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_4106560
_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_sum            'C60 H86 B2 F8 N6 Ni P4'
_chemical_formula_weight         1247.56
_chemical_name_common            '[Ni(PCy2NPh2)2(MeCN)](BF4)2'
_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                 96.356(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.14(2)
_cell_length_b                   13.213(8)
_cell_length_c                   26.165(15)
_cell_measurement_temperature    123(2)
_cell_volume                     12074(12)
_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      123(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  0.1136
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            63277
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.9072
_exptl_absorpt_correction_T_min  0.8653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             5264
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         11228
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0478P)^2^+50.5109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                7815
_reflns_number_total             11228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204489e_si_003.cif
_cod_data_source_block           js03_2
_cod_database_code               4106560