Mechanistic Insights into Catalytic H2 Oxidation by Ni Complexes Containing a Diphosphine Ligand with a Positioned Amine Base
Jenny Y. Yang; R. Morris Bullock; Wendy J. Shaw; Brendan Twamley; Kendra Fraze; M. Rakowski DuBois; Daniel L. DuBois; Journal of the American Chemical Society 131 (2009) 5935–5945; doi:10.1021/ja900483x

data_4104249
_publ_section_title
;
 Mechanistic Insights into Catalytic H2 Oxidation by Ni Complexes
 Containing a Diphosphine Ligand with a Positioned Amine Base
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5935
_journal_page_last               5945
_journal_paper_doi               10.1021/ja900483x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C57 H58 N2 Ni P4, C2 H3 N'
_chemical_formula_sum            'C59 H61 N3 Ni P4'
_chemical_formula_weight         994.70
_chemical_name_common            'DpppNippbbbme2, MeCN'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.353(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3808(7)
_cell_length_b                   11.6486(4)
_cell_length_c                   23.6805(9)
_cell_measurement_reflns_used    6048
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.19
_cell_volume                     5028.6(3)
_computing_cell_refinement       'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics    'XP, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'XS, SHELXTL  v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            74657
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_correction_T_min  0.8645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0475P)^2^+1.3731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                6751
_reflns_number_total             9108
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja900483x_si_002.cif
_cod_data_source_block           bt1151
_cod_original_cell_volume        5028.5(3)
_cod_database_code               4104249