Construction of octanuclear polyoxomolybdenum(v)-based porous materials with lithium additives
Liu, Cheng; Xie, Zhen-Lang; Dong, Xin; Jin, Wan-Ting; Lian, Yi-Xin; Zhou, Zhao-Hui; RSC Advances 15 (2025) 30062–30070; doi:10.1039/D5RA03010B

data_7250800
_publ_section_title
;
 Construction of octanuclear polyoxomolybdenum(v)-based porous materials
 with lithium additives
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              30062
_journal_page_last               30070
_journal_paper_doi               10.1039/D5RA03010B
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C32 H52 Mo8 N24 O20, 4.8[NH4], 61.6[H2O]'
_chemical_formula_sum            'C32 H52 Mo8 N24 O20'
_chemical_formula_weight         1860.49
_chemical_name_systematic        'MO with NH4'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-04-14 deposited with the CCDC.	2025-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            10
_cell_length_a                   29.8259(3)
_cell_length_b                   46.5268(6)
_cell_length_c                   24.3732(3)
_cell_measurement_reflns_used    21411
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      68.3220
_cell_measurement_theta_min      2.9580
_cell_volume                     33734.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00 -75.00   1.00    2.50    --  -41.98 -57.00-150.00   35
  2  \w    -91.00  -2.00   1.00    2.50    --  -41.98 125.00 120.00   89
  3  \w     23.00  89.00   1.00    2.50    --   41.98-125.00 120.00   66
  4  \w      4.00  30.00   1.00    2.50    --   41.98 -99.00 150.00   26
  5  \w    134.00 163.00   1.00   11.00    --   95.52 125.00  30.00   29
  6  \w     22.00  79.00   1.00   11.00    --   95.52 -30.00  90.00   57
  7  \w     22.00  99.00   1.00   11.00    --   95.52 -77.00 -60.00   77
  8  \w     25.00 121.00   1.00   11.00    --   95.52 -61.00   0.00   96
  9  \w     76.00 128.00   1.00   11.00    --   95.52  45.00   0.00   52
 10  \w     72.00 146.00   1.00   11.00    --   95.52  30.00 -60.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62493
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.089
_diffrn_reflns_theta_max         65.089
_diffrn_reflns_theta_min         2.608
_exptl_absorpt_coefficient_mu    6.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.916
_exptl_crystal_description       block
_exptl_crystal_F_000             9080
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         28854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0584P)^2^+217.2748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18538
_reflns_number_total             28854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03010b2.cif
_cod_data_source_block           exp_20101_auto
_cod_database_code               7250800
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.575
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
3.a Riding coordinates:
 O11(H11), O16(H16), O23(H23), O2(H2), O6(H6)
3.b Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C21(H21a,H21b,H21c), C25(H25a,H25b,H25c), C28(H28a,H28b,
 H28c), C29(H29a,H29b,H29c), C32(H32a,H32b,H32c), C17(H17a,H17b,H17c), C20(H20a,
 H20b,H20c), C37(H37a,H37b,H37c), C33(H33a,H33b,H33c), C40(H40a,H40b,H40c),
 C36(H36a,H36b,H36c), C13(H13a,H13b,H13c), C16(H16a,H16b,H16c), C12(H12a,H12b,
 H12c), C9(H9a,H9b,H9c), C1(H1a,H1b,H1c), C4(H4a,H4b,H4c), C8(H8a,H8b,H8c),
 C5(H5a,H5b,H5c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 6628 electrons were 
found in a volume of 21476\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[NH4], 62.4[H2O] per Asymmetric Unit 
which account for 6680 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1756
_shelx_fab_checksum              33151
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;