Semi-heterogeneous dual iron/photocatalytic decarboxylative C(sp3)–C(sp3) cross-coupling via radical sorting
Sun, Yajun; Kang, Tengfei; Feng, Yingdi; Sun, Huaming; Song, Geyang; Xue, Dong; Green Chemistry 28 (2026) 3270–3278; doi:10.1039/D5GC05705A

data_7251604
_publ_section_title
;
 Semi-heterogeneous dual iron/photocatalytic decarboxylative
 C(sp3)--C(sp3) cross-coupling via radical sorting
;
_journal_issue                   7
_journal_name_full               'Green Chemistry'
_journal_page_first              3270
_journal_page_last               3278
_journal_paper_doi               10.1039/D5GC05705A
_journal_volume                  28
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H38 O'
_chemical_formula_sum            'C32 H38 O'
_chemical_formula_weight         438.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-10 deposited with the CCDC.	2026-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2977(4)
_cell_length_b                   14.2719(9)
_cell_length_c                   27.7472(18)
_cell_measurement_reflns_used    9471
_cell_measurement_temperature    229.00
_cell_measurement_theta_max      68.235
_cell_measurement_theta_min      3.186
_cell_volume                     2493.9(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      229.00
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            45421
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.304
_diffrn_reflns_theta_min         3.185
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0958 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.9082.
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    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.115
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 1855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.3561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4448
_reflns_number_total             4510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc05705a2.cif
_cod_data_source_block           s
_cod_database_code               7251604
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.861
_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 Ternary CH refined with riding coordinates:
 C002(H002), C003(H003), C004(H004), C006(H006)
2.b Secondary CH2 refined with riding coordinates:
 C00A(H00A,H00B), C00B(H00C,H00D), C00G(H00I,H00J), C00H(H00K,H00L), C00J(H00P,
 H00Q), C00N(H00U,H00V), C00O(H00W,H00X), C00S(H00,H), C00T(H1,HA)
2.c Aromatic/amide H refined with riding coordinates:
 C00F(H00H), C00K(H00R), C00L(H00S), C00M(H00T), C00P(H00Y), C00R(H00Z),
 C00U(H2), C00V(H3), C00W(H4), C00X(H5)
2.d Idealised Me refined as rotating group:
 C00C(H00E,H00F,H00G), C00I(H00M,H00N,H00O)
;
_shelx_res_checksum              47452
_shelx_hkl_checksum              25041
_olex2_submission_special_instructions 'No special instructions were received'