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_1574674
_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 N3 O10 Zr, C14 H6 N2 O6, 1.8[C3H7NO]'
_chemical_formula_sum            'C35 H12 N5 O16 Zr'
_chemical_formula_weight         849.72
_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             2024-03-21
_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                 102.996(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6563(15)
_cell_length_b                   21.5556(19)
_cell_length_c                   11.8123(12)
_cell_measurement_reflns_used    4470
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.22
_cell_volume                     3636.2(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19175
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.219
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6737
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1215 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.9038.
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    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         6343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0790P)^2^+15.4023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4751
_reflns_number_total             6343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01242b2.cif
_cod_data_source_block           '__tmp___sq'
_cod_depositor_comments
'Adding full bibliography for 1574674--1574675.cif.'
_cod_database_code               1574674
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00Z(H00Z), C013(H013), C017(H017), C018(H018), C019(H019),
 C01C(H01C), C01H(H01H), C01K(H01K), C01M(H01M)
2.b Idealised tetrahedral OH refined as rotating group:
 O00D(H00D), O00H(H00H)
;
_shelx_res_checksum              50729
_shelx_fab_checksum              80725
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'