011 0.6303 -0.0352 0.060 Uiso 1 1 calc R . . H7B H 0.1322 0.7264 -0.0250 0.060 Uiso 1 1 calc R . . C8 C 0.1165(3) 0.6459(2) 0.07365(14) 0.0482(6) Uani 1 1 d . . . H8A H 0.0141 0.6747 0.0864 0.058 Uiso 1 1 calc R . . H8B H 0.1292 0.5685 0.0908 0.058 Uiso 1 1 calc R . . C9 C 0.2475(4) 0.7314(2) 0.18808(14) 0.0493(6) Uani 1 1 d . . . H9A H 0.1332 0.7344 0.1954 0.059 Uiso 1 1 calc R . . H9B H 0.2966 0.8044 0.2016 0.059 Uiso 1 1 calc R . . C10 C 0.3362(3) 0.64526(19) 0.24013(14) 0.0473(6) Uani 1 1 d . . . H10A H 0.4483 0.6366 0.2304 0.057 Uiso 1 1 calc R . . H10B H 0.3419 0.6695 0.2921 0.057 Uiso 1 1 calc R . . C11 C 0.3240(3) 0.45603(19) 0.27937(12) 0.0433(5) Uani 1 1 d . . . H11A H 0.3017 0.4704 0.3299 0.052 Uiso 1 1 calc R . . H11B H 0.4429 0.4545 0.2814 0.052 Uiso 1 1 calc R . . C12 C 0.2486(3) 0.34501(19) 0.25020(12) 0.0419(5) Uani 1 1 d . . . H12A H 0.1291 0.3479 0.2448 0.050 Uiso 1 1 calc R . . H12B H 0.2891 0.2845 0.2847 0.050 Uiso 1 1 calc R . . C13 C 0.2492(3) 0.18524(18) 0.13613(12) 0.0341(5) 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 S1 0.0537(4) 0.0364(3) 0.0516(4) -0.0058(3) 0.0184(3) -0.0087(3) S2 0.0375(3) 0.0481(3) 0.0403(3) -0.0001(3) 0.0127(2) -0.0030(3) S3 0.0663(4) 0.0349(3) 0.0389(3) -0.0028(2) 0.0220(3) -0.0101(3) S4 0.0486(3) 0.0424(3) 0.0500(3) 0.0028(3) 0.0235(3) -0.0041(3) O1 0.0556(11) 0.0494(11) 0.0826(14) 0.0037(9) 0.0217(10) -0.0176(9) O2 0.0569(10) 0.0486(10) 0.0338(8) -0.0020(7) 0.0010(7) -0.0058(8) O3 0.0503(9) 0.0531(10) 0.0352(8) 0.0020(7) 0.0043(7) 0.0061(8) O4 0.0503(9) 0.0497(10) 0.0401(9) 0.0009(7) 0.0097(7) -0.0143(8) O5 0.0558(10) 0.0330(8) 0.0436(9) 0.0047(7) 0.0001(7) -0.0015(7) C1 0.0434(12) 0.0401(13) 0.0479(13) 0.0057(10) 0.0085(10) -0.0049(11) C2 0.0364(11) 0.0332(11) 0.0331(11) 0.0028(9) 0.0078(9) -0.0029(9) C3 0.0494(13) 0.0447(13) 0.0331(11) -0.0055(10) 0.0144(10) -0.0107(11) C4 0.0470(13) 0.0506(14) 0.0339(12) -0.0066(10) 0.0024(10) 0.0009(11) C5 0.0621(16) 0.0556(16) 0.0403(13) -0.0026(11) 0.0183(12) -0.0176(13) C6 0.0691(16) 0.0466(14) 0.0344(13) 0.0057(10) 0.0045(11) -0.0096(12) C7 0.0474(13) 0.0479(15) 0.0512(15) -0.0015(12) -0.0021(11) 0.0042(11) C8 0.0429(13) 0.0534(15) 0.0498(14) -0.0064(12) 0.0121(11) -0.0093(11) C9 0.0712(17) 0.0330(13) 0.0447(14) -0.0019(10) 0.0126(12) -0.0044(12) C10 0.0614(15) 0.0354(13) 0.0434(13) -0.0032(10) 0.0039(11) -0.0054(11) C11 0.0600(14) 0.0377(12) 0.0320(12) 0.0012(9) 0.0075(10) 0.0030(11) C12 0.0585(14) 0.0354(12) 0.0339(12) 0.0043(9) 0.0142(10) 0.0015(11) C13 0.0377(11) 0.0337(11) 0.0315(11) 0.0045(9) 0.0074(9) -0.0018(9) _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 C2 1.753(2) . ? S1 C1 1.759(2) . ? S2 C2 1.754(2) . ? S2 C3 1.814(2) . ? S3 C13 1.744(2) . ? S3 C12 1.812(2) . ? S4 C13 1.749(2) . ? S4 C1 1.779(3) . ? O1 C1 1.207(3) . ? O2 C4 1.423(3) . ? O2 C5 1.424(3) . ? O3 C7 1.418(3) . ? O3 C6 1.420(3) . ? O4 C8 1.416(3) . ? O4 C9 1.421(3) . ? O5 C11 1.415(3) . ? O5 C10 1.416(3) . ? C2 C13 1.347(3) . ? C3 C4 1.500(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.491(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.494(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.490(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.513(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 C2 S1 C1 96.71(11) . . ? C2 S2 C3 103.01(10) . . ? C13 S3 C12 103.54(10) . . ? C13 S4 C1 96.74(10) . . ? C4 O2 C5 114.18(18) . . ? C7 O3 C6 112.40(18) . . ? C8 O4 C9 113.90(18) . . ? C11 O5 C10 113.24(18) . . ? O1 C1 S1 124.3(2) . . ? O1 C1 S4 123.24(19) . . ? S1 C1 S4 112.41(12) . . ? C13 C2 S1 117.41(16) . . ? C13 C2 S2 125.22(17) . . ? S1 C2 S2 117.29(12) . . ? C4 C3 S2 112.41(16) . . ? C4 C3 H3A 109.1 . . ? S2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? S2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? O2 C4 C3 108.20(18) . . ? O2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O2 C5 C6 114.4(2) . . ? O2 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? O2 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? O3 C6 C5 110.1(2) . . ? O3 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O3 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O3 C7 C8 110.5(2) . . ? O3 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O3 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O4 C8 C7 110.07(19) . . ? O4 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O4 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? O4 