#------------------------------------------------------------------------------
#$Date: 2020-11-18 07:09:42 +0200 (Wed, 18 Nov 2020) $
#$Revision: 259161 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/36/2243679.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_2243679
loop_
_publ_author_name
'Jochim, Aleksej'
'Radulovic, Rastko'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 bis(tetramethylthiourea-κS)bis(thiocyanato-κN)nickel(II)
;
_journal_coeditor_code           TX2033
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1841
_journal_page_last               1845
_journal_paper_doi               10.1107/S2056989020015121
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ni (N C S)2 (C5 H12 N2 S1)2]'
_chemical_formula_sum            'C12 H24 N6 Ni S4'
_chemical_formula_weight         439.32
_chemical_name_systematic
;
Bis(tetramethylthiourea-κS)bis(thiocyanato-κN)nickel(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 103.140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7245(3)
_cell_length_b                   6.2050(3)
_cell_length_c                   15.1579(5)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.001
_cell_measurement_theta_min      1.950
_cell_volume                     982.28(6)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008) and DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.001
_diffrn_reflns_theta_min         1.950
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.8741
_exptl_absorpt_correction_T_min  0.7156
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red and X-Shape; Stoe & Cie, 2002)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0560P)²+0.1275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                1607
_reflns_number_total             1945
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tx2033sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2243679
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.500000 0.29112(8) 0.750000 0.03467(16) Uani d 1 . .
N N1 0.3260(3) 0.2587(4) 0.70613(16) 0.0416(6) Uani d 1 . .
C C1 0.2221(3) 0.1954(5) 0.67755(18) 0.0375(6) Uani d 1 . .
S S1 0.07891(8) 0.10731(15) 0.63716(6) 0.0536(2) Uani d 1 . .
S S11 0.51467(7) 0.31221(13) 0.60612(5) 0.0421(2) Uani d 1 . .
C C11 0.6634(3) 0.4138(5) 0.60210(18) 0.0368(6) Uani d 1 . .
N N11 0.7271(2) 0.3274(4) 0.54463(16) 0.0402(5) Uani d 1 . .
C C12 0.7000(4) 0.1112(6) 0.5071(2) 0.0551(8) Uani d 1 . .
H H12A 0.658143 0.026358 0.546631 0.083 Uiso calc 1 . .
H H12B 0.780347 0.041141 0.502878 0.083 Uiso calc 1 . .
H H12C 0.643405 0.121046 0.446582 0.083 Uiso calc 1 . .
C C13 0.8112(3) 0.4537(6) 0.5012(2) 0.0495(8) Uani d 1 . .
H H13A 0.801002 0.607219 0.513061 0.074 Uiso calc 1 . .
H H13B 0.788670 0.427747 0.435733 0.074 Uiso calc 1 . .
H H13C 0.900282 0.410930 0.525696 0.074 Uiso calc 1 . .
N N12 0.7143(2) 0.5845(4) 0.65156(16) 0.0410(5) Uani d 1 . .
C C14 0.6379(4) 0.7320(5) 0.6929(2) 0.0522(8) Uani d 1 . .
H H14A 0.549871 0.735359 0.656431 0.078 Uiso calc 1 . .
H H14B 0.674874 0.876929 0.695780 0.078 Uiso calc 1 . .
H H14C 0.637766 0.682513 0.754302 0.078 Uiso calc 1 . .
C C15 0.8524(3) 0.6057(6) 0.6875(2) 0.0522(8) Uani d 1 . .
H H15A 0.894942 0.470956 0.677642 0.078 Uiso calc 1 . .
H H15B 0.869414 0.636391 0.752599 0.078 Uiso calc 1 . .
H H15C 0.885381 0.723850 0.656457 0.078 Uiso calc 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 . 2_656 167.47(16) y
N1 Ni1 S11 . . 86.80(8) y
N1 Ni1 S11 2_656 . 93.93(8) y
S11 Ni1 S11 2_656 . 173.26(5) y
C1 N1 Ni1 . . 166.5(3) ?
N1 C1 S1 . . 179.4(3) ?
C11 S11 Ni1 . . 109.10(9) ?
N11 C11 N12 . . 118.6(3) ?
N11 C11 S11 . . 119.3(2) ?
N12 C11 S11 . . 122.0(2) ?
C11 N11 C13 . . 122.6(3) ?
C11 N11 C12 . . 122.5(3) ?
C13 N11 C12 . . 113.9(2) ?
C11 N12 C14 . . 122.6(3) ?
C11 N12 C15 . . 121.9(3) ?
C14 N12 C15 . . 113.7(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 1.844(3) y
Ni1 S11 . 2.2259(7) y
N1 C1 . 1.168(4) ?
C1 S1 . 1.614(3) ?
S11 C11 . 1.729(3) ?
C11 N11 . 1.335(4) ?
C11 N12 . 1.340(4) ?
N11 C13 . 1.460(4) ?
N11 C12 . 1.460(4) ?
N12 C14 . 1.461(4) ?
N12 C15 . 1.464(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C12 H12B S1 3_656 0.98 3.01 3.821(3) 140.3 yes
C13 H13C S1 1_655 0.98 2.93 3.798(3) 147.7 yes

_cod_database_fobs_code 2243679
