Crystal structure of 1,1′-(1,2-ethanediyl)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2 S:S)nickel(II), C20H14N6NiS4
Yan, Wei-Hong; Chen, Wan-Yao; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 235–236; doi:10.1515/ncrs-2021-0433

data_8105189
_publ_section_title
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 Crystal structure of 1,1&#x2032;-(1,2-ethanediyl)bis(pyridin-1-ium)
 bis(1,2-dicyanoethene-1,2-dithiolato-\k2 S:S)nickel(II), C20H14N6NiS4
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_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              235
_journal_page_last               236
_journal_paper_doi               10.1515/ncrs-2021-0433
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C8 N4 Ni S4, C12 H14 N2'
_chemical_formula_sum            'C20 H14 N6 Ni S4'
_chemical_formula_weight         525.32
_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     iterative
_cell_angle_alpha                116.404(3)
_cell_angle_beta                 94.574(4)
_cell_angle_gamma                103.031(4)
_cell_formula_units_Z            1
_cell_length_a                   8.519(3)
_cell_length_b                   8.5956(16)
_cell_length_c                   8.6531(17)
_cell_measurement_reflns_used    878
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.51
_cell_volume                     541.0(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3974
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.524
_diffrn_reflns_theta_min         2.508
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0472 before and 0.0327 after correction.
The Ratio of minimum to maximum transmission is 0.8723.
The \l/2 correction factor is 0.0015.
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_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0468P)^2^+0.4529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1147
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2157
_reflns_number_total             2708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0433_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105189
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C9(H9)
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