Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Leonard F. Lindoy' _publ_contact_author_address ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; _publ_contact_author_email Lindoy@chem.usyd.edu.au _publ_contact_author_fax '+61 2 9351 3329' _publ_contact_author_phone '+61 2 9351 4400' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Interaction of cobalt(II) and nickel(II) with a linked, bis-b-diketone ligand to yield an unusual coordination motif ; loop_ _publ_author_name _publ_author_address 'Bai Shu Zhen' ; School of Physics and Chemistry, Guizhou Normal University, Guiyang, Guizhou 550001, P. R. China ; 'Xiao Yi Zhang' ; School of Physics and Chemistry, Guizhou Normal University, Guiyang, Guizhou 550001, P. R. China ; 'Huai Wu Zhu' ; School of Physics and Chemistry, Guizhou Normal University, Guiyang, Guizhou 550001, P. R. China ; 'Shi Xia Luo' ; School of Physics and Chemistry, Guizhou Normal University, Guiyang, Guizhou 550001, P. R. China ; 'Leonard F. Lindoy' ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; 'John C. McMurtrie' ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; 'Peter Turner' ; Crystal Structure Analysis Facility School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; 'Gang Wei' ; CSIRO, Telecommunications and Industrial Physics, PO Box 218, Linfield, NSW, 2070, Australia ; #========================================================================= # Complex 1 is lflj30 and Complex 2 is lfl73 #========================================================================= data_lflj30_g _database_code_depnum_ccdc_archive 'CCDC 263748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Co O7 S2' _chemical_formula_weight 401.35 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' 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 16.367(4) _cell_length_b 14.423(3) _cell_length_c 7.4705(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.490(4) _cell_angle_gamma 90.00 _cell_volume 1721.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 892 _cell_measurement_theta_min 2.825 _cell_measurement_theta_max 28.229 _exptl_crystal_description columnar _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.588 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 145 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 8259 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2038 _reflns_number_gt 1916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2038 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 C1 C 0.63741(10) 0.26344(13) 0.79556(19) 0.0442(4) Uani 1 1 d . . . H1A H 0.5957 0.2308 0.8485 0.066 Uiso 1 1 calc R . . H1B H 0.6435 0.3272 0.8422 0.066 Uiso 1 1 calc R . . H1C H 0.6913 0.2314 0.8299 0.066 Uiso 1 1 calc R . . C2 C 0.60937(7) 0.26502(9) 0.59030(16) 0.0235(2) Uani 1 1 d . . . C3 C 0.64769(7) 0.32227(8) 0.48015(16) 0.0210(2) Uani 1 1 d . . . C4 C 0.72387(7) 0.37335(8) 0.54716(17) 0.0236(2) Uani 1 1 d . . . C5 C 0.75888(10) 0.43456(11) 0.4180(2) 