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_4127381
_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_sum            'C11 H13 N5 Ni O S4'
_chemical_formula_weight         418.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90.107(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.576(2)
_cell_length_b                   24.360(8)
_cell_length_c                   9.895(3)
_cell_measurement_reflns_used    1664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.65
_cell_volume                     1585.1(9)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.639
_diffrn_reflns_theta_min         1.672
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 1041 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3694
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0301P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                2816
_reflns_number_total             3694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04937_si_003.cif
_cod_data_source_block           Ni(HL)2_DMF_100K
_cod_original_cell_volume        1585.0(9)
_cod_database_code               4127381
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              53145
_shelx_hkl_checksum              10712