A dinuclear nickel catalyst based on metal–metal cooperation for electrochemical hydrogen production
Hamaguchi, Tomohiko; Kai, Keisuke; Ando, Isao; Kawano, Ken; Yamauchi, Kosei; Sakai, Ken; Inorganica Chimica Acta 505 (2020) 119498–; doi:10.1016/j.ica.2020.119498

data_1565224
_publ_section_title
;
 A dinuclear nickel catalyst based on metal--metal cooperation for
 electrochemical hydrogen production
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119498
_journal_paper_doi               10.1016/j.ica.2020.119498
_journal_volume                  505
_journal_year                    2020
_chemical_formula_sum            'C68 H72 B2 F8 N4 Ni2 O P4 S4'
_chemical_formula_weight         1504.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.0500(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2930(4)
_cell_length_b                   14.6432(3)
_cell_length_c                   20.5612(4)
_cell_measurement_reflns_used    66101
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.99
_cell_volume                     7007.3(2)
_computing_cell_refinement       'CrystalClear (Rigaku, 2010)'
_computing_data_collection       '<i>RAPID-AUTO</i> (Rigaku, 2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 2010)'
_computing_molecular_graphics
;
Yadokari-XG (Wakita, Nemoto et al., 2009) and ORTEP-3
 for Windows (Farrugia ,1997))
;
_computing_publication_material
;
Yadokari-XG (Wakita, Nemoto et al., 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            110234
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.459
_diffrn_reflns_theta_min         2.988
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.832
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_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     860
_refine_ls_number_reflns         15971
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+12.7731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13797
_reflns_number_total             15971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-505-119498.cif
_cod_data_source_block           Ni_dppp_tzs_dimer
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565224
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.923