0.0405(4) Uani 1 1 d . . . H5A H 0.7318 0.4955 0.4101 0.061 Uiso 1 1 calc R . . H5B H 0.7483 0.4060 0.2961 0.061 Uiso 1 1 calc R . . H5C H 0.8193 0.4419 0.4640 0.061 Uiso 1 1 calc R . . C6 C 0.53452(10) 0.41558(9) 0.1973(2) 0.0382(3) Uani 1 1 d . . . H6A H 0.5675 0.4733 0.2268 0.046 Uiso 1 1 calc R . . H6B H 0.5087 0.4169 0.0646 0.046 Uiso 1 1 calc R . . O1 O 0.54723(5) 0.21276(6) 0.52275(11) 0.02478(18) Uani 1 1 d . . . O2 O 0.76223(5) 0.36989(6) 0.70934(12) 0.0286(2) Uani 1 1 d . . . O3 O 0.57755(6) 0.09138(6) 0.19000(13) 0.02582(19) Uani 1 1 d . . . H3O H 0.5651(11) 0.0424(13) 0.215(2) 0.040(5) Uiso 1 1 d . . . H3OB H 0.6299(12) 0.0987(12) 0.223(2) 0.042(5) Uiso 1 1 d . . . O4 O 0.5000 -0.07008(10) 0.2500 0.0383(4) Uani 1 2 d S . . H4O H 0.5040(14) -0.1018(15) 0.171(3) 0.062(6) Uiso 1 1 d . . . S1 S 0.60592(2) 0.31718(2) 0.24205(4) 0.02462(8) Uani 1 1 d . . . Co1 Co 0.5000 0.195068(14) 0.2500 0.01831(7) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0452(8) 0.0682(11) 0.0168(6) 0.0008(6) 0.0013(5) -0.0301(8) C2 0.0232(5) 0.0289(6) 0.0176(5) -0.0021(4) 0.0027(4) -0.0042(4) C3 0.0225(5) 0.0226(5) 0.0168(5) -0.0018(4) 0.0018(4) -0.0027(4) C4 0.0222(5) 0.0216(5) 0.0266(6) -0.0026(5) 0.0044(5) -0.0021(4) C5 0.0360(7) 0.0435(8) 0.0384(8) 0.0109(6) 0.0001(6) -0.0175(6) C6 0.0426(8) 0.0228(6) 0.0401(8) 0.0094(6) -0.0114(6) -0.0065(5) O1 0.0240(4) 0.0315(4) 0.0174(4) 0.0014(3) 0.0014(3) -0.0083(3) O2 0.0230(4) 0.0359(5) 0.0256(5) -0.0055(4) 0.0023(3) -0.0067(4) O3 0.0187(4) 0.0221(4) 0.0355(5) -0.0023(4) 0.0034(4) -0.0003(3) O4 0.0733(11) 0.0192(6) 0.0267(7) 0.000 0.0206(7) 0.000 S1 0.02934(16) 0.02617(15) 0.01702(15) 0.00250(10) 0.00206(12) -0.00667(11) Co1 0.01973(12) 0.01861(12) 0.01524(12) 0.000 0.00084(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.5027(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O1 1.2788(14) . ? C2 C3 1.4055(17) . ? C3 C4 1.4416(16) . ? C3 S1 1.7637(12) . ? C4 O2 1.2391(15) . ? C4 C5 1.5093(18) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C6 1.510(3) 2_655 ? C6 S1 1.8228(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O1 Co1 2.0330(9) . ? O3 Co1 2.0723(9) . ? O3 H3O 0.769(18) . ? O3 H3OB 0.845(19) . ? O4 H4O 0.761(19) . ? S1 Co1 2.4810(5) . ? Co1 O1 2.0330(9) 2_655 ? Co1 O3 2.0723(9) 2_655 ? Co1 S1 2.4810(5) 2_655 ? 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 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.19(11) . . ? O1 C2 C1 115.79(11) . . ? C3 C2 C1 122.00(11) . . ? C2 C3 C4 123.98(11) . . ? C2 C3 S1 116.19(9) . . ? C4 C3 S1 119.28(9) . . ? O2 C4 C3 122.43(11) . . ? O2 C4 C5 117.81(11) . . ? C3 C4 C5 119.76(11) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C6 S1 115.25(8) 2_655 . ? C6 C6 H6A 108.5 2_655 . ? S1 C6 H6A 108.5 . . ? C6 C6 H6B 108.5 2_655 . ? S1 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C2 O1 Co1 124.55(8) . . ? Co1 O3 H3O 113.8(13) . . ? Co1 O3 H3OB 118.5(12) . . ? H3O O3 H3OB 110.5(18) . . ? C3 S1 C6 104.23(6) . . ? C3 S1 Co1 97.23(4) . . ? C6 S1 Co1 97.67(5) . . ? O1 Co1 O1 165.58(5) . 