Isolation, Structure, and Reactivity of an Arylnickel(II) Pivalate Complex in Catalytic C-H/C-O Biaryl Coupling
Kei Muto; Junichiro Yamaguchi; Aiwen Lei; Kenichiro Itami; Journal of the American Chemical Society 135 (2013) 16384–16387; doi:10.1021/ja409803x

data_4121101
_publ_section_title
;
 Isolation, Structure, and Reactivity of an Arylnickel(II) Pivalate
 Complex in Catalytic C-H/C-O Biaryl Coupling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16384
_journal_page_last               16387
_journal_paper_doi               10.1021/ja409803x
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C42.5 H67.5 Ni O2 P2'
_chemical_formula_weight         731.12
_chemical_name_systematic
; 
 ? 
;
_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                 136.700(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   35.830(12)
_cell_length_b                   25.083(6)
_cell_length_c                   27.462(8)
_cell_measurement_reflns_used    17311
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.2839
_cell_measurement_theta_min      3.0162
_cell_volume                     16927(9)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56141
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.8952
_exptl_absorpt_correction_T_min  0.8952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       Block
_exptl_crystal_F_000             6344
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         14770
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0926
_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^)+(0.0709P)^2^+102.7954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2198
_reflns_number_gt                11539
_reflns_number_total             14770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409803x_si_002.cif
_cod_data_source_block           NiNapO
_cod_original_cell_volume        16926(9)
_cod_original_formula_sum        'C42.50 H67.50 Ni O2 P2'
_cod_database_code               4121101