Intramolecular Redox-Active Ligand-to-Substrate Single-Electron Transfer: Radical Reactivity with a Palladium(II) Complex.
Broere, Daniël L J; de Bruin, Bas; Reek, Joost N. H.; Lutz, Martin; Dechert, Sebastian; van der Vlugt, Jarl Ivar; Journal of the American Chemical Society 136 (2014) 11574–11577; doi:10.1021/ja502164f

data_4122056
_publ_section_title
;
 Intramolecular Redox-Active Ligand-to-Substrate Single-Electron Transfer:
 Radical Reactivity with a Palladium(II) Complex.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11574
_journal_page_last               11577
_journal_paper_doi               10.1021/ja502164f
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C22 H30 Cl N2 O Pd, C10 H10 Co, C6 H6, 0.5(O)'
_chemical_formula_sum            'C38 H46 Cl Co N2 O1.5 Pd'
_chemical_formula_weight         755.55
_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
_cell_angle_alpha                98.706(5)
_cell_angle_beta                 90.011(5)
_cell_angle_gamma                117.738(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0399(5)
_cell_length_b                   9.7093(5)
_cell_length_c                   23.0313(13)
_cell_measurement_reflns_used    20629
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.679
_cell_measurement_theta_min      1.795
_cell_volume                     1762.79(18)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         1.795
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.9269
_exptl_absorpt_correction_T_min  0.8127
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.530
_refine_diff_density_min         -2.116
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+4.5408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5858
_reflns_number_total             6630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502164f_si_003.cif
_cod_data_source_block           jarl-db
_cod_depositor_comments
'Adding full bibliography for 4122055--4122056.cif.'
_cod_original_formula_sum        'C38 H46 Cl Co N2 O1.50 Pd'
_cod_database_code               4122056
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.899
_shelxl_version_number           2013-4
_shelx_res_checksum              95322
_shelx_hkl_checksum              31608