Secondary phosphine oxide-triggered selective oxygenation of a benzyl ligand on palladium.
Oka, Sayaka; Shigehiro, Yuma; Kataoka, Yasutaka; Ura, Yasuyuki; Chemical communications (Cambridge, England) 56 (2020) 12977–12980; doi:10.1039/d0cc05572g

data_7127277
_publ_section_title
;
 Secondary phosphine oxide-triggered selective oxygenation of a benzyl
 ligand on palladium.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12977
_journal_page_last               12980
_journal_paper_doi               10.1039/d0cc05572g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C48 H42 Cl2 O4 P4 Pd2'
_chemical_formula_weight         1090.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-03-13 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                68.772(6)
_cell_angle_beta                 78.937(8)
_cell_angle_gamma                63.277(5)
_cell_formula_units_Z            2
_cell_length_a                   11.8642(15)
_cell_length_b                   13.1675(15)
_cell_length_c                   17.343(2)
_cell_measurement_reflns_used    6798
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.2689
_cell_measurement_theta_min      1.8242
_cell_volume                     2254.4(5)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'Mercury 3.10.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17758
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.9783
_exptl_absorpt_correction_T_min  0.8097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DTABSCOR
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/hexane'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         9460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+1.6539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                7335
_reflns_number_total             9460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cc05572g2.cif
_cod_data_source_block           complex_2a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7127277--7127278.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7127277