#------------------------------------------------------------------------------
#$Date: 2023-07-03 10:27:15 +0300 (Mon, 03 Jul 2023) $
#$Revision: 284753 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/74/8107428.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8107428
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Crystal structure of
 trans-tetrakis(3-phenylpyridine-\kN)bis(thiocyanato-\kN)nickel(II),
 C46H36N6NiS2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              319
_journal_page_last               321
_journal_paper_doi               10.1515/ncrs-2023-0020
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C46 H36 N6 Ni S2'
_chemical_formula_sum            'C46 H36 N6 Ni S2'
_chemical_formula_weight         795.64
_chemical_name_systematic
;
trans-tetrakis(3-phenylpyridine-κN)bis(thiocyanato-κN)
nickel(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                107.377(3)
_cell_angle_beta                 107.333(3)
_cell_angle_gamma                91.254(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1007(10)
_cell_length_b                   9.8108(10)
_cell_length_c                   11.8638(12)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.51
_cell_volume                     957.84(18)
_computing_cell_refinement       'Bruker SAINT [1]'
_computing_data_collection       'Bruker APEX2 [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'ORTEP-III [3]'
_computing_publication_material  'SHELXL-2014/7 [2]'
_computing_structure_refinement  'SHELXL-2014/7 [2]'
_computing_structure_solution    'SHELXL-2014/7 [2]'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'PHOTON II M14'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24392
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.077
_diffrn_reflns_theta_min         2.397
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016) [1]'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       Block
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0258P)²+0.4351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3541
_reflns_number_total             3730
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0020_suppl.cif
_cod_data_source_block           Ni(NCS)2(3ppy)4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        957.84(17)
_cod_database_code               8107428
_shelx_shelxl_version_number     2014/7
_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   0.842
_shelx_estimated_absorpt_t_max   0.937
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.02508(8) Uani 1 2 d S . P . .
S1 S 0.09684(4) -0.08293(5) 0.11583(4) 0.04324(11) Uani 1 1 d . . . . .
N1 N 0.30462(14) -0.06254(13) 0.34818(11) 0.0316(3) Uani 1 1 d . . . . .
N2 N 0.43703(14) 0.22062(12) 0.54120(11) 0.0296(2) Uani 1 1 d . . . . .
N3 N 0.62806(13) 0.03851(12) 0.38655(10) 0.0291(2) Uani 1 1 d . . . . .
C1 C 0.21722(15) -0.07426(14) 0.25091(13) 0.0270(3) Uani 1 1 d . . . . .
C2 C 0.32977(17) 0.26771(15) 0.46075(13) 0.0300(3) Uani 1 1 d . . . . .
H2 H 0.2760 0.2012 0.3823 0.036 Uiso 1 1 calc R U . . .
C3 C 0.29287(17) 0.40783(15) 0.48551(14) 0.0313(3) Uani 1 1 d . . . . .
C4 C 0.3688(2) 0.50171(16) 0.60447(15) 0.0409(4) Uani 1 1 d . . . . .
H4 H 0.3468 0.5974 0.6269 0.049 Uiso 1 1 calc R U . . .
C5 C 0.4760(2) 0.45479(17) 0.68931(15) 0.0419(4) Uani 1 1 d . . . . .
H5 H 0.5262 0.5174 0.7703 0.050 Uiso 1 1 calc R U . . .
C6 C 0.50899(19) 0.31508(16) 0.65426(14) 0.0358(3) Uani 1 1 d . . . . .
H6 H 0.5850 0.2847 0.7119 0.043 Uiso 1 1 calc R U . . .
C7 C 0.18229(18) 0.45600(15) 0.38894(15) 0.0349(3) Uani 1 1 d . . . . .
C8 C 0.1561(2) 0.38721(18) 0.26255(16) 0.0439(4) Uani 1 1 d . . . . .
H8 H 0.2038 0.3045 0.2375 0.053 Uiso 1 1 calc R U . . .
C9 C 0.0613(2) 0.4382(2) 0.17305(18) 0.0537(5) Uani 1 1 d . . . . .
H9 H 0.0449 0.3899 0.0882 0.064 Uiso 1 1 calc R U . . .
C10 C -0.0091(2) 0.5590(2) 0.2076(2) 0.0596(5) Uani 1 1 d . . . . .
H10 H -0.0714 0.5953 0.1470 0.071 Uiso 1 1 calc R U . . .
C11 C 0.0124(3) 0.6264(2) 0.3320(2) 0.0679(6) Uani 1 1 d . . . . .
H11 H -0.0375 0.7078 0.3561 0.082 Uiso 1 1 calc R U . . .
C12 C 0.1068(2) 0.57574(19) 0.42207(19) 0.0541(5) Uani 1 1 d . . . . .
H12 H 0.1200 0.6230 0.5066 0.065 Uiso 1 1 calc R U . . .
C13 C 0.56711(16) 0.09388(14) 0.29509(12) 0.0278(3) Uani 1 1 d . . . . .
H13 H 0.4646 0.1159 0.2821 0.033 Uiso 1 1 calc R U . . .
C14 C 0.64443(16) 0.12129(14) 0.21771(12) 0.0274(3) Uani 1 1 d . . . . .
