Synthesis and reductive elimination of arylPd(ii) trifluoromethyl complexes: a remarkable concentration effect on chemoselectivity.
Zhang, Song-Lin; Deng, Zhu-Qin; Physical chemistry chemical physics : PCCP 18 (2016) 32664–32667; doi:10.1039/c6cp07093k

data_7227137
_publ_section_title
;
 Synthesis and reductive elimination of arylPd(ii) trifluoromethyl
 complexes: a remarkable concentration effect on chemoselectivity.
;
_journal_issue                   48
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              32664
_journal_page_last               32667
_journal_paper_doi               10.1039/c6cp07093k
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C47 H40 F6 O3 P2 Pd'
_chemical_formula_sum            'C47 H40 F6 O3 P2 Pd'
_chemical_formula_weight         935.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.725(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5019(10)
_cell_length_b                   9.8634(5)
_cell_length_c                   25.5915(15)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.40
_cell_volume                     4184.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            118559
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.078
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+34.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                6489
_reflns_number_total             7777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cp07093k2.cif
_cod_data_source_block           jiang150401den_0m_a
_cod_depositor_comments          'Adding full bibliography for 7227137.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7227137