#------------------------------------------------------------------------------
#$Date: 2021-12-22 04:13:55 +0100 (Wed 22 de Dec de 2021) $
#$Revision: 271580 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/39/2243961.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_2243961
loop_
_publ_author_name
'Krebs, Christoph'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Synthesis, crystal structure and thermal properties of
 bis(1,3-dicyclohexylthiourea-κS)bis(isothiocyanato-κN)cobalt(II)
;
_journal_coeditor_code           ZQ2269
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205698902101327X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Co (N C S)2 (C13 H24 N2 S)2]'
_chemical_formula_moiety         'C28 H48 Co N6 S4'
_chemical_formula_sum            'C28 H48 Co N6 S4'
_chemical_formula_weight         655.89
_chemical_name_systematic
;
Bis(1,3-dicyclohexylthiourea-κS)bis(isothiocyanato-κN)cobalt(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                90
_cell_angle_beta                 125.619(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0667(4)
_cell_length_b                   8.82820(10)
_cell_length_c                   18.8910(3)
_cell_measurement_reflns_used    13904
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.4760
_cell_measurement_theta_min      2.8510
_cell_volume                     3262.76(12)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20399
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.987
_diffrn_reflns_theta_min         4.520
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'intense blue'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0345
_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)+(0.0540P)²+5.0479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                3462
_reflns_number_total             3503
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            zq2269sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        3262.76(11)
_cod_database_code               2243961
_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.500000 0.91248(4) 0.750000 0.02073(12) Uani d 1 . .
N N1 0.57874(8) 1.03449(18) 0.78063(11) 0.0283(3) Uani d 1 . .
C C1 0.62890(10) 1.1041(2) 0.82549(13) 0.0241(4) Uani d 1 . .
S S1 0.69885(2) 1.19936(6) 0.88857(3) 0.02946(13) Uani d 1 . .
S S11 0.53579(2) 0.76716(5) 0.87146(3) 0.02478(12) Uani d 1 . .
C C11 0.59547(9) 0.6489(2) 0.87525(12) 0.0221(3) Uani d 1 . .
N N11 0.63300(8) 0.70206(18) 0.84996(11) 0.0257(3) Uani d 1 . .
H H11 0.628830 0.799458 0.837934 0.031 Uiso calc 1 . .
C C12 0.68063(9) 0.6182(2) 0.83960(13) 0.0250(4) Uani d 1 . .
H H12 0.664260 0.511209 0.823464 0.030 Uiso calc 1 . .
C C13 0.67862(11) 0.6900(3) 0.76500(14) 0.0377(5) Uani d 1 . .
H H13A 0.691074 0.798367 0.777936 0.045 Uiso calc 1 . .
H H13B 0.631610 0.683568 0.710954 0.045 Uiso calc 1 . .
C C14 0.72780(12) 0.6107(3) 0.75124(15) 0.0433(6) Uani d 1 . .
H H14A 0.712524 0.504987 0.732404 0.052 Uiso calc 1 . .
H H14B 0.727319 0.662885 0.704507 0.052 Uiso calc 1 . .
C C15 0.80009(11) 0.6105(3) 0.83419(15) 0.0342(5) Uani d 1 . .
H H15A 0.817213 0.715832 0.849578 0.041 Uiso calc 1 . .
H H15B 0.830355 0.553156 0.824289 0.041 Uiso calc 1 . .
C C16 0.80239(10) 0.5391(2) 0.90921(14) 0.0297(4) Uani d 1 . .
H H16A 0.849393 0.546680 0.963165 0.036 Uiso calc 1 . .
H H16B 0.790582 0.430304 0.896754 0.036 Uiso calc 1 . .
C C17 0.75272(10) 0.6167(2) 0.92332(13) 0.0276(4) Uani d 1 . .
H H17A 0.752748 0.562352 0.969193 0.033 Uiso calc 1 . .