2_655 ? O1 Co1 O3 89.53(4) . 2_655 ? O1 Co1 O3 100.92(4) 2_655 2_655 ? O1 Co1 O3 100.92(4) . . ? O1 Co1 O3 89.53(4) 2_655 . ? O3 Co1 O3 87.62(6) 2_655 . ? O1 Co1 S1 79.55(3) . . ? O1 Co1 S1 90.18(3) 2_655 . ? O3 Co1 S1 168.90(3) 2_655 . ? O3 Co1 S1 92.48(3) . . ? O1 Co1 S1 90.18(3) . 2_655 ? O1 Co1 S1 79.55(3) 2_655 2_655 ? O3 Co1 S1 92.48(3) 2_655 2_655 ? O3 Co1 S1 168.90(3) . 2_655 ? S1 Co1 S1 89.55(2) . 2_655 ? 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 O1 C2 C3 C4 -171.99(11) . . . . ? C1 C2 C3 C4 9.8(2) . . . . ? O1 C2 C3 S1 -0.67(17) . . . . ? C1 C2 C3 S1 -178.91(12) . . . . ? C2 C3 C4 O2 0.61(19) . . . . ? S1 C3 C4 O2 -170.46(10) . . . . ? C2 C3 C4 C5 -178.70(13) . . . . ? S1 C3 C4 C5 10.23(17) . . . . ? C3 C2 O1 Co1 5.30(17) . . . . ? C1 C2 O1 Co1 -176.36(10) . . . . ? C2 C3 S1 C6 97.05(11) . . . . ? C4 C3 S1 C6 -91.20(11) . . . . ? C2 C3 S1 Co1 -2.80(10) . . . . ? C4 C3 S1 Co1 168.95(9) . . . . ? C6 C6 S1 C3 -58.35(13) 2_655 . . . ? C6 C6 S1 Co1 41.16(13) 2_655 . . . ? C2 O1 Co1 O1 -50.64(10) . . . 2_655 ? C2 O1 Co1 O3 172.60(10) . . . 2_655 ? C2 O1 Co1 O3 85.12(10) . . . . ? C2 O1 Co1 S1 -5.41(9) . . . . ? C2 O1 Co1 S1 -94.91(10) . . . 2_655 ? C3 S1 Co1 O1 3.65(5) . . . . ? C6 S1 Co1 O1 -101.84(6) . . . . ? C3 S1 Co1 O1 173.47(5) . . . 2_655 ? C6 S1 Co1 O1 67.97(6) . . . 2_655 ? C3 S1 Co1 O3 -6.72(16) . . . 2_655 ? C6 S1 Co1 O3 -112.22(16) . . . 2_655 ? C3 S1 Co1 O3 -97.00(5) . . . . ? C6 S1 Co1 O3 157.51(6) . . . . ? C3 S1 Co1 S1 93.92(4) . . . 2_655 ? C6 S1 Co1 S1 -11.58(5) . . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O4 0.769(18) 1.989(19) 2.7352(16) 163.4(19) . O3 H3OB O2 0.845(19) 1.79(2) 2.6271(14) 172.5(18) 7_656 O4 H4O O1 0.761(19) 2.15(2) 2.8779(13) 160(2) 6 _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.385 _refine_diff_density_min -0.181 _refine_diff_density_rms 0.047 #===END data_lfl73 _database_code_depnum_ccdc_archive 'CCDC 263749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H22 Ni O7 S2' _chemical_formula_weight 401.13 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' 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' 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 'C 2/c ' _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 16.236(3) _cell_length_b 14.445(3) _cell_length_c 7.4624(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.493(3) _cell_angle_gamma 90.00 _cell_volume 1715.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 944 _cell_measurement_theta_min 3.257 _cell_measurement_theta_max 28.110 _exptl_crystal_description columnar _exptl_crystal_colour blue _exptl_crystal_size_max 0.562 _exptl_crystal_size_mid 0.094 _exptl_crystal_size_min 0.078 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.631 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ; Gaussian (Coppens et al., 1965) XPREP (Bruker, 1995) ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Cryosystems Cryostream. