Highly-stable Silverton-type UIV-containing polyoxomolybdate frameworks for the heterogeneous catalytic synthesis of quinazolinones
Li, Ke; Liu, Yufeng; Yang, Guoping; Zheng, Zhijian; Lin, Xiaoling; Zhang, Zhibin; Li, Shujun; Liu, Yunhai; Wei, Yongge; Green Chemistry 26 (2024) 6454–6460; doi:10.1039/D4GC00877D

data_7248368
_publ_section_title
;
 Highly-stable Silverton-type UIV-containing polyoxomolybdate frameworks
 for the heterogeneous catalytic synthesis of quinazolinones
;
_journal_issue                   11
_journal_name_full               'Green Chemistry'
_journal_page_first              6454
_journal_page_last               6460
_journal_paper_doi               10.1039/D4GC00877D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'Fe1 Mo12 Na3 O51 U1, 4.5(O)'
_chemical_formula_sum            'Fe H30 Mo12 Na3 O55.5 U'
_chemical_formula_weight         2432.37
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-07-20 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.0130(2)
_cell_length_b                   26.0130(2)
_cell_length_c                   26.0130(2)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.053
_cell_measurement_theta_min      2.217
_cell_volume                     17602.4(2)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18752
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.013
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_min         1.918
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.450
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0444 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.9325.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.671
_exptl_crystal_description       block
_exptl_crystal_F_000             18064
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2600
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0144P)^2^+283.1758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2465
_reflns_number_total             2600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4gc00877d2.cif
_cod_data_source_block           Fe1
_cod_depositor_comments
'Adding full bibliography for 7248368--7248371.cif.'
_cod_original_cell_volume        17602.4(4)
_cod_original_formula_sum        'Fe H30 Mo12 Na3 O55.50 U'
_cod_database_code               7248368
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O16) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O17A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Na2) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(Mo1A) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of
0.001
2. Others
 Fixed Sof: Mo1(0.962) Na1(0.8) Na2(0.2) O16(0.7) O16A(0.3) O17(0.7) O17A(0.3)
 Mo1A(0.038)
;
_shelx_res_checksum              17242
_olex2_submission_special_instructions 'No special instructions were received'