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_7250798
_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
'0.091(C32 Mo8 N24 O20), 0.182(C4 N3), 2.818[H2O]'
_chemical_formula_sum            'C40 H95 Li4 Mo8 N30 O34.5'
_chemical_formula_weight         2343.73
_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     iterative
_audit_creation_date             2024-11-12
_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                90.435(3)
_cell_angle_beta                 115.999(3)
_cell_angle_gamma                107.431(2)
_cell_formula_units_Z            1
_cell_length_a                   13.3591(3)
_cell_length_b                   14.9668(4)
_cell_length_c                   15.2348(6)
_cell_measurement_reflns_used    11797
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.0160
_cell_measurement_theta_min      3.7570
_cell_volume                     2577.61(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -88.00 -39.00   1.00    1.00    --  -41.98 -57.00  30.00   49
  2  \w    -86.00  -5.00   1.00    1.00    --  -41.98 125.00  60.00   81
  3  \w   -108.00 -16.00   1.00    1.00    --  -41.98 -57.00-180.00   92
  4  \w    -73.00  19.00   1.00    1.00    --  -41.98  77.00 -30.00   92
  5  \w     22.00 115.00   1.00    1.00    --   41.98  38.00 -60.00   93
  6  \w    141.00 167.00   1.00    2.43    --  110.54  77.00 -30.00   26
  7  \w     87.00 177.00   1.00    2.43    --  110.54  30.00 -30.00   90
  8  \w     43.00 140.00   1.00    2.43    --  110.54 -77.00-150.00   97
  9  \w     37.00 107.00   1.00    2.43    --  110.54 -30.00  30.00   70
 10  \w     46.00 117.00   1.00    2.43    --  110.54-125.00  60.00   71
 11  \w     37.00 129.00   1.00    2.43    --  110.54 -30.00 150.00   92
 12  \w     85.00 110.00   1.00    2.43    --  110.54  77.00 -30.00   25
 13  \w     40.00 123.00   1.00    2.43    --  110.54 -77.00  30.00   83
 14  \w     42.00 116.00   1.00    2.43    --  110.54-125.00-150.00   74
 15  \w    130.00 155.00   1.00    2.43    --  110.54 -15.00 -60.00   25
 16  \w     85.00 110.00   1.00    2.43    --  110.54-101.00-137.00   25
 17  \w     36.00 122.00   1.00    2.43    --  110.54 -15.00 -60.00   86
;
_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      -0.0279537000
_diffrn_orient_matrix_UB_12      -0.0078741000
_diffrn_orient_matrix_UB_13      -0.1097742000
_diffrn_orient_matrix_UB_21      0.0040631000
_diffrn_orient_matrix_UB_22      0.1039830000
_diffrn_orient_matrix_UB_23      0.0013876000
_diffrn_orient_matrix_UB_31      0.1333138000
_diffrn_orient_matrix_UB_32      0.0328408000
_diffrn_orient_matrix_UB_33      0.0307660000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17187
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.585
_diffrn_reflns_theta_max         66.585
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.386
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51232
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             1169
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9096
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7958
_reflns_number_total             9096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03010b2.cif
_cod_data_source_block           exp_20216_auto
_cod_original_cell_volume        2577.61(15)
_cod_original_formula_sum        'C40 H95 Li4 Mo8 N30 O34.50'
_cod_database_code               7250798
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.366
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 Li21-H8A \\sim Li21-H8B
 with sigma of 0.02
 O13-Li21 \\sim O19-Li21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O17 \\sim O14 \\sim O20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O17 \\sim O23 \\sim O14: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O13 \\sim O19: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O17 \\sim O14: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O22 \\sim O20: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O16 \\sim O18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O22 \\sim O23 \\sim O20: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O17, Li1W, O14, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O13, O19, Li21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O17, O23, Li1W, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O17, Li1W, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O22, Li1W, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O16, O18, Li21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O22, O23, Li1W, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 1*[Sof(O13)+Sof(H13A)+Sof(H13B)+Sof(O16)+Sof(H16A)+Sof(H16B)+Sof(O17)+
 Sof(H17A)+Sof(H17B)+Sof(O18)+Sof(H18A)+Sof(H18B)+Sof(O19)+Sof(H19A)+Sof(H19B)+
 Sof(O14)+Sof(H14A)+Sof(H14B)+Sof(O20)+Sof(H20A)+Sof(H20B)]+1*[Sof(O22)+
 Sof(H22A)+Sof(H22B)]+1*[Sof(O23)+Sof(H23A)+Sof(H23B)]=1 with esd of 0.002
 Sof(O13)=Sof(H13A)=Sof(H13B)=Sof(O18)=Sof(H18A)=Sof(H18B)=Sof(O14)=Sof(H14A)=
 Sof(H14B)=1-FVAR(1)
 Sof(O16)=Sof(H16A)=Sof(H16B)=Sof(O17)=Sof(H17A)=Sof(H17B)=Sof(O19)=Sof(H19A)=
 Sof(H19B)=Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(1)
 Sof(O22)=Sof(H22A)=Sof(H22B)=FVAR(2)
 Sof(O23)=Sof(H23A)=Sof(H23B)=FVAR(3)
 Fixed Sof: O15(0.5) H15A(0.5) H15B(0.5) O21(0.75) H21A(0.75) H21B(0.75)
6.a Riding coordinates:
 O3(H3), O7(H7), O14(H14A,H14B), O21(H21A,H21B)
6.b Free rotating group:
 O8(H8A,H8B), O20(H20A,H20B)
6.c Rotating group:
 O12(H12A,H12B), O13(H13A,H13B), O17(H17A,H17B), O18(H18A,H18B), O19(H19A,
 H19B), O22(H22A,H22B), O23(H23A,H23B)
6.d Secondary CH2 refined with riding coordinates:
 O16(H16A,H16B)
6.e Aromatic/amide H refined with riding coordinates:
 N9(H9)
6.f X=CH2 refined with riding coordinates:
 O15(H15A,H15B)
6.g Idealised Me refined as rotating group:
 C01A(H01A,H01B,H01C), C01E(H01D,H01E,H01F), C01F(H01G,H01H,H01I), C01G(H01J,
 H01K,H01L), C01H(H01M,H01N,H01O), C01L(H01P,H01Q,H01R), C017(H01S,H01T,H01U),
 C019(H01V,H01W,H01X), C01P(H01Y,H,HA), C01Y(H01Z,HB,HC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 182 electrons were 
found in a volume of 521\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
20[H2O] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2262
_shelx_fab_checksum              89687
_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 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.690