Electrocatalytic Oxidation of Formate by [Ni(PR2NR'2)2(CH3CN)]2+ Complexes
Brandon R. Galan; Julia Schöffel; John C. Linehan; Candace Seu; Aaron M. Appel; John A. S. Roberts; Monte L. Helm; Uriah J. Kilgore; Jenny Y. Yang; Daniel L. DuBois; Clifford P. Kubiak; Journal of the American Chemical Society 133 (2011) 12767–12779; doi:10.1021/ja204489e

data_4106564
_publ_section_title
;
 Electrocatalytic Oxidation of Formate by [Ni(PR2NR'2)2(CH3CN)]2+
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12767
_journal_page_last               12779
_journal_paper_doi               10.1021/ja204489e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C62 H67 N4 Ni O2 P4, C4 H10 O, B F4'
_chemical_formula_sum            'C66 H77 B F4 N4 Ni O3 P4'
_chemical_formula_weight         1243.72
_chemical_name_common            '[Ni(PPh2NBn2)2(OAc)]BF4'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   24.0216(11)
_cell_length_b                   17.6157(8)
_cell_length_c                   14.6064(7)
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      2.20
_cell_volume                     6180.8(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            91964
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.9536
_exptl_absorpt_correction_T_min  0.9536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         12749
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0422P)^2^+1.8072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                10311
_reflns_number_total             12749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204489e_si_007.cif
_cod_data_source_block           helm015
_cod_database_code               4106564