Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Paola Deplano' _publ_contact_author_address ; Dipartimento di Chimica Inorganica e Analitica Universita degli Studi di Cagliari Cittadella di Monserrato Monserrato Cagliari 1-09042 ITALY ; _publ_contact_author_email DEPLANO@UNICA.IT _publ_section_title ; Synthesis, Crystal Structure and Properties of the semiconducting salts (TTF)2[Ni(dtcr)2] and (ET)2[Ni(dtcr)2] based on the [Ni(dtcr)2] dianions (dtcr = dithiocroconate) ; loop_ _publ_author_name 'P. Deplano' 'Christophe Faulmann' 'Maria Laura Mercuri' 'Luca Pilia' 'Marco Salidu' 'Angela Serpe' # Attachment 'ETNidtcr_fin.cif' data_(ET)2[Ni(dtcroc)2] _database_code_depnum_ccdc_archive 'CCDC 294420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C10 H8 S8), C10 Ni O6 S4' _chemical_formula_sum 'C30 H16 Ni O6 S20' _chemical_formula_weight 1172.34 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' 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 'P 21/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 9.3700(7) _cell_length_b 7.4410(6) _cell_length_c 28.278(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.039(6) _cell_angle_gamma 90.00 _cell_volume 1947.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1268 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 30.7 _exptl_crystal_description bar _exptl_crystal_colour black _exptl_crystal_size_max 0.625 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6053 _exptl_absorpt_correction_T_max 0.8302 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'XCalibur Oxford Diffraction' _diffrn_measurement_method '\f scan ' _diffrn_standards_decay_% negligible _diffrn_reflns_number 20052 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 32.14 _reflns_number_total 6442 _reflns_number_gt 4443 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin et al., 1996); Ortep3 (Farrugia, 1997); Mercury (CCDC, 2005)' _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^)+(0.0233P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6442 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.01381(8) Uani 1 2 d S . . S1 S 0.30646(5) 0.63564(7) 0.463924(17) 0.01758(11) Uani 1 1 d . . . S2 S 0.58404(5) 0.44917(7) 0.433776(17) 0.01654(11) Uani 1 1 d . . . C1 C 0.3313(2) 0.6231(3) 0.40621(6) 0.0138(4) Uani 1 1 d . . . C2 C 0.4537(2) 0.5415(3) 0.39255(6) 0.0136(4) Uani 1 1 d . . . C3 C 0.2360(2) 0.6939(3) 0.36437(7) 0.0157(4) Uani 1 1 d . . . C5 C 0.3128(2) 0.6543(3) 0.32239(7) 0.0166(4) Uani 1 1 d . . . C4 C 0.4481(2) 0.5506(3) 0.34100(7) 0.0152(4) Uani 1 1 d . . . O1 O 0.11942(15) 0.7676(2) 0.36240(5) 0.0248(3) Uani 1 1 d . . . O2 O 0.27117(16) 0.6981(2) 0.28083(5) 0.0277(4) Uani 1 1 d . . . O3 O 0.53388(14) 0.49195(19) 