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_4106561
_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         'C32 H46 N4 Ni P2, C2 H3 N, 2(B F4)'
_chemical_formula_sum            'C34 H49 B2 F8 N5 Ni P2'
_chemical_formula_weight         822.05
_chemical_name_common            '[Ni(PCy2NPh2)(ACN)2](BF4)2*ACN'
_chemical_name_systematic
; 
 [Ni(PCy2NPh2)2(ACN)2](BF4)2*ACN
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.202(4)
_cell_angle_beta                 102.372(4)
_cell_angle_gamma                102.077(4)
_cell_formula_units_Z            2
_cell_length_a                   9.481(3)
_cell_length_b                   12.340(4)
_cell_length_c                   17.657(5)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.44
_cell_volume                     1910.3(10)
_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      150(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX2'
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36003
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.8788
_exptl_absorpt_correction_T_min  0.7327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       Needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+1.6453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                5771
_reflns_number_total             7013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204489e_si_004.cif
_cod_data_source_block           js03
_cod_original_cell_volume        1910.5(10)
_cod_database_code               4106561