C9 C10 114.1(2) . . ? O4 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? O4 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O5 C10 C9 109.8(2) . . ? O5 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O5 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? O5 C11 C12 107.48(18) . . ? O5 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O5 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 C12 S3 106.04(15) . . ? C11 C12 H12A 110.5 . . ? S3 C12 H12A 110.5 . . ? C11 C12 H12B 110.5 . . ? S3 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C2 C13 S3 122.68(16) . . ? C2 C13 S4 116.71(16) . . ? S3 C13 S4 120.44(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 S1 C1 O1 179.2(2) . . . . ? C2 S1 C1 S4 -1.26(15) . . . . ? C13 S4 C1 O1 -179.1(2) . . . . ? C13 S4 C1 S1 1.35(15) . . . . ? C1 S1 C2 C13 0.7(2) . . . . ? C1 S1 C2 S2 177.64(13) . . . . ? C3 S2 C2 C13 -98.8(2) . . . . ? C3 S2 C2 S1 84.50(14) . . . . ? C2 S2 C3 C4 89.11(18) . . . . ? C5 O2 C4 C3 -151.5(2) . . . . ? S2 C3 C4 O2 177.46(14) . . . . ? C4 O2 C5 C6 -86.0(3) . . . . ? C7 O3 C6 C5 -179.0(2) . . . . ? O2 C5 C6 O3 69.0(3) . . . . ? C6 O3 C7 C8 175.2(2) . . . . ? C9 O4 C8 C7 167.2(2) . . . . ? O3 C7 C8 O4 79.7(3) . . . . ? C8 O4 C9 C10 90.8(3) . . . . ? C11 O5 C10 C9 -176.90(19) . . . . ? O4 C9 C10 O5 -67.1(3) . . . . ? C10 O5 C11 C12 -167.11(19) . . . . ? O5 C11 C12 S3 63.8(2) . . . . ? C13 S3 C12 C11 170.79(16) . . . . ? S1 C2 C13 S3 -175.07(12) . . . . ? S2 C2 C13 S3 8.2(3) . . . . ? S1 C2 C13 S4 0.2(2) . . . . ? S2 C2 C13 S4 -176.50(12) . . . . ? C12 S3 C13 C2 -157.47(19) . . . . ? C12 S3 C13 S4 27.43(17) . . . . ? C1 S4 C13 C2 -1.0(2) . . . . ? C1 S4 C13 S3 174.43(14) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.299 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.057 # Attachment '- Na[Ni(S2O4)2].cif' data_import_OJI112_150K_08mar10 _database_code_depnum_ccdc_archive 'CCDC 848303' #TrackingRef '- Na[Ni(S2O4)2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Na Ni O8 S8' _chemical_formula_sum 'C24 H40 Na Ni O8 S8' _chemical_formula_weight 794.74 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.6588(14) _cell_length_b 10.1920(6) _cell_length_c 17.5265(12) _cell_angle_alpha 90.00 _cell_angle_beta 127.742(2) _cell_angle_gamma 90.00 _cell_volume 3342.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_theta_min 2.35 _cell_measurement_reflns_used 2228 _cell_measurement_theta_max 25.71 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.934 _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12062 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3800 _reflns_number_gt 2562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (ALtomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0836P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3800 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Ni Ni 0.7500 -0.2500 0.0000 0.0215(2) Uani 1 2 d S . . Na1 Na 0.5000 -0.6588(2) -0.2500 0.0407(7) Uani 1 2 d S . . S1 S 0.66354(6) -0.15493(10) -0.12939(7) 0.0283(3) Uani 1 1 d . . . S2 S 0.77502(6) -0.36448(10) -0.07919(7) 0.0243(3) Uani 1 1 d . . . S3 S 0.58851(6) -0.18672(11) -0.34051(8) 0.0293(3) Uani 1 1 d . . . S4 S 0.69877(6) -0.41972(11) -0.29077(7) 0.0294(3) Uani 1 1 d . . . O1 O 0.46117(15) -0.4728(3) -0.3617(2) 0.0338(7) Uani 1 1 d . . . O2 O 0.37685(16) -0.6893(3) -0.4077(2) 0.0318(7) Uani 1 1 d . . . O3 O 0.49922(16) -0.8403(3) -0.3424(2) 0.0317(7) Uani 1 1 d . . . O4 O 0.61255(16) -0.6740(3) -0.2897(2) 0.0348(8) Uani 1 1 d . . . C1 C 0.6568(2) -0.2373(4) -0.2207(3) 0.0256(9) Uani 1 1 d . . . C2 C 0.7050(2) -0.3337(4) -0.1988(3) 0.0221(9) Uani 1 1 d . . . C3 C 0.5102(2) -0.2608(4) -0.3618(3) 0.0322(10) Uani 1 1 d . . . H3A H 0.5035 -0.2256 -0.3163 0.039 Uiso 1 1 calc R . . H3B H 0.4681 -0.2398 -0.4265 0.039 Uiso 1 1 calc R . . C4 C 0.5192(2) -0.4082(4) -0.3500(3) 0.0375(11) Uani 1 1 d . . . H4A H 0.5244 -0.4425 -0.3971 0.045 Uiso 1 1 calc R . . H4B H 0.5629 -0.4279 -0.2864 0.045 Uiso 1 1 calc R . . C5 C 0.4018(2) -0.4926(4) -0.4603(3) 0.0330(11) Uani 1 1 d . . . H5A H 0.4165 -0.5402 -0.4934 0.040 Uiso 1 1 calc R . . H5B H 0.3818 -0.4090 -0.4924 0.040 Uiso 1 1 calc R . . C6 C 0.3475(2) -0.5704(4) -0.4611(3) 0.0339(11) Uani 1 1 d . . . H6A H 0.3298 -0.5178 -0.4336 0.041 Uiso 1 1 calc R . . H6B H 0.3074 -0.5909 -0.5272 0.041 Uiso 1 1 calc R . . C7 C 0.3720(2) -0.7964(5) -0.4636(3) 