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#$Date: 2022-11-10 12:27:05 +0200 (Thu, 10 Nov 2022) $
#$Revision: 279202 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/60/8106062.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_8106062
loop_
_publ_author_name
'Lin, Long'
'Zhu, Ling-Hao'
'Wang, Yuan'
_publ_section_title
;
 Crystal structure of
 bis(N′-((1H-pyrrol-2-yl)methylene)-1-methylthio-methanethiohydrazido-κ2
 S,N)nickel(II), C14H16N6NiS4
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              105
_journal_page_last               106
_journal_paper_doi               10.1515/ncrs-2017-0192
_journal_volume                  233
_journal_year                    2018
_chemical_formula_sum            'C14 H16 N6 Ni S4'
_chemical_formula_weight         455.28
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.77(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.817(16)
_cell_length_b                   10.172(17)
_cell_length_c                   10.043(17)
_cell_measurement_reflns_used    374
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.63
_cell_measurement_theta_min      2.86
_cell_volume                     892(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_sigmaI/netI    0.1338
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4772
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  0.8591
_exptl_absorpt_correction_T_min  0.7991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.260
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0788
_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)+(0.0690P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1962
_reflns_number_gt                991
_reflns_number_total             1761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0192_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               8106062
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.0000 0.0420(5) Uani 1 2 d S . .
N2 N -0.1032(6) 0.0017(6) 0.1518(6) 0.0395(13) Uani 1 1 d . . .
N3 N -0.2360(7) -0.0751(6) 0.1514(6) 0.0447(15) Uani 1 1 d . . .
N1 N -0.2512(7) -0.0030(6) 0.4098(6) 0.0490(16) Uani 1 1 d . . .
H1A H -0.2974 -0.0628 0.3590 0.059 Uiso 1 1 calc R . .
C5 C -0.0713(8) 0.0674(7) 0.2599(7) 0.0435(17) Uani 1 1 d . . .
H5A H 0.0142 0.1210 0.2600 0.052 Uiso 1 1 calc R . .
C4 C -0.1367(8) 0.0758(7) 0.3766(7) 0.0447(18) Uani 1 1 d . . .
C2 C -0.1899(9) 0.1268(8) 0.5797(7) 0.054(2) Uani 1 1 d . . .
H2B H -0.1885 0.1682 0.6624 0.064 Uiso 1 1 calc R . .
C3 C -0.0992(9) 0.1567(7) 0.4827(7) 0.0483(19) Uani 1 1 d . . .
H3A H -0.0245 0.2218 0.4891 0.058 Uiso 1 1 calc R . .
C1 C -0.2805(9) 0.0269(8) 0.5326(8) 0.056(2) Uani 1 1 d . . .
H1B H -0.3521 -0.0146 0.5783 0.067 Uiso 1 1 calc R . .
S1 S -0.2078(2) -0.0784(2) -0.10602(18) 0.0528(6) Uani 1 1 d . . .
S2 S -0.4626(2) -0.1937(2) 0.00517(17) 0.0511(6) Uani 1 1 d . . .
C6 C -0.2907(8) -0.1106(7) 0.0351(7) 0.0407(17) Uani 1 1 d . . .
C7 C -0.5171(9) -0.2047(8) 0.1666(7) 0.061(2) Uani 1 1 d . . .
H7A H -0.6131 -0.2502 0.1618 0.091 Uiso 1 1 calc R . .
H7B H -0.5277 -0.1179 0.2018 0.091 Uiso 1 1 calc R . .
H7C H -0.4404 -0.2520 0.2246 0.091 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 0.0294(7) 0.0554(9) 0.0420(8) 0.0020(6) 0.0079(5) -0.0009(6)
N2 0.023(3) 0.054(3) 0.041(3) -0.001(3) 0.006(2) -0.001(3)
N3 0.034(4) 0.056(4) 0.045(4) -0.003(3) 0.009(3) -0.005(3)
N1 0.036(4) 0.068(4) 0.043(3) -0.010(3) 0.005(3) -0.009(3)
C5 0.027(4) 0.055(5) 0.049(4) 0.007(4) 0.009(3) 0.003(3)
C4 0.032(4) 0.054(5) 0.048(4) 0.001(4) 0.005(3) -0.003(4)
C2 0.053(5) 0.064(5) 0.045(4) -0.007(4) 0.009(4) 0.006(4)
C3 0.042(5) 0.053(5) 0.051(4) -0.011(4) 0.009(4) -0.001(4)
C1 0.036(4) 0.083(6) 0.052(5) -0.003(4) 0.020(4) -0.002(4)
S1 0.0359(11) 0.0817(15) 0.0418(11) 0.0001(10) 0.0085(9) -0.0072(10)
S2 0.0352(11) 0.0736(14) 0.0454(11) -0.0044(10) 0.0083(9) -0.0120(10)
C6 0.026(4) 0.051(5) 0.046(4) -0.002(3) 0.009(3) -0.001(3)
C7 0.043(5) 0.086(6) 0.054(5) 0.000(4) 0.009(4) -0.017(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'
N N 0.0061 0.0033 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Ni1 N2 180.0(3) . 3
N2 Ni1 S1 94.0(2) . 3
N2 Ni1 S1 86.0(2) 3 3
N2 Ni1 S1 86.0(2) . .
N2 Ni1 S1 94.0(2) 3 .
S1 Ni1 S1 180.0 3 .
C5 N2 N3 112.5(6) . .
C5 N2 Ni1 128.4(5) . .
N3 N2 Ni1 119.1(4) . .
C6 N3 N2 112.2(6) . .
C1 N1 C4 109.6(6) . .
N2 C5 C4 133.5(7) . .
C3 C4 N1 105.9(7) . .
C3 C4 C5 128.5(7) . .
N1 C4 C5 125.5(7) . .
C1 C2 C3 107.1(7) . .
C4 C3 C2 108.7(7) . .
N1 C1 C2 108.6(7) . .
C6 S1 Ni1 95.3(3) . .
C6 S2 C7 102.3(3) . .
N3 C6 S1 124.2(6) . .
N3 C6 S2 121.4(5) . .
S1 C6 S2 114.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 1.878(6) .
Ni1 N2 1.878(6) 3
Ni1 S1 2.145(3) 3
Ni1 S1 2.145(3) .
N2 C5 1.273(9) .
N2 N3 1.407(8) .
N3 C6 1.255(8) .
N1 C1 1.329(8) .
N1 C4 1.366(9) .
C5 C4 1.377(9) .
C4 C3 1.352(10) .
C2 C1 1.339(10) .
C2 C3 1.375(9) .
S1 C6 1.712(7) .
S2 C6 1.726(7) .
S2 C7 1.756(7) .
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
N1 H1A N3 0.86 2.23 2.718(9) 116.1 .
