Hydrogen Oxidation and Production Using Nickel-Based Molecular Catalysts with Positioned Proton Relays
Aaron D. Wilson; Rachel H. Newell; Michael J. McNevin; James T. Muckerman; M. Rakowski DuBois; Daniel L. DuBois; Journal of the American Chemical Society 128 (2006) 358–366; doi:10.1021/ja056442y

data_4110341
_publ_contact_author_address     '215 UCB, Boulder, CO, 80309-0215, USA'
_publ_contact_author_name        'Michael McNevin'
_publ_section_title
;
 Hydrogen Oxidation and Production Using Nickel-Based Molecular Catalysts
 with Positioned Proton Relays
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              358
_journal_page_last               366
_journal_paper_doi               10.1021/ja056442y
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C58 H59 B2 F8 N5 Ni P4'
_chemical_formula_weight         1182.31
_chemical_name_common            '[Ni(P(Ph)2N(Ph)2)2(CH3CN)](BF4)2'
_chemical_name_systematic        6a
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   12.9803(5)
_cell_length_b                   18.2873(7)
_cell_length_c                   23.0460(8)
_cell_measurement_reflns_used    4058
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      21.03
_cell_measurement_theta_min      2.36
_cell_volume                     5470.5(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      152(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.2061
_diffrn_reflns_av_sigmaI/netI    0.2330
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43782
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.9892
_exptl_absorpt_correction_T_min  0.8760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption correction applied 
using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38)' 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       'cut prism'
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         12544
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                6607
_reflns_number_total             12544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056442ysi20050928_044604_1.cif
_cod_data_source_block           6a
_cod_database_code               4110341