Diastereoselective construction of complex spiroheterocycles via γ-C(sp3)–H functionalization of 1,1-disubstituted cyclohexanes with diverse bifunctional reagents
Mutra, Mohana Reddy; Chandana, T. L.; Chen, Hsing-Yin; Wang, Yun-Jou; Wang, Jeh-Jeng; Green Chemistry 28 (2026) 5753–5766; doi:10.1039/D5GC06338H

data_7251771
_publ_section_title
;
 Diastereoselective construction of complex spiroheterocycles via
 \g-C(sp3)--H functionalization of 1,1-disubstituted cyclohexanes with
 diverse bifunctional reagents
;
_journal_issue                   13
_journal_name_full               'Green Chemistry'
_journal_page_first              5753
_journal_page_last               5766
_journal_paper_doi               10.1039/D5GC06338H
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C31 H33 N O5 S2'
_chemical_formula_sum            'C31 H33 N O5 S2'
_chemical_formula_weight         563.70
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2026-02-04 deposited with the CCDC.	2026-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.7640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9254(8)
_cell_length_b                   20.1083(8)
_cell_length_c                   17.3647(7)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.73
_cell_volume                     5636.9(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61998
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0808P)^2^+14.0167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4389
_reflns_number_total             4950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc06338h2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7251770--7251775.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7251771
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              64909