<i>In situ</i> confinement of ultra-small metal nanoparticles in redox-active zirconium MOFs for catalysis.
Li, Fugang; Huang, Jinyi; Meng, Yuxuan; Li, Ji; Zhang, Liangliang; Sheng, Daopeng; Chemical communications (Cambridge, England) 60 (2024) 8708–8711; doi:10.1039/d4cc01976h

data_7133366
_publ_section_title
;
 <i>In situ</i> confinement of ultra-small metal nanoparticles in
 redox-active zirconium MOFs for catalysis.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8708
_journal_page_last               8711
_journal_paper_doi               10.1039/d4cc01976h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C68.5 H40 Eu6 F8 N4 O24.5, 1280[C3H7NO], 320[H2O]'
_chemical_formula_sum            'C68.5 H40 Eu6 F8 N4 O24.5'
_chemical_formula_weight         2374.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-08 deposited with the CCDC.	2024-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.893(3)
_cell_length_b                   30.475(4)
_cell_length_c                   31.958(5)
_cell_measurement_reflns_used    9611
_cell_measurement_temperature    168.00
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.27
_cell_volume                     19374(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      168.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1111
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            98114
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.269
_diffrn_source_current           1.6
_diffrn_source_power             0.08
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.814
_exptl_crystal_description       block
_exptl_crystal_F_000             4500
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.495
_refine_diff_density_min         -3.291
_refine_diff_density_rms         0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         4583
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.1510
_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^)+(0.0195P)^2^+7125.4561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3230
_refine_ls_wR_factor_ref         0.3461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3638
_reflns_number_total             4583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01976h2.cif
_cod_data_source_block           Eu
_cod_depositor_comments
'Adding full bibliography for 7133365--7133366.cif.'
_cod_original_cell_volume        19375(5)
_cod_original_formula_sum        'C68.50 H40 Eu6 F8 N4 O24.50'
_cod_database_code               7133366
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 11(10)
 -10(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 O1, O2, F2, F1, O5, O6, N1, C1, C10, C3, C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C2, O36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim F2 \\sim F1 \\sim O5 \\sim O6 \\sim N1 \\sim C1 \\sim C10
\\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9: within 3.7A
with sigma of 0.005 and sigma for terminal atoms of 0.001 within 3.7A
O36 \\sim C2 \\sim O5: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Others
 Fixed Sof: C2(0.0625) O36(0.0625)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9)
;
_shelx_res_checksum              12688
_shelx_hkl_checksum              96599
_olex2_submission_special_instructions 'No special instructions were received'