Remarkable Ligand Effect of P(2-MeOC6H4)3on Palladium-Catalyzed Direct Arylation
Wakioka, Masayuki; Nakamura, Yuki; Montgomery, Michelle; Ozawa, Fumiyuki; Organometallics 34 (2015) 198–; doi:10.1021/om501052g

data_4085092
_publ_section_title
;
 Remarkable Ligand Effect of P(2-MeOC6H4)3on Palladium-Catalyzed Direct
 Arylation
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              198
_journal_paper_doi               10.1021/om501052g
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C31 H33 O5 P Pd'
_chemical_formula_weight         622.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                81.235(4)
_cell_angle_beta                 78.161(4)
_cell_angle_gamma                76.153(3)
_cell_formula_units_Z            8
_cell_length_a                   14.9591(15)
_cell_length_b                   16.4861(18)
_cell_length_c                   23.666(3)
_cell_measurement_reflns_used    16829
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      31.1653
_cell_measurement_theta_min      2.2443
_cell_volume                     5513.4(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37267
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.9409
_exptl_absorpt_correction_T_min  0.9065
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_recrystallization_method THF/pentane
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1393
_refine_ls_number_reflns         19949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0383P)^2^+23.3308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                16709
_reflns_number_total             19949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501052g_si_002.cif
_cod_data_source_block           5b
_cod_depositor_comments
'Adding full bibliography for 4085091--4085092.cif.'
_cod_original_cell_volume        5513.4(10)
_cod_database_code               4085092