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#$Date: 2020-10-31 07:24:54 +0200 (Sat, 31 Oct 2020) $
#$Revision: 258662 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/36/2243643.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_2243643
loop_
_publ_author_name
'Setifi, Zouaoui'
'Ferjani, Hela'
'Setifi, Fatima'
'Ezzine, Safa'
'Al-Douh, Mohammed Hadi'
_publ_section_title
;
 Synthesis, crystal structure and Hirshfeld surface analysis of
 bis{2-[(pyridin-2-yl)amino]pyridinium} tetracyanonickelate(II)
;
_journal_coeditor_code           HB7948
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1794
_journal_page_last               1798
_journal_paper_doi               10.1107/S205698902001419X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C10 H10 N3)2 [Ni (C N)4]'
_chemical_formula_moiety         '2(C10 H10 N3), C4 N4 Ni 2-'
_chemical_formula_sum            'C24 H20 N10 Ni'
_chemical_formula_weight         507.21
_chemical_name_common
;
Bis{2-[(pyridin-2-yl)amino]pyridinium} tetracyanonickelate(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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.182(2)
_cell_angle_beta                 98.729(2)
_cell_angle_gamma                97.444(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1046(4)
_cell_length_b                   9.1467(4)
_cell_length_c                   9.3833(4)
_cell_measurement_reflns_used    7173
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.875
_cell_measurement_theta_min      2.818
_cell_volume                     585.49(5)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur Sapphire CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16272
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.559
_diffrn_reflns_theta_min         2.241
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       plate
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.344
_refine_ls_extinction_coef       0.091(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick 2014
;
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0475
_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)+(0.0546P)²+0.3025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                2659
_reflns_number_total             3572
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7948sup1.cif
_cod_data_source_block           I
_cod_database_code               2243643
_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'
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 0.5000 0.0000 0.0000 0.04195(19) Uani d 1 . .
C C1 0.6743(4) 0.0656(3) 0.1772(3) 0.0508(6) Uani d 1 . .
N N1 0.7800(5) 0.1080(3) 0.2861(3) 0.0745(8) Uani d 1 . .
C C2 0.3639(4) 0.1552(3) 0.0568(2) 0.0455(5) Uani d 1 . .
N N2 0.2831(4) 0.2503(3) 0.0942(3) 0.0624(6) Uani d 1 . .
N N4 0.1820(3) 0.7199(2) 0.3981(2) 0.0445(4) Uani d 1 . .
H H4A 0.1949 0.7110 0.4886 0.053 Uiso calc 1 . .
N N5 0.2473(3) 0.5418(2) 0.5852(2) 0.0484(5) Uani d 1 . .
N N3 0.2311(3) 0.4715(2) 0.3342(2) 0.0492(5) Uani d 1 . .
H H3A 0.2354 0.3997 0.2625 0.059 Uiso calc 1 . .
C C3 0.1977(3) 0.6028(3) 0.2949(3) 0.0422(5) Uani d 1 . .
C C8 0.2592(3) 0.4356(3) 0.4722(3) 0.0443(5) Uani d 1 . .
C C5 0.1462(4) 0.8522(3) 0.3626(3) 0.0508(6) Uani d 1 . .
H H5 0.1351 0.9313 0.4365 0.061 Uiso calc 1 . .
C C4 0.1807(4) 0.6192(3) 0.1479(3) 0.0503(6) Uani d 1 . .
H H4 0.1942 0.5397 0.0753 0.060 Uiso calc 1 . .
C C12 0.3276(4) 0.2629(3) 0.6262(4) 0.0595(7) Uani d 1 . .
H H12 0.3538 0.1690 0.6407 0.071 Uiso calc 1 . .
C C7 0.1442(4) 0.7522(3) 0.1118(3) 0.0557(6) Uani d 1 . .
H H7 0.1314 0.7635 0.0144 0.067 Uiso calc 1 . .
C C10 0.2763(4) 0.5097(3) 0.7197(3) 0.0553(6) Uani d 1 . .
H H10 0.2695 0.5836 0.7998 0.066 Uiso calc 1 . .
C C6 0.1264(4) 0.8713(3) 0.2224(3) 0.0564(7) Uani d 1 . .
H H6 0.1013 0.9625 0.1994 0.068 Uiso calc 1 . .
