#------------------------------------------------------------------------------
#$Date: 2020-08-01 08:02:09 +0300 (Sat, 01 Aug 2020) $
#$Revision: 254728 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/35/2243515.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_2243515
loop_
_publ_author_name
'Jochim, Aleksej'
'Radulovic, Rastko'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structure of
 bis(tetramethylthiourea-κS)bis(thiocyanato-κN)cobalt(II)
;
_journal_coeditor_code           TX2029
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1373
_journal_page_last               1377
_journal_paper_doi               10.1107/S205698902001021X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Co (N C S)2 (C5 H12 N2 S)2]'
_chemical_formula_sum            'C12 H24 Co N6 S4'
_chemical_formula_weight         439.54
_chemical_name_systematic
;
Bis(tetramethylthiourea-κS)bis(thiocyanato-κN)cobalt(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 97.667(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3288(13)
_cell_length_b                   11.2140(8)
_cell_length_c                   13.8579(13)
_cell_measurement_reflns_used    14562
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.002
_cell_measurement_theta_min      2.345
_cell_volume                     2052.8(3)
_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 0.986
_diffrn_measured_fraction_theta_max 0.985
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14562
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.002
_diffrn_reflns_theta_min         2.345
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.8046
_exptl_absorpt_correction_T_min  0.6441
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red and X-Shape; Stoe & Cie, 2002)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.390
_refine_ls_extinction_coef       0.0092(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2018)
;
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0308
_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)+(0.0593P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                3826
_reflns_number_total             4409
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tx2029sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243515
_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+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_disorder_assembly
_atom_site_disorder_group
Co Co1 0.31466(2) 0.44406(2) 0.18631(2) 0.03623(10) Uani d 1 . .
N N1 0.26892(14) 0.28853(15) 0.13540(11) 0.0473(4) Uani d 1 . .
C C1 0.22426(14) 0.20050(17) 0.11758(12) 0.0400(4) Uani d 1 . .
S S1 0.16309(4) 0.07801(5) 0.09170(4) 0.05239(14) Uani d 1 . .
N N2 0.23001(14) 0.56237(15) 0.11124(12) 0.0476(4) Uani d 1 . .
C C2 0.18324(14) 0.63196(16) 0.06226(12) 0.0389(4) Uani d 1 . .
S S2 0.11944(5) 0.73069(6) -0.00388(4) 0.05992(16) Uani d 1 . .
S S11 0.31339(4) 0.42243(5) 0.35233(3) 0.04323(13) Uani d 1 . .
C C11 0.20254(13) 0.33900(15) 0.34598(11) 0.0346(3) Uani d 1 . .
N N11 0.11381(12) 0.39071(14) 0.31533(11) 0.0410(3) Uani d 1 . .
C C12 0.09967(18) 0.51955(19) 0.32179(17) 0.0551(5) Uani d 1 . .
H H12A 0.150522 0.552429 0.372410 0.083 Uiso calc 1 . .
H H12B 0.031805 0.536217 0.338259 0.083 Uiso calc 1 . .
H H12C 0.107221 0.556414 0.259049 0.083 Uiso calc 1 . .
C C13 0.02995(16) 0.3274(2) 0.25917(16) 0.0580(5) Uani d 1 . .
H H13A 0.053452 0.249499 0.239227 0.087 Uiso calc 1 . .
H H13B 0.004558 0.374051 0.201245 0.087 Uiso calc 1 . .
H H13C -0.024519 0.316034 0.299316 0.087 Uiso calc 1 . .
N N12 0.20637(12) 0.22456(14) 0.37071(10) 0.0392(3) Uani d 1 . .
C C14 0.12200(18) 0.1612(2) 0.40544(16) 0.0538(5) Uani d 1 . .
H H14A 0.071235 0.218979 0.420747 0.081 Uiso calc 1 . .
H H14B 0.147061 0.115724 0.464096 0.081 Uiso calc 1 . .
H H14C 0.091237 0.106630 0.354706 0.081 Uiso calc 1 . .
C C15 0.29981(18) 0.1561(2) 0.37811(16) 0.0561(5) Uani d 1 . .
H H15A 0.345116 0.191657 0.335874 0.084 Uiso calc 1 . .
H H15B 0.284447 0.073696 0.357751 0.084 Uiso calc 1 . .
H H15C 0.332793 0.156901 0.445679 0.084 Uiso calc 1 . .
S S21 0.47009(4) 0.51223(5) 0.15128(3) 0.04435(13) Uani d 1 . .
C C21 0.56218(13) 0.43472(14) 0.22564(11) 0.0333(3) Uani d 1 . .
