#------------------------------------------------------------------------------
#$Date: 2022-10-07 04:53:21 +0300 (Fri, 07 Oct 2022) $
#$Revision: 278482 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244195.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_2244195
loop_
_publ_author_name
'Näther, Christian'
'Jess, Inke'
'Krebs, Christoph'
_publ_section_title
;
 Synthesis, crystal structure and properties of
 catena-poly[[[bis(3-methylpyridine-κN)nickel(II)]-di-μ-1,3-thiocyanato]
 acetonitrile monosolvate]
;
_journal_coeditor_code           JY2022
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022009598
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Ni (N C S)2 (C6 H7 N1)2], C2 H3 N'
_chemical_formula_moiety         'C14 H14 N4 Ni S2, C2 H3 N'
_chemical_formula_sum            'C16 H17 N5 Ni S2'
_chemical_formula_weight         402.17
_chemical_name_systematic
'catena-Poly[[[bis(3-methylpyridine-κN)nickel(II)]-di-μ-1,3-thiocyanato] acetonitrile monosolvate]'
_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                 117.043(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2934(9)
_cell_length_b                   11.7472(4)
_cell_length_c                   9.7341(5)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.2380
_cell_measurement_theta_min      4.5780
_cell_volume                     1863.11(18)
_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      99.99(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 0.987
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_unetI/netI     0.0063
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11840
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.664
_diffrn_reflns_theta_min         4.640
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0240
_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)+(0.0356P)²+1.9913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                1955
_reflns_number_total             1966
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jy2022sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1863.11(17)
_cod_database_code               2244195
_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 0.11950(2) 0.250000 0.01509(10) Uani d 1 . .
N N1 0.54965(7) 0.11278(9) 0.10148(12) 0.0185(2) Uani d 1 . .
C C1 0.57231(7) 0.08251(10) 0.01406(14) 0.0165(2) Uani d 1 . .
S S1 0.60344(2) 0.03798(3) -0.11091(4) 0.01977(10) Uani d 1 . .
N N11 0.58540(6) 0.24076(9) 0.38595(12) 0.0181(2) Uani d 1 . .
C C11 0.62454(8) 0.22828(11) 0.53994(15) 0.0204(3) Uani d 1 . .
H H11 0.607248 0.168907 0.584775 0.025 Uiso calc 1 . .
C C12 0.68901(8) 0.29758(12) 0.63729(16) 0.0244(3) Uani d 1 . .
C C13 0.71270(9) 0.38429(13) 0.56974(18) 0.0297(3) Uani d 1 . .
H H13 0.756660 0.433386 0.631780 0.036 Uiso calc 1 . .
C C14 0.67207(10) 0.39913(13) 0.41148(19) 0.0309(3) Uani d 1 . .
H H14 0.687354 0.458893 0.363972 0.037 Uiso calc 1 . .
C C15 0.60876(9) 0.32557(12) 0.32326(16) 0.0240(3) Uani d 1 . .
H H15 0.581066 0.335802 0.214608 0.029 Uiso calc 1 . .
C C16 0.73170(9) 0.27472(15) 0.80794(17) 0.0336(3) Uani d 1 . .
H H16A 0.696992 0.226009 0.835783 0.050 Uiso calc 1 . .
H H16B 0.741856 0.346916 0.864123 0.050 Uiso calc 1 . .
H H16C 0.784063 0.236346 0.835127 0.050 Uiso calc 1 . .
N N21 0.4958(3) 0.5343(3) 0.0380(4) 0.0525(8) Uani d 0.5 A -1
C C21 0.4990(2) 0.5882(3) 0.1369(4) 0.0366(7) Uani d 0.5 A -1
C C22 0.4981(19) 0.6557(4) 0.238(3) 0.059(3) Uani d 0.5 A -1
H H22A 0.511446 0.613590 0.333381 0.089 Uiso calc 0.5 A -1
H H22B 0.443345 0.689575 0.200183 0.089 Uiso calc 0.5 A -1
H H22C 0.538683 0.716083 0.258413 0.089 Uiso calc 0.5 A -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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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 Ni1 N1 . 2_655 175.54(6) y
N1 Ni1 S1 . 6_556 83.43(3) y
N1 Ni1 S1 2_655 6_556 93.32(3) ?
