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_7248371
_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 Na3.3 Ni0.576 O51 U1, 4.5(O)'
_chemical_formula_sum            'H29.7 Mo12 Na3.3 Ni0.58 O55.5 U'
_chemical_formula_weight         2416.94
_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                   25.9532(8)
_cell_length_b                   25.9532(8)
_cell_length_c                   25.9532(8)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.458
_cell_measurement_theta_min      2.937
_cell_volume                     17481.3(9)
_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      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            23550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         2.719
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.426
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1427 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.7949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.673
_exptl_crystal_description       block
_exptl_crystal_F_000             17954
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.791
_refine_diff_density_min         -2.372
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3353
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0164P)^2^+223.2881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3160
_reflns_number_total             3353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4gc00877d2.cif
_cod_data_source_block           Ni1
_cod_depositor_comments
'Adding full bibliography for 7248368--7248371.cif.'
_cod_original_cell_volume        17481.3(16)
_cod_original_formula_sum        'H29.70 Mo12 Na3.30 Ni0.58 O55.50 U'
_cod_database_code               7248371
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.423
_shelx_estimated_absorpt_t_min   0.348
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Na2) \\sim Ueq, Uanis(Na1) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O16A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
2. Others
 Fixed Sof: Ni1(0.192) Na1(0.76667) Na2(0.33333) O16(0.65) O16A(0.35)
 O17(0.65) O17A(0.35)
;
_shelx_res_checksum              92898
_olex2_submission_special_instructions 'No special instructions were received'