#------------------------------------------------------------------------------
#$Date: 2017-07-29 07:50:41 +0200 (Sat 29 de Jul de 2017) $
#$Revision: 199401 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/81/2108137.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_2108137
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            'C18 H12 N6 Ni S4'
_chemical_formula_weight         499.29
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.1670(10)
_cell_angle_beta                 94.7270(10)
_cell_angle_gamma                108.5250(10)
_cell_formula_units_Z            1
_cell_length_a                   7.4307(2)
_cell_length_b                   8.9072(2)
_cell_length_c                   9.2445(2)
_cell_measurement_reflns_used    131084
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      33.29
_cell_measurement_theta_min      1.46
_cell_volume                     507.94(2)
_computing_cell_refinement       ' '
_computing_data_collection       ' '
_computing_data_reduction        ' '
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      15(2)
_diffrn_measured_fraction_theta_full 0.817
_diffrn_measured_fraction_theta_max 0.817
_diffrn_measurement_device_type  'APEX II CCD detector'
_diffrn_radiation_monochromator  DCM
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            130961
_diffrn_reflns_theta_full        33.29
_diffrn_reflns_theta_max         33.29
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.9634
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.826
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         16291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0296P)²+0.0397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                14895
_reflns_number_total             16291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lc5076sup1.cif
_cod_data_source_block           CCDC_1544718
_cod_database_code               2108137
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ni Ni 0.0000 0.5000 1.5000 0.004130(10) Uani d S 1 2
S S1 0.317618(9) 0.603163(9) 1.579636(9) 0.005930(10) Uani d . 1 1
S S2 0.012018(9) 0.581040(9) 1.308949(9) 0.006160(10) Uani d . 1 1
C C1 0.39474(3) 0.70368(3) 1.45924(3) 0.00597(3) Uani d . 1 1
C C2 0.26156(3) 0.69072(3) 1.33830(3) 0.00608(3) Uani d . 1 1
N N2 0.36226(4) 0.80414(4) 1.13119(4) 0.01179(4) Uani d . 1 1
C C4 0.32093(4) 0.75749(4) 1.22776(4) 0.00769(3) Uani d . 1 1
C C3 0.59890(3) 0.80103(3) 1.48805(3) 0.00709(3) Uani d . 1 1
N N1 0.76412(3) 0.88561(4) 1.51355(4) 0.01002(3) Uani d . 1 1
N N3 0.87136(3) 0.86159(3) 1.19702(3) 0.00776(3) Uani d . 1 1
C C9 0.85642(4) 1.01879(3) 1.22929(4) 0.00804(3) Uani d . 1 1
C C8 0.78291(4) 1.04088(3) 1.10109(4) 0.00795(3) Uani d . 1 1
C C7 0.72426(4) 0.89928(3) 0.94116(4) 0.00820(3) Uani d . 1 1
C C6 0.74185(4) 0.73830(4) 0.91130(4) 0.00921(3) Uani d . 1 1
C C5 0.81664(4) 0.72187(4) 1.04315(4) 0.00888(3) Uani d . 1 1
H H5 0.8355(16) 0.6178(14) 1.0364(14) 0.028(3) Uiso d . 1 1
H H7 0.6677(13) 0.9102(12) 0.8533(12) 0.0156(19) Uiso d . 1 1
H H9 0.9024(14) 1.1078(12) 1.3380(12) 0.017(2) Uiso d . 1 1
H H6 0.6975(14) 0.6343(12) 0.8005(12) 0.021(2) Uiso d . 1 1
H H8 0.7733(14) 1.1521(12) 1.1242(12) 0.021(2) Uiso d . 1 1
H H3 0.9178(14) 0.8491(12) 1.2818(13) 0.020(2) 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 -0.0020 0.0005 '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 -0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0366 0.0409 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.1862 0.4106 '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
S1 Ni S1 2_568 . 179.999(4)
S1 Ni S2 2_568 . 87.677(3)
S1 Ni S2 . . 92.324(3)
S1 Ni S2 2_568 2_568 92.324(3)
S1 Ni S2 . 2_568 87.676(3)
S2 Ni S2 . 2_568 180.0
C1 S1 Ni . . 103.123(8)
C2 S2 Ni . . 103.152(8)
C2 C1 C3 . . 120.31(2)
C2 C1 S1 . . 120.661(17)
C3 C1 S1 . . 119.032(17)
C1 C2 C4 . . 121.96(2)
C1 C2 S2 . . 120.477(18)
C4 C2 S2 . . 117.490(17)
N2 C4 C2 . . 176.58(3)
N1 C3 C1 . . 177.70(3)
C9 N3 C5 . . 122.83(2)
N3 C9 C8 . . 119.57(3)
C9 C8 C7 . . 119.06(2)
C8 C7 C6 . . 120.14(2)
C5 C6 C7 . . 118.96(3)
N3 C5 C6 . . 119.43(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni S1 2_568 2.1718
Ni S1 . 2.1718
Ni S2 . 2.1720
Ni S2 2_568 2.1721
S1 C1 . 1.7308(2)
S2 C2 . 1.7340(2)
C1 C2 . 1.3704(3)
C1 C3 . 1.4232(3)
C2 C4 . 1.4202(4)
N2 C4 . 1.1592(4)
C3 N1 . 1.1592(3)
N3 C9 . 1.3457(3)
N3 C5 . 1.3472(4)
C9 C8 . 1.3789(4)
C8 C7 . 1.3875(4)
C7 C6 . 1.3921(4)
C6 C5 . 1.3811(4)

_cod_database_fobs_code 2108137
