Hexnuclear, octanuclear, dodecanuclear, and hexadecnuclear polyoxomolybdenum(v)-based porous materials for selective adsorption of gases
Lin, Rong-Yan; Dai, Ru-Dan; Dong, Xin; Zhou, Zhao-Hui; CrystEngComm 25 (2023) 5942–5950; doi:10.1039/D3CE00736G

data_7247408
_publ_section_title
;
 Hexnuclear, octanuclear, dodecanuclear, and hexadecnuclear
 polyoxomolybdenum(v)-based porous materials for selective adsorption of
 gases
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              5942
_journal_page_last               5950
_journal_paper_doi               10.1039/D3CE00736G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C16 H23 Mo12 N32 Na4 O30, 12[H2O]'
_chemical_formula_sum            'C16 H47 Mo12 N32 Na4 O42'
_chemical_formula_weight         2603.09
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-01-20 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                98.134(2)
_cell_angle_beta                 97.651(2)
_cell_angle_gamma                91.857(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8391(3)
_cell_length_b                   11.9219(2)
_cell_length_c                   25.7883(6)
_cell_measurement_reflns_used    16317
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.2480
_cell_measurement_theta_min      3.7510
_cell_volume                     3566.31(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.965
_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     48.00 108.00   0.50   18.00    --   92.20-108.00   5.00  120
  2  \w     88.00 125.00   0.50   18.00    --   92.20 108.00 102.00   74
  3  \w   -102.00 -76.00   0.50   18.00    --  -94.70 108.00 102.00   52
  4  \w   -166.00 -85.00   0.50   18.00    --  -94.70-108.00   5.00  162
  5  \w    -15.00  26.00   0.50    0.70    --   -1.25 -99.00-180.00   82
  6  \w    -18.00  21.00   0.50    0.70    --   -1.25 -99.00  30.00   78
  7  \w    -17.00  31.00   0.50    0.70    --   -1.25 -99.00 -30.00   96
  8  \w    -60.00 -13.00   0.50    0.70    --   -1.25 -38.00 -60.00   94
  9  \w    -70.00   8.00   0.50    0.70    --   -1.25 -38.00-120.00  156
 10  \w     81.00 107.00   0.50   18.00    --   92.20-125.00  60.00   52
 11  \w     61.00 102.00   0.50   18.00    --   92.20 -99.00-150.00   82
 12  \w     21.00  51.00   0.50   18.00    --   92.20 -99.00-150.00   60
 13  \w     21.00  62.00   0.50   18.00    --   92.20-125.00  60.00   82
 14  \w     30.00  56.00   0.50   18.00    --   92.20-125.00-150.00   52
 15  \w     23.00  67.00   0.50   18.00    --   92.20 -57.00-150.00   88
 16  \w     42.00  68.00   0.50   18.00    --   92.20-125.00 150.00   52
 17  \w     80.00 111.00   0.50   18.00    --   92.20-125.00 150.00   62
 18  \w     78.00 164.00   0.50   18.00    --   92.20  57.00  30.00  172
 19  \w     63.00 107.00   0.50   18.00    --   92.20 -77.00  90.00   88
 20  \w     61.00 112.00   0.50   18.00    --   92.20-125.00-150.00  102
 21  \w     80.00 110.00   0.50   18.00    --   92.20  57.00-150.00   60
 22  \w     21.00  67.00   0.50   18.00    --   92.20 -57.00-120.00   92
 23  \w     49.00  74.00   0.50   18.00    --   92.20 -99.00-180.00   50
 24  \w     29.00  56.00   0.50   18.00    --   92.20 -77.00  90.00   54
 25  \w     70.00  95.00   0.50   18.00    --   92.20 -99.00   0.00   50
 26  \w   -164.00 -95.00   0.50   18.00    --  -94.70 -38.00-150.00  138
 27  \w    -71.00 -27.00   0.50   18.00    --  -94.70 125.00-120.00   88
 28  \w   -160.00 -89.00   0.50   18.00    --  -94.70 -99.00  30.00  142
 29  \w   -105.00 -80.00   0.50   18.00    --  -94.70 125.00-120.00   50
 30  \w    -64.00 -24.00   0.50   18.00    --  -94.70  57.00  60.00   80
 31  \w    -63.00 -24.00   0.50   18.00    --  -94.70  57.00  90.00   78
 32  \w   -167.00 -74.00   0.50   18.00    --  -94.70-125.00 -30.00  186
 33  \w   -110.00 -85.00   0.50   18.00    --  -94.70 -38.00  30.00   50
 34  \w   -105.00 -45.00   0.50   18.00    --  -94.70 125.00 -90.00  120
 35  \w   -111.00 -81.00   0.50   18.00    --  -94.70 -57.00 -30.00   60
 36  \w   -165.00-128.00   0.50   18.00    --  -94.70 -57.00 -30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0862935000
_diffrn_orient_matrix_UB_12      0.0535291000
_diffrn_orient_matrix_UB_13      0.0346501000
_diffrn_orient_matrix_UB_21      0.0943064000
_diffrn_orient_matrix_UB_22      0.0201760000
_diffrn_orient_matrix_UB_23      0.0481167000
_diffrn_orient_matrix_UB_31      0.0307430000
_diffrn_orient_matrix_UB_32      0.1175330000
_diffrn_orient_matrix_UB_33      -0.0140675000
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39596
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.249
_diffrn_reflns_theta_min         3.497
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_description       block
_exptl_crystal_F_000             2502
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.025
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         13354
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+36.1429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10564
_reflns_number_total             13354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00736g2.cif
_cod_data_source_block           exp_793_auto
_cod_depositor_comments
'Adding full bibliography for 7247406--7247409.cif.'
_cod_database_code               7247408
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo C H O N'
_chemical_oxdiff_usercomment     'Ag Cu I P C'
_shelx_estimated_absorpt_t_max   0.468
_shelx_estimated_absorpt_t_min   0.267
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Rigid bond restraints
 N15, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 N9, N11, C5, N24, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 N12, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 N4, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
3. Others
 Fixed Sof: Na5(0.5) Na6(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C11(H11), C15(H15), C3(H3), C5(H5), C7(H7)
4.c X=CH2 refined with riding coordinates:
 N20(H20A,H20B), N32(H32A,H32B), N28(H28A,H28B), N8(H8A,H8B), N16(H16A,H16B),
 N12(H12A,H12B), N24(H24A,H24B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65373
_shelx_fab_checksum              89889
_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 1.710
_oxdiff_exptl_absorpt_empirical_full_min 0.722