0.0364(11) Uani 1 1 d . . . H7A H 0.3789 -0.7658 -0.5098 0.044 Uiso 1 1 calc R . . H7B H 0.3252 -0.8370 -0.4987 0.044 Uiso 1 1 calc R . . C8 C 0.4286(2) -0.8929(5) -0.3963(3) 0.0382(11) Uani 1 1 d . . . H8A H 0.4202 -0.9238 -0.3517 0.046 Uiso 1 1 calc R . . H8B H 0.4251 -0.9678 -0.4331 0.046 Uiso 1 1 calc R . . C9 C 0.5246(2) -0.8273(4) -0.3976(3) 0.0342(11) Uani 1 1 d . . . H9A H 0.4997 -0.7561 -0.4435 0.041 Uiso 1 1 calc R . . H9B H 0.5155 -0.9075 -0.4332 0.041 Uiso 1 1 calc R . . C10 C 0.6025(2) -0.7999(4) -0.3314(3) 0.0333(11) Uani 1 1 d . . . H10A H 0.6269 -0.8662 -0.2812 0.040 Uiso 1 1 calc R . . H10B H 0.6218 -0.8011 -0.3667 0.040 Uiso 1 1 calc R . . C11 C 0.6855(2) -0.6471(4) -0.2116(3) 0.0350(11) Uani 1 1 d . . . H11A H 0.7088 -0.7287 -0.1786 0.042 Uiso 1 1 calc R . . H11B H 0.6870 -0.5899 -0.1661 0.042 Uiso 1 1 calc R . . C12 C 0.7275(2) -0.5834(4) -0.2411(3) 0.0313(10) Uani 1 1 d . . . H12A H 0.7242 -0.6390 -0.2886 0.038 Uiso 1 1 calc R . . H12B H 0.7774 -0.5796 -0.1850 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 Ni 0.0245(4) 0.0223(4) 0.0164(4) -0.0029(3) 0.0119(3) -0.0007(3) Na1 0.0573(18) 0.0260(13) 0.0197(13) 0.000 0.0138(13) 0.000 S1 0.0328(6) 0.0287(6) 0.0197(5) -0.0015(4) 0.0141(5) 0.0061(5) S2 0.0261(6) 0.0270(5) 0.0187(5) -0.0023(4) 0.0131(4) 0.0019(5) S3 0.0322(6) 0.0318(6) 0.0195(5) 0.0040(4) 0.0135(5) 0.0010(5) S4 0.0370(7) 0.0339(6) 0.0218(5) -0.0044(5) 0.0203(5) -0.0014(5) O1 0.0275(17) 0.0412(18) 0.0224(16) 0.0053(13) 0.0101(14) -0.0012(15) O2 0.0383(18) 0.0316(16) 0.0270(16) 0.0005(13) 0.0207(15) 0.0021(15) O3 0.0296(17) 0.0361(17) 0.0274(16) -0.0025(13) 0.0163(15) -0.0021(15) O4 0.0326(18) 0.0281(16) 0.0362(18) -0.0043(14) 0.0172(15) 0.0006(15) C1 0.028(2) 0.029(2) 0.018(2) -0.0009(17) 0.0135(18) -0.0044(19) C2 0.026(2) 0.023(2) 0.019(2) -0.0024(16) 0.0145(18) -0.0031(18) C3 0.029(2) 0.040(3) 0.022(2) 0.0006(19) 0.0129(19) 0.005(2) C4 0.026(2) 0.035(3) 0.040(3) 0.005(2) 0.015(2) 0.000(2) C5 0.029(2) 0.040(3) 0.024(2) 0.006(2) 0.013(2) 0.005(2) C6 0.032(2) 0.041(3) 0.030(2) 0.005(2) 0.019(2) 0.006(2) C7 0.031(3) 0.044(3) 0.027(2) -0.012(2) 0.014(2) -0.006(2) C8 0.038(3) 0.035(3) 0.040(3) -0.010(2) 0.023(2) -0.009(2) C9 0.039(3) 0.035(3) 0.028(2) -0.005(2) 0.020(2) -0.001(2) C10 0.034(3) 0.030(2) 0.034(3) -0.006(2) 0.020(2) 0.002(2) C11 0.037(3) 0.031(2) 0.028(2) -0.0063(19) 0.016(2) -0.005(2) C12 0.032(2) 0.032(2) 0.028(2) -0.0070(19) 0.017(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S1 2.1417(11) 7_645 ? Ni S1 2.1417(11) . ? Ni S2 2.1551(10) . ? Ni S2 2.1551(10) 7_645 ? Na1 O3 2.452(3) 2_654 ? Na1 O3 2.452(3) . ? Na1 O1 2.463(3) 2_654 ? Na1 O1 2.463(3) . ? Na1 O2 2.523(3) 2_654 ? Na1 O2 2.523(3) . ? S1 C1 1.726(4) . ? S2 C2 1.728(4) . ? S3 C1 1.770(4) . ? S3 C3 1.816(5) . ? S4 C2 1.760(4) . ? S4 C12 1.810(4) . ? O1 C4 1.421(5) . ? O1 C5 1.425(5) . ? O2 C7 1.424(5) . ? O2 C6 1.425(5) . ? O3 C9 1.422(5) . ? O3 C8 1.428(5) . ? O4 C10 1.422(5) . ? O4 C11 1.426(5) . ? C1 C2 1.370(6) . ? C3 C4 1.514(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.503(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.489(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.485(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.519(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 S1 Ni S1 180.00(13) 7_645 . ? S1 Ni S2 88.63(4) 7_645 . ? S1 Ni S2 91.37(4) . . ? S1 Ni S2 91.37(4) 7_645 7_645 ? S1 Ni S2 88.63(4) . 7_645 ? S2 Ni S2 180.00(4) . 7_645 ? O3 Na1 O3 82.01(15) 2_654 . ? O3 Na1 O1 101.97(10) 2_654 2_654 ? O3 Na1 O1 162.58(10) . 2_654 ? O3 Na1 O1 162.58(10) 2_654 . ? O3 Na1 O1 101.97(10) . . ? O1 Na1 O1 79.37(16) 2_654 . ? O3 Na1 O2 69.31(10) 2_654 2_654 ? O3 Na1 O2 99.62(11) . 2_654 ? O1 Na1 O2 66.77(10) 2_654 2_654 ? O1 Na1 O2 125.74(11) . 