#------------------------------------------------------------------------------
#$Date: 2017-02-04 16:10:19 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191707 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/59/7055904.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_7055904
loop_
_publ_author_name
'Saha, Pinaki'
'Samanta, Debasish'
'Ghosh, Prasanta'
_publ_section_title
;
 Glyoxalbis(2-methylmercaptoanil) complexes of nickel and ruthenium:
 radical versus non-radical states
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              1149
_journal_paper_doi               10.1039/C6NJ02903E
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C16 H16 Cl2 N2 Ni S2'
_chemical_formula_sum            'C17 H18 Cl4 N2 Ni S2'
_chemical_formula_weight         514.96
_chemical_name_systematic        1_CH2Cl2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-12-11 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1597(19)
_cell_length_b                   16.2161(18)
_cell_length_c                   6.9479(7)
_cell_measurement_reflns_used    6214
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.52
_cell_volume                     2046.0(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21735
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.987
_diffrn_reflns_theta_min         2.243
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0438P)²+1.2465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2269
_reflns_number_total             2541
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj02903e2.cif
_cod_data_source_block           1_CH2Cl2
_cod_depositor_comments
'Adding full bibliography for 7055903--7055906.cif.'
_cod_database_code               7055904
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.61082(2) 0.7500 0.36434(4) 0.02535(10) Uani 1 2 d S T P
Cl1 Cl 0.51371(3) 0.7500 0.59972(9) 0.03696(15) Uani 1 2 d S T P
Cl2 Cl 0.70436(3) 0.7500 0.12352(8) 0.03276(14) Uani 1 2 d S T P
S1 S 0.55201(2) 0.62496(3) 0.24547(6) 0.03215(12) Uani 1 1 d . . .
N1 N 0.66922(7) 0.66953(8) 0.52797(19) 0.0260(3) Uani 1 1 d . . .
C1 C 0.66039(9) 0.58354(10) 0.5116(2) 0.0281(3) Uani 1 1 d . . .
C2 C 0.70364(11) 0.52640(12) 0.6115(3) 0.0358(4) Uani 1 1 d . . .
H2A H 0.7416 0.5446 0.6905 0.043 Uiso 1 1 calc R U .
C3 C 0.69002(12) 0.44315(12) 0.5930(3) 0.0427(5) Uani 1 1 d . . .
H3A H 0.7194 0.4053 0.6579 0.051 Uiso 1 1 calc R U .
C4 C 0.63283(12) 0.41567(12) 0.4784(3) 0.0446(5) Uani 1 1 d . . .
H4A H 0.6230 0.3595 0.4692 0.054 Uiso 1 1 calc R U .
C5 C 0.59031(11) 0.47146(12) 0.3775(3) 0.0396(4) Uani 1 1 d . . .
H5A H 0.5516 0.4527 0.3016 0.048 Uiso 1 1 calc R U .
C6 C 0.60495(9) 0.55544(11) 0.3886(2) 0.0307(4) Uani 1 1 d . . .
C7 C 0.58319(13) 0.59609(14) 0.0071(3) 0.0451(5) Uani 1 1 d . . .
H7A H 0.5586 0.6294 -0.0872 0.068 Uiso 1 1 calc R U .
H7B H 0.6354 0.6045 -0.0022 0.068 Uiso 1 1 calc R U .
H7C H 0.5721 0.5390 -0.0155 0.068 Uiso 1 1 calc R U .
C8 C 0.70955(9) 0.70499(10) 0.6548(2) 0.0291(3) Uani 1 1 d . . .
H8A H 0.7374 0.6749 0.7424 0.035 Uiso 1 1 calc R U .
C9 C 0.88077(19) 0.7500 0.3586(5) 0.0557(8) Uani 1 2 d S T P
H9A H 0.8377 0.7500 0.2759 0.067 Uiso 1 2 calc R U P
H9B H 0.9241 0.7500 0.2770 0.067 Uiso 1 2 calc R U P
Cl3 Cl 0.88051(4) 0.66048(5) 0.50064(10) 0.06454(18) Uani 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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
N1 Ni1 N1 80.02(8) . 7_575
N1 Ni1 Cl2 91.19(4) . .
N1 Ni1 Cl2 91.19(4) 7_575 .
N1 Ni1 Cl1 90.13(4) . .
N1 Ni1 Cl1 90.13(4) 7_575 .
Cl2 Ni1 Cl1 178.28(3) . .
N1 Ni1 S1 162.57(4) . 7_575
N1 Ni1 S1 83.33(4) 7_575 7_575
Cl2 Ni1 S1 94.267(16) . 7_575
Cl1 Ni1 S1 84.785(16) . 7_575
N1 Ni1 S1 83.33(4) . .
N1 Ni1 S1 162.57(4) 7_575 .
Cl2 Ni1 S1 94.268(16) . .
Cl1 Ni1 S1 84.785(16) . .
S1 Ni1 S1 112.69(2) 7_575 .
C6 S1 C7 100.24(9) . .
C6 S1 Ni1 95.78(6) . .
C7 S1 Ni1 112.83(7) . .
C8 N1 C1 124.37(15) . .
C8 N1 Ni1 113.27(11) . .
C1 N1 Ni1 122.14(11) . .
C6 C1 C2 119.49(16) . .
C6 C1 N1 117.02(15) . .
C2 C1 N1 123.50(16) . .
C3 C2 C1 120.10(18) . .
C2 C3 C4 120.28(19) . .
C5 C4 C3 120.09(18) . .
C4 C5 C6 120.48(18) . .
C5 C6 C1 119.42(17) . .
C5 C6 S1 119.03(14) . .
C1 C6 S1 121.55(13) . .
N1 C8 C8 116.65(10) . 7_575
Cl3 C9 Cl3 111.57(18) . 7_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.0298(14) .
Ni1 N1 2.0298(14) 7_575
Ni1 Cl2 2.3844(7) .
Ni1 Cl1 2.4051(7) .
Ni1 S1 2.4359(5) 7_575
Ni1 S1 2.4360(5) .
S1 C6 1.7844(18) .
S1 C7 1.812(2) .
N1 C8 1.282(2) .
N1 C1 1.408(2) .
C1 C6 1.397(2) .
C1 C2 1.399(2) .
C2 C3 1.379(3) .
C3 C4 1.383(3) .
C4 C5 1.380(3) .
C5 C6 1.390(3) .
C8 C8 1.460(3) 7_575
C9 Cl3 1.7556(19) .
C9 Cl3 1.7556(19) 7_575
