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_7250801
_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, 2(H8 Li O4), H14 Li2 O7, 2(C4 H7 N3), 20.5[H2O]'
_chemical_formula_sum            'C40 H137 Li4 Mo8 N30 O55.5'
_chemical_formula_weight         2722.07
_chemical_name_systematic        MO1
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2025-04-14 deposited with the CCDC.	2025-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                81.012(2)
_cell_angle_beta                 89.971(2)
_cell_angle_gamma                72.593(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3561(3)
_cell_length_b                   14.9592(4)
_cell_length_c                   27.3998(7)
_cell_measurement_reflns_used    18028
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      66.9380
_cell_measurement_theta_min      3.1380
_cell_volume                     5153.3(2)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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    -91.00 -10.00   1.00    1.02    --  -41.98 125.00-150.00   81
  2  \w   -115.00 -19.00   1.00    1.02    --  -41.98 -38.00  30.00   96
  3  \w   -109.00 -21.00   1.00    1.02    --  -41.98 -38.00 120.00   88
  4  \w     54.00  80.00   1.00    1.02    --   41.98  57.00 -30.00   26
  5  \w     34.00 117.00   1.00    4.10    --   91.68 -77.00 -30.00   83
  6  \w     90.00 117.00   1.00    4.10    --   91.68-125.00 120.00   27
  7  \w     17.00 115.00   1.00    4.10    --   91.68 -30.00 -60.00   98
  8  \w     22.00  80.00   1.00    4.10    --   91.68 -30.00 120.00   58
  9  \w     83.00 108.00   1.00    4.10    --   91.68-125.00-120.00   25
 10  \w     94.00 123.00   1.00    4.10    --   91.68 125.00 -30.00   29
 11  \w    128.00 158.00   1.00    4.10    --   91.68 125.00 -30.00   30
 12  \w    126.00 152.00   1.00    4.10    --   91.68 125.00  60.00   26
 13  \w     15.00 128.00   1.00    4.10    --   91.68 -15.00-180.00  113
 14  \w     26.00 115.00   1.00    4.10    --   91.68 -30.00  30.00   89
 15  \w     31.00 105.00   1.00    4.10    --   91.68 -94.00 -90.00   74
 16  \w     37.00 109.00   1.00    4.10    --   91.68 -77.00  90.00   72
;
_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      0.0044876000
_diffrn_orient_matrix_UB_12      0.0430732000
_diffrn_orient_matrix_UB_13      0.0471801000
_diffrn_orient_matrix_UB_21      0.0326274000
_diffrn_orient_matrix_UB_22      -0.1002451000
_diffrn_orient_matrix_UB_23      0.0310535000
_diffrn_orient_matrix_UB_31      0.1164596000
_diffrn_orient_matrix_UB_32      -0.0080001000
_diffrn_orient_matrix_UB_33      -0.0076123000
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34837
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        66.917
_diffrn_reflns_theta_max         66.917
_diffrn_reflns_theta_min         3.138
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64092
_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_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             2758
_exptl_crystal_preparation       1
_exptl_crystal_recrystallization_method 1
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         17849
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0461P)^2^+0.2275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14821
_reflns_number_total             17849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03010b2.cif
_cod_data_source_block           exp_21679_auto
_cod_original_formula_sum        'C40 H137 Li4 Mo8 N30 O55.50'
_cod_database_code               7250801
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 97.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O4W-H4WB = O4W-H4WA
 0.85 with sigma of 0.02
 O7W-H7WB = O7W-H7WA
 0.85 with sigma of 0.02
 O7W-H7WA = O7W-H7WB
 0.85 with sigma of 0.02
 O02G-H02A = O02G-H02B
 0.85 with sigma of 0.02
 Li4-H14A \\sim Li4-H14B
 with sigma of 0.02
 Li2-H5WA \\sim Li2-H5WB
 with sigma of 0.02
 N5-H9 \\sim N4-H9
 with sigma of 0.02
 N10-H10 \\sim N11-H10
 with sigma of 0.02
 N22-C22 \\sim N19-H12 \\sim N20-H12
 with sigma of 0.02
 N13-H11 \\sim N14-H11
 with sigma of 0.02
 Li3-H9WA \\sim Li3-H9WB
 with sigma of 0.02
 Li3-H10A \\sim Li3-H10B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 H10, N10, N11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N5, N4, H9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N19, N20, H12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 H11, N14, N13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4.a Riding coordinates:
 O9(H9), O11(H11), O12(H12), O10(H10), O8W(H8WA,H8WB), O1W(H1WA,H1WB),
 O7W(H7WA,H7WB), O5W(H5WA,H5WB)
4.b Free rotating group:
 O14W(H14A,H14B), O10W(H10A,H10B), O9W(H9WA,H9WB)
4.c Rotating group:
 O6W(H6WA,H6WB), O12W(H12A,H12B), O2W(H2WA,H2WB), O11W(H11A,H11B), O13W(H13A,
 H13B), O02G(H02A,H02B)
4.d Aromatic/amide H refined with riding coordinates:
 N28(H28)
4.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21936
_shelx_fab_checksum              65757
_olex2_exptl_crystal_mounting_method 1
_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 1.374
_oxdiff_exptl_absorpt_empirical_full_min 0.736