2_654 ? O3 Na1 O2 99.62(11) 2_654 . ? O3 Na1 O2 69.31(10) . . ? O1 Na1 O2 125.74(11) 2_654 . ? O1 Na1 O2 66.77(10) . . ? O2 Na1 O2 165.83(17) 2_654 . ? C1 S1 Ni 104.37(15) . . ? C2 S2 Ni 104.23(14) . . ? C1 S3 C3 101.4(2) . . ? C2 S4 C12 102.86(19) . . ? C4 O1 C5 112.8(3) . . ? C4 O1 Na1 112.6(2) . . ? C5 O1 Na1 117.8(3) . . ? C7 O2 C6 113.5(3) . . ? C7 O2 Na1 113.6(3) . . ? C6 O2 Na1 112.7(3) . . ? C9 O3 C8 113.3(3) . . ? C9 O3 Na1 122.9(3) . . ? C8 O3 Na1 104.6(2) . . ? C10 O4 C11 113.0(3) . . ? C2 C1 S1 120.0(3) . . ? C2 C1 S3 122.7(3) . . ? S1 C1 S3 117.2(2) . . ? C1 C2 S2 119.0(3) . . ? C1 C2 S4 120.8(3) . . ? S2 C2 S4 120.1(2) . . ? C4 C3 S3 110.0(3) . . ? C4 C3 H3A 109.7 . . ? S3 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? S3 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O1 C4 C3 113.3(4) . . ? O1 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? O1 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? O1 C5 C6 106.7(4) . . ? O1 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O1 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? O2 C6 C5 111.9(4) . . ? O2 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? O2 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? O2 C7 C8 107.9(4) . . ? O2 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O2 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O3 C8 C7 113.4(4) . . ? O3 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? O3 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? O3 C9 C10 108.9(4) . . ? O3 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O3 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O4 C10 C9 108.0(4) . . ? O4 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O4 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O4 C11 C12 114.6(4) . . ? O4 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? O4 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 S4 115.2(3) . . ? C11 C12 H12A 108.5 . . ? S4 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? S4 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ni S1 C1 7.34(15) . . . . ? S2 Ni S1 C1 -172.66(15) 7_645 . . . ? S1 Ni S2 C2 171.20(14) 7_645 . . . ? S1 Ni S2 C2 -8.80(14) . . . . ? O3 Na1 O1 C4 169.6(4) 2_654 . . . ? O3 Na1 O1 C4 -88.8(3) . . . . ? O1 Na1 O1 C4 73.5(3) 2_654 . . . ? O2 Na1 O1 C4 22.5(3) 2_654 . . . ? O2 Na1 O1 C4 -149.8(3) . . . . ? O3 Na1 O1 C5 -56.3(5) 2_654 . . . ? O3 Na1 O1 C5 45.3(3) . . . . ? O1 Na1 O1 C5 -152.4(3) 2_654 . . . ? O2 Na1 O1 C5 156.6(3) 2_654 . . . ? O2 Na1 O1 C5 -15.7(3) . . . . ? O3 Na1 O2 C7 -75.5(3) 2_654 . . . ? O3 Na1 O2 C7 2.1(3) . . . . ? O1 Na1 O2 C7 172.1(3) 2_654 . . . ? O1 Na1 O2 C7 115.9(3) . . . . ? O2 Na1 O2 C7 -37.9(3) 2_654 . . . ? O3 Na1 O2 C6 153.6(3) 2_654 . . . ? O3 Na1 O2 C6 -128.8(3) . . . . ? O1 Na1 O2 C6 41.2(3) 2_654 . . . ? O1 Na1 O2 C6 -15.0(2) . . . . ? O2 Na1 O2 C6 -168.8(3) 2_654 . . . ? O3 Na1 O3 C9 -156.0(3) 2_654 . . . ? O1 Na1 O3 C9 -51.4(5) 2_654 . . . ? O1 Na1 O3 C9 41.3(3) . . . . ? O2 Na1 O3 C9 -88.7(3) 2_654 . . . ? O2 Na1 O3 C9 100.5(3) . . . . ? O3 Na1 O3 C8 73.1(2) 2_654 . . . ? O1 Na1 O3 C8 177.7(4) 2_654 . . . ? O1 Na1 O3 C8 -89.7(3) . . . . ? O2 Na1 O3 C8 140.4(3) 2_654 . . . ? O2 Na1 O3 C8 -30.4(3) . . . . ? Ni S1 C1 C2 -3.9(4) . . . . ? Ni S1 C1 S3 178.81(19) . . . . ? C3 S3 C1 C2 105.7(4) . . . . ? C3 S3 C1 S1 -77.1(3) . . . . ? S1 C1 C2 S2 -3.6(5) . . . . ? S3 C1 C2 S2 173.6(2) . . . . ? S1 C1 C2 S4 179.6(2) . . . . ? S3 C1 C2 S4 -3.3(5) . . . . ? Ni S2 C2 C1 9.0(3) . . . . ? Ni S2 C2 S4 -174.09(19) . . . . ? C12 S4 C2 C1 -144.8(3) . . . . ? C12 S4 C2 S2 38.4(3) . . . . ? C1 S3 C3 C4 -59.4(4) . . . . ? C5 O1 C4 C3 81.1(5) . . . . ? Na1 O1 C4 C3 -142.5(3) . . . . ? S3 C3 C4 O1 177.6(3) . . . . ? C4 O1 C5 C6 175.7(3) . . . . ? Na1 O1 C5 C6 41.7(4) . . . . ? C7 O2 C6 C5 -88.0(5) . . . . ? Na1 O2 C6 C5 42.9(4) . . . . ? O1 C5 C6 O2 -55.3(5) . . . . ? C6 O2 C7 C8 156.4(4) . . . . ? Na1 O2 C7 C8 25.9(4) . . . . ? C9 O3 C8 C7 -75.7(5) . . . . ? Na1 O3 C8 C7 60.6(4) . . . . ? O2 C7 C8 O3 -60.3(5) . . . . ? C8 O3 C9 C10 -167.9(4) . . . . ? Na1 O3 C9 C10 64.8(4) . . . . ? C11 O4 C10 C9 169.0(4) . . . . ? O3 C9 C10 O4 -66.6(5) . . . . ? C10 O4 C11 C12 89.1(4) . . . . ? O4 C11 C12 S4 65.7(4) . . . . ? C2 S4 C12 C11 56.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.523 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.163 data_import _database_code_depnum_ccdc_archive 'CCDC 848304' #TrackingRef '- Ni[Ni(S2O4)2]__rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Ni O8 S8, Ni0.5, O0.5' _chemical_formula_sum 'C24 H40 Ni1.5 O8.5 S8 ' _chemical_formula_weight 809.14 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.4074(4) _cell_length_b 14.0031(4) _cell_length_c 19.1875(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.5930(10) _cell_angle_gamma 90.00 _cell_volume 3486.15(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8871 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.878 _exptl_absorpt_correction_T_max 0.917 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.882163 #-------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15378 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3991 _reflns_number_gt 3469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (ALtomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1081P)^2^+7.4622P] 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 3991 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1811 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Ni2 Ni 1.0000 -0.42404(8) 0.7500 0.0589(3) Uani 0.50 2 d SP . . O5 O 1.0000 -0.42404(8) 0.7500 0.0589(3) Uani 0.50 2 d SP . . Ni1 Ni 1.0000 0.0000 0.5000 0.0451(2) Uani 1 2 d S . . S1 S 1.08158(9) -0.13434(7) 0.50983(7) 0.0677(3) Uani 1 1 d . . . S2 S 0.92169(7) -0.04419(6) 0.57890(5) 0.0474(2) Uani 1 1 d . . . S4 S 0.91623(7) -0.21549(6) 0.66946(4) 0.0467(2) Uani 1 1 d . . . C1 C 1.0393(3) -0.1982(3) 0.5740(2) 0.0527(8) Uani 1 1 d . . . C2 C 0.9670(2) -0.1582(2) 0.60405(17) 0.0430(6) Uani 1 1 d . . . C3 C 0.7973(3) -0.2645(3) 0.61459(19) 0.0493(7) Uani 1 1 d . B . H3A H 0.7573 -0.2893 0.6462 0.059 Uiso 1 1 calc R . . H3B H 0.7580 -0.2131 0.5867 0.059 Uiso 1 1 calc R . . C4 C 0.8100(3) -0.3419(3) 0.56416(19) 0.0543(8) Uani 1 1 d . . . H4A H 0.7431 -0.3594 0.5337 0.065 Uiso 1 1 calc R A 1 H4B H 0.8525 -0.3193 0.5335 0.065 Uiso 1 1 calc R A 1 O1 O 0.8567(2) -0.42282(17) 0.60359(12) 0.0517(6) Uani 1 1 d . B 1 C5 C 0.8664(4) -0.4999(3) 0.5575(2) 0.0653(11) Uani 1 1 d . B 1 H5A H 0.9098 -0.4809 0.5264 0.078 Uiso 1 1 calc R B 1 H5B H 0.7991 -0.5167 0.5274 0.078 Uiso 1 1 calc R B 1 C6 C 0.9120(4) -0.5829(3) 0.6009(3) 0.0745(12) Uani 1 1 d . B 1 H6A H 0.8719 -0.5992 0.6348 0.089 Uiso 1 1 calc R B 1 H6B H 0.9128 -0.6376 0.5701 0.089 Uiso 1 1 calc R B 1 O2 O 1.0149(3) -0.5578(3) 0.6387(2) 0.1025(14) Uani 1 1 d . B 1 C7 C 1.0797(5) -0.6300(4) 0.6665(4) 0.0941(17) Uani 1 1 d . B 1 H7A H 1.0797 -0.6773 0.6295 0.113 Uiso 1 1 calc R B 1 H7B H 1.0570 -0.6608 0.7051 0.113 Uiso 1 1 calc R B 1 C8 C 1.1851(4) -0.5914(4) 0.6945(3) 0.0770(12) Uani 1 1 d . B 1 H8A H 1.2328 -0.6434 0.7115 0.092 Uiso 1 1 calc R B 1 H8B H 1.2067 -0.5589 0.6561 0.092 Uiso 1 1 calc R B 1 O3 O 1.1874(2) -0.5277(3) 0.75085(18) 0.0739(8) Uani 1 1 d . B 1 C9 C 1.2880(4) -0.4951(3) 0.7865(3) 0.0690(11) Uani 1 1 d . B 1 H9A H 1.3338 -0.5497 0.7974 0.083 Uiso 1 1 calc R B 1 H9B H 1.2854 -0.4658 0.8318 0.083 Uiso 1 1 calc R B 1 C10 C 1.3318(4) -0.4248(4) 0.7437(3) 0.0786(13) Uani 1 1 d . B 1 H10A H 1.4004 -0.4060 0.7704 0.094 Uiso 1 1 calc R B 1 H10B H 1.3370 -0.4537 0.6988 0.094 Uiso 1 1 calc R B 1 O4 O 1.2669(4) -0.3439(3) 0.72933(18) 0.0933(12) Uani 1 1 d . B 1 C11 C 1.2764(6) -0.2851(4) 0.6707(3) 0.0957(17) Uani 1 1 d . B 1 H11A H 1.3482 -0.2832 0.6693 0.115 Uiso 1 1 calc R B 1 H11B H 1.2560 -0.2205 0.6790 0.115 Uiso 1 1 calc R B 1 C12 C 1.2148(3) -0.3174(4) 0.6012(2) 0.0708(11) Uani 1 1 d . B 1 H12A H 1.2363 -0.3815 0.5927 0.085 Uiso 1 1 calc R B 1 H12B H 1.2291 -0.2765 0.5641 0.085 Uiso 1 1 calc R B 1 S3 S 1.07911(10) -0.31807(8) 0.59232(8) 0.0774(4) Uani 1 1 d . B 1 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 Ni2 0.0729(8) 0.0408(5) 0.0526(6) 0.000 -0.0034(5) 0.000 O5 0.0729(8) 0.0408(5) 0.0526(6) 0.000 -0.0034(5) 0.000 Ni1 0.0464(3) 0.0392(3) 0.0527(4) -0.0002(2) 0.0180(3) -0.0065(2) S1 0.0750(7) 0.0495(5) 0.0959(8) 0.0111(5) 0.0536(6) 0.0063(4) S2 0.0509(5) 0.0434(4) 0.0516(5) 0.0018(3) 0.0196(4) 0.0002(3) S4 0.0522(5) 0.0522(5) 0.0344(4) 0.0049(3) 0.0083(3) 0.0017(3) C1 0.0523(18) 0.0445(17) 0.065(2) 0.0042(15) 0.0216(16) -0.0005(14) C2 0.0408(15) 0.0440(15) 0.0427(15) 0.0006(12) 0.0079(12) -0.0051(12) C3 0.0419(16) 0.0550(18) 0.0508(17) 0.0137(14) 0.0111(13) -0.0007(14) C4 0.0521(18) 0.062(2) 0.0431(16) 0.0055(15) 0.0021(14) -0.0086(16) O1 0.0605(14) 0.0499(13) 0.0436(12) -0.0034(10) 0.0114(10) -0.0045(11) C5 0.062(2) 0.074(3) 0.056(2) -0.0194(18) 0.0095(18) -0.0085(19) C6 0.086(3) 0.052(2) 0.081(3) -0.023(2) 0.014(2) -0.008(2) O2 0.100(3) 0.069(2) 0.112(3) -0.034(2) -0.022(2) 0.0193(19) C7 0.099(4) 0.071(3) 0.114(4) -0.017(3) 0.032(3) 0.012(3) C8 0.075(3) 0.078(3) 0.082(3) -0.012(2) 0.027(2) 0.015(2) O3 0.0619(17) 0.087(2) 0.0764(19) -0.0134(17) 0.0234(15) 0.0111(15) C9 0.065(3) 0.077(3) 0.066(3) 0.003(2) 0.017(2) 0.016(2) C10 0.081(3) 0.086(3) 0.072(3) -0.010(2) 0.027(2) 0.002(3) O4 0.144(4) 0.078(2) 0.0568(18) 0.0034(16) 0.022(2) 0.026(2) C11 0.114(4) 0.068(3) 0.097(4) -0.004(3) 0.013(3) -0.020(3) C12 0.068(3) 