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_7248369
_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         'Mo12 Na5.8 O54 U, 1.5(O)'
_chemical_formula_sum            'H29.2 Mo12 Na5.8 O55.5 U'
_chemical_formula_weight         2440.08
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.0319(3)
_cell_length_b                   19.0319(3)
_cell_length_c                   11.4460(5)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.294
_cell_measurement_theta_min      2.167
_cell_volume                     3590.45(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11019
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         2.140
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.584
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1481 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.6383.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.386
_exptl_crystal_description       block
_exptl_crystal_F_000             3399
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1985
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0211P)^2^+28.3595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1918
_reflns_number_total             1985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4gc00877d2.cif
_cod_data_source_block           naumo12
_cod_depositor_comments
'Adding full bibliography for 7248368--7248371.cif.'
_cod_original_cell_volume        3590.45(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'H29.20 Mo12 Na5.80 O55.50 U'
_cod_database_code               7248369
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.621
_shelx_estimated_absorpt_t_min   0.459
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O9A) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O8A) \\sim Ueq, Uanis(O8B)
\\sim Ueq, Uanis(O8C) \\sim Ueq, Uanis(O8D) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(Na2) \\sim Ueq, Uanis(Na2A) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
2. Others
 Fixed Sof: Na2(0.5) Na2A(0.3) O8(0.45) O8C(0.2) O8D(0.1) O9(0.75) O9A(0.25)
 O8A(0.25) O8B(0.25)
;
_shelx_res_checksum              92163
_olex2_submission_special_instructions 'No special instructions were received'