N N21 0.57661(12) 0.45344(13) 0.32191(10) 0.0369(3) Uani d 1 . .
C C22 0.54437(16) 0.56303(18) 0.36544(14) 0.0463(4) Uani d 1 . .
H H22A 0.540529 0.627600 0.317434 0.069 Uiso calc 1 . .
H H22B 0.593316 0.584178 0.422032 0.069 Uiso calc 1 . .
H H22C 0.477595 0.550936 0.386096 0.069 Uiso calc 1 . .
C C23 0.60727(17) 0.3590(2) 0.39199(12) 0.0507(5) Uani d 1 . .
H H23A 0.610361 0.283021 0.357553 0.076 Uiso calc 1 . .
H H23B 0.557930 0.352888 0.438242 0.076 Uiso calc 1 . .
H H23C 0.674128 0.377561 0.427288 0.076 Uiso calc 1 . .
N N22 0.62202(12) 0.35804(13) 0.18656(9) 0.0384(3) Uani d 1 . .
C C24 0.72499(16) 0.3301(2) 0.23060(14) 0.0509(5) Uani d 1 . .
H H24A 0.745874 0.386147 0.283738 0.076 Uiso calc 1 . .
H H24B 0.771017 0.336746 0.181307 0.076 Uiso calc 1 . .
H H24C 0.727201 0.248577 0.256314 0.076 Uiso calc 1 . .
C C25 0.59760(19) 0.3148(2) 0.08646(13) 0.0536(5) Uani d 1 . .
H H25A 0.523941 0.309911 0.069608 0.080 Uiso calc 1 . .
H H25B 0.627351 0.235605 0.080900 0.080 Uiso calc 1 . .
H H25C 0.625178 0.370024 0.041890 0.080 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'
Co Co 0.3494 0.9721 '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 Co1 N2 . . 106.56(7) y
N1 Co1 S11 . . 102.86(5) y
N2 Co1 S11 . . 121.40(5) y
N1 Co1 S21 . . 117.66(5) y
N2 Co1 S21 . . 97.67(6) y
S11 Co1 S21 . . 111.564(19) y
C1 N1 Co1 . . 164.57(16) ?
N1 C1 S1 . . 179.27(18) ?
C2 N2 Co1 . . 175.96(17) ?
N2 C2 S2 . . 178.70(18) ?
C11 S11 Co1 . . 97.16(5) ?
N12 C11 N11 . . 120.27(16) ?
N12 C11 S11 . . 120.22(13) ?
N11 C11 S11 . . 119.51(14) ?
C11 N11 C13 . . 122.80(17) ?
C11 N11 C12 . . 121.74(17) ?
C13 N11 C12 . . 114.72(17) ?
C11 N12 C15 . . 122.09(17) ?
C11 N12 C14 . . 123.28(16) ?
C15 N12 C14 . . 114.12(17) ?
C21 S21 Co1 . . 107.02(6) ?
N22 C21 N21 . . 119.39(15) ?
N22 C21 S21 . . 119.81(12) ?
N21 C21 S21 . . 120.76(13) ?
C21 N21 C23 . . 122.68(15) ?
C21 N21 C22 . . 122.21(15) ?
C23 N21 C22 . . 114.11(15) ?
C21 N22 C24 . . 123.21(14) ?
C21 N22 C25 . . 121.86(16) ?
C24 N22 C25 . . 113.75(16) ?
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
Co1 N1 . 1.9484(17) y
Co1 N2 . 1.9499(17) y
Co1 S11 . 2.3157(5) y
Co1 S21 . 2.3196(6) y
N1 C1 . 1.162(3) ?
C1 S1 . 1.613(2) ?
N2 C2 . 1.160(2) ?
C2 S2 . 1.6066(18) ?
S11 C11 . 1.7411(18) ?
C11 N12 . 1.327(2) ?
C11 N11 . 1.335(2) ?
N11 C13 . 1.459(3) ?
N11 C12 . 1.461(3) ?
N12 C15 . 1.455(3) ?
N12 C14 . 1.465(3) ?
S21 C21 . 1.7282(17) ?
C21 N22 . 1.336(2) ?
C21 N21 . 1.339(2) ?
N21 C23 . 1.458(2) ?
N21 C22 . 1.459(2) ?
N22 C24 . 1.460(3) ?
N22 C25 . 1.464(2) ?
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 2 0.98 2.93 3.906(2) 174.0 yes
C14 H14A S2 2_545 0.98 2.93 3.741(2) 140.8 yes
C22 H22C S11 . 0.98 2.61 3.442(2) 142.8 yes
C24 H24A S1 2_655 0.98 2.92 3.878(2) 166.2 yes

_cod_database_fobs_code 2243515
