#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:43:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/50/2205057.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_2205057
loop_
_publ_author_name
'Gai-Xian Li'
'Jian-Qing Li'
'Xu-Zhen Kang'
_publ_section_title
trans-Bis[(2E)-3-(N,N-dimethylamino)-1-(2-pyridyl)prop-2-en-1-one]diisothiocyanatonickel(II)
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m410
_journal_page_last               m411
_journal_paper_doi               10.1107/S1600536805002795
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni (N C S)2 (C10 H12 N2 O)2]'
_chemical_formula_moiety         'C22 H24 N6 Ni O2 S2'
_chemical_formula_sum            'C22 H24 N6 Ni O2 S2'
_chemical_formula_weight         527.30
_chemical_name_systematic
;
trans-Bis[(2E)-3-(N,N-dimethylamino)-1-(2-pyridyl)prop-2-en-1-
one]diisothiocyanatonickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.614(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.086(4)
_cell_length_b                   10.635(5)
_cell_length_c                   14.519(7)
_cell_measurement_reflns_used    912
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.74
_cell_measurement_theta_min      3.41
_cell_volume                     1213.5(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT and SHELXTL (Bruker, 1998)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_sigmaI/netI    0.1123
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6213
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.8560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0482P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                1325
_reflns_number_total             2217
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn6198.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2205057
_cod_database_fobs_code          2205057
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_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_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
C1 -0.1093(7) 0.1639(5) 0.1449(4) 0.0495(15) Uani d . 1 C
H1 -0.0022 0.1484 0.1838 0.059 Uiso calc R 1 H
C2 -0.2178(8) 0.2426(5) 0.1765(4) 0.0607(16) Uani d . 1 C
H2 -0.1834 0.2811 0.2354 0.073 Uiso calc R 1 H
C3 -0.3760(7) 0.2644(5) 0.1216(4) 0.0587(16) Uani d . 1 C
H3 -0.4510 0.3176 0.1423 0.070 Uiso calc R 1 H
C4 -0.4236(7) 0.2053(5) 0.0333(3) 0.0468(14) Uani d . 1 C
H4 -0.5318 0.2176 -0.0052 0.056 Uiso calc R 1 H
C5 -0.3096(6) 0.1297(4) 0.0047(3) 0.0370(12) Uani d . 1 C
C6 -0.3403(6) 0.0616(5) -0.0887(4) 0.0390(12) Uani d . 1 C
C7 -0.4967(6) 0.0784(5) -0.1549(3) 0.0418(13) Uani d . 1 C
H7 -0.5756 0.1364 -0.1434 0.050 Uiso calc R 1 H
C8 -0.5313(6) 0.0084(5) -0.2365(4) 0.0467(13) Uani d . 1 C
H8 -0.4489 -0.0502 -0.2422 0.056 Uiso calc R 1 H
C9 -0.8030(7) 0.1016(6) -0.3107(4) 0.0674(18) Uani d . 1 C
H9A -0.8802 0.0684 -0.2757 0.101 Uiso calc R 1 H
