Plausible PEPPSI catalysts for direct C–H functionalization of five-membered heterocyclic bioactive motifs: synthesis, spectral, X-ray crystallographic characterizations and catalytic activity
Bensalah, Donia; Mansour, Lamjed; Sauthier, Mathieu; Gurbuz, Nevin; Özdemir, Ismail; Beji, Lotfi; Gatri, Rafik; Hamdi, Naceur; RSC Advances 13 (2023) 31386–31410; doi:10.1039/D3RA06334H

data_7247684
_publ_section_title
;
 Plausible PEPPSI catalysts for direct C--H functionalization of
 five-membered heterocyclic bioactive motifs: synthesis, spectral, X-ray
 crystallographic characterizations and catalytic activity
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              31386
_journal_page_last               31410
_journal_paper_doi               10.1039/D3RA06334H
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C31 H40 Br2 N4 O Pd'
_chemical_formula_sum            'C31 H40 Br2 N4 O Pd'
_chemical_formula_weight         750.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-09-12 deposited with the CCDC.	2023-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.464(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7681(12)
_cell_length_b                   15.3486(11)
_cell_length_c                   17.0756(11)
_cell_measurement_reflns_used    2380
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      1.54
_cell_volume                     6383.4(7)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material
'OLEX2 (Dolomanov et al., 2009) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.8 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.827
_diffrn_reflns_theta_min         1.568
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_T_max  0.6781
_exptl_absorpt_correction_T_min  0.3240
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED32 (Stoe & Cie, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       prism
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.610
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3840
_reflns_number_total             6796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra06334h2.cif
_cod_data_source_block           db24
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7247684
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.252
_shelx_estimated_absorpt_t_max   0.670
_shelx_res_checksum              83621