#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/01/2200100.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200100 loop_ _publ_author_name 'Mahmoudkhani, Amir H.' 'Langer, Vratislav' _publ_section_title ; On the reaction of nickel(II) ions with thiolacetic acid ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m92 _journal_page_last m94 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Ni (C2 H3 S3)2]' _chemical_formula_sum 'C4 H6 Ni S6' _chemical_formula_weight 305.16 _chemical_name_common Bis(methylperthiocarboxylato)nickel(II) _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXTL _cell_angle_alpha 90.00 _cell_angle_beta 92.500(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.3169(3) _cell_length_b 6.1524(3) _cell_length_c 15.9722(8) _cell_measurement_reflns_used 3360 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 1 _cell_volume 521.98(5) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT and SADABS (Sheldrick, 2001)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 1997)' _diffrn_ambient_temperature 297(2) _diffrn_detector_area_resol_mean no _diffrn_measured_fraction_theta_full .998 _diffrn_measured_fraction_theta_max .998 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0473 _diffrn_reflns_av_sigmaI/netI .0315 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 4984 _diffrn_reflns_theta_full 25.68 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_min 2.55 _diffrn_standards_decay_% none _diffrn_standards_interval_count no _diffrn_standards_interval_time no _diffrn_standards_number no _exptl_absorpt_coefficient_mu 2.99 _exptl_absorpt_correction_T_max .890 _exptl_absorpt_correction_T_min .467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing (1995)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_description parallepide _exptl_crystal_F_000 308 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .04 _refine_diff_density_max .561 _refine_diff_density_min -.458 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 53 _refine_ls_number_reflns 992 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all .0394 _refine_ls_R_factor_gt .0339 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0565P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0872 _reflns_number_gt 848 _reflns_number_total 992 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6010.cif _[local]_cod_data_source_block BMN _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2200100 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ni1 .0000 .0000 .0000 .0387(2) Uani d S 1 . . Ni S3 .07836(17) -.17320(15) .11602(5) .0607(3) Uani d . 1 . . S S2 .35389(19) -.00717(14) .18086(6) .0579(3) Uani d . 1 . . S S1 .27462(17) .25107(13) .02763(5) .0542(3) Uani d . 1 . . S C2 .6249(6) .3537(6) .1523(2) .0622(9) Uani d . 1 . . C H2A .6870 .3053 .2065 .093 Uiso calc R 1 . . H H2B .5583 .4981 .1568 .093 Uiso calc R 1 . . H H2C .7600 .3541 .1143 .093 Uiso calc R 1 . . H C1 .4217(6) .2036(5) .12013(18) .0464(7) Uani d . 1 . . C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 .0409(3) .0398(3) .0349(3) -.0043(2) -.0047(2) -.00078(19) S3 .0718(6) .0588(5) .0495(5) -.0227(4) -.0204(4) .0135(4) S2 .0594(6) .0647(6) .0477(5) -.0121(4) -.0191(4) .0079(3) S1 .0613(5) .0536(5) .0466(5) -.0189(4) -.0124(4) .0057(3) C2 .0541(19) .074(2) .057(2) -.0187(17) -.0132(16) -.0069(17) C1 .0419(15) .0531(18) .0436(16) -.0037(13) -.0034(12) -.0053(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 S1 . 2.1579(8) yes Ni1 S1 3 2.1579(8) ? Ni1 S3 3 2.1623(8) ? Ni1 S3 . 2.1623(8) yes S3 S2 . 2.0322(12) yes S2 C1 . 1.668(3) yes S1 C1 . 1.667(3) yes C2 C1 . 1.496(4) yes C2 H2A . .96 ? C2 H2B . .96 ? C2 H2C . .96 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 Ni1 S1 . 3 180.00(5) yes S1 Ni1 S3 . 3 85.75(3) yes S1 Ni1 S3 3 3 94.25(3) ? S1 Ni1 S3 . . 94.25(3) yes S1 Ni1 S3 3 . 85.75(3) ? S3 Ni1 S3 3 . 180.00(5) yes S2 S3 Ni1 . . 107.26(4) yes C1 S2 S3 . . 105.29(11) yes C1 S1 Ni1 . . 110.05(11) yes C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C2 C1 S1 . . 120.0(2) yes C2 C1 S2 . . 116.8(2) yes S1 C1 S2 . . 123.14(18) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2C Ni1 1_655 .96 3.15 3.880(4) 134.3 _cod_database_fobs_code 2200100 _journal_paper_doi 10.1107/S1600536801001994