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_7712580
_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_moiety         'C38 H46 Cl2 O P2 Pd'
_chemical_formula_sum            'C38 H46 Cl2 O P2 Pd'
_chemical_formula_weight         757.99
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-12-28 deposited with the CCDC.	2023-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                97.385(2)
_cell_angle_beta                 94.546(2)
_cell_angle_gamma                110.352(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6484(5)
_cell_length_b                   10.6341(6)
_cell_length_c                   18.3612(10)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.597
_cell_measurement_theta_min      3.309
_cell_volume                     1736.00(17)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36109
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.605
_diffrn_reflns_theta_min         3.309
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         9733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.6911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8774
_reflns_number_total             9733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00033h2.cif
_cod_data_source_block           hhh005
_cod_original_cell_volume        1736.00(16)
_cod_database_code               7712580
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.875
_shelx_res_checksum              7150