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_4346731
_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         'C4 H2 N2 Ni0.5 S2, C16 H36 N'
_chemical_formula_sum            'C20 H38 N3 Ni0.5 S2'
_chemical_formula_weight         414.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-21 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 97.122(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9683(19)
_cell_length_b                   20.411(5)
_cell_length_c                   14.249(4)
_cell_measurement_reflns_used    5662
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      2.418
_cell_measurement_theta_min      27.520
_cell_volume                     2299.6(10)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.34
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.320
_diffrn_reflns_theta_min         1.752
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_preparation       'slow evporation'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0798P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3041
_reflns_number_total             5659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02035_si_002.cif
_cod_data_source_block           srk1s
_cod_original_cell_volume        2299.5(10)
_cod_original_formula_sum        'C20 H38 N3 Ni0.50 S2'
_cod_database_code               4346731
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.842
_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:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              79447
_shelx_hkl_checksum              69706
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'paratone oil on a loop'
_olex2_submission_special_instructions 'No special instructions were received'