EnT-catalysis-enabled, radical-relay cascade cyclization to access multisubstituted cyclohexane/cyclohexene.
Xiang, Mei; Huang, Cong; Gao, Jie; Chen, Kai; Xie, Zhen-Zhen; Yang, Hua; Chemical communications (Cambridge, England) 62 (2026) 1941–1944; doi:10.1039/d5cc06259d

data_7135509
_publ_section_title
;
 EnT-catalysis-enabled, radical-relay cascade cyclization to access
 multisubstituted cyclohexane/cyclohexene.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1941
_journal_page_last               1944
_journal_paper_doi               10.1039/d5cc06259d
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C39 H37 N O4 S2'
_chemical_formula_sum            'C39 H37 N O4 S2'
_chemical_formula_weight         647.81
_chemical_name_systematic        XM-2
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-16
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-08-14 deposited with the CCDC.	2025-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                109.2000(10)
_cell_angle_beta                 98.0810(10)
_cell_angle_gamma                104.6550(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1879(6)
_cell_length_b                   12.0483(6)
_cell_length_c                   16.9670(8)
_cell_measurement_reflns_used    8504
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.605
_cell_measurement_theta_min      2.464
_cell_volume                     2025.94(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  BrukerD8Quest
_diffrn_measurement_method       none
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27165
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         2.234
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.8504.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_preparation       NONE
_exptl_crystal_recrystallization_method NONE
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0084(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0487P)^2^+1.7170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4742
_reflns_number_total             7040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06259d2.cif
_cod_data_source_block           0613_5150_2_0m
_cod_database_code               7135509
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C21(H21a,H21b), C00E(H00a,H00b)
2.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00O(H00O), C00P(H00P), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C015(H015),
 C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B),
 C01C(H01C)
2.c Idealised Me refined as rotating group:
 C00L(H00c,H00d,H00e), C00M(H00f,H00g,H00h)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36733
_shelx_fab_checksum              25256
_olex2_exptl_crystal_mounting_method NONE
_olex2_submission_special_instructions 'No special instructions were received'