Achieving highly efficient carbon radical-mediated cross-coupling reaction in a confined radical microenvironment within a metal–organic framework
Li, Ying-Lin; Li, Ning; Mei, Zhi-Bin; Li, Jun-Rong; Yao, Su-Juan; Yu, Fei; Li, Shun-Li; Lin, Jiao-Min; Liu, Jiang; Lan, Ya-Qian; Chemical Science 16 (2025) 11939–11948; doi:10.1039/D5SC01242B

data_1574675
_publ_section_title
;
 Achieving highly efficient carbon radical-mediated cross-coupling
 reaction in a confined radical microenvironment within a metal--organic
 framework
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              11939
_journal_page_last               11948
_journal_paper_doi               10.1039/D5SC01242B
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C21 H6 Hf0.986 N3 O10, C14 H6 N2 O6, C3 H7 N O, 0.6[C3H7NO]'
_chemical_formula_sum            'C38 H19 Hf0.99 N6 O17'
_chemical_formula_weight         1008.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-27 deposited with the CCDC.	2025-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.015(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6361(14)
_cell_length_b                   21.520(2)
_cell_length_c                   11.8409(13)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.22
_cell_volume                     3633.7(6)
_computing_cell_refinement       Zr9L3
_computing_data_reduction        Zr9L3
_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)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            72921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.003
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.935
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1568 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.8866.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_description       block
_exptl_crystal_F_000             1985
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.368
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+11.5693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6060
_reflns_number_total             6406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01242b2.cif
_cod_data_source_block           '__tmp___sq_CCDC1'
_cod_depositor_comments
'Adding full bibliography for 1574674--1574675.cif.'
_cod_original_cell_volume        3633.8(7)
_cod_database_code               1574675
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.720
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C00Y(H00Y), C012(H012), C013(H013), C014(H014), C019(H019),
 C01I(H01I), C01L(H01L), C01M(H01M), C01O(H01O), C01Q(H01Q)
2.b Idealised Me refined as rotating group:
 C01P(H01A,H01B,H01C), C01R(H01D,H01E,H01F)
2.c Idealised tetrahedral OH refined as rotating group:
 O00E(H00E), O00J(H00J)
;
_shelx_res_checksum              7841
_shelx_fab_checksum              59925
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'