0.31609(5) 0.0199(3) Uani 1 1 d . . . S11 S 0.18729(5) 0.13993(7) 0.673312(17) 0.01841(11) Uani 1 1 d . . . S12 S 0.50338(5) -0.03139(7) 0.638144(18) 0.01942(12) Uani 1 1 d . . . S13 S 0.09723(5) 0.20112(7) 0.568995(17) 0.01625(11) Uani 1 1 d . . . S14 S 0.35689(5) 0.04407(7) 0.541266(17) 0.01800(11) Uani 1 1 d . . . S15 S -0.01925(5) 0.29431(7) 0.456793(17) 0.01681(11) Uani 1 1 d . . . S16 S 0.24384(5) 0.14012(7) 0.431449(17) 0.01815(11) Uani 1 1 d . . . S17 S -0.14977(5) 0.39219(7) 0.359430(18) 0.01835(11) Uani 1 1 d . . . S18 S 0.17537(5) 0.22366(7) 0.328031(18) 0.01934(12) Uani 1 1 d . . . C11 C 0.3621(2) 0.1043(3) 0.70930(7) 0.0181(4) Uani 1 1 d . . . C12 C 0.4420(2) -0.0592(3) 0.69499(7) 0.0190(4) Uani 1 1 d . . . C13 C 0.2269(2) 0.1209(3) 0.61538(6) 0.0141(4) Uani 1 1 d . . . C14 C 0.3494(2) 0.0505(3) 0.60213(7) 0.0149(4) Uani 1 1 d . . . C15 C 0.1937(2) 0.1487(3) 0.52371(7) 0.0145(4) Uani 1 1 d . . . C16 C 0.1438(2) 0.1889(3) 0.47572(7) 0.0144(4) Uani 1 1 d . . . C17 C -0.0021(2) 0.2992(3) 0.39623(6) 0.0147(4) Uani 1 1 d . . . C18 C 0.1228(2) 0.2306(3) 0.38455(6) 0.0146(4) Uani 1 1 d . . . C19 C -0.0775(2) 0.4216(3) 0.30420(7) 0.0169(4) Uani 1 1 d . . . C20 C 0.0038(2) 0.2599(3) 0.28987(7) 0.0182(4) Uani 1 1 d . . . H122 H 0.384(2) -0.168(3) 0.6930(7) 0.024(6) Uiso 1 1 d . . . H112 H 0.420(2) 0.211(3) 0.7098(7) 0.017(5) Uiso 1 1 d . . . H111 H 0.341(2) 0.084(2) 0.7406(7) 0.015(5) Uiso 1 1 d . . . H192 H -0.021(2) 0.528(3) 0.3069(7) 0.022(6) Uiso 1 1 d . . . H201 H -0.047(2) 0.155(3) 0.2898(7) 0.023(6) Uiso 1 1 d . . . H202 H 0.033(2) 0.273(3) 0.2607(8) 0.021(6) Uiso 1 1 d . . . H191 H -0.168(2) 0.449(3) 0.2812(8) 0.034(7) Uiso 1 1 d . . . H121 H 0.534(2) -0.075(3) 0.7161(8) 0.030(6) 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 Ni1 0.01460(17) 0.01812(19) 0.00865(17) 0.00068(14) 0.00163(13) 0.00156(15) S1 0.0170(2) 0.0255(3) 0.0106(2) 0.0003(2) 0.00314(19) 0.0052(2) S2 0.0164(2) 0.0241(3) 0.0093(2) 0.00155(19) 0.00236(19) 0.0060(2) C1 0.0155(9) 0.0162(10) 0.0100(9) -0.0009(7) 0.0022(7) -0.0017(8) C2 0.0151(9) 0.0161(10) 0.0091(9) 0.0019(7) 0.0007(7) -0.0017(8) C3 0.0158(10) 0.0182(11) 0.0128(9) -0.0018(8) 0.0011(8) -0.0026(8) C5 0.0185(10) 0.0180(11) 0.0122(9) -0.0005(8) -0.0015(8) -0.0002(8) C4 0.0190(10) 0.0135(10) 0.0127(9) 0.0016(7) 0.0009(8) -0.0018(8) O1 0.0177(8) 0.0344(9) 0.0215(8) 0.0007(7) 0.0009(6) 0.0071(7) O2 0.0308(9) 0.0398(10) 0.0112(7) 0.0029(7) -0.0007(6) 0.0130(7) O3 0.0215(7) 0.0260(8) 0.0130(7) 0.0002(6) 0.0051(6) 0.0044(7) S11 0.0204(3) 0.0246(3) 0.0108(2) 0.0022(2) 0.0043(2) 0.0064(2) S12 0.0168(2) 0.0275(3) 0.0132(2) 0.0006(2) -0.00006(19) 0.0084(2) S13 0.0159(2) 0.0224(3) 0.0105(2) 0.00148(19) 0.00231(19) 0.0052(2) S14 0.0166(2) 