Synthesis, crystal structure and Hirshfeld surface analysis of bis{2-[(pyridin-2-yl)amino]pyridinium} tetracyanonickelate(II)
Setifi, Zouaoui; Ferjani, Hela; Setifi, Fatima; Ezzine, Safa; Al-Douh, Mohammed Hadi; Acta Crystallographica Section E 76 (2020) 1794–1798; doi:10.1107/S205698902001419X

data_2243643
_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
;
<i>SHELXL2014/7</i> (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       '\w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0546P)^2^+0.3025P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            hb7948sup1.cif
_cod_data_source_block           I
_cod_database_code               2243643
_shelx_hkl_checksum              70627
_shelx_res_checksum              18513
_cod_database_fobs_code 2243643