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_7247407
_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 H40 Mo16 N32 Na8 O53, 24[H2O]'
_chemical_formula_sum            'C16 H88 Mo16 N32 Na8 O77'
_chemical_formula_weight         3680.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9900(2)
_cell_length_b                   31.7213(4)
_cell_length_c                   46.9852(6)
_cell_measurement_reflns_used    14167
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.5210
_cell_measurement_theta_min      3.3800
_cell_volume                     22341.6(5)
_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 0.984
_diffrn_measured_fraction_theta_max 0.938
_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     35.00  60.00   0.50    2.40    --  102.99 -57.00-120.00   50
  2  \w     32.00 112.00   0.50    2.40    --  102.99-126.00 -80.00  160
  3  \w     43.00  68.00   0.50    2.40    --  102.99 -57.00   0.00   50
  4  \w     35.00  60.00   0.50    2.40    --  102.99 -57.00 -30.00   50
  5  \w    -25.00  14.00   0.50    0.70    --   47.87 -19.00-150.00   78
  6  \w    114.00 143.00   0.50    2.40    --  102.99  28.00 -61.00   58
  7  \w    110.00 171.00   0.50    2.40    --  102.99  95.00 104.00  122
  8  \w   -103.00 -56.00   0.50    0.70    --  -47.87 146.00 164.00   94
  9  \w   -109.00 -83.00   0.50    2.40    --  -99.00 125.00  30.00   52
 10  \w    -64.00 -27.00   0.50    2.40    --  -99.00 125.00  30.00   74
 11  \w    -64.00 -39.00   0.50    2.40    --  -99.00  57.00-120.00   50
 12  \w    -60.00 -35.00   0.50    2.40    --  -99.00  57.00  30.00   50
 13  \w    -18.00  22.00   0.50    0.70    --  -47.87  19.00  30.00   80
 14  \w   -116.00 -78.00   0.50    0.70    --  -47.87-125.00 150.00   76
;
_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      -0.0765409000
_diffrn_orient_matrix_UB_12      0.0292049000
_diffrn_orient_matrix_UB_13      -0.0094974000
_diffrn_orient_matrix_UB_21      0.0681980000
_diffrn_orient_matrix_UB_22      0.0346906000
_diffrn_orient_matrix_UB_23      -0.0072797000
_diffrn_orient_matrix_UB_31      0.0075095000
_diffrn_orient_matrix_UB_32      -0.0173630000
_diffrn_orient_matrix_UB_33      -0.0305262000
_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  0.0206
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            19930
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.901
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64554
_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 light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_description       plate
_exptl_crystal_F_000             14272
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.208
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5475
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+392.4980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5034
_reflns_number_total             5475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00736g2.cif
_cod_data_source_block           exp_344_auto
_cod_depositor_comments
'Adding full bibliography for 7247406--7247409.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7247407
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.306
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All Na(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H3-O3
 0.85 with sigma of 0.02
 O2-H2
 0.87 with sigma of 0.02
 H2-O2W
 2.15 with sigma of 0.02
 H4-O4
 0.85 with sigma of 0.02
3. Rigid bond restraints
 O3W, C1
 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
4. Uiso/Uaniso restraints and constraints
N2 \\sim N1 \\sim N3 \\sim N5 \\sim N6 \\sim N7 \\sim N4 \\sim N8: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
5. Others
 Fixed Sof: H2W(0.5) Na3(0.5) Na2(0.5) O3W(0.5) H3W(0.5) Na5(0.25)
6.a Riding coordinates:
 O4(H4), O2W(H2W), Na2(H1,H3,H2)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4A)
6.c X=CH2 refined with riding coordinates:
 N4(H4B,H4C), N8(H8A,H8B)
6.d Idealised tetrahedral OH refined as rotating group:
 O3W(H3W)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45087
_shelx_fab_checksum              61877
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.762