Beckmann rearrangement of ketoximes for accessing amides and lactams promoted by a perimidine-2-thione supported Hg(ii) complex: a mechanistic perception
Velmurugan, Priyanka; Kanniyappan, Poovarasan; Ghatak, Tapas; RSC Advances 15 (2025) 24317–24330; doi:10.1039/D5RA02843D

data_7250679
_publ_section_title
;
 Beckmann rearrangement of ketoximes for accessing amides and lactams
 promoted by a perimidine-2-thione supported Hg(ii) complex: a mechanistic
 perception
;
_journal_issue                   30
_journal_name_full               'RSC Advances'
_journal_page_first              24317
_journal_page_last               24330
_journal_paper_doi               10.1039/D5RA02843D
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C28 H28 Cl2 Hg N4 S2, C2 H6 O S'
_chemical_formula_sum            'C30 H34 Cl2 Hg N4 O S3'
_chemical_formula_weight         834.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-04-23 deposited with the CCDC.	2025-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                74.558(2)
_cell_angle_beta                 76.599(2)
_cell_angle_gamma                79.748(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2166(7)
_cell_length_b                   13.6839(9)
_cell_length_c                   13.6960(9)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.51
_cell_volume                     1607.14(19)
_computing_cell_refinement       'Bruker APEX4/SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker APEX4/SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  ?\
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44824
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.300
_diffrn_reflns_theta_min         1.935
_diffrn_source                   'i-mu-s microfocus source'
_exptl_absorpt_coefficient_mu    5.180
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BRUKER)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.969
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0886P)^2^+3.0316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4532
_reflns_number_total             7971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra02843d2.cif
_cod_data_source_block           VP_8_Tol_220523_0m_a
_cod_database_code               7250679
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.345
_shelx_estimated_absorpt_t_max   0.569
_shelx_res_checksum              48612