#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:07:53 +0300 (Wed, 07 Aug 2024) $
#$Revision: 294007 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023177.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_2023177
loop_
_publ_author_name
'Näther, Christian'
'Mangelsen, Sebastian'
_publ_section_title
;
 Synthesis, crystal structure and thermal properties of
 catena-poly[[bis-(4-methyl-pyridine)-nickel(II)]-di-μ-thio-cyanato],
 which shows an alternating all-trans and
 cis-cis-trans-coordination of the
 NiS₂Np ₂Nt ₂
 octa-hedra (p = 4-methyl-pyridine, t = thio-cyanate).
;
_journal_coeditor_code           HB8101
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              771
_journal_page_last               776
_journal_paper_doi               10.1107/S2056989024005887
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Ni (N C S)2 (C6 H7 N)2]'
_chemical_formula_moiety         'C14 H14 N4 Ni S2'
_chemical_formula_sum            'C14 H14 N4 Ni S2'
_chemical_formula_weight         361.12
_chemical_name_systematic
catena-Poly[[bis(4-methylpyridine-κN)nickel(II)]-di-μ-thiocyanato-κ²N:S;κ²S:N]
_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
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.783(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0352(12)
_cell_length_b                   9.1536(5)
_cell_length_c                   19.2268(12)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.37
_cell_volume                     3147.8(4)
_computing_cell_refinement
;
X-AREA (Stoe, 2008)
;
_computing_data_collection
;
X-AREA (Stoe, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe, 2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999) and XP in SHELXTL-PC (Sheldrick,
2008)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/4 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      220.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         2.373
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.8636
_exptl_absorpt_correction_T_min  0.6910
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red and X-Shape; Stoe, 2008)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.468
_refine_ls_extinction_coef       0.0034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0344
_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)+(0.0616P)²+0.1916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                3113
_reflns_number_total             3805
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb8101.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023177.cif.'
_cod_database_code               2023177
_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
Ni Ni1 0.500000 0.49095(4) 0.250000 0.02030(11) Uani d 1 . .
Ni Ni2 0.750000 0.250000 0.500000 0.02012(11) Uani d 1 . .
S S1 0.66327(3) 0.42321(6) 0.52157(3) 0.02554(14) Uani d 1 . .
C C1 0.60061(10) 0.4565(2) 0.43118(11) 0.0199(4) Uani d 1 . .
N N1 0.55720(9) 0.4797(2) 0.36824(10) 0.0240(4) Uani d 1 . .
S S2 0.58017(3) 0.29192(7) 0.23054(3) 0.03120(15) Uani d 1 . .
C C2 0.64768(11) 0.2743(2) 0.31946(11) 0.0213(4) Uani d 1 . .
N N2 0.69454(10) 0.2631(2) 0.38228(10) 0.0256(4) Uani d 1 . .
N N11 0.57268(9) 0.6535(2) 0.24781(9) 0.0230(3) Uani d 1 . .
C C11 0.59509(11) 0.6616(2) 0.19194(11) 0.0260(4) Uani d 1 . .
H H11 0.576619 0.592325 0.151505 0.031 Uiso calc 1 . .
C C12 0.64407(12) 0.7668(2) 0.19100(12) 0.0271(4) Uani d 1 . .
H H12 0.657378 0.769083 0.149963 0.033 Uiso calc 1 . .
C C13 0.67375(11) 0.8695(2) 0.25052(12) 0.0264(4) Uani d 1 . .
C C14 0.64970(13) 0.8611(3) 0.30801(13) 0.0332(5) Uani d 1 . .
H H14 0.667379 0.928794 0.349211 0.040 Uiso calc 1 . .
C C15 0.60000(13) 0.7538(3) 0.30461(13) 0.0308(5) Uani d 1 . .
H H15 0.584526 0.750894 0.344048 0.037 Uiso calc 1 . .
C C16 0.72901(14) 0.9821(3) 0.25378(16) 0.0391(6) Uani d 1 . .
H H16A 0.758663 0.943774 0.229594 0.059 Uiso calc 1 . .
H H16B 0.761580 1.006536 0.307691 0.059 Uiso calc 1 . .
H H16C 0.702696 1.069001 0.226168 0.059 Uiso calc 1 . .
N N21 0.68081(9) 0.0707(2) 0.49738(10) 0.0246(4) Uani d 1 . .
