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_4120000
_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            'C48 H96 N4 Ni P4'
_chemical_formula_weight         911.88
_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                 93.999(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1553(9)
_cell_length_b                   19.2316(11)
_cell_length_c                   17.9082(11)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.51
_cell_volume                     5206.8(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 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56881
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.9106
_exptl_absorpt_correction_T_min  0.8923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         19708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0375P)^2^+0.9108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                14073
_reflns_number_total             19708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400705a_si_002.cif
_cod_data_source_block           pnl073
_cod_database_code               4120000