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#$Date: 2023-01-13 10:42:35 +0200 (Fri, 13 Jan 2023) $
#$Revision: 280329 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/64/8106463.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_8106463
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Crystal structure of
 cis-bis(2,2′-bipyrimidine-κ2N,N′)bis(thiocyanato-\kN)nickel(II),
 C18H12N10NiS2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              147
_journal_page_last               148
_journal_paper_doi               10.1515/ncrs-2016-0202
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C18 H12 N10 Ni S2'
_chemical_formula_sum            'C18 H12 N10 Ni S2'
_chemical_formula_weight         491.21
_chemical_name_systematic
;
cis-bis(2,2'-bipyrimidine-κ²N,N')bis(thiocyanato-κN)nickel(II)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.1303(5)
_cell_length_b                   12.1303(5)
_cell_length_c                   28.7471(12)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.71
_cell_volume                     4230.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            84487
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.351
_diffrn_reflns_theta_min         2.709
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0329
_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)+(0.0388P)²+6.1341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2250
_reflns_number_total             2635
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2016-0202_suppl.cif
_cod_data_source_block           Ni(NCS)2(bpym)2
_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        4230.0(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               8106463
_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   0.804
_shelx_estimated_absorpt_t_max   0.914
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.2500 0.08549(2) 0.02397(10) Uani 1 2 d S T P . .
S1 S 0.18497(5) 0.27959(6) -0.01505(2) 0.05311(18) Uani 1 1 d . . . . .
N1 N 0.48201(12) 0.41965(12) 0.08796(5) 0.0261(3) Uani 1 1 d . . . . .
N2 N 0.34557(14) 0.55420(14) 0.10439(6) 0.0370(4) Uani 1 1 d . . . . .
N3 N 0.23769(15) 0.39851(16) 0.15792(7) 0.0440(4) Uani 1 1 d . . . . .
N4 N 0.37278(13) 0.26797(12) 0.13417(5) 0.0281(3) Uani 1 1 d . . . . .
N5 N 0.37660(13) 0.24483(13) 0.03621(6) 0.0333(3) Uani 1 1 d . . . . .
C1 C 0.53861(16) 0.49300(15) 0.06289(7) 0.0318(4) Uani 1 1 d . . . . .
H1 H 0.6062 0.4725 0.0494 0.038 Uiso 1 1 calc R U . . .
C2 C 0.49911(18) 0.59865(16) 0.05651(7) 0.0366(4) Uani 1 1 d . . . . .
H2 H 0.5371 0.6503 0.0381 0.044 Uiso 1 1 calc R U . . .
C3 C 0.40206(19) 0.62486(16) 0.07814(7) 0.0396(5) Uani 1 1 d . . . . .
H3 H 0.3738 0.6964 0.0743 0.047 Uiso 1 1 calc R U . . .
C4 C 0.38812(14) 0.45409(14) 0.10792(6) 0.0269(3) Uani 1 1 d . . . . .
C5 C 0.32795(15) 0.36888(15) 0.13538(6) 0.0288(4) Uani 1 1 d . . . . .
C6 C 0.1886(2) 0.3175(2) 0.18221(10) 0.0549(6) Uani 1 1 d . . . . .
H6 H 0.1242 0.3342 0.1990 0.066 Uiso 1 1 calc R U . . .
C7 C 0.2281(2) 0.2120(2) 0.18358(9) 0.0523(6) Uani 1 1 d . . . . .
H7 H 0.1928 0.1571 0.2012 0.063 Uiso 1 1 calc R U . . .
C8 C 0.32110(18) 0.18927(17) 0.15825(7) 0.0391(5) Uani 1 1 d . . . . .
H8 H 0.3490 0.1170 0.1578 0.047 Uiso 1 1 calc R U . . .
C9 C 0.29653(16) 0.25984(15) 0.01548(6) 0.0300(4) Uani 1 1 d . . . . .
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
N5 Ni1 N5 93.21(9) . 6_554
N5 Ni1 N1 88.70(6) . .
N5 Ni1 N1 94.01(6) 6_554 .
N5 Ni1 N1 94.01(6) . 6_554
N5 Ni1 N1 88.70(6) 6_554 6_554
N1 Ni1 N1 176.06(8) . 6_554
N5 Ni1 N4 172.19(6) . 6_554
N5 Ni1 N4 85.83(6) 6_554 6_554
N1 Ni1 N4 99.10(6) . 6_554
N1 Ni1 N4 78.23(6) 6_554 6_554
N5 Ni1 N4 85.83(6) . .
