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_7250799
_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, H20 Li4 O10, 27[H2O]'
_chemical_formula_sum            'C32 H126 Li4 Mo8 N24 O57'
_chemical_formula_weight         2554.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-28
_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                 106.7668(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6874(2)
_cell_length_b                   19.52258(17)
_cell_length_c                   23.33101(19)
_cell_measurement_reflns_used    12959
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9450
_cell_measurement_theta_min      3.8640
_cell_volume                     10330.49(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.941
_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    -62.00  -3.00   1.00    2.24    --  -41.98  38.00  90.00   59
  2  \w    -65.00  28.00   1.00    2.24    --  -41.98  38.00-150.00   93
  3  \w     25.00  66.00   1.00    2.24    --   41.98-125.00 120.00   41
  4  \w     26.00  76.00   1.00    2.24    --   41.98-125.00 -30.00   50
  5  \w     59.00 115.00   1.00    8.96    --  110.54-125.00   0.00   56
  6  \w     91.00 132.00   1.00    8.96    --  110.54 -30.00 150.00   41
  7  \w    101.00 176.00   1.00    8.96    --  110.54  30.00   0.00   75
  8  \w     41.00 116.00   1.00    8.96    --  110.54-125.00-120.00   75
  9  \w     56.00 134.00   1.00    8.96    --  110.54 -45.00-120.00   78
 10  \w     66.00 176.00   1.00    8.96    --  110.54  15.00 120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0424228000
_diffrn_orient_matrix_UB_12      0.0236420000
_diffrn_orient_matrix_UB_13      -0.0352283000
_diffrn_orient_matrix_UB_21      0.0300169000
_diffrn_orient_matrix_UB_22      -0.0707996000
_diffrn_orient_matrix_UB_23      0.0093673000
_diffrn_orient_matrix_UB_31      -0.0437284000
_diffrn_orient_matrix_UB_32      -0.0256292000
_diffrn_orient_matrix_UB_33      -0.0585115000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19901
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.997
_diffrn_reflns_theta_min         3.257
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.000027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10176
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0643P)^2^+18.2775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8717
_reflns_number_total             10176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03010b2.cif
_cod_data_source_block           exp_20214_auto
_cod_original_cell_volume        10330.49(17)
_cod_database_code               7250799
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, All O(H,H) groups
2. Restrained distances
 H18-N00P \\sim N00P-N00L
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O017 \\sim O1L: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Li36 \\sim O017 \\sim Li1P \\sim O1L \\sim O14 \\sim O5 \\sim O37 \\sim O9:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O1L) \\sim Ueq, Uanis(O017) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O017) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O017) \\sim Ueq, Uanis(O1L) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O1L(0.5) H1LA(0.5) H1LB(0.5) O14(0.5) H14A(0.5) H14B(0.5)
5.a Riding coordinates:
 O006(H006), O18(H18)
5.b Rotating group:
 O017(H01V,H01W), O5(H5A,H5B), O9(H9A,H9B)
5.c Secondary CH2 refined with riding coordinates:
 O1L(H1LA,H1LB)
5.d X=CH2 refined with riding coordinates:
 O14(H14A,H14B), O37(H37A,H37B)
5.e Idealised Me refined as rotating group:
 C00V(H00C,H00B,H00A), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C013(H01G,
 H01H,H01I), C015(H01J,H01K,H01L), C016(H01M,H01N,H01O), C01A(H01P,H01Q,H01R),
 C01B(H01S,H01T,H01U)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45749
_shelx_fab_checksum              62945
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.047
_oxdiff_exptl_absorpt_empirical_full_min 0.657