C15 C 0.79570(17) 0.08788(17) 0.23867(14) 0.0362(3) Uani 1 1 d . . . . .
H15 H 0.8538 0.1045 0.1895 0.043 Uiso 1 1 calc R U . . .
C16 C 0.86002(18) 0.02991(19) 0.33247(15) 0.0413(4) Uani 1 1 d . . . . .
H16 H 0.9620 0.0062 0.3471 0.050 Uiso 1 1 calc R U . . .
C17 C 0.77415(18) 0.00716(17) 0.40410(14) 0.0366(3) Uani 1 1 d . . . . .
H17 H 0.8195 -0.0319 0.4679 0.044 Uiso 1 1 calc R U . . .
C18 C 0.56687(16) 0.18355(14) 0.11902(12) 0.0274(3) Uani 1 1 d . . . . .
C19 C 0.40607(17) 0.16579(15) 0.06732(13) 0.0310(3) Uani 1 1 d . . . . .
H19 H 0.3450 0.1118 0.0942 0.037 Uiso 1 1 calc R U . . .
C20 C 0.33515(18) 0.22672(17) -0.02318(14) 0.0372(3) Uani 1 1 d . . . . .
H20 H 0.2264 0.2154 -0.0561 0.045 Uiso 1 1 calc R U . . .
C21 C 0.4230(2) 0.30394(18) -0.06533(16) 0.0436(4) Uani 1 1 d . . . . .
H21 H 0.3746 0.3448 -0.1271 0.052 Uiso 1 1 calc R U . . .
C22 C 0.5819(2) 0.3206(2) -0.01617(17) 0.0468(4) Uani 1 1 d . . . . .
H22 H 0.6424 0.3722 -0.0453 0.056 Uiso 1 1 calc R U . . .
C23 C 0.65361(18) 0.26206(17) 0.07575(15) 0.0382(3) Uani 1 1 d . . . . .
H23 H 0.7624 0.2755 0.1094 0.046 Uiso 1 1 calc R U . . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ni1 N1 180.0 2_656 .
N1 Ni1 N3 89.74(5) 2_656 2_656
N1 Ni1 N3 90.26(5) . 2_656
N1 Ni1 N3 90.26(5) 2_656 .
N1 Ni1 N3 89.74(5) . .
N3 Ni1 N3 180.0 2_656 .
N1 Ni1 N2 91.18(5) 2_656 .
N1 Ni1 N2 88.82(5) . .
N3 Ni1 N2 88.25(4) 2_656 .
N3 Ni1 N2 91.75(4) . .
N1 Ni1 N2 88.82(5) 2_656 2_656
N1 Ni1 N2 91.18(5) . 2_656
N3 Ni1 N2 91.75(4) 2_656 2_656
N3 Ni1 N2 88.25(4) . 2_656
N2 Ni1 N2 180.0 . 2_656
C1 N1 Ni1 160.75(12) . .
C6 N2 C2 117.21(12) . .
C6 N2 Ni1 118.31(10) . .
C2 N2 Ni1 124.48(9) . .
C13 N3 C17 117.21(12) . .
C13 N3 Ni1 121.93(9) . .
C17 N3 Ni1 120.86(10) . .
N1 C1 S1 177.39(13) . .
N2 C2 C3 124.51(13) . .
N2 C2 H2 117.7 . .
C3 C2 H2 117.7 . .
C2 C3 C4 116.31(14) . .
C2 C3 C7 121.83(13) . .
C4 C3 C7 121.83(13) . .
C5 C4 C3 120.09(14) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C6 119.23(14) . .
C4 C5 H5 120.4 . .
C6 C5 H5 120.4 . .
N2 C6 C5 122.57(14) . .
N2 C6 H6 118.7 . .
C5 C6 H6 118.7 . .
C12 C7 C8 117.65(15) . .
C12 C7 C3 120.91(15) . .
C8 C7 C3 121.37(13) . .
C9 C8 C7 121.26(16) . .
C9 C8 H8 119.4 . .
C7 C8 H8 119.4 . .
C10 C9 C8 120.29(19) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C9 C10 C11 119.24(17) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
C10 C11 C12 120.79(18) . .
C10 C11 H11 119.6 . .
C12 C11 H11 119.6 . .
C11 C12 C7 120.73(18) . .
C11 C12 H12 119.6 . .
C7 C12 H12 119.6 . .
N3 C13 C14 124.71(13) . .
N3 C13 H13 117.6 . .
C14 C13 H13 117.6 . .
C15 C14 C13 116.57(13) . .
C15 C14 C18 122.77(13) . .
C13 C14 C18 120.66(12) . .
C16 C15 C14 119.39(14) . .
C16 C15 H15 120.3 . .
C14 C15 H15 120.3 . .
C17 C16 C15 119.63(14) . .
C17 C16 H16 120.2 . .
C15 C16 H16 120.2 . .
N3 C17 C16 122.50(14) . .
N3 C17 H17 118.8 . .
C16 C17 H17 118.8 . .
C23 C18 C19 118.13(13) . .
C23 C18 C14 120.53(13) . .
