#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:02:21 +0100 (vie 25 de mar de 2016) $
#$Revision: 179948 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/43/7024342.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7024342
loop_
_publ_author_name
'Mas-Ballesté, Rubén'
'Guijarro, Alejandro'
'González-Prieto, Rodrigo'
'Castillo, Oscar'
'Sanz Miguel, Pablo J.'
'Zamora, Félix'
_publ_section_title
;
 S-S bond reactivity in metal-perthiocarboxylato compounds.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1511
_journal_page_last               1518
_journal_paper_doi               10.1039/b915518j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_iupac          '[Ni(C2H3S2)(C2H3S3)]'
_chemical_formula_moiety         'C4 H6 Ni S5'
_chemical_formula_sum            'C4 H6 Ni S5'
_chemical_formula_weight         273.10
_chemical_name_common
;
(dithioacetato-k2S,S')(perthioacetato-k2S,S')nickel(II)
;
_chemical_name_systematic
;
(dithioacetato-k2S,S')(perthioacetato-k2S,S')nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.74(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.755(3)
_cell_length_b                   11.059(3)
_cell_length_c                   12.411(5)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.57
_cell_volume                     974.3(7)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altamore et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4953
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction, 2003)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         4953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[σ²(Fo²)+(0.1345P)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2298
_reflns_number_gt                2506
_reflns_number_total             4953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915518j.txt
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7024342
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'
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
Ni1 Ni 0.76656(12) 0.13125(7) 0.34797(7) 0.0572(3) Uani 1 1 d .
S11 S 0.7356(3) 0.01926(15) 0.47898(14) 0.0647(5) Uani 1 1 d .
S12 S 0.7245(3) -0.16398(16) 0.30771(18) 0.0722(6) Uani 1 1 d .
S13 S 0.7474(3) -0.00912(16) 0.22704(15) 0.0714(6) Uani 1 1 d .
C11 C 0.7129(9) -0.1247(5) 0.4319(6) 0.0593(17) Uani 1 1 d .
C12 C 0.6956(11) -0.2247(6) 0.5094(6) 0.072(2) Uani 1 1 d .
H12A H 0.5764 -0.2645 0.4707 0.108 Uiso 1 1 calc R
H12B H 0.7039 -0.1912 0.5827 0.108 Uiso 1 1 calc R
H12C H 0.7955 -0.2820 0.5240 0.108 Uiso 1 1 calc R
S21 S 0.7985(3) 0.27140(15) 0.22851(15) 0.0654(5) Uani 1 1 d .
S22 S 0.7794(3) 0.30015(16) 0.44500(16) 0.0722(6) Uani 1 1 d .
C21 C 0.7912(10) 0.3739(6) 0.3272(6) 0.0621(18) Uani 1 1 d .
C22 C 0.7961(10) 0.5024(5) 0.3169(6) 0.0688(19) Uani 1 1 d .
H22A H 0.8743 0.5365 0.3918 0.103 Uiso 1 1 calc R
H22B H 0.6708 0.5342 0.2917 0.103 Uiso 1 1 calc R
H22C H 0.8466 0.5228 0.2601 0.103 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 0.0601(6) 0.0608(6) 0.0559(5) -0.0054(4) 0.0286(5) -0.0029(4)
S11 0.0756(15) 0.0634(10) 0.0614(10) -0.0039(8) 0.0341(11) -0.0011(10)
S12 0.0941(17) 0.0594(10) 0.0770(12) -0.0019(8) 0.0489(13) -0.0005(10)
S13 0.0944(16) 0.0655(11) 0.0672(11) -0.0043(8) 0.0458(12) 0.0013(10)
C11 0.045(4) 0.062(4) 0.074(4) 0.000(3) 0.027(4) 0.005(3)
C12 0.075(6) 0.077(5) 0.069(4) 0.019(4) 0.034(4) 0.002(4)
S21 0.0793(14) 0.0640(10) 0.0607(10) 0.0022(8) 0.0364(11) -0.0032(9)
S22 0.0946(16) 0.0696(11) 0.0624(11) -0.0051(9) 0.0420(12) -0.0071(10)
C21 0.058(5) 0.062(4) 0.065(4) -0.003(3) 0.023(4) -0.005(3)
C22 0.065(5) 0.062(4) 0.077(4) -0.001(3) 0.027(5) -0.001(4)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S13 Ni1 S11 96.73(7)
S13 Ni1 S22 169.00(8)
S11 Ni1 S22 94.00(7)
S13 Ni1 S21 91.90(7)
S11 Ni1 S21 171.35(7)
S22 Ni1 S21 77.36(7)
C11 S11 Ni1 108.2(2)
C11 S12 S13 106.8(2)
S12 S13 Ni1 105.29(9)
C12 C11 S12 117.3(5)
C12 C11 S11 119.8(5)
S12 C11 S11 122.7(4)
C11 C12 H12A 109.5
C11 C12 H12B 109.5
H12A C12 H12B 109.5
C11 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C21 S21 Ni1 86.5(2)
C21 S22 Ni1 86.7(2)
C22 C21 S21 126.4(5)
C22 C21 S22 124.3(5)
S21 C21 S22 109.3(4)
C21 C22 H22A 109.5
C21 C22 H22B 109.5
H22A C22 H22B 109.5
C21 C22 H22C 109.5
H22A C22 H22C 109.5
H22B C22 H22C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 S13 2.1225(18)
Ni1 S11 2.1331(18)
Ni1 S22 2.2028(19)
Ni1 S21 2.2267(18)
S11 C11 1.681(6)
S12 C11 1.638(6)
S12 S13 2.027(2)
C11 C12 1.506(8)
C12 H12A 0.9600
C12 H12B 0.9600
C12 H12C 0.9600
S21 C21 1.686(6)
S22 C21 1.709(6)
C21 C22 1.429(8)
C22 H22A 0.9600
C22 H22B 0.9600
C22 H22C 0.9600