H H17B 0.767965 0.721974 0.943308 0.033 Uiso calc 1 . .
N N12 0.60327(7) 0.50735(18) 0.90351(10) 0.0224(3) Uani d 1 . .
H H12A 0.635837 0.452301 0.908415 0.027 Uiso calc 1 . .
C C18 0.56066(9) 0.4371(2) 0.92713(12) 0.0212(3) Uani d 1 . .
H H18 0.550070 0.515812 0.955748 0.025 Uiso calc 1 . .
C C19 0.49330(9) 0.3789(2) 0.84687(12) 0.0244(4) Uani d 1 . .
H H19A 0.502584 0.301113 0.817278 0.029 Uiso calc 1 . .
H H19B 0.468264 0.463403 0.805576 0.029 Uiso calc 1 . .
C C20 0.44955(10) 0.3106(2) 0.87343(13) 0.0262(4) Uani d 1 . .
H H20A 0.437460 0.390552 0.898999 0.031 Uiso calc 1 . .
H H20B 0.406622 0.270325 0.821191 0.031 Uiso calc 1 . .
C C21 0.48772(10) 0.1834(2) 0.93957(13) 0.0281(4) Uani d 1 . .
H H21A 0.495221 0.098353 0.911865 0.034 Uiso calc 1 . .
H H21B 0.459693 0.145614 0.958672 0.034 Uiso calc 1 . .
C C22 0.55656(10) 0.2392(2) 1.01863(12) 0.0256(4) Uani d 1 . .
H H22A 0.581609 0.153099 1.058555 0.031 Uiso calc 1 . .
H H22B 0.548684 0.315490 1.050304 0.031 Uiso calc 1 . .
C C23 0.60031(10) 0.3096(2) 0.99230(13) 0.0264(4) Uani d 1 . .
H H23A 0.643242 0.349894 1.044513 0.032 Uiso calc 1 . .
H H23B 0.612306 0.231184 0.965832 0.032 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 0.0181 0.0091 '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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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 N1 . 2_656 113.00(10) y
N1 Co1 S11 . 2_656 109.67(5) y
N1 Co1 S11 . . 106.00(5) y
N1 Co1 S11 2_656 2_656 106.00(5) ?
N1 Co1 S11 2_656 . 109.67(5) ?
S11 Co1 S11 . 2_656 112.63(3) ?
C1 N1 Co1 . . 157.11(17) ?
N1 C1 S1 . . 179.39(19) ?
C11 S11 Co1 . . 101.24(6) ?
N11 C11 S11 . . 119.32(14) ?
N12 C11 S11 . . 120.02(13) ?
N12 C11 N11 . . 120.67(16) ?
C11 N11 H11 . . 116.0 ?
C11 N11 C12 . . 127.98(16) ?
C12 N11 H11 . . 116.0 ?
N11 C12 H12 . . 108.5 ?
N11 C12 C13 . . 107.87(16) ?
N11 C12 C17 . . 111.80(16) ?
C13 C12 H12 . . 108.5 ?
C13 C12 C17 . . 111.64(16) ?
C17 C12 H12 . . 108.5 ?
C12 C13 H13A . . 109.4 ?
C12 C13 H13B . . 109.4 ?
C12 C13 C14 . . 111.01(18) ?
H13A C13 H13B . . 108.0 ?
C14 C13 H13A . . 109.4 ?
C14 C13 H13B . . 109.4 ?
C13 C14 H14A . . 109.4 ?
C13 C14 H14B . . 109.4 ?
H14A C14 H14B . . 108.0 ?
C15 C14 C13 . . 111.2(2) ?
C15 C14 H14A . . 109.4 ?
C15 C14 H14B . . 109.4 ?
C14 C15 H15A . . 109.4 ?
C14 C15 H15B . . 109.4 ?
C14 C15 C16 . . 111.08(17) ?
H15A C15 H15B . . 108.0 ?
C16 C15 H15A . . 109.4 ?