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 136 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 8020 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.25 _reflns_number_total 2059 _reflns_number_gt 1941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.02P)^2^+1.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2059 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0521 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 1.272 _refine_ls_restrained_S_all 1.272 _refine_ls_shift/su_max 0.007 _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 0.198463(15) 0.2500 0.01334(7) Uani 1 2 d S . . S1 S 0.39548(2) 0.31539(2) 0.26116(4) 0.01824(9) Uani 1 1 d . . . O1 O 0.45195(6) 0.20622(6) -0.02145(12) 0.01769(19) Uani 1 1 d . . . O2 O 0.24034(6) 0.36974(7) -0.20435(12) 0.0209(2) Uani 1 1 d . . . O3 O 0.42178(6) 0.09567(7) 0.30784(13) 0.01827(19) Uani 1 1 d . . . H3O H 0.3713(13) 0.1014(13) 0.272(3) 0.035(5) Uiso 1 1 d . . . H3OB H 0.4329(12) 0.0467(14) 0.279(3) 0.038(6) Uiso 1 1 d . . . O4 O 0.5000 -0.06607(10) 0.2500 0.0262(3) Uani 1 2 d S . . H4O H 0.5037(13) -0.0965(14) 0.169(3) 0.042(6) Uiso 1 1 d . . . C1 C 0.36263(10) 0.25837(13) -0.29260(19) 0.0337(4) Uani 1 1 d . . . H1A H 0.4029 0.2228 -0.3468 0.051 Uiso 1 1 calc R . . H1B H 0.3593 0.3218 -0.3403 0.051 Uiso 1 1 calc R . . H1C H 0.3071 0.2292 -0.3239 0.051 Uiso 1 1 calc R . . C2 C 0.39121(8) 0.26047(9) -0.08780(17) 0.0178(3) Uani 1 1 d . . . C3 C 0.35362(8) 0.31999(9) 0.02359(17) 0.0157(2) Uani 1 1 d . . . C4 C 0.27807(8) 0.37240(9) -0.04210(18) 0.0177(3) Uani 1 1 d . . . C5 C 0.24309(10) 0.43504(11) 0.0876(2) 0.0286(3) Uani 1 1 d . . . H5A H 0.2678 0.4969 0.0867 0.043 Uiso 1 1 calc R . . H5B H 0.2570 0.4095 0.2116 0.043 Uiso 1 1 calc R . . H5C H 0.1819 0.4393 0.0485 0.043 Uiso 1 1 calc R . . C6 C 0.46525(9) 0.41570(10) 0.3039(2) 0.0278(3) Uani 1 1 d . . . H6A H 0.4313 0.4726 0.2738 0.033 Uiso 1 1 calc R . . H6B H 0.4908 0.4179 0.4359 0.033 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 Ni1 0.01539(12) 0.01262(12) 0.01131(12) 0.000 0.00099(8) 0.000 S1 0.02325(17) 0.01793(16) 0.01273(15) -0.00188(11) 0.00162(12) 0.00478(12) O1 0.0183(4) 0.0202(5) 0.0137(4) -0.0010(3) 0.0012(3) 0.0048(4) O2 0.0181(4) 0.0251(5) 0.0187(5) 0.0040(4) 0.0019(3) 0.0045(4) O3 0.0148(5) 0.0158(5) 0.0235(5) 0.0009(4) 0.0021(4) 0.0006(4) O4 0.0490(10) 0.0142(7) 0.0180(7) 0.000 0.0131(7) 0.000 C1 0.0366(8) 0.0493(10) 0.0138(7) -0.0007(6) 0.0015(6) 0.0246(7) C2 0.0184(6) 0.0207(6) 0.0141(6) 0.0016(5) 0.0026(5) 0.0024(5) C3 0.0178(6) 0.0162(6) 0.0126(6) 0.0009(4) 0.0018(5) 0.0014(5) C4 0.0188(6) 0.0139(6) 0.0207(6) 0.0019(5) 0.0047(5) -0.0001(5) C5 0.0282(8) 0.0282(8) 0.0273(7) -0.0062(6) 0.0006(6) 0.0119(6) C6 0.0315(8) 0.0155(6) 0.0302(8) -0.0068(6) -0.0087(6) 0.0042(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 Ni1 O1 2.0235(9) 2_655 ? Ni1 O1 2.0235(9) . ? Ni1 O3 2.0549(10) . ? Ni1 