0.084(3) 0.068(2) 0.014(2) 0.031(2) 0.013(2) S3 0.0694(7) 0.0540(6) 0.1186(10) 0.0198(6) 0.0416(7) 0.0153(5) _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 Ni1 S2 2.1397(8) 5_756 ? Ni1 S2 2.1397(8) . ? Ni1 S1 2.1603(10) 5_756 ? Ni1 S1 2.1603(10) . ? S1 C1 1.729(4) . ? S2 C2 1.733(3) . ? S4 C2 1.764(3) . ? S4 C3 1.809(3) . ? C1 C2 1.367(5) . ? C1 S3 1.769(4) . ? C3 C4 1.491(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O1 1.418(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? O1 C5 1.423(5) . ? C5 C6 1.470(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O2 1.431(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O2 C7 1.353(7) . ? C7 C8 1.482(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3 1.397(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O3 C9 1.425(6) . ? C9 C10 1.494(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O4 1.413(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O4 C11 1.426(7) . ? C11 C12 1.453(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 S3 1.784(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni1 S2 180.0 5_756 . ? S2 Ni1 S1 90.82(3) 5_756 5_756 ? S2 Ni1 S1 89.18(3) . 5_756 ? S2 Ni1 S1 89.18(3) 5_756 . ? S2 Ni1 S1 90.82(3) . . ? S1 Ni1 S1 180.0 5_756 . ? C1 S1 Ni1 105.27(13) . . ? C2 S2 Ni1 105.27(11) . . ? C2 S4 C3 101.53(15) . . ? C2 C1 S1 118.8(3) . . ? C2 C1 S3 121.1(3) . . ? S1 C1 S3 119.7(2) . . ? C1 C2 S2 119.8(3) . . ? C1 C2 S4 123.7(3) . . ? S2 C2 S4 116.48(19) . . ? C4 C3 S4 115.2(3) . . ? C4 C3 H3A 108.5 . . ? S4 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? S4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? O1 C4 C3 110.0(3) . . ? O1 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O1 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O1 C5 111.8(3) . . ? O1 C5 C6 109.7(4) . . ? O1 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O1 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? O2 C6 C5 107.6(4) . . ? O2 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O2 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C7 O2 C6 117.3(4) . . ? O2 C7 C8 109.2(5) . . ? O2 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O2 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O3 C8 C7 110.3(4) . . ? O3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 O3 C9 114.1(4) . . ? O3 C9 C10 113.8(4) . . ? O3 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? O3 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? O4 C10 C9 109.1(4) . . ? O4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C10 O4 C11 116.4(5) . . ? O4 C11 C12 113.7(5) . . ? O4 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? O4 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 S3 114.8(4) . . ? C11 C12 H12A 108.6 . . ? S3 C12 H12A 108.6 . . ? C11 C12 H12B 108.6 . . ? S3 C12 H12B 108.6 . . ? H12A C12 H12B 107.5 . . ? C1 S3 C12 105.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ni1 S1 C1 179.56(15) 5_756 . . . ? S2 Ni1 S1 C1 -0.44(15) . . . . ? S1 Ni1 S1 C1 -53(12) 5_756 . . . ? S2 Ni1 S2 C2 2(100) 5_756 . . . ? S1 Ni1 S2 C2 179.86(11) 5_756 . . . ? S1 Ni1 S2 C2 -0.14(11) . . . . ? Ni1 S1 C1 C2 1.2(3) . . . . ? Ni1 S1 C1 S3 174.21(19) . . . . ? S1 C1 C2 S2 -1.4(4) . . . . ? S3 C1 C2 S2 -174.4(2) . . . . ? S1 C1 C2 S4 179.44(19) . . . . ? S3 C1 C2 S4 6.5(5) . . . . ? Ni1 S2 C2 C1 0.9(3) . . . . ? Ni1 S2 C2 S4 -179.89(13) . . . . ? C3 S4 C2 C1 -97.2(3) . . . . ? C3 S4 C2 S2 83.6(2) . . . . ? C2 S4 C3 C4 67.2(3) . . . . ? S4 C3 C4 O1 65.0(3) . . . . ? C3 C4 O1 C5 177.6(3) . . . . ? C4 O1 C5 C6 -178.1(4) . . . . ? O1 C5 C6 O2 -65.2(5) . . . . ? C5 C6 O2 C7 -162.9(5) . . . . ? C6 O2 C7 C8 172.4(5) . . . . ? O2 C7 C8 O3 63.1(7) . . . . ? C7 C8 O3 C9 173.3(4) . . . . ? C8 O3 C9 C10 73.7(5) . . . . ? O3 C9 C10 O4 60.1(5) . . . . ? C9 C10 O4 C11 -159.8(4) . . . . ? C10 O4 C11 C12 85.1(7) . . . . ? O4 C11 C12 S3 62.2(6) . . . . ? C2 C1 S3 C12 -140.4(3) . . . . ? S1 C1 S3 C12 46.7(3) . . . . ? C11 C12 S3 C1 80.