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_4085091
_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            'C59 H60 Cl2 O10 P2 Pd2'
_chemical_formula_weight         1274.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.9811(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3173(9)
_cell_length_b                   18.9616(17)
_cell_length_c                   28.180(3)
_cell_measurement_reflns_used    15309
_cell_measurement_temperature    103(2)
_cell_measurement_theta_min      2.1481
_cell_volume                     5499.6(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47336
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_recrystallization_method CH2Cl2/Et2O
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.616
_refine_diff_density_min         -1.909
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         10216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0563P)^2^+15.7213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                9482
_reflns_number_total             10216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501052g_si_002.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 4085091--4085092.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085091