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_7712581
_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            'C40 H62 Cl4 O2 P2 Pd2'
_chemical_formula_weight         991.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 105.1584(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7915(4)
_cell_length_b                   16.4016(5)
_cell_length_c                   12.2069(4)
_cell_measurement_reflns_used    26754
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.899
_cell_measurement_theta_min      3.0265
_cell_volume                     2278.67(13)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.992
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41419
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.898
_diffrn_reflns_theta_min         3.675
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+3.3768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4960
_reflns_number_total             5394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00033h2.cif
_cod_data_source_block           popd2ad_sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7712581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.841
_shelx_res_checksum              51148
_shelx_fab_checksum              30602