Electron-deficient olefin ligands enable generation of quaternary carbons by Ni-catalyzed cross-coupling.
Huang, Chung-Yang Dennis; Doyle, Abigail G.; Journal of the American Chemical Society 137 (2015) 5638–5641; doi:10.1021/jacs.5b02503

data_4129411
_publ_section_title
;
 Electron-deficient olefin ligands enable generation of quaternary carbons
 by Ni-catalyzed cross-coupling.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5638
_journal_page_last               5641
_journal_paper_doi               10.1021/jacs.5b02503
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C36 H43 N3 Ni O7 S2'
_chemical_formula_weight         752.56
_chemical_name_common            DCY1
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.007(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.678(3)
_cell_length_b                   14.028(2)
_cell_length_c                   14.858(3)
_cell_measurement_reflns_used    9582
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.1984
_cell_measurement_theta_min      4.8686
_cell_volume                     3433.3(11)
_computing_cell_refinement       'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37324
_diffrn_reflns_theta_full        66.53
_diffrn_reflns_theta_max         66.53
_diffrn_reflns_theta_min         4.14
_diffrn_source                   'ImuS micro-focus source'
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.837
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         5936
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1140P)^2^+2.3877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                5120
_reflns_number_total             5936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b02503_si_003.cif
_cod_data_source_block           I
_cod_original_cell_volume        3433.3(10)
_cod_database_code               4129411