C C9 0.3006(4) 0.2930(3) 0.4869(3) 0.0524(6) Uani d 1 . .
H H9 0.3096 0.2214 0.4055 0.063 Uiso calc 1 . .
C C11 0.3157(4) 0.3727(4) 0.7447(3) 0.0591(7) Uani d 1 . .
H H11 0.3341 0.3540 0.8397 0.071 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'
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
C2 Ni1 C2 . 2_655 180.0 ?
C2 Ni1 C1 . . 89.06(10) ?
C2 Ni1 C1 2_655 . 90.94(10) ?
C2 Ni1 C1 . 2_655 90.94(10) ?
C2 Ni1 C1 2_655 2_655 89.06(10) ?
C1 Ni1 C1 . 2_655 180.0 ?
N1 C1 Ni1 . . 178.8(2) ?
N2 C2 Ni1 . . 178.6(2) ?
C3 N4 C5 . . 121.3(2) ?
C3 N4 H4A . . 119.4 ?
C5 N4 H4A . . 119.4 ?
C8 N5 C10 . . 117.8(2) ?
C3 N3 C8 . . 129.7(2) ?
C3 N3 H3A . . 115.1 ?
C8 N3 H3A . . 115.1 ?
N4 C3 N3 . . 119.7(2) ?
N4 C3 C4 . . 119.0(2) ?
N3 C3 C4 . . 121.3(2) ?
N5 C8 N3 . . 117.0(2) ?
N5 C8 C9 . . 123.4(2) ?
N3 C8 C9 . . 119.6(2) ?
C6 C5 N4 . . 121.3(2) ?
C6 C5 H5 . . 119.4 ?
N4 C5 H5 . . 119.4 ?
C7 C4 C3 . . 119.8(2) ?
C7 C4 H4 . . 120.1 ?
C3 C4 H4 . . 120.1 ?
C9 C12 C11 . . 119.7(3) ?
C9 C12 H12 . . 120.2 ?
C11 C12 H12 . . 120.2 ?
C4 C7 C6 . . 119.5(2) ?
C4 C7 H7 . . 120.3 ?
C6 C7 H7 . . 120.3 ?
N5 C10 C11 . . 122.9(3) ?
N5 C10 H10 . . 118.5 ?
C11 C10 H10 . . 118.5 ?
C5 C6 C7 . . 119.1(2) ?
C5 C6 H6 . . 120.4 ?
C7 C6 H6 . . 120.4 ?
C12 C9 C8 . . 117.4(3) ?
C12 C9 H9 . . 121.3 ?
C8 C9 H9 . . 121.3 ?
C10 C11 C12 . . 118.8(3) ?
C10 C11 H11 . . 120.6 ?
C12 C11 H11 . . 120.6 ?
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 C2 . 1.865(2) ?
Ni1 C2 2_655 1.865(2) ?
Ni1 C1 . 1.867(3) ?
Ni1 C1 2_655 1.867(3) ?
C1 N1 . 1.145(4) ?
C2 N2 . 1.136(3) ?
N4 C3 . 1.340(3) ?
N4 C5 . 1.355(3) ?
N4 H4A . 0.8600 ?
N5 C8 . 1.326(3) ?
N5 C10 . 1.337(3) ?
N3 C3 . 1.355(3) ?
N3 C8 . 1.383(3) ?
N3 H3A . 0.8600 ?
C3 C4 . 1.402(3) ?
C8 C9 . 1.399(3) ?
C5 C6 . 1.346(4) ?
C5 H5 . 0.9300 ?
C4 C7 . 1.365(4) ?
C4 H4 . 0.9300 ?
C12 C9 . 1.373(4) ?
C12 C11 . 1.381(4) ?
C12 H12 . 0.9300 ?
C7 C6 . 1.399(4) ?
C7 H7 . 0.9300 ?
C10 C11 . 1.371(4) ?
C10 H10 . 0.9300 ?
C6 H6 . 0.9300 ?
C9 H9 . 0.9300 ?
C11 H11 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N3 H3A N2 . 0.86 2.00 2.853(3) 172
N4 H4A N5 . 0.86 1.97 2.629(3) 132
N4 H4A N1 2_666 0.86 2.41 3.055(3) 132
C5 H5 N1 2_666 0.93 2.68 3.206(4) 117

_cod_database_fobs_code 2243643
