Bifunctional ligands in combination with phosphines and Lewis acidic phospheniums for the carbonylative Sonogashira reaction
Chen Tan; Peng Wang; Huan Liu; Xiao-Li Zhao; Yong Lu; Ye Liu; Chem.Commun. 51 (2015) 10871–; doi:10.1039/C5cc03697F

data_7117384
_publ_section_title
;
 Bifunctional ligands in combination with phosphines and Lewis acidic
 phospheniums for the carbonylative Sonogashira reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              10871
_journal_paper_doi               10.1039/C5cc03697F
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration .
_chemical_formula_sum            'C27 H21 Cl2 I N P2 Pd'
_chemical_formula_weight         725.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.413(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2622(7)
_cell_length_b                   18.5110(15)
_cell_length_c                   9.5911(8)
_cell_measurement_temperature    296(2)
_cell_volume                     1520.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17622
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.8460
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.799
_refine_diff_density_min         -1.798
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5326
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0727
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1714P)^2^+2.3864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                4853
_reflns_number_total             5326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc03697f2.cif
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7117384