Two Pathways for Electrocatalytic Oxidation of Hydrogen by a Nickel Bis(diphosphine) Complex with Pendant Amines in the Second Coordination Sphere
Jenny Y. Yang; Stuart E. Smith; Tianbiao Liu; William G. Dougherty; Wesley A. Hoffert; W. Scott Kassel; M. Rakowski DuBois; Daniel L. DuBois; R. Morris Bullock; Journal of the American Chemical Society 135 (2013) 9700–9712; doi:10.1021/ja400705a

data_4120001
_publ_contact_author
; 
Tianbiao Leo Liu 
Pacific Northwest National Laboratory 
Richland, WA, 99354 
USA 
;
_publ_contact_author_email       Tianbiao.Liu@pnl.gov
_publ_section_title
;
 Two Pathways for Electrocatalytic Oxidation of Hydrogen by a Nickel
 Bis(diphosphine) Complex with Pendant Amines in the Second Coordination
 Sphere
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9700
_journal_page_last               9712
_journal_paper_doi               10.1021/ja400705a
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C36 H72 B F4 N3 Ni0.75 P3'
_chemical_formula_weight         770.72
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.7955(8)
_cell_length_b                   25.7955(8)
_cell_length_c                   25.7955(8)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.23
_cell_volume                     17164.5(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            141922
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.9468
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             6656
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.098
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.004
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3623
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.969
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.2250
_reflns_number_gt                3479
_reflns_number_total             3623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400705a_si_003.cif
_cod_data_source_block           jy
_cod_database_code               4120001