#------------------------------------------------------------------------------
#$Date: 2021-10-20 05:24:09 +0300 (Wed, 20 Oct 2021) $
#$Revision: 270046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243941.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_2243941
loop_
_publ_author_name
'Krebs, Christoph'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Comparison of the crystal structures of the low- and high-temperature
 forms of bis[4-(dimethylamino)pyridine]dithiocyanatocobalt(II)
;
_journal_coeditor_code           HB7987
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021010422
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Co (N C S)2 (C7 H10 N2)2]'
_chemical_formula_moiety         'C16 H20 Co N6 S2'
_chemical_formula_sum            'C16 H20 Co N6 S2'
_chemical_formula_weight         419.43
_chemical_name_systematic
;
Bis[4-(dimethylamino)pyridine]dithiocyanatocobalt(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                 99.0760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.37080(10)
_cell_length_b                   15.2200(2)
_cell_length_c                   11.80140(10)
_cell_measurement_reflns_used    13880
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.2720
_cell_measurement_theta_min      3.7810
_cell_volume                     952.61(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16411
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.047
_diffrn_reflns_theta_min         3.793
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.202
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0237
_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)+(0.0348P)²+0.4033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                2081
_reflns_number_total             2100
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7987sup1.cif
_cod_data_source_block           Form_I
_cod_database_code               2243941
_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.
;
_shelx_estimated_absorpt_t_min   0.260
_shelx_estimated_absorpt_t_max   0.710
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.93113(6) 0.750000 0.27609(3) 0.01820(10) Uani d 1 . .
N N1 1.1349(3) 0.750000 0.15392(15) 0.0236(4) Uani d 1 . .
C C1 1.2586(4) 0.750000 0.08142(17) 0.0197(4) Uani d 1 . .
S S1 1.43347(10) 0.750000 -0.01905(4) 0.02516(13) Uani d 1 . .
N N2 1.1055(3) 0.750000 0.43574(15) 0.0228(4) Uani d 1 . .
C C2 1.2525(4) 0.750000 0.52018(17) 0.0202(4) Uani d 1 . .
S S2 1.46184(10) 0.750000 0.63528(4) 0.02618(13) Uani d 1 . .
N N11 0.7113(2) 0.64220(8) 0.26788(10) 0.0186(2) Uani d 1 . .
C C11 0.5802(3) 0.62788(9) 0.35490(12) 0.0194(3) Uani d 1 . .
H H11 0.614076 0.664879 0.420344 0.023 Uiso calc 1 . .
C C12 0.4021(3) 0.56372(9) 0.35509(12) 0.0197(3) Uani d 1 . .
H H12 0.318372 0.556780 0.419671 0.024 Uiso calc 1 . .
C C13 0.3428(3) 0.50769(9) 0.25904(12) 0.0196(3) Uani d 1 . .
C C14 0.4861(3) 0.52099(10) 0.16919(12) 0.0216(3) Uani d 1 . .
H H14 0.460807 0.483952 0.103587 0.026 Uiso calc 1 . .
C C15 0.6609(3) 0.58727(9) 0.17704(12) 0.0203(3) Uani d 1 . .
H H15 0.752119 0.595055 0.115020 0.024 Uiso calc 1 . .
N N12 0.1612(2) 0.44622(8) 0.25328(11) 0.0229(3) Uani d 1 . .
C C16 0.0279(3) 0.43142(10) 0.34987(14) 0.0265(3) Uani d 1 . .
H H16A 0.147210 0.410913 0.416077 0.040 Uiso calc 1 . .
H H16B -0.103220 0.386937 0.329058 0.040 Uiso calc 1 . .
H H16C -0.049866 0.486459 0.369491 0.040 Uiso calc 1 . .
C C17 0.1036(3) 0.38967(11) 0.15329(15) 0.0320(4) Uani d 1 . .
H H17A 0.053675 0.425800 0.084731 0.048 Uiso calc 1 . .
H H17B -0.034880 0.349998 0.163508 0.048 Uiso calc 1 . .
H H17C 0.253102 0.355095 0.144230 0.048 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 N2 . . 118.16(8) y
N1 Co1 N11 . . 111.03(4) y
N1 Co1 N11 . 4_575 111.03(4) ?
N2 Co1 N11 . . 103.47(4) y
N2 Co1 N11 . 4_575 103.47(4) ?
N11 Co1 N11 . 4_575 109.04(7) y
C1 N1 Co1 . . 179.48(17) y
N1 C1 S1 . . 179.51(19) ?
C2 N2 Co1 . . 166.24(16) y
N2 C2 S2 . . 178.57(18) ?
C11 N11 Co1 . . 117.81(9) n
C11 N11 C15 . . 116.08(12) ?
C15 N11 Co1 . . 125.71(9) ?
N11 C11 H11 . . 117.8 ?
N11 C11 C12 . . 124.41(13) ?
C12 C11 H11 . . 117.8 ?
C11 C12 H12 . . 120.0 ?
C11 C12 C13 . . 119.91(13) ?
C13 C12 H12 . . 120.0 ?
C12 C13 C14 . . 115.63(13) ?
N12 C13 C12 . . 121.99(13) ?
N12 C13 C14 . . 122.38(13) ?
C13 C14 H14 . . 120.0 ?
C15 C14 C13 . . 120.05(13) ?
C15 C14 H14 . . 120.0 ?
N11 C15 C14 . . 123.86(13) ?
N11 C15 H15 . . 118.1 ?
C14 C15 H15 . . 118.1 ?
C13 N12 C16 . . 120.66(12) ?
C13 N12 C17 . . 120.83(13) ?
C17 N12 C16 . . 118.42(12) ?
N12 C16 H16A . . 109.5 ?
N12 C16 H16B . . 109.5 ?
N12 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N12 C17 H17A . . 109.5 ?
N12 C17 H17B . . 109.5 ?
N12 C17 H17C . . 109.5 ?
H17A C17 H17B . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
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 . 1.9429(18) y
Co1 N2 . 1.9672(19) y
Co1 N11 . 2.0148(12) y
Co1 N11 4_575 2.0148(12) ?
N1 C1 . 1.163(3) ?
C1 S1 . 1.625(2) ?
N2 C2 . 1.170(3) ?
C2 S2 . 1.621(2) ?
N11 C11 . 1.3512(17) ?
N11 C15 . 1.3529(18) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.367(2) ?
C12 H12 . 0.9500 ?
C12 C13 . 1.414(2) ?
C13 C14 . 1.4195(19) ?
C13 N12 . 1.3454(19) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.371(2) ?
C15 H15 . 0.9500 ?
N12 C16 . 1.4559(19) ?
N12 C17 . 1.454(2) ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C17 H17A . 0.9800 ?
C17 H17B . 0.9800 ?
C17 H17C . 0.9800 ?
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
C16 H16B S2 3_666 0.98 2.91 3.8367(15) 158
C17 H17B S1 3_665 0.98 2.94 3.7291(16) 138
C17 H17C S1 3_765 0.98 2.89 3.8018(18) 155

_cod_database_fobs_code 2243941
