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_4064113
_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         'C26 H34 Cl2 N4 O2 P2 Pd2'
_chemical_formula_sum            'C26 H34 Cl2 N4 O2 P2 Pd2'
_chemical_formula_weight         780.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.133(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4095(3)
_cell_length_b                   16.1661(6)
_cell_length_c                   19.8026(7)
_cell_measurement_reflns_used    13367
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.1451
_cell_measurement_theta_min      2.4117
_cell_volume                     3007.77(18)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 16.0690
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega 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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27250
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.8636
_exptl_absorpt_correction_T_min  0.7521
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                5497
_reflns_number_total             7262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101132t_si_001.cif
_cod_data_source_block           hong171m
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064113