A coordinatively saturated nickel complex supported by triazenido ligands: a new electrocatalyst for hydrogen generation via ligand-centered proton-transfer
Xue, Dan; Luo, Su-Ping; Zhan, Shu-Zhong; New Journal of Chemistry 41 (2017) 8503–8508; doi:10.1039/C7NJ01705G

data_1546581
_publ_section_title
;
 A coordinatively saturated nickel complex supported by triazenido
 ligands: a new electrocatalyst for hydrogen generation via
 ligand-centered proton-transfer
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8503
_journal_page_last               8508
_journal_paper_doi               10.1039/C7NJ01705G
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C28 H16 N10 Ni S4'
_chemical_formula_weight         679.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.256(8)
_cell_length_b                   10.256(8)
_cell_length_c                   13.160(10)
_cell_measurement_reflns_used    1221
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.52
_cell_volume                     1384.2(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.2740
_diffrn_reflns_av_sigmaI/netI    0.1433
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5830
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_correction_T_min  0.8850
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                1108
_reflns_number_total             1221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj01705g2.cif
_cod_data_source_block           m101024e1
_cod_original_sg_symbol_H-M      i_-4
_cod_database_code               1546581