Role of <i>d</i>-Elements in a Proton-Electron Coupling of <i>d</i>-π Hybridized Electron Systems.
Hayashi, Mikihiro; Takahashi, Yuki; Yoshida, Yukihiro; Sugimoto, Kunihisa; Kitagawa, Hiroshi; Journal of the American Chemical Society 141 (2019) 11686–11693; doi:10.1021/jacs.9b04937

data_4127378
_publ_section_title
;
 Role of <i>d</i>-Elements in a Proton-Electron Coupling of <i>d</i>-\p
 Hybridized Electron Systems.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11686
_journal_page_last               11693
_journal_paper_doi               10.1021/jacs.9b04937
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C11 H13 N5 Ni O S4 '
_chemical_formula_sum            'C11 H13 N5 Ni O S4'
_chemical_formula_weight         418.20
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.339(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   6.6990(10)
_cell_length_b                   9.9020(13)
_cell_length_c                   12.655(8)
_cell_measurement_reflns_used    4039
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      3.4
_cell_volume                     809.5(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Large cylindrical IP camera'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Synchrotron (SPring-8 BL02B1)'
_diffrn_radiation_wavelength     0.55981
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4200
_diffrn_reflns_theta_full        23.61
_diffrn_reflns_theta_max         23.61
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             428.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.45
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1585 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.42(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4039
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.4791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                2886
_reflns_number_total             4039
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9b04937_si_002.cif
_cod_data_source_block           Ni(HL)2_DMF_296K
_cod_original_formula_sum        'C11 H13 N5 Ni O S4 '
_cod_database_code               4127378