Oxidative cyclization of active methylene amides: efficient synthesis of functionalized 3-azabicyclo[<i>n</i>.1.0]alkanes.
Nemichand, ?; Waghmode, Amol G.; Awchar, Vilas M.; Baskaran, Sundarababu; Chemical communications (Cambridge, England)  (2025) –; doi:10.1039/d5cc05248c

data_7135186
_publ_section_title
;
 Oxidative cyclization of active methylene amides: efficient synthesis of
 functionalized 3-azabicyclo[<i>n</i>.1.0]alkanes.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d5cc05248c
_journal_year                    2025
_chemical_formula_sum            'C23 H23 Cl2 N O4'
_chemical_formula_weight         448.32
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-05-29 deposited with the CCDC.	2025-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   29.7421(16)
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_cell_measurement_temperature    296(2)
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_cell_volume                     4369.5(4)
_computing_cell_refinement       'Bruker SAINT'
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_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.290
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_exptl_crystal_size_min          0.040
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_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3840
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_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0470P)^2^+2.3172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             3840
_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              58257
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