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_4110342
_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            'C64 H94 B2 F8 N6 Ni P4'
_chemical_formula_weight         1303.66
_chemical_name_common            '[Ni(P(Cy)2N(Bz)2)2](BF4)'
_chemical_name_systematic        6b
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 99.754(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.571(13)
_cell_length_b                   16.235(11)
_cell_length_c                   23.576(17)
_cell_measurement_reflns_used    7786
_cell_measurement_temperature    157(2)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      2.31
_cell_volume                     6628(8)
_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      157(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0973
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22550
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.9559
_exptl_absorpt_correction_T_min  0.8043
_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    1.306
_exptl_crystal_description       'cut prism'
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0651
_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^)+(0.1228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1888
_reflns_number_gt                4801
_reflns_number_total             7320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja056442ysi20050928_044604_2.cif
_cod_data_source_block           6b
_cod_database_code               4110342