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.352 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.144 # Attachment '- [Ni(S2O4)2].cif' data_import3 _database_code_depnum_ccdc_archive 'CCDC 848305' #TrackingRef '- [Ni(S2O4)2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 Ni O8 S8' _chemical_formula_sum 'C24 H40 Ni O8 S8' _chemical_formula_weight 771.75 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1918(4) _cell_length_b 9.5486(4) _cell_length_c 10.6697(4) _cell_angle_alpha 67.4590(10) _cell_angle_beta 74.151(2) _cell_angle_gamma 84.463(2) _cell_volume 832.01(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6645 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.935 #----------------------------- Remark ------------------------------# # Tmax and Tmin values correspond to EXPECTED values calculated # # from crystal size. In the case of absorption correction performed # # with SADABS program, Tmax should be given as Tmax_expected and # # and Tmin = Tmax * 'relative-correction-factor'. # # SADABS output: # # Ratio of minimum to maximum apparent transmission: 0.799223 #-------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10148 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3777 _reflns_number_gt 3498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0407P)^2^+0.1129P] 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 3777 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _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 Ni Ni 1.0000 0.0000 1.0000 0.01349(9) Uani 1 2 d S . . S1 S 1.17741(4) 0.03250(4) 1.08034(4) 0.01672(10) Uani 1 1 d . . . S2 S 1.07717(4) -0.22157(4) 1.01078(4) 0.01644(10) Uani 1 1 d . . . S3 S 1.43548(4) -0.16531(5) 1.17611(4) 0.01903(11) Uani 1 1 d . . . S4 S 1.34466(4) -0.41019(4) 1.09677(4) 0.01868(11) Uani 1 1 d . . . O1 O 1.39488(13) -0.13100(12) 1.46127(11) 0.0197(2) Uani 1 1 d . . . O2 O 1.28106(13) -0.41272(13) 1.72339(12) 0.0234(3) Uani 1 1 d . . . O3 O 1.18330(13) -0.60502(13) 1.58317(12) 0.0239(3) Uani 1 1 d . . . O4 O 1.16122(13) -0.67208(13) 1.34473(11) 0.0235(3) Uani 1 1 d . . . C1 C 1.27536(16) -0.13347(17) 1.11060(15) 0.0143(3) Uani 1 1 d . . . C2 C 1.23180(16) -0.24856(17) 1.07729(15) 0.0141(3) Uani 1 1 d . . . C3 C 1.44929(18) 0.00171(18) 1.21406(16) 0.0188(3) Uani 1 1 d . . . H3A H 1.5535 0.0148 1.2117 0.023 Uiso 1 1 calc R . . H3B H 1.4222 0.0899 1.1411 0.023 Uiso 1 1 calc R . . C4 C 1.34893(18) -0.00575(18) 1.35519(16) 0.0192(3) Uani 1 1 d . . . H4A H 1.3585 0.0874 1.3689 0.023 Uiso 1 1 calc R . . H4B H 1.2440 -0.0183 1.3594 0.023 Uiso 1 1 calc R . . C5 C 1.31667(18) -0.13759(18) 1.59869(16) 0.0205(3) Uani 1 1 d . . . H5A H 1.2085 -0.1344 1.6082 0.025 Uiso 1 1 calc R . . H5B H 1.3445 -0.0503 1.6128 0.025 Uiso 1 1 calc R . . C6 C 1.35501(19) -0.28063(19) 1.70808(17) 0.0226(3) Uani 1 1 d . . . H6A H 1.4635 -0.2954 1.6836 0.027 Uiso 1 1 calc R . . H6B H 1.3279 -0.2683 1.7977 0.027 Uiso 1 1 calc R . . C7 C 1.36729(18) -0.48493(18) 1.63191(17) 0.0208(3) Uani 1 1 d . . . H7A H 1.4686 -0.5043 1.6454 0.025 Uiso 1 1 calc R . . H7B H 1.3755 -0.4182 1.5351 0.025 Uiso 1 1 calc R . . C8 C 1.29383(18) -0.63188(18) 1.66070(17) 0.0210(3) Uani 1 1 d . . . H8A H 1.3700 -0.7002 1.6342 0.025 Uiso 1 1 calc R . . H8B H 1.2462 -0.6794 1.7603 0.025 Uiso 1 1 calc R . . C9 C 1.1276(2) -0.74215(19) 1.59023(18) 0.0251(4) Uani 1 1 d . . . H9A H 1.0573 -0.7904 1.6809 0.030 Uiso 1 1 calc R . . H9B H 1.2108 -0.8110 1.5801 0.030 Uiso 1 1 calc R . . C10 C 1.04918(19) -0.7099(2) 1.47548(17) 0.0246(4) Uani 1 1 d . . . H10A H 0.9919 -0.7985 1.4924 0.030 Uiso 1 1 calc R . . H10B H 0.9797 -0.6264 1.4734 0.030 Uiso 1 1 calc R . . C11 C 1.09802(18) -0.60895(19) 1.22777(16) 0.0214(3) Uani 1 1 d . . . H11A H 1.0312 -0.5264 1.2368 0.026 Uiso 1 1 calc R . . H11B H 1.0397 -0.6854 1.2231 0.026 Uiso 1 1 calc R . . C12 C 1.22579(18) -0.55105(18) 1.09607(16) 0.0198(3) Uani 1 1 d . . . H12A H 1.1835 -0.5070 1.0155 0.024 Uiso 1 1 calc R . . H12B H 1.2879 -0.6360 1.0856 0.024 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 Ni 0.01246(14) 0.01412(15) 0.01474(15) -0.00443(11) -0.00679(10) 0.00183(10) S1 0.0165(2) 0.0148(2) 0.0219(2) -0.00675(16) -0.01060(16) 0.00223(15) S2 0.0158(2) 0.0169(2) 0.0207(2) -0.00850(16) -0.00970(15) 0.00270(15) S3 0.0182(2) 0.0204(2) 0.0242(2) -0.00977(17) -0.01363(16) 0.00439(15) S4 0.0160(2) 0.0163(2) 0.0255(2) -0.00816(16) -0.00892(16) 0.00413(15) O1 0.0246(6) 0.0185(6) 0.0148(5) -0.0051(4) -0.0060(4) 0.0041(4) O2 0.0239(6) 0.0236(6) 0.0209(6) -0.0102(5) 0.0013(5) -0.0034(5) O3 0.0271(6) 0.0177(6) 0.0324(7) -0.0099(5) -0.0167(5) 0.0046(5) O4 0.0216(6) 0.0259(6) 0.0185(6) -0.0038(5) -0.0063(5) 0.0043(5) C1 0.0119(7) 0.0172(7) 0.0128(7) -0.0035(6) -0.0050(5) 0.0009(6) C2 0.0124(7) 0.0159(7) 0.0124(7) -0.0038(6) -0.0033(5) 0.0017(5) C3 0.0205(8) 0.0194(8) 