Non-directed Pd-catalysed electrooxidative olefination of arenes
Panja, Subir; Ahsan, Salman; Pal, Tanay; Kolb, Simon; Ali, Wajid; Sharma, Sulekha; Das, Chandan; Grover, Jagrit; Dutta, Arnab; Werz, Daniel B.; Paul, Amit; Maiti, Debabrata; Chemical Science 13 (2022) 9432–9439; doi:10.1039/D2SC03288K

data_1567429
_publ_section_title
;
 Non-directed Pd-catalysed electrooxidative olefination of arenes
;
_journal_issue                   32
_journal_name_full               'Chemical Science'
_journal_page_first              9432
_journal_page_last               9439
_journal_paper_doi               10.1039/D2SC03288K
_journal_volume                  13
_journal_year                    2022
_chemical_formula_sum            'C20 H12 Cl4 N8 Na2 O14 Pd'
_chemical_formula_weight         882.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-06 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_c                   35.708(4)
_cell_measurement_reflns_used    4678
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.8
_cell_volume                     6088.3(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Axs Kappa Apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1294
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            31132
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.208
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_description       block
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.229
_refine_diff_density_min         -2.777
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.00021(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         5284
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1709
_refine_ls_R_factor_gt           0.1177
_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^)+(0.0354P)^2^+264.2243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3391
_reflns_number_total             5284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03288k2.cif
_cod_data_source_block           DMAJ241
_cod_depositor_comments          'Adding full bibliography for 1567429.cif.'
_cod_original_cell_volume        6088.2(9)
_cod_database_code               1567429
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.814
_shelx_estimated_absorpt_t_max   0.856
_shelx_res_checksum              41763
_shelx_hkl_checksum              37586