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_7247409
_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         'C36 H30 Mo6 N18 O15, H O, 20[H2O]'
_chemical_formula_sum            'C36 H31 Mo6 N18 O16'
_chemical_formula_weight         1547.43
_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             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                83.745(2)
_cell_angle_beta                 81.094(2)
_cell_angle_gamma                84.215(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1739(2)
_cell_length_b                   12.6845(3)
_cell_length_c                   27.1349(6)
_cell_measurement_reflns_used    18664
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      73.3030
_cell_measurement_theta_min      3.3110
_cell_volume                     3763.17(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      99.98(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.961
_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    120.00 145.00   0.50    4.50    --   96.34 133.00-111.00   50
  2  \w     91.00 117.00   0.50    4.50    --   96.34-133.00 179.00   52
  3  \w     29.00  72.00   0.50    4.50    --   96.34-137.00   2.00   86
  4  \w     75.00 120.00   0.50    4.50    --   96.34-137.00   2.00   90
  5  \w   -110.00 -84.00   0.50    4.50    --  -98.84 133.00-111.00   52
  6  \w   -111.00 -59.00   0.50    4.50    --  -98.84 137.00  65.00  104
  7  \w   -143.00-118.00   0.50    4.50    --  -98.84-137.00   2.00   50
  8  \w   -156.00 -69.00   0.50    4.50    --  -98.84-133.00 179.00  174
  9  \w    -13.00  29.00   0.50    0.15    --   -1.25 -99.00 -30.00   84
 10  \w    -18.00  10.00   0.50    0.15    --   -1.25 -99.00-150.00   56
 11  \w    -49.00   3.00   0.50    0.15    --   -1.25   0.00-150.00  104
 12  \w    -18.00   8.00   0.50    0.15    --   -1.25 -99.00 150.00   52
 13  \w    -47.00  -5.00   0.50    0.15    --   -1.25   0.00 150.00   84
 14  \w    -16.00  16.00   0.50    0.15    --   -1.25 -99.00 -90.00   64
 15  \w    -17.00  26.00   0.50    0.15    --   -1.25 -99.00 120.00   86
 16  \w    -13.00  13.00   0.50    0.15    --   -1.25 -99.00-180.00   52
 17  \w     76.00 102.00   0.50    4.50    --   96.34 -77.00  30.00   52
 18  \w     31.00 106.00   0.50    4.50    --   96.34 -99.00 150.00  150
 19  \w     33.00  68.00   0.50    4.50    --   96.34 -99.00-150.00   70
 20  \w     42.00 107.00   0.50    4.50    --   96.34-125.00  30.00  130
 21  \w     66.00 105.00   0.50    4.50    --   96.34 -99.00   0.00   78
 22  \w     71.00  99.00   0.50    4.50    --   96.34 -99.00-150.00   56
 23  \w     27.00  55.00   0.50    4.50    --   96.34 -77.00  30.00   56
 24  \w     55.00 103.00   0.50    4.50    --   96.34   0.00  60.00   96
 25  \w     26.00  68.00   0.50    4.50    --   96.34 -57.00  60.00   84
 26  \w     64.00 103.00   0.50    4.50    --   96.34   0.00 150.00   78
 27  \w     52.00  96.00   0.50    4.50    --   96.34   0.00 120.00   88
 28  \w     86.00 111.00   0.50    4.50    --   96.34-125.00-120.00   50
 29  \w     27.00  76.00   0.50    4.50    --   96.34 -99.00-180.00   98
 30  \w     27.00 106.00   0.50    4.50    --   96.34 -77.00-120.00  158
 31  \w     51.00  98.00   0.50    4.50    --   96.34   0.00 -90.00   94
 32  \w     95.00 120.00   0.50    4.50    --   96.34 137.00  65.00   50
 33  \w     81.00 112.00   0.50    4.50    --   96.34-125.00 150.00   62
 34  \w    -79.00 -32.00   0.50    4.50    --  -98.84  77.00  90.00   94
 35  \w   -169.00 -79.00   0.50    4.50    --  -98.84 -77.00  30.00  180
 36  \w   -154.00 -79.00   0.50    4.50    --  -98.84 -77.00 -90.00  150
 37  \w    -73.00 -27.00   0.50    4.50    --  -98.84  77.00 -90.00   92
 38  \w   -166.00 -79.00   0.50    4.50    --  -98.84 -77.00   0.00  174
 39  \w    -64.00 -39.00   0.50    4.50    --  -98.84  57.00 -90.00   50
 40  \w    -70.00 -32.00   0.50    4.50    --  -98.84  77.00  60.00   76
 41  \w   -147.00-106.00   0.50    4.50    --  -98.84   0.00-120.00   82
 42  \w    -59.00 -29.00   0.50    4.50    --  -98.84  57.00-120.00   60
;
_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      -0.0006756000
_diffrn_orient_matrix_UB_12      0.0552260000
_diffrn_orient_matrix_UB_13      0.0478849000
_diffrn_orient_matrix_UB_21      -0.0390649000
_diffrn_orient_matrix_UB_22      -0.1018370000
_diffrn_orient_matrix_UB_23      0.0322308000
_diffrn_orient_matrix_UB_31      0.1345070000
_diffrn_orient_matrix_UB_32      -0.0402122000
_diffrn_orient_matrix_UB_33      0.0008582000
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47835
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.164
_diffrn_reflns_theta_min         3.312
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61992
_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    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             1506
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.490
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         14696
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1566P)^2^+4.0484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11670
_reflns_number_total             14696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00736g2.cif
_cod_data_source_block           exp_154_auto
_cod_depositor_comments
'Adding full bibliography for 7247406--7247409.cif.'
_cod_database_code               7247409
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.486
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H1W-O13
 1.8 with sigma of 0.02
 H21_$1-H16
 2.3 with sigma of 0.02
 H16-H21_$1
 2.5 with sigma of 0.02
 H18_$2-H1W
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O1W: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
O13: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
Uanis(C14) = Uanis(C13) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) =
Uanis(N7) = Uanis(N8) = Uanis(N9)
4.a Free rotating group:
 O1W(H1W)
4.b Aromatic/amide H refined with riding coordinates:
 N18(H18), N3(H3), N15(H15), C33(H33), N6(H6), C4(H4), C35(H35), C6(H6A),
 C34(H34), C3(H3A), N12(H12), C29(H29), C5(H5), C30(H30), C36(H36), C28(H28),
 C11(H11), C9(H9), C27(H27), C10(H10), C12(H12A), N9(H9A), C21(H21), C15(H15A),
 C18(H18A), C17(H17), C16(H16), C24(H24), C22(H22), C23(H23)
4.c Fitted hexagon refined as free rotating group:
 C15(C14,C13,C18,C17,C16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89863
_shelx_fab_checksum              57214
_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 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.652