C C21 0.70854(12) -0.0404(3) 0.54745(13) 0.0313(5) Uani d 1 . .
H H21 0.760343 -0.043195 0.579938 0.038 Uiso calc 1 . .
C C22 0.66472(13) -0.1516(3) 0.55383(13) 0.0343(5) Uani d 1 . .
H H22 0.686953 -0.227367 0.590015 0.041 Uiso calc 1 . .
C C23 0.58782(12) -0.1514(3) 0.50670(13) 0.0286(4) Uani d 1 . .
C C24 0.55988(12) -0.0385(3) 0.45291(13) 0.0298(5) Uani d 1 . .
H H24 0.508574 -0.034966 0.418356 0.036 Uiso calc 1 . .
C C25 0.60707(11) 0.0684(3) 0.44994(12) 0.0277(4) Uani d 1 . .
H H25 0.586557 0.143308 0.412862 0.033 Uiso calc 1 . .
C C26 0.53820(14) -0.2658(3) 0.51501(16) 0.0367(5) Uani d 1 . .
H H26A 0.548385 -0.359533 0.498245 0.055 Uiso calc 1 . .
H H26B 0.486273 -0.239712 0.483032 0.055 Uiso calc 1 . .
H H26C 0.547883 -0.272090 0.569101 0.055 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'
Ni Ni 0.3393 1.1124 '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'
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_655 174.18(10) y
N1 Ni1 S2 2_655 . 82.84(5) ?
N1 Ni1 S2 . 2_655 82.84(5) ?
N1 Ni1 S2 2_655 2_655 93.01(5) ?
N1 Ni1 S2 . . 93.01(5) ?
N1 Ni1 N11 . 2_655 93.45(7) ?
N1 Ni1 N11 2_655 2_655 90.68(7) ?
N1 Ni1 N11 . . 90.68(7) ?
N1 Ni1 N11 2_655 . 93.45(7) ?
S2 Ni1 S2 . 2_655 89.50(3) y
N11 Ni1 S2 2_655 2_655 90.86(5) ?
N11 Ni1 S2 . . 90.85(5) ?
N11 Ni1 S2 2_655 . 173.52(5) ?
N11 Ni1 S2 . 2_655 173.52(5) ?
N11 Ni1 N11 . 2_655 89.52(9) y
S1 Ni2 S1 . 7_656 180.0 y
N2 Ni2 S1 . 7_656 85.71(5) ?
N2 Ni2 S1 7_656 . 85.71(5) ?
N2 Ni2 S1 . . 94.29(5) ?
N2 Ni2 S1 7_656 7_656 94.29(5) ?
N2 Ni2 N2 . 7_656 180.0 y
N2 Ni2 N21 7_656 . 90.24(7) ?
N2 Ni2 N21 . 7_656 90.23(7) ?
N2 Ni2 N21 . . 89.76(7) ?
N2 Ni2 N21 7_656 7_656 89.77(7) ?
N21 Ni2 S1 7_656 7_656 89.95(5) ?
N21 Ni2 S1 7_656 . 90.05(5) ?
N21 Ni2 S1 . 7_656 90.05(5) ?
N21 Ni2 S1 . . 89.95(5) ?
N21 Ni2 N21 . 7_656 180.0 y
C1 S1 Ni2 . . 101.33(7) ?
N1 C1 S1 . . 179.8(2) ?
C1 N1 Ni1 . . 164.70(17) ?
C2 S2 Ni1 . . 101.18(7) ?
N2 C2 S2 . . 179.1(2) ?
C2 N2 Ni2 . . 162.45(17) ?
C11 N11 Ni1 . . 122.82(14) ?
C11 N11 C15 . . 117.01(18) ?
C15 N11 Ni1 . . 120.16(14) ?
N11 C11 H11 . . 118.5 ?
N11 C11 C12 . . 123.06(19) ?
C12 C11 H11 . . 118.5 ?
C11 C12 H12 . . 119.9 ?
C11 C12 C13 . . 120.2(2) ?
C13 C12 H12 . . 119.9 ?
C12 C13 C14 . . 116.3(2) ?
C12 C13 C16 . . 122.4(2) ?
C14 C13 C16 . . 121.3(2) ?
C13 C14 H14 . . 119.9 ?
C15 C14 C13 . . 120.1(2) ?
C15 C14 H14 . . 119.9 ?
N11 C15 C14 . . 123.2(2) ?
N11 C15 H15 . . 118.4 ?
