Preparation of New Buchwald-Type Secondary Phosphine Oxide Ligands and Applications in Suzuki−Miyaura Reactions
Hu, Dan-Fu; Weng, Chia-Ming; Hong, Fung-E; Organometallics 30 (2011) 1139–; doi:10.1021/om101132t

data_4064112
_publ_section_title
;
 Preparation of New Buchwald-Type Secondary Phosphine Oxide Ligands and
 Applications in Suzuki&#x2212;Miyaura Reactions
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1139
_journal_paper_doi               10.1021/om101132t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C28 H38 Br2 N4 O4 P2 Pd, 3(C H2 Cl2)'
_chemical_formula_sum            'C31 H44 Br2 Cl6 N4 O4 P2 Pd'
_chemical_formula_weight         1077.54
_chemical_name_systematic
; 
 ? 
;
_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                69.137(7)
_cell_angle_beta                 83.972(6)
_cell_angle_gamma                72.689(7)
_cell_formula_units_Z            2
_cell_length_a                   10.7115(8)
_cell_length_b                   13.4221(10)
_cell_length_c                   16.4598(12)
_cell_measurement_reflns_used    8063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1967
_cell_measurement_theta_min      2.8681
_cell_volume                     2111.1(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15913
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0.0(1)
_diffrn_standards_interval_count 20
_diffrn_standards_interval_time  20
_diffrn_standards_number         20
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78781
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       CUBIC
_exptl_crystal_F_000             1076.0
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                6802
_reflns_number_total             11498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101132t_si_001.cif
_cod_data_source_block           hong178m
_cod_database_code               4064112