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_4127382
_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            'C24 H41 N5 Ni S4'
_chemical_formula_weight         586.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                72.7210(10)
_cell_angle_beta                 79.4010(10)
_cell_angle_gamma                89.3780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8084(13)
_cell_length_b                   10.0948(13)
_cell_length_c                   15.219(2)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.32
_cell_volume                     1412.8(3)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16434
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.520
_diffrn_reflns_theta_min         1.427
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.391
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.391
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0402
_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^)+2.8107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6204
_reflns_number_total             6519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04937_si_007.cif
_cod_data_source_block           (TBA)[Ni(HL)(L)]_100K
_cod_database_code               4127382
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              41703
_shelx_hkl_checksum              1722