C19 C18 C14 121.34(13) . .
C20 C19 C18 120.69(14) . .
C20 C19 H19 119.7 . .
C18 C19 H19 119.7 . .
C21 C20 C19 120.42(15) . .
C21 C20 H20 119.8 . .
C19 C20 H20 119.8 . .
C22 C21 C20 119.42(15) . .
C22 C21 H21 120.3 . .
C20 C21 H21 120.3 . .
C21 C22 C23 120.50(15) . .
C21 C22 H22 119.7 . .
C23 C22 H22 119.7 . .
C22 C23 C18 120.82(15) . .
C22 C23 H23 119.6 . .
C18 C23 H23 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.0411(12) 2_656
Ni1 N1 2.0411(12) .
Ni1 N3 2.1287(12) 2_656
Ni1 N3 2.1287(12) .
Ni1 N2 2.2004(12) .
Ni1 N2 2.2004(12) 2_656
S1 C1 1.6261(14) .
N1 C1 1.1608(18) .
N2 C6 1.3395(19) .
N2 C2 1.3436(18) .
N3 C13 1.3367(17) .
N3 C17 1.3405(19) .
C2 C3 1.3880(19) .
C2 H2 0.9400 .
C3 C4 1.390(2) .
C3 C7 1.485(2) .
C4 C5 1.374(2) .
C4 H4 0.9400 .
C5 C6 1.376(2) .
C5 H5 0.9400 .
C6 H6 0.9400 .
C7 C12 1.388(2) .
C7 C8 1.392(2) .
C8 C9 1.383(2) .
C8 H8 0.9400 .
C9 C10 1.372(3) .
C9 H9 0.9400 .
C10 C11 1.375(3) .
C10 H10 0.9400 .
C11 C12 1.384(3) .
C11 H11 0.9400 .
C12 H12 0.9400 .
C13 C14 1.3908(19) .
C13 H13 0.9400 .
C14 C15 1.389(2) .
C14 C18 1.4819(19) .
C15 C16 1.382(2) .
C15 H15 0.9400 .
C16 C17 1.373(2) .
C16 H16 0.9400 .
C17 H17 0.9400 .
C18 C23 1.390(2) .
C18 C19 1.392(2) .
C19 C20 1.383(2) .
C19 H19 0.9400 .
C20 C21 1.379(2) .
C20 H20 0.9400 .
C21 C22 1.375(3) .
C21 H21 0.9400 .
C22 C23 1.383(2) .
C22 H22 0.9400 .
C23 H23 0.9400 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C6 N2 C2 C3 2.3(2) . . . .
Ni1 N2 C2 C3 -178.23(11) . . . .
N2 C2 C3 C4 -3.1(2) . . . .
N2 C2 C3 C7 174.93(13) . . . .
C2 C3 C4 C5 1.3(2) . . . .
C7 C3 C4 C5 -176.80(15) . . . .
C3 C4 C5 C6 1.2(3) . . . .
C2 N2 C6 C5 0.4(2) . . . .
Ni1 N2 C6 C5 -179.07(13) . . . .
C4 C5 C6 N2 -2.1(3) . . . .
C2 C3 C7 C12 158.14(16) . . . .
C4 C3 C7 C12 -23.9(2) . . . .
C2 C3 C7 C8 -24.9(2) . . . .
C4 C3 C7 C8 153.03(16) . . . .
C12 C7 C8 C9 1.5(3) . . . .
C3 C7 C8 C9 -175.52(16) . . . .
C7 C8 C9 C10 0.2(3) . . . .
C8 C9 C10 C11 -1.7(3) . . . .
C9 C10 C11 C12 1.5(3) . . . .
C10 C11 C12 C7 0.2(3) . . . .
C8 C7 C12 C11 -1.7(3) . . . .
C3 C7 C12 C11 175.35(18) . . . .
C17 N3 C13 C14 -0.2(2) . . . .
Ni1 N3 C13 C14 -179.87(10) . . . .
N3 C13 C14 C15 0.0(2) . . . .
N3 C13 C14 C18 -179.76(12) . . . .
C13 C14 C15 C16 0.3(2) . . . .
C18 C14 C15 C16 -179.93(14) . . . .
C14 C15 C16 C17 -0.5(2) . . . .
C13 N3 C17 C16 0.0(2) . . . .
Ni1 N3 C17 C16 179.71(12) . . . .
C15 C16 C17 N3 0.3(3) . . . .
C15 C14 C18 C23 -25.2(2) . . . .
C13 C14 C18 C23 154.51(14) . . . .
C15 C14 C18 C19 154.95(14) . . . .
C13 C14 C18 C19 -25.30(19) . . . .
C23 C18 C19 C20 -1.0(2) . . . .
C14 C18 C19 C20 178.83(13) . . . .
C18 C19 C20 C21 1.2(2) . . . .
C19 C20 C21 C22 -0.3(2) . . . .
C20 C21 C22 C23 -0.7(3) . . . .
C21 C22 C23 C18 0.9(3) . . . .
C19 C18 C23 C22 -0.1(2) . . . .
C14 C18 C23 C22 -179.90(15) . . . .
