Isolated molybdenum-based microporous POMs for selective adsorption of gases
Deng, Lan; Lin, Rong-Yan; Zhou, Zhao-Hui; Dalton Transactions  (2022) –; doi:10.1039/D2DT00134A

data_7709624
_publ_section_title
;
 Isolated molybdenum-based microporous POMs for selective adsorption of
 gases
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00134A
_journal_year                    2022
_chemical_formula_moiety         '2(C16 H24 Mo8 N24 O20)'
_chemical_formula_sum            'C32 H48 Mo16 N48 O40'
_chemical_formula_weight         3280.22
_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             2022-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-01-15 deposited with the CCDC.	2022-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                89.8000(10)
_cell_angle_beta                 82.5470(10)
_cell_angle_gamma                83.1880(10)
_cell_formula_units_Z            1
_cell_length_a                   9.74720(10)
_cell_length_b                   18.7620(2)
_cell_length_c                   20.4530(2)
_cell_measurement_reflns_used    48469
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      77.9430
_cell_measurement_theta_min      2.3840
_cell_volume                     3682.33(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -25.00   0.00   0.50    0.20    --  -47.87  25.00-151.00   50
  2  \w   -104.00 -55.00   0.50    0.20    --  -47.87 -25.00  44.00   98
  3  \w    -22.00  33.00   0.50    0.20    --   47.87 -25.00  44.00  110
  4  \w     43.00 122.00   0.50    0.20    --   47.87  25.00-151.00  158
  5  \w   -148.00-123.00   0.50    0.80    --  -99.00 -25.00  44.00   50
  6  \w    120.00 165.00   0.50    0.80    --  108.50  25.00-151.00   90
  7  \w    -22.00  14.00   0.50    0.20    --  -47.87  19.00  30.00   72
  8  \w    -58.00 -14.00   0.50    0.20    --  -47.87  57.00 150.00   88
  9  \w    -99.00 -74.00   0.50    0.20    --  -47.87-125.00-120.00   50
 10  \w    -21.00  23.00   0.50    0.20    --  -47.87  19.00  60.00   88
 11  \w    -22.00  14.00   0.50    0.20    --  -47.87  19.00   0.00   72
 12  \w   -116.00 -80.00   0.50    0.20    --  -47.87-125.00 150.00   72
 13  \w     25.00  92.00   0.50    0.20    --   47.87-125.00 -90.00  134
 14  \w   -106.00 -73.00   0.50    0.80    --  -99.00 111.00-104.57   66
 15  \w    -58.00 -28.00   0.50    0.80    --  -99.00  61.00-180.00   60
 16  \w   -126.00-100.00   0.50    0.80    --  -99.00 144.00  58.60   52
 17  \w   -108.00 -83.00   0.50    0.80    --  -99.00 109.00 -73.67   50
 18  \w   -121.00 -87.00   0.50    0.80    --  -99.00 138.00 163.17   68
 19  \w   -131.00-105.00   0.50    0.80    --  -99.00 153.00 173.63   52
 20  \w   -124.00 -93.00   0.50    0.80    --  -99.00 143.00 -43.33   62
 21  \w    -72.00 -28.00   0.50    0.80    --  -99.00 141.00 -73.90   88
 22  \w   -109.00 -84.00   0.50    0.80    --  -99.00 115.00 -46.95   50
 23  \w   -108.00 -81.00   0.50    0.80    --  -99.00 111.00 -58.97   54
 24  \w    -60.00 -35.00   0.50    0.80    --  -99.00 109.00 -73.67   50
 25  \w     73.00  99.00   0.50    0.80    --  108.50 -95.00  90.00   52
 26  \w     62.00 105.00   0.50    0.80    --  108.50 -95.00  60.00   86
 27  \w     37.00  64.00   0.50    0.80    --  108.50 -61.00-180.00   54
 28  \w    114.00 155.00   0.50    0.80    --  108.50  45.00 150.00   82
 29  \w     36.00  73.00   0.50    0.80    --  108.50 -61.00  60.00   74
 30  \w     66.00  92.00   0.50    0.80    --  108.50 -95.00 -60.00   52
 31  \w     36.00 107.00   0.50    0.80    --  108.50-110.00  66.06  142
 32  \w     41.00  79.00   0.50    0.80    --  108.50 -77.00 -90.00   76
 33  \w     36.00  71.00   0.50    0.80    --  108.50 -95.00   0.00   70
 34  \w     74.00 105.00   0.50    0.80    --  108.50 -95.00   0.00   62
 35  \w     61.00  98.00   0.50    0.80    --  108.50 -95.00-180.00   74
 36  \w    103.00 176.00   0.50    0.80    --  108.50  30.00 120.00  146
 37  \w     36.00  73.00   0.50    0.80    --  108.50 -61.00-150.00   74
