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_7033758
_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
'C41 H26 F10 O2 P2 Pd, 0.48(C6 H6) 0.11(C6 H14)'
_chemical_formula_sum            'C44.52 H30.36 F10 O2 P2 Pd'
_chemical_formula_weight         955.57
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 92.097(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6907(10)
_cell_length_b                   11.8192(9)
_cell_length_c                   25.115(2)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.43
_cell_volume                     4061.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 2008)'
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38724
_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         26.476
_diffrn_reflns_theta_min         1.623
_exptl_absorpt_coefficient_mu    0.620
_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    1.563
_exptl_crystal_description       needle
_exptl_crystal_F_000             1918
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/hexane'
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8374
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0322P)^2^+3.1557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6639
_reflns_number_total             8374
_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_original_cell_volume        4061.3(5)
_cod_database_code               7033758
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2013-4
_shelx_res_checksum              39398
_shelx_hkl_checksum              81561