Construction of robust Cu-MOFs from bifunctional pyridine-hydroxamate linkers for photocatalytic CO<sub>2</sub> reduction.
Xiong, Li; Tang, Wenlei; Xiong, Chaozhi; Du, Jiajun; Zhang, Zhiyuan; Qiu, Yuqing; Shao, Zhen-Wu; Zhou, Xuemei; Liu, Chong; Chemical communications (Cambridge, England) 61 (2025) 4030–4033; doi:10.1039/d4cc06778a

data_7134253
_publ_section_title
;
 Construction of robust Cu-MOFs from bifunctional pyridine-hydroxamate
 linkers for photocatalytic CO<sub>2</sub> reduction.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4030
_journal_page_last               4033
_journal_paper_doi               10.1039/d4cc06778a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C48 H40 Cu10 N16 O20, H4 O2'
_chemical_formula_sum            'C48 H44 Cu10 N16 O22'
_chemical_formula_weight         1832.39
_chemical_name_systematic        SUM-23A
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-12-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-01-25 deposited with the CCDC.	2025-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1107(2)
_cell_length_b                   23.1107(2)
_cell_length_c                   18.0067(4)
_cell_measurement_reflns_used    9752
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      79.58
_cell_measurement_theta_min      4.93
_cell_volume                     9617.5(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74193
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.010
_diffrn_reflns_theta_min         2.704
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.849
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0664 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8758.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0458P)^2^+21.1737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4958
_reflns_number_total             5155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06778a2.cif
_cod_data_source_block           SUM-23A
_cod_depositor_comments
'Adding full bibliography for 7134253--7134255.cif.'
_cod_original_cell_volume        9617.5(3)
_cod_database_code               7134253
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.764
_shelx_estimated_absorpt_t_min   0.708
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(4)
 0.05(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Cu2-O6 \\sim Cu2-O6A
 with sigma of 0.02
 Cu1-O7 \\sim Cu1-O7A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O7 \\sim O7A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O6A \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O7) \\sim Ueq, Uanis(O7A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O6A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: O6A(0.5) H6AA(0.5) H6AB(0.5) O7(0.25) H7A(0.25) H7B(0.25) O6(0.5)
 H6A(0.5) H6B(0.5) O7A(0.25) H7AA(0.25) H7AB(0.25)
6.a Riding coordinates:
 O6A(H6AA,H6AB), O7(H7A,H7B), O6(H6A,H6B), O7A(H7AA,H7AB)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C3(H3), C6(H6), C11(H11), C12(H12), C4(H4), C5(H5)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1094 electrons were 
found in a volume of 4366\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 27.4[H2O] per Formula Unit 
which account for 1095 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              229
_shelx_hkl_checksum              76272
_shelx_fab_checksum              74942
_olex2_submission_special_instructions 'No special instructions were received'