 38  \w     52.00 105.00   0.50    0.80    --  108.50 -98.00-134.29  106
 39  \w     37.00 104.00   0.50    0.80    --  108.50 -95.00 150.00  134
 40  \w    107.00 178.00   0.50    0.80    --  108.50  77.00  60.00  142
 41  \w    133.00 164.00   0.50    0.80    --  108.50   0.00   0.00   62
 42  \w     46.00  71.00   0.50    0.80    --  108.50-125.00-180.00   50
 43  \w     74.00 117.00   0.50    0.80    --  108.50   0.00   0.00   86
 44  \w     38.00  72.00   0.50    0.80    --  108.50 -61.00 -30.00   68
 45  \w     80.00 105.00   0.50    0.80    --  108.50 -95.00  30.00   50
 46  \w     73.00 111.00   0.50    0.80    --  108.50-125.00-180.00   76
 47  \w    117.00 143.00   0.50    0.80    --  108.50  45.00-120.00   52
 48  \w     47.00  72.00   0.50    0.80    --  108.50 -61.00 150.00   50
 49  \w     98.00 176.00   0.50    0.80    --  108.50  30.00  60.00  156
 50  \w     36.00 111.00   0.50    0.80    --  108.50-125.00   0.00  150
 51  \w     98.00 156.00   0.50    0.80    --  108.50  45.00-180.00  116
 52  \w     74.00 108.00   0.50    0.80    --  108.50-125.00 -60.00   68
 53  \w     37.00  78.00   0.50    0.80    --  108.50 -77.00  60.00   82
 54  \w     84.00 109.00   0.50    0.80    --  108.50-125.00 -90.00   50
 55  \w     71.00  97.00   0.50    0.80    --  108.50 -95.00 120.00   52
 56  \w     38.00  89.00   0.50    0.80    --  108.50 -77.00-150.00  102
 57  \w     87.00 120.00   0.50    0.80    --  108.50  77.00 150.00   66
 58  \w    153.00 178.00   0.50    0.80    --  108.50  77.00 150.00   50
 59  \w    103.00 178.00   0.50    0.80    --  108.50  45.00   0.00  150
 60  \w     43.00  70.00   0.50    0.80    --  108.50 -61.00  90.00   54
 61  \w     37.00  69.00   0.50    0.80    --  108.50-125.00 -60.00   64
 62  \w     68.00  93.00   0.50    0.80    --  108.50 -77.00 -60.00   50
 63  \w     69.00 111.00   0.50    0.80    --  108.50-125.00 150.00   84
 64  \w    145.00 175.00   0.50    0.80    --  108.50  45.00-150.00   60
 65  \w    137.00 163.00   0.50    0.80    --  108.50 125.00  60.00   52
 66  \w     92.00 129.00   0.50    0.80    --  108.50 125.00  60.00   74
 67  \w     50.00  99.00   0.50    0.80    --  108.50 -95.00 -30.00   98
 68  \w     37.00  62.00   0.50    0.80    --  108.50 -61.00-120.00   50
 69  \w     45.00  73.00   0.50    0.80    --  108.50 -95.00  30.00   56
;
_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      0.1153897000
_diffrn_orient_matrix_UB_12      -0.0634831000
_diffrn_orient_matrix_UB_13      -0.0150456000
_diffrn_orient_matrix_UB_21      -0.1069591000
_diffrn_orient_matrix_UB_22      -0.0529427000
_diffrn_orient_matrix_UB_23      0.0200209000
_diffrn_orient_matrix_UB_31      -0.0319203000
_diffrn_orient_matrix_UB_32      -0.0025200000
_diffrn_orient_matrix_UB_33      -0.0717226000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67878
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.612
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36875
_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 dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.422
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         15575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0812P)^2^+12.7776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14681
_reflns_number_total             15575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00134a2.cif
_cod_data_source_block           exp_475-dl_auto
_cod_database_code               7709624
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.397
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N13(H13), N1(H1), N19(H19), N7(H7), C1(H1a), C3(H3), N16(H16), C7(H7a),
 C11(H11), C2(H2), C5(H5), C9(H9), C13(H13a), N22(H22), N4(H4), C14(H14),
 C10(H10a), C6(H6), C12(H12), N10(H10), C15(H15), C16(H16a), C4(H4a), C8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              55299
_shelx_fab_checksum              69938
_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 2.198
_oxdiff_exptl_absorpt_empirical_full_min 0.714