C14 C15 H15 . . 118.4 ?
C13 C16 H16A . . 109.5 ?
C13 C16 H16B . . 109.5 ?
C13 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C21 N21 Ni2 . . 120.87(14) ?
C21 N21 C25 . . 116.78(19) ?
C25 N21 Ni2 . . 122.18(15) ?
N21 C21 H21 . . 118.4 ?
N21 C21 C22 . . 123.25(19) ?
C22 C21 H21 . . 118.4 ?
C21 C22 H22 . . 120.0 ?
C21 C22 C23 . . 120.1(2) ?
C23 C22 H22 . . 120.0 ?
C22 C23 C26 . . 121.4(2) ?
C24 C23 C22 . . 116.3(2) ?
C24 C23 C26 . . 122.3(2) ?
C23 C24 H24 . . 119.8 ?
C25 C24 C23 . . 120.31(19) ?
C25 C24 H24 . . 119.8 ?
N21 C25 C24 . . 123.2(2) ?
N21 C25 H25 . . 118.4 ?
C24 C25 H25 . . 118.4 ?
C23 C26 H26A . . 109.5 ?
C23 C26 H26B . . 109.5 ?
C23 C26 H26C . . 109.5 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 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
Ni1 N1 . 2.0358(17) y
Ni1 N1 2_655 2.0358(17) n
Ni1 S2 2_655 2.5653(6) n
Ni1 S2 . 2.5653(6) y
Ni1 N11 2_655 2.0955(17) n
Ni1 N11 . 2.0956(18) y
Ni2 S1 7_656 2.5208(5) n
Ni2 S1 . 2.5208(5) y
Ni2 N2 . 2.0261(17) y
Ni2 N2 7_656 2.0262(17) n
Ni2 N21 . 2.1345(18) y
Ni2 N21 7_656 2.1345(18) n
S1 C1 . 1.6501(19) ?
C1 N1 . 1.148(3) ?
S2 C2 . 1.6414(19) ?
C2 N2 . 1.153(3) ?
N11 C11 . 1.340(3) ?
N11 C15 . 1.340(3) ?
C11 H11 . 0.9400 ?
C11 C12 . 1.381(3) ?
C12 H12 . 0.9400 ?
C12 C13 . 1.390(3) ?
C13 C14 . 1.393(3) ?
C13 C16 . 1.493(3) ?
C14 H14 . 0.9400 ?
C14 C15 . 1.379(3) ?
C15 H15 . 0.9400 ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C16 H16C . 0.9700 ?
N21 C21 . 1.337(3) ?
N21 C25 . 1.342(3) ?
C21 H21 . 0.9400 ?
C21 C22 . 1.385(3) ?
C22 H22 . 0.9400 ?
C22 C23 . 1.392(3) ?
C23 C24 . 1.389(3) ?
C23 C26 . 1.501(3) ?
C24 H24 . 0.9400 ?
C24 C25 . 1.380(3) ?
C25 H25 . 0.9400 ?
C26 H26A . 0.9700 ?
C26 H26B . 0.9700 ?
C26 H26C . 0.9700 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 N11 C11 C12 . . . . -178.77(16) ?
Ni1 N11 C15 C14 . . . . 178.07(19) ?
Ni2 N21 C21 C22 . . . . 173.01(19) ?
Ni2 N21 C25 C24 . . . . -172.91(17) ?
N11 C11 C12 C13 . . . . 1.2(3) ?
C11 N11 C15 C14 . . . . -0.8(3) ?
C11 C12 C13 C14 . . . . -1.7(3) ?
C11 C12 C13 C16 . . . . 177.7(2) ?
C12 C13 C14 C15 . . . . 1.0(3) ?
C13 C14 C15 N11 . . . . 0.2(4) ?
C15 N11 C11 C12 . . . . 0.0(3) ?
C16 C13 C14 C15 . . . . -178.4(2) ?
N21 C21 C22 C23 . . . . 0.0(4) ?
C21 N21 C25 C24 . . . . 2.4(3) ?
C21 C22 C23 C24 . . . . 2.3(3) ?
C21 C22 C23 C26 . . . . -176.7(2) ?
C22 C23 C24 C25 . . . . -2.2(3) ?
C23 C24 C25 N21 . . . . -0.1(4) ?
C25 N21 C21 C22 . . . . -2.4(3) ?
C26 C23 C24 C25 . . . . 176.8(2) ?
