[Ni(PPh2NC6H4X2)2]2+ Complexes as Electrocatalysts for H2 Production: Effect of Substituents, Acids, and Water on Catalytic Rates
Uriah J. Kilgore; John A. S. Roberts; Douglas H. Pool; Aaron M. Appel; Michael P. Stewart; M. Rakowski DuBois; William G. Dougherty; W. Scott Kassel; R. Morris Bullock; Daniel L. DuBois; Journal of the American Chemical Society 133 (2011) 5861–5872; doi:10.1021/ja109755f

data_4105941
_publ_section_title
;
 [Ni(PPh2NC6H4X2)2]2+ Complexes as Electrocatalysts for H2 Production:
 Effect of Substituents, Acids, and Water on Catalytic Rates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5861
_journal_page_last               5872
_journal_paper_doi               10.1021/ja109755f
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C68 H80 B2 F8 N4 Ni O2 P4'
_chemical_formula_weight         1341.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.6150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2120(7)
_cell_length_b                   21.4165(9)
_cell_length_c                   17.7094(7)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.23
_cell_volume                     6436.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            90133
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.9367
_exptl_absorpt_correction_T_min  0.9113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.231
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         24371
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0470P)^2^+2.1833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                17074
_reflns_number_total             24371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109755f_si_002.cif
_cod_data_source_block           pnl052
_cod_original_cell_volume        6436.4(5)
_cod_database_code               4105941