0.0269(3) 0.0105(2) 0.0000(2) 0.00238(19) 0.0067(2) S15 0.0152(2) 0.0245(3) 0.0108(2) 0.0011(2) 0.00241(19) 0.0046(2) S16 0.0165(2) 0.0274(3) 0.0107(2) 0.0018(2) 0.00268(19) 0.0075(2) S17 0.0166(2) 0.0249(3) 0.0131(2) 0.0022(2) 0.00070(19) 0.0063(2) S18 0.0181(2) 0.0295(3) 0.0110(2) 0.0019(2) 0.00381(19) 0.0053(2) C11 0.0239(11) 0.0194(11) 0.0111(10) 0.0006(8) 0.0027(8) 0.0003(9) C12 0.0216(11) 0.0216(12) 0.0134(10) 0.0036(8) 0.0016(9) 0.0040(9) C13 0.0165(9) 0.0162(10) 0.0090(9) 0.0018(7) 0.0000(7) 0.0010(8) C14 0.0179(10) 0.0164(10) 0.0099(9) 0.0013(7) 0.0009(8) -0.0008(8) C15 0.0146(9) 0.0147(10) 0.0144(9) 0.0002(8) 0.0029(8) 0.0019(8) C16 0.0139(9) 0.0188(11) 0.0109(9) -0.0002(7) 0.0026(7) 0.0011(8) C17 0.0178(10) 0.0166(10) 0.0092(9) 0.0013(7) 0.0007(7) -0.0012(8) C18 0.0158(9) 0.0173(10) 0.0109(9) 0.0009(7) 0.0026(8) 0.0007(8) C19 0.0195(10) 0.0196(11) 0.0108(10) 0.0010(8) 0.0001(8) 0.0006(9) C20 0.0206(10) 0.0232(12) 0.0105(10) -0.0023(8) 0.0017(8) -0.0004(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 Ni1 S2 2.1756(5) . ? Ni1 S2 2.1756(5) 3_666 ? Ni1 S1 2.1833(5) 3_666 ? Ni1 S1 2.1833(5) . ? S1 C1 1.6869(19) . ? S2 C2 1.6954(19) . ? C1 C2 1.405(3) . ? C1 C3 1.464(3) . ? C2 C4 1.452(3) . ? C3 O1 1.216(2) . ? C3 C5 1.511(3) . ? C5 O2 1.223(2) . ? C5 C4 1.507(3) . ? C4 O3 1.229(2) . ? S11 C13 1.7413(19) . ? S11 C11 1.807(2) . ? S12 C14 1.740(2) . ? S12 C12 1.802(2) . ? S13 C15 1.7246(19) . ? S13 C13 1.7472(19) . ? S14 C15 1.7178(19) . ? S14 C14 1.7340(19) . ? S15 C16 1.7257(19) . ? S15 C17 1.7452(19) . ? S16 C16 1.7167(19) . ? S16 C18 1.7394(19) . ? S17 C17 1.7387(19) . ? S17 C19 1.810(2) . ? S18 C18 1.7457(19) . ? S18 C20 1.810(2) . ? C11 C12 1.517(3) . ? C11 H112 0.96(2) . ? C11 H111 0.951(19) . ? C12 H122 0.97(2) . ? C12 H121 0.97(2) . ? C13 C14 1.367(3) . ? C15 C16 1.397(3) . ? C17 C18 1.365(3) . ? C19 C20 1.513(3) . ? C19 H192 0.94(2) . ? C19 H191 1.00(2) . ? C20 H201 0.92(2) . ? C20 H202 0.92(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni1 S2 180.0 . 3_666 ? S2 Ni1 S1 86.299(19) . 3_666 ? S2 Ni1 S1 93.701(18) 3_666 3_666 ? S2 Ni1 S1 93.701(18) . . ? S2 Ni1 S1 86.299(18) 3_666 . ? S1 Ni1 S1 180.00(2) 3_666 . ? C1 S1 Ni1 101.28(7) . . ? C2 S2 Ni1 101.69(6) . . ? C2 C1 C3 110.74(16) . . ? C2 C1 S1 122.21(15) . . ? C3 C1 S1 127.04(14) . . ? C1 C2 C4 110.69(16) . . ? C1 C2 S2 121.12(14) . . ? C4 C2 S2 128.19(14) . . ? O1 C3 C1 128.99(18) . . ? O1 C3 C5 125.96(18) . . ? C1 C3 C5 105.04(16) . . ? O2 C5 C4 126.57(18) . . ? O2 C5 C3 125.74(18) . . ? C4 C5 C3 107.68(16) . . ? O3 C4 C2 129.39(18) . . ? O3 C4 C5 124.88(18) . . ? C2 C4 C5 105.71(16) . . ? C13 S11 C11 102.09(9) . . ? C14 S12 C12 102.19(10) . . ? C15 S13 C13 95.52(9) . . ? C15 S14 C14 