#------------------------------------------------------------------------------
#$Date: 2016-02-20 04:06:23 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/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_paper_doi               10.1107/S1600536801001994
_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       ω
_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/[σ²(Fo²)+(0.0565P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0872
_reflns_number_gt                848
_reflns_number_total             992
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6010.cif
_cod_data_source_block           BMN
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2200100
_cod_database_fobs_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_
_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_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_
_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