O3 2.0549(10) 2_655 ? Ni1 S1 2.4074(5) 2_655 ? Ni1 S1 2.4074(5) . ? S1 C3 1.7689(13) . ? S1 C6 1.8277(15) . ? O1 C2 1.2795(15) . ? O2 C4 1.2438(16) . ? O3 H3O 0.81(2) . ? O3 H3OB 0.77(2) . ? O4 H4O 0.762(18) . ? C1 C2 1.5065(18) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.4159(18) . ? C3 C4 1.4417(18) . ? C4 C5 1.5159(18) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C6 1.510(3) 2_655 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 Ni1 O1 173.65(5) 2_655 . ? O1 Ni1 O3 87.76(4) 2_655 . ? O1 Ni1 O3 96.84(4) . . ? O1 Ni1 O3 96.84(4) 2_655 2_655 ? O1 Ni1 O3 87.76(4) . 2_655 ? O3 Ni1 O3 87.46(6) . 2_655 ? O1 Ni1 S1 82.07(3) 2_655 2_655 ? O1 Ni1 S1 93.46(3) . 2_655 ? O3 Ni1 S1 169.63(3) . 2_655 ? O3 Ni1 S1 91.73(3) 2_655 2_655 ? O1 Ni1 S1 93.46(3) 2_655 . ? O1 Ni1 S1 82.07(3) . . ? O3 Ni1 S1 91.73(3) . . ? O3 Ni1 S1 169.63(3) 2_655 . ? S1 Ni1 S1 90.89(2) 2_655 . ? C3 S1 C6 104.24(6) . . ? C3 S1 Ni1 97.15(4) . . ? C6 S1 Ni1 98.37(5) . . ? C2 O1 Ni1 122.34(8) . . ? Ni1 O3 H3O 118.8(13) . . ? Ni1 O3 H3OB 114.7(15) . . ? H3O O3 H3OB 106.2(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.27(12) . . ? O1 C2 C1 115.98(11) . . ? C3 C2 C1 121.75(11) . . ? C2 C3 C4 123.80(12) . . ? C2 C3 S1 116.17(9) . . ? C4 C3 S1 119.44(10) . . ? O2 C4 C3 122.38(12) . . ? O2 C4 C5 117.75(12) . . ? C3 C4 C5 119.86(12) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C6 S1 114.20(8) 2_655 . ? C6 C6 H6A 108.7 2_655 . ? S1 C6 H6A 108.7 . . ? C6 C6 H6B 108.7 2_655 . ? S1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? 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 O1 Ni1 S1 C3 176.13(5) 2_655 . . . ? O1 Ni1 S1 C3 0.66(5) . . . . ? O3 Ni1 S1 C3 -96.01(5) . . . . ? O3 Ni1 S1 C3 -10.64(18) 2_655 . . . ? S1 Ni1 S1 C3 94.03(4) 2_655 . . . ? O1 Ni1 S1 C6 70.53(6) 2_655 . . . ? O1 Ni1 S1 C6 -104.95(6) . . . . ? O3 Ni1 S1 C6 158.39(6) . . . . ? O3 Ni1 S1 C6 -116.25(18) 2_655 . . . ? S1 Ni1 S1 C6 -11.58(5) 2_655 . . . ? O1 Ni1 O1 C2 -46.29(10) 2_655 . . . ? O3 Ni1 O1 C2 89.95(10) . . . . ? O3 Ni1 O1 C2 177.12(10) 2_655 . . . ? S1 Ni1 O1 C2 -91.28(10) 2_655 . . . ? S1 Ni1 O1 C2 -0.86(10) . . . . ? Ni1 O1 C2 C3 0.73(18) . . . . ? Ni1 O1 C2 C1 179.90(10) . . . . ? O1 C2 C3 C4 -171.06(12) . . . . ? C1 C2 C3 C4 9.8(2) . . . . ? O1 C2 C3 S1 0.05(18) . . . . ? C1 C2 C3 S1 -179.07(12) . . . . ? C6 S1 C3 C2 99.97(11) . . . . ? Ni1 S1 C3 C2 -0.58(10) . . . . ? C6 S1 C3 C4 -88.50(11) . . . . ? Ni1 S1 C3 C4 170.94(9) . . . . ? C2 C3 C4 O2 -0.7(2) . . . . ? S1 C3 C4 O2 -171.57(10) . . . . ? C2 C3 C4 C5 -179.43(13) . . . . ? S1 C3 C4 C5 9.73(17) . . . . ? C3 S1 C6 C6 -58.97(13) . . . 2_655 ? Ni1 S1 C6 C6 40.65(13) . . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O2 0.81(2) 1.83(2) 2.6390(14) 172.2(19) 7 O3 H3OB O4 0.77(2) 2.00(2) 2.7342(16) 160(2) . O4 H4O O1 0.762(18) 2.133(19) 2.8542(14) 158(2) 5_655 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.390 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.052