Effect of Protonation upon Electronic Coupling in the Mixed Valence and Mixed Protonated Complex, [Ni(2,3-pyrazinedithiol)2].
Kennedy, Steven R.; Goyal, Puja; Kozar, Morgan N.; Yennawar, Hemant P.; Hammes-Schiffer, Sharon; Lear, Benjamin J.; Inorganic chemistry 55 (2016) 1433–1445; doi:10.1021/acs.inorgchem.5b02035

data_4346730
_publ_section_title
;
 Effect of Protonation upon Electronic Coupling in the Mixed Valence and
 Mixed Protonated Complex, [Ni(2,3-pyrazinedithiol)2].
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1433
_journal_page_last               1445
_journal_paper_doi               10.1021/acs.inorgchem.5b02035
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C8 H4 N4 Ni S4, C16 H36 N'
_chemical_formula_sum            'C24 H40 N5 Ni S4'
_chemical_formula_weight         585.58
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-21 # Formatted by publCIF

;
_cell_angle_alpha                72.931(2)
_cell_angle_beta                 79.621(2)
_cell_angle_gamma                89.431(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8856(13)
_cell_length_b                   10.1476(13)
_cell_length_c                   15.386(2)
_cell_measurement_reflns_used    2993
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.104
_cell_measurement_theta_min      2.299
_cell_volume                     1449.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13550
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.9903
_exptl_absorpt_correction_T_min  0.7644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         7006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+0.1687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                4784
_reflns_number_total             7006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02035_si_003.cif
_cod_data_source_block           srk11s
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4346730