#------------------------------------------------------------------------------
#$Date: 2017-07-29 08:50:41 +0300 (Sat, 29 Jul 2017) $
#$Revision: 199401 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/81/2108134.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_2108134
loop_
_publ_author_name
'Chuang, Yu-Chun'
'Sheu, Chou-Fu'
'Lee, Gene-Hsiang'
'Chen, Yu-Sheng'
'Wang, Yu'
_publ_section_title
;
 Charge density studies of 3d metal (Ni/Cu) complexes with a
 non-innocent ligand
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              634
_journal_page_last               642
_journal_paper_doi               10.1107/S2052520617007119
_journal_volume                  73
_journal_year                    2017
_chemical_formula_sum            'C13 H6 N5 Ni S4'
_chemical_formula_weight         419.18
_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                 116.837(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1805(10)
_cell_length_b                   6.3567(5)
_cell_length_c                   17.0872(7)
_cell_measurement_reflns_used    16292
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      1.41
_cell_volume                     1568.20(18)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16292
_diffrn_reflns_theta_full        50.00
_diffrn_reflns_theta_max         50.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  0.7182
_exptl_absorpt_correction_T_min  0.5026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.470
_refine_ls_extinction_coef       0.0065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         16292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0317P)²+0.3858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                14166
_reflns_number_total             16292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lc5076sup1.cif
_cod_data_source_block           CCDC_1525430
_cod_original_cell_volume        1568.20(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2108134
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_type_symbol
_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_occupancy
_atom_site_symmetry_multiplicity
Ni Ni1 0.633099(5) 0.513914(13) 0.503857(5) 0.00990(2) Uani d 1 1
S S1 0.718112(11) 0.79137(3) 0.544576(10) 0.01244(3) Uani d 1 1
S S2 0.712140(12) 0.35970(3) 0.627215(10) 0.01296(3) Uani d 1 1
S S3 0.547816(12) 0.67530(3) 0.383680(11) 0.01362(3) Uani d 1 1
S S4 0.551011(11) 0.23250(3) 0.462853(10) 0.01241(2) Uani d 1 1
N N1 0.92449(6) 1.01174(12) 0.72942(5) 0.02236(12) Uani d 1 1
N N2 0.90642(5) 0.45331(12) 0.84827(4) 0.01999(11) Uani d 1 1
N N3 0.33551(5) 0.59238(12) 0.17317(4) 0.01947(10) Uani d 1 1
N N4 0.33876(5) 0.03446(11) 0.26528(4) 0.01799(10) Uani d 1 1
N N5 0.79905(4) 0.42283(10) 0.41538(4) 0.01507(8) Uani d 1 1
C C1 0.79871(4) 0.73158(10) 0.64971(4) 0.01219(8) Uani d 1 1
C C2 0.79550(4) 0.54197(10) 0.68679(4) 0.01214(8) Uani d 1 1
C C3 0.86802(5) 0.88515(11) 0.69516(4) 0.01519(9) Uani d 1 1
C C4 0.85810(5) 0.49211(11) 0.77552(4) 0.01438(9) Uani d 1 1
C C5 0.46594(4) 0.49220(10) 0.32538(4) 0.01209(8) Uani d 1 1
C C6 0.46731(4) 0.29523(10) 0.36044(4) 0.01181(8) Uani d 1 1
C C7 0.39438(5) 0.54811(11) 0.24117(4) 0.01397(8) Uani d 1 1
C C8 0.39751(5) 0.14632(10) 0.31021(4) 0.01361(8) Uani d 1 1
C C9 0.83363(5) 0.61377(12) 0.41451(4) 0.01628(10) Uani d 1 1
C C10 0.90564(5) 0.69132(12) 0.48989(5) 0.01650(10) Uani d 1 1
C C11 0.94043(5) 0.56886(12) 0.56549(4) 0.01594(9) Uani d 1 1
C C12 0.90282(5) 0.37159(12) 0.56416(5) 0.01640(10) Uani d 1 1
C C13 0.83052(5) 0.30060(11) 0.48721(5) 0.01598(9) Uani d 1 1
H H5 0.7589(14) 0.377(3) 0.3702(13) 0.044(5) Uiso d 1 1
H H9 0.8064(11) 0.686(3) 0.3608(10) 0.022(3) Uiso d 1 1
H H10 0.9300(11) 0.822(3) 0.4884(10) 0.024(4) Uiso d 1 1
H H11 0.9889(11) 0.619(3) 0.6170(10) 0.022(4) Uiso d 1 1
H H12 0.9231(11) 0.289(3) 0.6118(11) 0.028(4) Uiso d 1 1
H H13 0.8000(11) 0.173(3) 0.4804(10) 0.026(4) Uiso d 1 1
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
S2 Ni1 S4 86.934(9)
S2 Ni1 S3 176.207(8)
S4 Ni1 S3 92.874(9)
S2 Ni1 S1 92.657(9)
S4 Ni1 S1 178.517(8)
S3 Ni1 S1 87.628(9)
C1 S1 Ni1 103.26(2)
C2 S2 Ni1 103.53(2)
C5 S3 Ni1 103.11(2)
C6 S4 Ni1 103.14(2)
C9 N5 C13 123.11(6)
C2 C1 C3 122.31(6)
C2 C1 S1 120.47(5)
C3 C1 S1 117.22(5)
C1 C2 C4 121.88(6)
C1 C2 S2 120.07(5)
C4 C2 S2 118.02(5)
N1 C3 C1 177.62(8)
N2 C4 C2 177.60(8)
C6 C5 C7 120.62(6)
C6 C5 S3 120.53(5)
C7 C5 S3 118.82(5)
C5 C6 C8 119.12(6)
C5 C6 S4 120.34(5)
C8 C6 S4 120.54(5)
N3 C7 C5 179.12(8)
N4 C8 C6 175.77(7)
N5 C9 C10 119.61(6)
C9 C10 C11 118.95(7)
C12 C11 C10 119.94(6)
C13 C12 C11 119.10(6)
N5 C13 C12 119.27(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 S2 2.1461(2)
Ni1 S4 2.1482(2)
Ni1 S3 2.1482(2)
Ni1 S1 2.1501(2)
S1 C1 1.7196(6)
S2 C2 1.7199(7)
S3 C5 1.7060(6)
S4 C6 1.7076(6)
N1 C3 1.1586(10)
N2 C4 1.1576(9)
N3 C7 1.1564(9)
N4 C8 1.1575(9)
N5 C9 1.3394(10)
N5 C13 1.3435(9)
C1 C2 1.3736(9)
C1 C3 1.4239(9)
C2 C4 1.4278(9)
C5 C6 1.3839(9)
C5 C7 1.4259(9)
C6 C8 1.4258(9)
C9 C10 1.3801(10)
C10 C11 1.3910(10)
C11 C12 1.3895(11)
C12 C13 1.3829(10)

_cod_database_fobs_code 2108134