N1 Ni1 S1 . 5_655 93.32(3) y
N1 Ni1 S1 2_655 5_655 83.43(3) ?
N1 Ni1 N11 . . 91.71(4) y
N1 Ni1 N11 . 2_655 91.34(4) y
N1 Ni1 N11 2_655 . 91.34(4) ?
N1 Ni1 N11 2_655 2_655 91.71(4) ?
S1 Ni1 S1 5_655 6_556 87.022(18) y
N11 Ni1 S1 2_655 6_556 173.74(3) ?
N11 Ni1 S1 . 5_655 173.74(3) y
N11 Ni1 S1 2_655 5_655 89.87(3) ?
N11 Ni1 S1 . 6_556 89.87(3) y
N11 Ni1 N11 . 2_655 93.73(6) y
C1 N1 Ni1 . . 163.89(10) ?
N1 C1 S1 . . 179.13(12) ?
C1 S1 Ni1 . 5_655 101.56(4) ?
C11 N11 Ni1 . . 119.96(9) ?
C15 N11 Ni1 . . 121.53(9) ?
C15 N11 C11 . . 118.17(11) ?
N11 C11 H11 . . 118.2 ?
N11 C11 C12 . . 123.56(12) ?
C12 C11 H11 . . 118.2 ?
C11 C12 C16 . . 120.10(13) ?
C13 C12 C11 . . 117.29(13) ?
C13 C12 C16 . . 122.58(13) ?
C12 C13 H13 . . 120.1 ?
C14 C13 C12 . . 119.72(13) ?
C14 C13 H13 . . 120.1 ?
C13 C14 H14 . . 120.5 ?
C13 C14 C15 . . 119.06(13) ?
C15 C14 H14 . . 120.5 ?
N11 C15 C14 . . 122.18(13) ?
N11 C15 H15 . . 118.9 ?
C14 C15 H15 . . 118.9 ?
C12 C16 H16A . . 109.5 ?
C12 C16 H16B . . 109.5 ?
C12 C16 H16C . . 109.5 ?
H16A C16 H16B . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N21 C21 C22 . . 174.4(12) ?
C21 C22 H22A . . 109.5 ?
C21 C22 H22B . . 109.5 ?
C21 C22 H22C . . 109.5 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 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 . 2.0285(11) y
Ni1 N1 2_655 2.0286(11) y
Ni1 S1 5_655 2.5508(4) ?
Ni1 S1 6_556 2.5508(4) y
Ni1 N11 2_655 2.0836(11) ?
Ni1 N11 . 2.0836(11) y
N1 C1 . 1.1590(17) ?
C1 S1 . 1.6456(13) ?
N11 C11 . 1.3435(16) ?
N11 C15 . 1.3360(17) ?
C11 H11 . 0.9500 ?
C11 C12 . 1.3912(18) ?
C12 C13 . 1.384(2) ?
C12 C16 . 1.504(2) ?
C13 H13 . 0.9500 ?
C13 C14 . 1.384(2) ?
C14 H14 . 0.9500 ?
C14 C15 . 1.386(2) ?
C15 H15 . 0.9500 ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
N21 C21 . 1.132(5) ?
C21 C22 . 1.270(19) ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
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 . . . . 172.20(10) ?
Ni1 N11 C15 C14 . . . . -172.51(11) ?
N11 C11 C12 C13 . . . . 0.6(2) ?
N11 C11 C12 C16 . . . . -177.52(13) ?
C11 N11 C15 C14 . . . . 0.8(2) ?
C11 C12 C13 C14 . . . . 0.4(2) ?
C12 C13 C14 C15 . . . . -0.8(2) ?
C13 C14 C15 N11 . . . . 0.2(2) ?
C15 N11 C11 C12 . . . . -1.20(19) ?
C16 C12 C13 C14 . . . . 178.47(15) ?

_cod_database_fobs_code 2244195
