Crystal structure of 1,1′-(methylene)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2 S:S)nickel(II), C42H30N14Ni2S8
Liu, Xue-Guo; Chen, Wan-Yao; Pan, Hui-Yan; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 231–233; doi:10.1515/ncrs-2021-0434

data_8105188
_publ_section_title
;
 Crystal structure of 1,1&#x2032;-(methylene)bis(pyridin-1-ium)
 bis(1,2-dicyanoethene-1,2-dithiolato-\k2 S:S)nickel(II), C42H30N14Ni2S8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              231
_journal_page_last               233
_journal_paper_doi               10.1515/ncrs-2021-0434
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         '2(C8 N4 Ni S4), 2(C11 H12 N2), 2(C2 H3 N)'
_chemical_formula_sum            'C42 H30 N14 Ni2 S8'
_chemical_formula_weight         1104.70
_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
_cell_angle_alpha                80.109(4)
_cell_angle_beta                 84.876(4)
_cell_angle_gamma                88.758(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5083(17)
_cell_length_b                   10.744(2)
_cell_length_c                   12.188(2)
_cell_measurement_reflns_used    7604
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.34
_cell_volume                     1221.7(4)
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.975
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14613
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.707
_diffrn_reflns_theta_min         1.703
_exptl_absorpt_coefficient_mu    1.160
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.8895.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.055
_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     302
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.2621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4890
_reflns_number_total             5581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0434_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105188
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C15(H15), C5(H5), C7(H7), C11(H11), C12(H12),
 C14(H14), C13(H13)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;