N5 Ni1 N4 172.19(6) 6_554 .
N1 Ni1 N4 78.23(6) . .
N1 Ni1 N4 99.10(6) 6_554 .
N4 Ni1 N4 96.16(8) 6_554 .
C1 N1 C4 117.37(15) . .
C1 N1 Ni1 126.13(12) . .
C4 N1 Ni1 114.43(11) . .
C4 N2 C3 115.68(17) . .
C5 N3 C6 115.0(2) . .
C8 N4 C5 116.69(17) . .
C8 N4 Ni1 128.15(14) . .
C5 N4 Ni1 114.30(12) . .
C9 N5 Ni1 163.96(16) . .
N1 C1 C2 120.79(18) . .
N1 C1 H1 119.6 . .
C2 C1 H1 119.6 . .
C3 C2 C1 116.99(18) . .
C3 C2 H2 121.5 . .
C1 C2 H2 121.5 . .
N2 C3 C2 123.40(18) . .
N2 C3 H3 118.3 . .
C2 C3 H3 118.3 . .
N2 C4 N1 125.72(17) . .
N2 C4 C5 119.06(16) . .
N1 C4 C5 115.20(15) . .
N3 C5 N4 126.67(18) . .
N3 C5 C4 118.44(17) . .
N4 C5 C4 114.89(15) . .
N3 C6 C7 123.0(2) . .
N3 C6 H6 118.5 . .
C7 C6 H6 118.5 . .
C6 C7 C8 117.5(2) . .
C6 C7 H7 121.3 . .
C8 C7 H7 121.3 . .
N4 C8 C7 121.2(2) . .
N4 C8 H8 119.4 . .
C7 C8 H8 119.4 . .
N5 C9 S1 178.46(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N5 2.0619(16) .
Ni1 N5 2.0619(16) 6_554
Ni1 N1 2.0706(14) .
Ni1 N1 2.0706(14) 6_554
Ni1 N4 2.0946(15) 6_554
Ni1 N4 2.0946(15) .
S1 C9 1.631(2) .
N1 C1 1.335(2) .
N1 C4 1.342(2) .
N2 C4 1.323(2) .
N2 C3 1.332(3) .
N3 C5 1.322(2) .
N3 C6 1.344(3) .
N4 C8 1.335(2) .
N4 C5 1.340(2) .
N5 C9 1.154(2) .
C1 C2 1.380(3) .
C1 H1 0.9400 .
C2 C3 1.369(3) .
C2 H2 0.9400 .
C3 H3 0.9400 .
C4 C5 1.491(2) .
C6 C7 1.368(4) .
C6 H6 0.9400 .
C7 C8 1.371(3) .
C7 H7 0.9400 .
C8 H8 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
C4 N1 C1 C2 -2.4(3) . . . .
Ni1 N1 C1 C2 160.20(15) . . . .
N1 C1 C2 C3 2.0(3) . . . .
C4 N2 C3 C2 -1.2(3) . . . .
C1 C2 C3 N2 -0.1(3) . . . .
C3 N2 C4 N1 0.7(3) . . . .
C3 N2 C4 C5 -177.96(17) . . . .
C1 N1 C4 N2 1.1(3) . . . .
Ni1 N1 C4 N2 -163.56(16) . . . .
C1 N1 C4 C5 179.81(16) . . . .
Ni1 N1 C4 C5 15.15(19) . . . .
C6 N3 C5 N4 0.9(3) . . . .
C6 N3 C5 C4 -179.4(2) . . . .
C8 N4 C5 N3 -0.1(3) . . . .
Ni1 N4 C5 N3 170.11(17) . . . .
C8 N4 C5 C4 -179.83(17) . . . .
Ni1 N4 C5 C4 -9.6(2) . . . .
N2 C4 C5 N3 -4.5(3) . . . .
N1 C4 C5 N3 176.66(17) . . . .
N2 C4 C5 N4 175.21(17) . . . .
N1 C4 C5 N4 -3.6(2) . . . .
C5 N3 C6 C7 -0.3(4) . . . .
N3 C6 C7 C8 -1.0(4) . . . .
C5 N4 C8 C7 -1.3(3) . . . .
Ni1 N4 C8 C7 -169.90(18) . . . .
C6 C7 C8 N4 1.8(4) . . . .