0.0184(7) -0.0050(6) -0.0102(6) -0.0021(6) C4 0.0210(8) 0.0167(8) 0.0210(8) -0.0058(6) -0.0093(6) 0.0013(6) C5 0.0222(8) 0.0236(8) 0.0189(8) -0.0120(7) -0.0043(6) 0.0002(6) C6 0.0272(9) 0.0253(9) 0.0172(8) -0.0096(7) -0.0053(6) -0.0021(7) C7 0.0189(8) 0.0215(8) 0.0206(8) -0.0085(7) -0.0021(6) 0.0006(6) C8 0.0210(8) 0.0187(8) 0.0211(8) -0.0039(6) -0.0077(6) 0.0025(6) C9 0.0325(9) 0.0204(8) 0.0202(8) -0.0043(7) -0.0066(7) -0.0047(7) C10 0.0249(9) 0.0262(9) 0.0219(8) -0.0078(7) -0.0044(7) -0.0047(7) C11 0.0224(8) 0.0197(8) 0.0226(8) -0.0057(7) -0.0093(7) -0.0008(6) C12 0.0250(8) 0.0163(7) 0.0213(8) -0.0086(6) -0.0089(6) 0.0011(6) _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 Ni S1 2.1344(4) 2_757 ? Ni S1 2.1344(4) . ? Ni S2 2.1356(4) 2_757 ? Ni S2 2.1356(4) . ? S1 C1 1.7081(15) . ? S2 C2 1.7117(15) . ? S3 C1 1.7492(14) . ? S3 C3 1.8127(16) . ? S4 C2 1.7505(15) . ? S4 C12 1.8163(16) . ? O1 C4 1.4197(18) . ? O1 C5 1.4258(18) . ? O2 C6 1.4236(19) . ? O2 C7 1.4297(19) . ? O3 C9 1.419(2) . ? O3 C8 1.4242(19) . ? O4 C11 1.4177(18) . ? O4 C10 1.4276(19) . ? C1 C2 1.399(2) . ? C3 C4 1.515(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.504(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.503(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.505(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.512(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 S1 Ni S1 180.0 2_757 . ? S1 Ni S2 92.227(13) 2_757 2_757 ? S1 Ni S2 87.773(13) . 2_757 ? S1 Ni S2 87.773(14) 2_757 . ? S1 Ni S2 92.227(13) . . ? S2 Ni S2 180.0 2_757 . ? C1 S1 Ni 104.34(5) . . ? C2 S2 Ni 104.61(5) . . ? C1 S3 C3 104.14(7) . . ? C2 S4 C12 104.61(7) . . ? C4 O1 C5 112.02(12) . . ? C6 O2 C7 112.10(12) . . ? C9 O3 C8 111.92(12) . . ? C11 O4 C10 112.53(12) . . ? C2 C1 S1 119.85(11) . . ? C2 C1 S3 117.25(11) . . ? S1 C1 S3 122.85(9) . . ? C1 C2 S2 118.94(11) . . ? C1 C2 S4 118.16(11) . . ? S2 C2 S4 122.81(9) . . ? C4 C3 S3 113.52(11) . . ? C4 C3 H3A 108.9 . . ? S3 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? S3 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? O1 C4 C3 108.17(12) . . ? O1 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O1 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O1 C5 C6 110.55(13) . . ? O1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? O1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O2 C6 C5 113.97(13) . . ? O2 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? O2 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 C8 110.73(13) . . ? O2 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O3 C8 C7 110.10(13) . . ? O3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? O3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? O3 C9 C10 109.97(14) . . ? O3 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? O3 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O4 C10 C9 108.40(14) . . ? O4 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O4 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? O4 C11 C12 108.36(13) . . ? O4 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? O4 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C11 C12 S4 113.31(11) . . ? C11 C12 H12A 108.9 . . ? S4 C12 H12A 108.9 . . ? C11 C12 H12B 108.9 . . ? S4 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ni S1 C1 178.74(5) 2_757 . . . ? S2 Ni S1 C1 -1.26(5) . . . . ? S1 Ni S2 C2 -179.43(5) 2_757 . . . ? S1 Ni S2 C2 0.57(5) . . . . ? Ni S1 C1 C2 1.95(13) . . . . ? Ni S1 C1 S3 179.31(8) . . . . ? C3 S3 C1 C2 -177.27(12) . . . . ? C3 S3 C1 S1 5.31(11) . . . . ? S1 C1 C2 S2 -1.69(18) . . . . ? S3 C1 C2 S2 -179.19(7) . . . . ? S1 C1 C2 S4 174.89(8) . . . . ? S3 C1 C2 S4 -2.61(17) . . . . ? Ni S2 C2 C1 0.48(13) . . . . ? Ni S2 C2 S4 -175.94(8) . . . . ? C12 S4 C2 C1 163.40(12) . . . . ? C12 S4 C2 S2 -20.16(11) . . . . ? C1 S3 C3 C4 82.92(12) . . . . ? C5 O1 C4 C3 173.97(12) . . . . ? S3 C3 C4 O1 61.40(15) . . . . ? C4 O1 C5 C6 173.64(12) . . . . ? C7 O2 C6 C5 89.58(17) . . . . ? O1 C5 C6 O2 -76.43(17) . . . . ? C6 O2 C7 C8 174.36(13) . . . . ? C9 O3 C8 C7 171.00(13) . . . . ? O2 C7 C8 O3 86.13(16) . . . . ? C8 O3 C9 C10 -163.09(14) . . . . ? C11 O4 C10 C9 -167.43(14) . . . . ? O3 C9 C10 O4 72.45(18) . . . . ? C10 O4 C11 C12 171.45(13) . . . . ? O4 C11 C12 S4 -58.25(15) . . . . ? C2 S4 C12 C11 -71.11(12) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.365 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.110