Preparation of carboxylic arylphosphines by hydrolysis of the trifluoromethyl group
Herrera, Daniel; Peral, Daniel; Bayón, J. Carles; RSC Advances 12 (2022) 7103–7114; doi:10.1039/D2RA00420H

data_7244562
_publ_section_title
;
 Preparation of carboxylic arylphosphines by hydrolysis of the
 trifluoromethyl group
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              7103
_journal_page_last               7114
_journal_paper_doi               10.1039/D2RA00420H
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C45 H32 Cl2 F12 O5 P2 Pd'
_chemical_formula_weight         1119.94
_chemical_name_common            'bis(p-Miranphos)palladium(II) dichloride'
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3938(7)
_cell_length_b                   15.6175(8)
_cell_length_c                   20.4211(10)
_cell_measurement_reflns_used    5981
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.185
_cell_measurement_theta_min      2.195
_cell_volume                     4871.8(4)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.13
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38513
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.804
_diffrn_reflns_theta_min         1.333
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2.05'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.39
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.862
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         11872
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0625P)^2^+2.6369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8672
_reflns_number_total             11872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra00420h2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7244562
_shelxl_version_number           2014-3
_shelx_res_checksum              84333