95.84(9) . . ? C16 S15 C17 95.77(9) . . ? C16 S16 C18 96.24(9) . . ? C17 S17 C19 101.20(9) . . ? C18 S18 C20 100.91(9) . . ? C12 C11 S11 114.15(15) . . ? C12 C11 H112 111.7(12) . . ? S11 C11 H112 110.2(12) . . ? C12 C11 H111 107.7(11) . . ? S11 C11 H111 104.1(12) . . ? H112 C11 H111 108.6(16) . . ? C11 C12 S12 112.69(14) . . ? C11 C12 H122 112.9(12) . . ? S12 C12 H122 107.4(13) . . ? C11 C12 H121 110.8(13) . . ? S12 C12 H121 100.8(13) . . ? H122 C12 H121 111.7(17) . . ? C14 C13 S11 126.98(15) . . ? C14 C13 S13 116.11(14) . . ? S11 C13 S13 116.91(11) . . ? C13 C14 S14 116.70(14) . . ? C13 C14 S12 128.93(15) . . ? S14 C14 S12 114.36(11) . . ? C16 C15 S14 121.69(14) . . ? C16 C15 S13 122.55(15) . . ? S14 C15 S13 115.76(11) . . ? C15 C16 S16 121.67(15) . . ? C15 C16 S15 122.96(14) . . ? S16 C16 S15 115.35(11) . . ? C18 C17 S17 129.51(15) . . ? C18 C17 S15 116.38(15) . . ? S17 C17 S15 114.12(11) . . ? C17 C18 S16 116.21(14) . . ? C17 C18 S18 127.51(15) . . ? S16 C18 S18 116.27(10) . . ? C20 C19 S17 114.02(15) . . ? C20 C19 H192 112.8(12) . . ? S17 C19 H192 108.1(12) . . ? C20 C19 H191 113.5(13) . . ? S17 C19 H191 100.9(13) . . ? H192 C19 H191 106.6(17) . . ? C19 C20 S18 113.35(15) . . ? C19 C20 H201 113.3(13) . . ? S18 C20 H201 106.8(13) . . ? C19 C20 H202 112.9(13) . . ? S18 C20 H202 100.8(13) . . ? H201 C20 H202 108.8(18) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 32.14 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.562 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.119 # Attachment 'TTFNidtcr_fin.cif' data_(TTF)2[Ni(dtcr)2] _database_code_depnum_ccdc_archive 'CCDC 294421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 Ni O6 S4, 2(C6 H4 S4)' _chemical_formula_sum 'C22 H8 Ni O6 S12' _chemical_formula_weight 811.81 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' 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 'P 21/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 8.6340(8) _cell_length_b 21.586(2) _cell_length_c 7.5960(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.625(11) _cell_angle_gamma 90.00 _cell_volume 1408.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 4645 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.9 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_T_max 0.7771 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS).The crystal-to-detector distance was 70 mm. 143 exposures (5 min per exposure) were obtained with 0 < \f < 2005\% and with the crystals rotated through 1.4\% in \f. Crystal decay was monitored by measuring 200 reflexions per image. ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE Imaging Plate Diffraction System' _diffrn_measurement_method '\f scan' _diffrn_standards_decay_% negligible _diffrn_reflns_number 11032 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2761 _reflns_number_gt 1622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS software (Stoe, 1996)' _computing_cell_refinement 'IPDS software (Stoe, 1996)' _computing_data_reduction 'IPDS software (Stoe, 1996)' _computing_structure_solution 'Sir97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin et al., 1996); Ortep3 (Farrugia, 1997); Mercury (CCDC, 2005)' _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^)+(0.0225P)^2^] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2761 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.0247(2) Uani 1 2 d S . . S1 S 0.32928(12) 0.55782(5) 0.62035(17) 0.0309(3) Uani 1 1 d . . . S2 S 0.61836(12) 0.58073(5) 0.40633(16) 0.0337(3) Uani 1 1 d . . . C1 C 0.3880(4) 0.63057(18) 0.5767(6) 0.0246(10) Uani 1 1 d . . . C2 C 0.5184(4) 0.64013(16) 0.4855(6) 0.0236(9) Uani 1 1 d . . . C3 C 0.3176(5) 0.68910(18) 0.6179(6) 0.0303(10) Uani 1 1 d . . . C4 C 0.5538(5) 0.7052(2) 0.4722(7) 0.0365(12) Uani 1 1 d . . . C5 C 0.4252(5) 0.73911(19) 0.5540(6) 0.0334(11) Uani 1 1 d . . . O1 O 0.1983(3) 0.69930(14) 0.6859(5) 0.0495(10) Uani 1 1 d . . . O2 O 0.4092(4) 0.79390(13) 0.5657(5) 0.0532(10) Uani 1 1 d . . . O3 O 0.6644(4) 0.72973(15) 0.4116(5) 0.0592(12) Uani 1 1 d . . . S3 S -0.04062(11) 0.55325(5) 0.30357(15) 0.0307(3) Uani 1 1 d . . . S4 S 0.21705(12) 0.59494(5) 0.11693(16) 0.0355(3) Uani 1 1 d . . . S5 S 0.05214(13) 0.41055(5) 0.23596(16) 0.0351(3) Uani 1 1 d . . . S6 S 0.30806(12) 0.45276(6) 0.04709(17) 0.0403(3) Uani 1 1 d . . . C6 C 0.1069(5) 0.6506(2) 0.2072(7) 0.0366(12) Uani 1 1 d . . . H6 H 0.132(5) 0.687(3) 0.197(6) 0.050(16) Uiso 1 1 d . . . C7 C -0.0117(5) 0.6318(2) 0.2918(7) 0.0346(11) Uani 1 1 d . . . H7 H -0.078(5) 0.661(2) 0.335(6) 0.050(14) Uiso 1 1 d . . . C8 C 0.1146(4) 0.5334(2) 0.1911(5) 0.0252(10) Uani 1 1 d . . . C9 C 0.1546(4) 0.4724(2) 0.1628(6) 0.0264(10) Uani 1 1 d . . . C10 C 0.2902(6) 0.3747(2) 0.0748(8) 0.0457(14) Uani 1 1 d . . . H10 H 0.351(5) 0.3482(19) 0.030(6) 0.031(12) Uiso 1 1 d . . . C11 C 0.1714(6) 0.3554(2) 0.1602(7) 0.0396(13) Uani 1 1 d . . . H11 H 0.147(4) 0.316(2) 0.179(5) 0.030(13) 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 Ni1 0.0207(4) 0.0200(4) 0.0349(5) -0.0011(4) 0.0112(3) 0.0007(3) S1 0.0273(5) 0.0211(5) 0.0475(8) -0.0001(5) 0.0193(5) 0.0007(4) S2 0.0296(5) 0.0239(5) 0.0513(8) -0.0022(5) 0.0231(6) 0.0007(5) C1 0.023(2) 0.024(2) 0.028(3) -0.0039(19) 0.0065(19) 0.0018(17) C2 0.025(2) 0.0165(19) 0.030(3) 0.000(2) 0.0057(19) 0.0016(17) C3 0.034(2) 0.023(2) 0.036(3) 0.001(2) 0.010(2) 0.0015(18) C4 0.031(2) 0.033(2) 0.048(3) 0.000(2) 0.016(2) -0.007(2) C5 0.036(2) 0.025(2) 0.041(3) -0.006(2) 