Highly Efficient and Well-Defined Phosphinous Acid-Ligated Pd(II) Precatalysts for Hirao Cross-Coupling Reaction
Hong, Li-Hui; Feng, Wei-Jung; Chen, Wei-Chih; Chang, Yu-Chang; Dalton Transactions  (2023) –; doi:10.1039/D3DT00033H

data_7712582
_publ_section_title
;
 Highly Efficient and Well-Defined Phosphinous Acid-Ligated Pd(II)
 Precatalysts for Hirao Cross-Coupling Reaction
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00033H
_journal_year                    2023
_chemical_formula_sum            'C26 H23 O P'
_chemical_formula_weight         382.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-12-28 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                77.950(2)
_cell_angle_beta                 88.0780(19)
_cell_angle_gamma                79.4227(18)
_cell_formula_units_Z            2
_cell_length_a                   9.3661(5)
_cell_length_b                   9.7124(5)
_cell_length_c                   11.4886(5)
_cell_measurement_reflns_used    11211
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8855
_cell_measurement_theta_min      2.5255
_cell_volume                     1004.68(9)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21500
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.909
_diffrn_reflns_theta_min         2.532
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+1.4732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4030
_reflns_number_total             4787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00033h2.cif
_cod_data_source_block           lhh004
_cod_database_code               7712582
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              82569