Investigating the Dearomative Rearrangement of Biaryl Phosphine-Ligated Pd(II) Complexes
Phillip J. Milner; Thomas J. Maimone; Mingjuan Su; Jiahao Chen; Peter Müller; Stephen L. Buchwald; Journal of the American Chemical Society 134 (2012) 19922–19934; doi:10.1021/ja310351e

data_4118967
_publ_section_title
;
 Investigating the Dearomative Rearrangement of Biaryl Phosphine-Ligated
 Pd(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19922
_journal_page_last               19934
_journal_paper_doi               10.1021/ja310351e
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C43.5 H68 I O2 P Pd'
_chemical_formula_weight         887.25
_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                68.638(2)
_cell_angle_beta                 70.570(2)
_cell_angle_gamma                88.106(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7507(9)
_cell_length_b                   13.3686(10)
_cell_length_c                   15.8562(12)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.35
_cell_volume                     2176.6(3)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatech ImuS multilayer optics'
_diffrn_radiation_source         'ImuS micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            93214
_diffrn_reflns_theta_full        30.32
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_correction_T_min  0.7947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       needle
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.841
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         13049
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0480P)^2^+3.9841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                10512
_reflns_number_total             13049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310351e_si_001_05.cif
_cod_data_source_block           x11207
_cod_original_formula_sum        'C43.50 H68 I O2 P Pd'
_cod_database_code               4118967