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_7247406
_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 H44 Mo8 N40 O20, 2(O), 26[H2O]'
_chemical_formula_sum            'C16 H42 Mo8 N40 O22'
_chemical_formula_weight         1914.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 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                90
_cell_angle_beta                 102.276(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2829(9)
_cell_length_b                   20.7000(9)
_cell_length_c                   10.4480(5)
_cell_measurement_reflns_used    7312
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      64.3520
_cell_measurement_theta_min      3.2420
_cell_volume                     3863.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (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      99.9(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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      1.00  26.00   0.50    1.00    --    0.28  59.00 160.00   50
  2  \w    -81.00 -38.00   0.50    1.00    --    0.28 178.00-150.00   86
  3  \w    -22.00  76.00   0.50    1.00    --    1.90  59.00 160.00  196
  4  \w     87.00 113.00   0.50    2.00    --   87.09  59.00 160.00   52
  5  \w    -42.00 -17.00   0.50    1.00    --    0.28 -37.00  30.00   50
  6  \w    -48.00 -23.00   0.50    1.00    --    0.28 -59.00  21.00   50
  7  \w    -30.00  16.00   0.50    1.00    --    1.90 -59.00  21.00   92
  8  \w     41.00  66.00   0.50    2.00    --   87.09 -61.00 150.00   50
  9  \w     16.00  41.00   0.50    2.00    --   87.09 -59.00  21.00   50
 10  \w     11.00  51.00   0.50    2.00    --   87.09 -45.00 -60.00   80
 11  \w     13.00  47.00   0.50    2.00    --   87.09 -45.00 -90.00   68
 12  \w     10.00  51.00   0.50    2.00    --   87.09 -45.00-120.00   82
 13  \w     10.00  38.00   0.50    2.00    --   87.09 -45.00-150.00   56
 14  \w     10.00  35.00   0.50    2.00    --   87.09 -30.00-120.00   50
 15  \w     14.00  42.00   0.50    2.00    --   87.09 -61.00-120.00   56
 16  \w      7.00  33.00   0.50    2.00    --   87.09 -30.00-180.00   52
 17  \w     46.00  71.00   0.50    2.00    --   87.09 -61.00-120.00   50
 18  \w      9.00  34.00   0.50    2.00    --   87.09 -30.00   0.00   50
 19  \w      9.00  34.00   0.50    2.00    --   87.09 -30.00  30.00   50
 20  \w    -34.00  -8.00   0.50    2.00    --  -84.91  30.00   0.00   52
 21  \w    -35.00  -6.00   0.50    2.00    --  -84.91  30.00  90.00   58
 22  \w    -70.00 -15.00   0.50    2.00    --  -84.91  61.00 120.00  110
 23  \w    -53.00 -10.00   0.50    2.00    --  -84.91  59.00 160.00   86
 24  \w    -51.00 -12.00   0.50    2.00    --  -84.91  45.00 120.00   78
 25  \w    -35.00  -8.00   0.50    2.00    --  -84.91  30.00 150.00   54
 26  \w    -35.00 -10.00   0.50    2.00    --  -84.91  30.00 120.00   50
 27  \w   -153.00 -60.00   0.50    2.00    --  -84.91 -59.00  21.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0657565000
_diffrn_orient_matrix_UB_12      0.0006017000
_diffrn_orient_matrix_UB_13      -0.0709547000
_diffrn_orient_matrix_UB_21      -0.0394953000
_diffrn_orient_matrix_UB_22      -0.0521674000
_diffrn_orient_matrix_UB_23      -0.0954800000
_diffrn_orient_matrix_UB_31      -0.0395182000
_diffrn_orient_matrix_UB_32      0.0529727000
_diffrn_orient_matrix_UB_33      -0.0929742000
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10565
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        64.342
_diffrn_reflns_theta_max         64.342
_diffrn_reflns_theta_min         3.268
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (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    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0899P)^2^+1.8864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2816
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00736g2.cif
_cod_data_source_block           exp_7020_auto
_cod_depositor_comments
'Adding full bibliography for 7247406--7247409.cif.'
_cod_database_code               7247406
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo C O N'
_shelx_estimated_absorpt_t_max   0.407
_shelx_estimated_absorpt_t_min   0.290
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     59.94
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H7B-H7B_$1
 2.3 with sigma of 0.02
 H7B_$1-H7B
 2.7 with sigma of 0.02
3. Others
 Fixed Sof: H1W(0.5)
4.a Riding coordinates:
 O1W(H1W)
4.b Rotating group:
 N11(H11A,H11B), N8(H8A,H8B)
4.c Aromatic/amide H refined with riding coordinates:
 N10(H10), N6(H6), N2(H2)
4.d X=CH2 refined with riding coordinates:
 N7(H7A,H7B), N3(H3A,H3B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61569
_shelx_fab_checksum              66305
_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 4.306
_oxdiff_exptl_absorpt_empirical_full_min 0.440