C16 C15 H15B . . 109.4 ?
C15 C16 H16A . . 109.3 ?
C15 C16 H16B . . 109.3 ?
C15 C16 C17 . . 111.61(17) ?
H16A C16 H16B . . 108.0 ?
C17 C16 H16A . . 109.3 ?
C17 C16 H16B . . 109.3 ?
C12 C17 C16 . . 110.88(16) ?
C12 C17 H17A . . 109.5 ?
C12 C17 H17B . . 109.5 ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 108.1 ?
C11 N12 H12A . . 118.1 ?
C11 N12 C18 . . 123.87(15) ?
C18 N12 H12A . . 118.1 ?
N12 C18 H18 . . 108.3 ?
N12 C18 C19 . . 111.41(15) ?
N12 C18 C23 . . 109.67(14) ?
C19 C18 H18 . . 108.3 ?
C23 C18 H18 . . 108.3 ?
C23 C18 C19 . . 110.89(16) ?
C18 C19 H19A . . 109.7 ?
C18 C19 H19B . . 109.7 ?
C18 C19 C20 . . 110.05(15) ?
H19A C19 H19B . . 108.2 ?
C20 C19 H19A . . 109.7 ?
C20 C19 H19B . . 109.7 ?
C19 C20 H20A . . 109.4 ?
C19 C20 H20B . . 109.4 ?
H20A C20 H20B . . 108.0 ?
C21 C20 C19 . . 110.96(16) ?
C21 C20 H20A . . 109.4 ?
C21 C20 H20B . . 109.4 ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
C20 C21 C22 . . 110.86(16) ?
H21A C21 H21B . . 108.1 ?
C22 C21 H21A . . 109.5 ?
C22 C21 H21B . . 109.5 ?
C21 C22 H22A . . 109.2 ?
C21 C22 H22B . . 109.2 ?
C21 C22 C23 . . 111.83(16) ?
H22A C22 H22B . . 107.9 ?
C23 C22 H22A . . 109.2 ?
C23 C22 H22B . . 109.2 ?
C18 C23 C22 . . 109.63(15) ?
C18 C23 H23A . . 109.7 ?
C18 C23 H23B . . 109.7 ?
C22 C23 H23A . . 109.7 ?
C22 C23 H23B . . 109.7 ?
H23A C23 H23B . . 108.2 ?
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 . 1.9516(16) y
Co1 N1 2_656 1.9517(16) ?
Co1 S11 . 2.3130(5) y
Co1 S11 2_656 2.3131(5) ?
N1 C1 . 1.167(3) ?
C1 S1 . 1.620(2) ?
S11 C11 . 1.7431(18) ?
C11 N11 . 1.330(2) ?
C11 N12 . 1.328(2) ?
N11 H11 . 0.8800 ?
N11 C12 . 1.470(2) ?
C12 H12 . 1.0000 ?
C12 C13 . 1.520(3) ?
C12 C17 . 1.522(3) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C13 C14 . 1.522(3) ?
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C14 C15 . 1.519(3) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C15 C16 . 1.522(3) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C16 C17 . 1.530(3) ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
N12 H12A . 0.8800 ?
N12 C18 . 1.472(2) ?
C18 H18 . 1.0000 ?
C18 C19 . 1.526(2) ?
C18 C23 . 1.525(2) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C19 C20 . 1.529(2) ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C20 C21 . 1.526(3) ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C21 C22 . 1.528(3) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C22 C23 . 1.534(3) ?
C23 H23A . 0.9900 ?
C23 H23B . 0.9900 ?
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
N11 H11 N1 . 0.88 2.33 3.169(2) 160.4
C12 H12 S1 1_545 1.00 2.93 3.774(2) 142.5
N12 H12A S1 1_545 0.88 2.84 3.6770(16) 158.5
C19 H19B S11 . 0.99 3.00 3.529(2) 114.3

_cod_database_fobs_code 2243961
