Cyclopalladated complexes containing 2-C6R4PPh2 ligands (R = H, F): one-electron electrochemical reduction leading to metal-carbon σ-bond cleavage via palladium(i).
Kar, Gopa; Privér, Steven H; Jones, Lathe A.; Guo, Si-Xuan; Torriero, Angel A. J.; Bond, Alan M.; Bennett, Martin A.; Bhargava, Suresh K.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3367–3377; doi:10.1039/c4dt03268c

data_7033756
_publ_section_title
;
 Cyclopalladated complexes containing 2-C6R4PPh2 ligands (R = H, F):
 one-electron electrochemical reduction leading to metal-carbon \s-bond
 cleavage via palladium(i).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3367
_journal_page_last               3377
_journal_paper_doi               10.1039/c4dt03268c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C23 H11 F10 O2 P Pd'
_chemical_formula_sum            'C23 H11 F10 O2 P Pd'
_chemical_formula_weight         646.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-09-16 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                75.895(2)
_cell_angle_beta                 78.581(2)
_cell_angle_gamma                82.601(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3594(9)
_cell_length_b                   14.5809(12)
_cell_length_c                   14.5984(12)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.43
_cell_volume                     2290.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51891
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.149
_diffrn_reflns_theta_min         1.809
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       needle
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: isopentane'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.1309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8766
_reflns_number_total             11173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03268c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7033756--7033759.cif.'
_cod_database_code               7033756
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2013-4
_shelx_res_checksum              70550
_shelx_hkl_checksum              98891