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_4120002
_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            'C49 H97.5 B2 F8 N4.5 Ni P4'
_chemical_formula_weight         1106.02
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.802(3)
_cell_angle_beta                 81.733(3)
_cell_angle_gamma                87.091(3)
_cell_formula_units_Z            4
_cell_length_a                   13.5841(6)
_cell_length_b                   22.1401(11)
_cell_length_c                   25.5216(13)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.77
_cell_volume                     7082.0(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            119382
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_correction_T_min  0.9597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       block
_exptl_crystal_F_000             2372
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.081
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1425
_refine_ls_number_reflns         35421
_refine_ls_number_restraints     661
_refine_ls_restrained_S_all      2.075
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.2511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                24971
_reflns_number_total             35421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400705a_si_004.cif
_cod_data_source_block           jy3_0m
_cod_original_formula_sum        'C49 H97.50 B2 F8 N4.50 Ni P4'
_cod_database_code               4120002