0.010(2) 0.005(2) O1 0.0427(18) 0.0351(18) 0.076(3) -0.0037(18) 0.0323(19) 0.0086(15) O2 0.0479(19) 0.0233(17) 0.092(3) -0.0048(19) 0.024(2) 0.0019(15) O3 0.054(2) 0.0315(17) 0.099(3) -0.0033(19) 0.043(2) -0.0117(15) S3 0.0291(5) 0.0270(6) 0.0384(7) -0.0015(5) 0.0155(5) 0.0000(5) S4 0.0286(6) 0.0327(6) 0.0474(8) 0.0009(6) 0.0153(6) -0.0047(5) S5 0.0420(6) 0.0279(6) 0.0370(7) 0.0025(5) 0.0118(6) 0.0023(5) S6 0.0298(6) 0.0419(7) 0.0515(9) -0.0038(6) 0.0157(6) 0.0068(5) C6 0.039(3) 0.027(3) 0.044(3) -0.002(2) 0.009(2) -0.007(2) C7 0.037(3) 0.024(2) 0.043(3) -0.005(2) 0.004(2) 0.001(2) C8 0.020(2) 0.033(2) 0.023(3) -0.0016(19) 0.0033(19) 0.0011(18) C9 0.0188(19) 0.034(2) 0.026(3) 0.000(2) 0.0030(19) 0.0026(17) C10 0.045(3) 0.042(3) 0.051(4) -0.007(3) 0.005(3) 0.018(2) C11 0.050(3) 0.023(3) 0.045(4) 0.001(2) 0.001(3) 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 Ni1 S2 2.1749(10) 3_666 ? Ni1 S2 2.1749(10) . ? Ni1 S1 2.1977(9) . ? Ni1 S1 2.1977(9) 3_666 ? S1 C1 1.693(4) . ? S2 C2 1.689(4) . ? C1 C2 1.394(5) . ? C1 C3 1.450(5) . ? C2 C4 1.444(5) . ? C3 O1 1.217(4) . ? C3 C5 1.533(6) . ? C4 O3 1.220(4) . ? C4 C5 1.513(5) . ? C5 O2 1.195(5) . ? S3 C8 1.713(4) . ? S3 C7 1.718(4) . ? S4 C6 1.716(5) . ? S4 C8 1.722(4) . ? S5 C11 1.710(5) . ? S5 C9 1.723(4) . ? S6 C10 1.706(5) . ? S6 C9 1.713(4) . ? C6 C7 1.325(6) . ? C6 H6 0.83(5) . ? C7 H7 0.94(5) . ? C8 C9 1.383(5) . ? C10 C11 1.333(7) . ? C10 H10 0.87(4) . ? C11 H11 0.89(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 S2 Ni1 S2 180.00(3) 3_666 . ? S2 Ni1 S1 87.89(4) 3_666 . ? S2 Ni1 S1 92.11(4) . . ? S2 Ni1 S1 92.11(4) 3_666 3_666 ? S2 Ni1 S1 87.89(4) . 3_666 ? S1 Ni1 S1 180.0 . 3_666 ? C1 S1 Ni1 102.66(12) . . ? C2 S2 Ni1 102.65(13) . . ? C2 C1 C3 110.8(3) . . ? C2 C1 S1 120.5(3) . . ? C3 C1 S1 128.8(3) . . ? C1 C2 C4 111.4(3) . . ? C1 C2 S2 122.0(3) . . ? C4 C2 S2 126.5(3) . . ? O1 C3 C1 129.8(4) . . ? O1 C3 C5 124.8(4) . . ? C1 C3 C5 105.4(3) . . ? O3 C4 C2 128.8(4) . . ? O3 C4 C5 125.3(4) . . ? C2 C4 C5 105.8(3) . . ? O2 C5 C4 127.1(4) . . ? O2 C5 C3 126.6(4) . . ? C4 C5 C3 106.3(3) . . ? C8 S3 C7 95.5(2) . . ? C6 S4 C8 95.0(2) . . ? C11 S5 C9 94.9(2) . . ? C10 S6 C9 95.6(2) . . ? C7 C6 S4 117.7(4) . . ? C7 C6 H6 124(3) . . ? S4 C6 H6 118(3) . . ? C6 C7 S3 116.7(4) . . ? C6 C7 H7 119(3) . . ? S3 C7 H7 124(3) . . ? C9 C8 S3 122.4(3) . . ? C9 C8 S4 122.7(3) . . ? S3 C8 S4 115.0(2) . . ? C8 C9 S6 122.2(3) . . ? C8 C9 S5 122.9(3) . . ? S6 C9 S5 114.9(2) . . ? C11 C10 S6 116.9(4) . . ? C11 C10 H10 121(3) . . ? S6 C10 H10 122(3) . . ? C10 C11 S5 117.5(4) . . ? C10 C11 H11 126(3) . . ? S5 C11 H11 117(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.346 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.087