Catalytic Oxidation of Alcohol via Nickel Phosphine Complexes with Pendant Amines
Weiss, Charles J.; Das, Parthapratim; Miller, Deanna L.; Helm, Monte L.; Appel, Aaron M.; ACS Catalysis 4 (2014) 2951–; doi:10.1021/cs500853f

data_4511782
_publ_section_title
;
 Catalytic Oxidation of Alcohol via Nickel Phosphine Complexes with
 Pendant Amines
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              2951
_journal_paper_doi               10.1021/cs500853f
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C32 H57 B2 F8 N3 Ni P2'
_chemical_formula_sum            'C32 H57 B2 F8 N3 Ni P2'
_chemical_formula_weight         778.08
_chemical_name_common            Ni(dcpe)2CH3CN2
_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                 102.370(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2559(7)
_cell_length_b                   15.9677(9)
_cell_length_c                   19.9262(10)
_cell_measurement_reflns_used    45022
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      1.65
_cell_volume                     3809.0(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45022
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.8268
_exptl_absorpt_correction_T_min  0.7784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocl
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.230
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         8753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+4.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                7400
_reflns_number_total             8753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs500853f_si_003.cif
_cod_data_source_block           miller007_0m
_cod_depositor_comments
'Adding full bibliography for 4511782--4511784.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4511782