H9B -0.8625 0.1147 -0.3755 0.101 Uiso calc R 1 H
H9C -0.7576 0.1801 -0.2834 0.101 Uiso calc R 1 H
C10 -0.6897(7) -0.0735(6) -0.3865(4) 0.0659(18) Uani d . 1 C
H10A -0.5860 -0.1189 -0.3837 0.099 Uiso calc R 1 H
H10B -0.7201 -0.0274 -0.4449 0.099 Uiso calc R 1 H
H10C -0.7789 -0.1316 -0.3833 0.099 Uiso calc R 1 H
C11 -0.1241(6) -0.2524(6) 0.0860(3) 0.0451(14) Uani d . 1 C
N1 -0.1516(5) 0.1090(4) 0.0607(3) 0.0410(11) Uani d . 1 N
N2 -0.6656(5) 0.0135(4) -0.3072(3) 0.0476(11) Uani d . 1 N
N3 -0.0731(6) -0.1605(5) 0.0623(3) 0.0605(14) Uani d . 1 N
Ni1 0.0000 0.0000 0.0000 0.0442(3) Uani d S 1 Ni
O1 -0.2233(4) -0.0064(3) -0.1032(2) 0.0525(10) Uani d . 1 O
S1 -0.1984(2) -0.38194(15) 0.12175(11) 0.0674(5) Uani d . 1 S
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'
O O 0.0106 0.0060 '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
N1 C1 C2 . . 122.1(5)
N1 C1 H1 . . 118.9
C2 C1 H1 . . 118.9
C3 C2 C1 . . 119.9(5)
C3 C2 H2 . . 120.1
C1 C2 H2 . . 120.1
C2 C3 C4 . . 118.7(5)
C2 C3 H3 . . 120.7
C4 C3 H3 . . 120.7
C5 C4 C3 . . 119.1(5)
C5 C4 H4 . . 120.5
C3 C4 H4 . . 120.5
C4 C5 N1 . . 121.4(4)
C4 C5 C6 . . 125.5(4)
N1 C5 C6 . . 113.1(4)
O1 C6 C7 . . 123.7(5)
O1 C6 C5 . . 117.4(4)
C7 C6 C5 . . 118.9(4)
C8 C7 C6 . . 119.2(5)
C8 C7 H7 . . 120.4
C6 C7 H7 . . 120.4
N2 C8 C7 . . 128.2(5)
N2 C8 H8 . . 115.9
C7 C8 H8 . . 115.9
N2 C9 H9A . . 109.5
N2 C9 H9B . . 109.5
H9A C9 H9B . . 109.5
N2 C9 H9C . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
N2 C10 H10A . . 109.5
N2 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
N2 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
N3 C11 S1 . . 178.7(5)
C1 N1 C5 . . 118.9(4)
C1 N1 Ni1 . . 126.9(4)
C5 N1 Ni1 . . 114.2(3)
C8 N2 C9 . . 122.9(5)
C8 N2 C10 . . 121.8(4)
C9 N2 C10 . . 115.2(4)
C11 N3 Ni1 . . 171.9(5)
N1 Ni1 N1 3 . 180.0(2)
N1 Ni1 O1 3 3 79.60(15)
N1 Ni1 O1 . 3 100.40(15)
N1 Ni1 O1 3 . 100.40(15)
N1 Ni1 O1 . . 79.60(15)
O1 Ni1 O1 3 . 180.0(3)
N1 Ni1 N3 3 3 91.00(18)
N1 Ni1 N3 . 3 89.00(18)
O1 Ni1 N3 3 3 89.92(16)
O1 Ni1 N3 . 3 90.08(16)
N1 Ni1 N3 3 . 89.00(18)
N1 Ni1 N3 . . 91.00(18)
O1 Ni1 N3 3 . 90.08(16)
O1 Ni1 N3 . . 89.92(16)
N3 Ni1 N3 3 . 180.0(3)
C6 O1 Ni1 . . 115.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.324(6)
C1 C2 . 1.368(7)
C1 H1 . 0.9300
C2 C3 . 1.358(7)
C2 H2 . 0.9300
C3 C4 . 1.397(7)
C3 H3 . 0.9300
C4 C5 . 1.360(6)
C4 H4 . 0.9300
C5 N1 . 1.362(5)
C5 C6 . 1.506(7)
C6 O1 . 1.247(5)
C6 C7 . 1.408(6)
C7 C8 . 1.372(6)
C7 H7 . 0.9300
C8 N2 . 1.308(6)
C8 H8 . 0.9300
C9 N2 . 1.445(6)
C9 H9A . 0.9600
C9 H9B . 0.9600
C9 H9C . 0.9600
C10 N2 . 1.454(6)
C10 H10A . 0.9600
C10 H10B . 0.9600
C10 H10C . 0.9600
C11 N3 . 1.145(6)
C11 S1 . 1.635(6)
N1 Ni1 . 2.033(4)
N3 Ni1 . 2.081(5)
Ni1 N1 3 2.033(4)
Ni1 O1 3 2.058(3)
Ni1 O1 . 2.058(3)
Ni1 N3 3 2.081(5)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139067400
