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_7709627
_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         'C16 H20 Mo12 N24 O28, C8 H12 Mo4 N12 O10'
_chemical_formula_sum            'C24 H32 Mo16 N36 O38'
_chemical_formula_weight         2967.89
_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             2022-01-06
_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                72.4920(10)
_cell_angle_beta                 79.1170(10)
_cell_angle_gamma                85.7130(10)
_cell_formula_units_Z            2
_cell_length_a                   13.58760(10)
_cell_length_b                   19.1998(2)
_cell_length_c                   21.9901(2)
_cell_measurement_reflns_used    69639
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      74.2080
_cell_measurement_theta_min      2.7070
_cell_volume                     5371.62(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_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    -40.00 -12.00   0.50    0.30    --  -43.22 -77.00  30.00   56
  2  \w    -80.00 -12.00   0.50    0.30    --  -43.22 -77.00 120.00  136
  3  \w    -82.00 -57.00   0.50    1.20    --  -90.25 -81.00  53.73   50
  4  \w    -84.00 -59.00   0.50    1.20    --  -90.25 -77.00   0.00   50
  5  \w    -85.00 -60.00   0.50    1.20    --  -90.25 -74.00 -11.36   50
  6  \w    -82.00 -57.00   0.50    1.20    --  -90.25 -82.00  29.12   50
  7  \w    -85.00 -60.00   0.50    1.20    --  -90.25 -74.00  81.24   50
  8  \w    -82.00 -57.00   0.50    1.20    --  -90.25 -82.00 111.22   50
  9  \w    -82.00 -57.00   0.50    1.20    --  -90.25 -83.00 149.36   50
 10  \w    -92.00 -57.00   0.50    1.20    --  -90.25 -83.00  66.97   70
 11  \w    -94.00 -57.00   0.50    1.20    --  -90.25 -81.00 -17.67   74
 12  \w    -91.00 -59.00   0.50    1.20    --  -90.25 -77.00 -33.50   64
 13  \w    -89.00 -57.00   0.50    1.20    --  -90.25 -81.00  18.99   64
 14  \w    -94.00 -57.00   0.50    1.20    --  -90.25 -81.00 -45.40   74
 15  \w    -94.00 -57.00   0.50    1.20    --  -90.25 -82.00-114.13   74
 16  \w    -92.00 -57.00   0.50    1.20    --  -90.25 -82.00-124.99   70
 17  \w    -91.00 -57.00   0.50    1.20    --  -90.25 -82.00-150.41   68
 18  \w    -92.00 -57.00   0.50    1.20    --  -90.25 -81.00-137.83   70
 19  \w   -101.00 -60.00   0.50    1.20    --  -90.25 -74.00 -79.27   82
 20  \w   -104.00 -57.00   0.50    1.20    --  -90.25 -82.00-104.54   94
 21  \w   -107.00 -81.00   0.50    1.20    --  -90.25-117.00-105.00   52
 22  \w   -109.00 -58.00   0.50    1.20    --  -90.25 -79.00 -59.96  102
 23  \w   -114.00 -62.00   0.50    1.20    --  -90.25 -71.00  27.41  104
 24  \w   -104.00 -58.00   0.50    1.20    --  -90.25 -82.00  81.72   92
 25  \w   -108.00 -81.00   0.50    0.30    --  -43.22-161.00 102.00   54
 26  \w    -87.00 -55.00   0.50    1.20    --  -90.25-161.00 102.00   64
 27  \w   -110.00 -57.00   0.50    1.20    --  -90.25 -83.00 171.68  106
 28  \w   -108.00 -82.00   0.50    0.30    --  -43.22 -77.00 120.00   52
 29  \w   -133.00-107.00   0.50    1.20    --  -90.25 -83.00 149.36   52
 30  \w   -117.00 -57.00   0.50    1.20    --  -90.25 -81.00 178.53  120
 31  \w   -125.00 -59.00   0.50    1.20    --  -90.25 -77.00 150.00  132
 32  \w   -118.00 -20.00   0.50    0.30    --  -43.22 -77.00   0.00  196
 33  \w     26.00  81.00   0.50    0.30    --   43.22-117.00-105.00  110
 34  \w     41.00 112.00   0.50    1.20    --  107.76-117.00-105.00  142
 35  \w     72.00 102.00   0.50    1.20    --  107.76 -94.00 -90.00   60
 36  \w     34.00  87.00   0.50    1.20    --  107.76-125.00 -60.00  106
 37  \w     43.00 106.00   0.50    1.20    --  107.76 -94.00   0.00  126
 38  \w    116.00 141.00   0.50    1.20    --  107.76-161.00 102.00   50
 39  \w     83.00 108.00   0.50    1.20    --  107.76 -94.00 150.00   50
 40  \w     63.00 109.00   0.50    1.20    --  107.76 -94.00  90.00   92
 41  \w     65.00  91.00   0.50    0.30    --   43.22-161.00 102.00   52
 42  \w     45.00  71.00   0.50    1.20    --  107.76 -94.00 150.00   52
 43  \w     32.00  58.00   0.50    1.20    --  107.76 -94.00  90.00   52
 44  \w     36.00 100.00   0.50    1.20    --  107.76 -77.00  30.00  128
 45  \w     36.00  71.00   0.50    1.20    --  107.76 -61.00 -60.00   70
 46  \w     34.00  59.00   0.50    1.20    --  107.76 -94.00 -90.00   50
 47  \w     34.00 116.00   0.50    1.20    --  107.76-125.00-150.00  164
 48  \w     33.00 114.00   0.50    1.20    --  107.76-125.00   0.00  162
 49  \w     37.00 111.00   0.50    1.20    --  107.76-125.00 150.00  148
 50  \w     33.00  71.00   0.50    1.20    --  107.76 -61.00 120.00   76
 51  \w     18.00  59.00   0.50    0.30    --   43.22  38.00  90.00   82
 52  \w     19.00  45.00   0.50    0.30    --   43.22  57.00 150.00   52
 53  \w     85.00 178.00   0.50    1.20    --  107.76  77.00  60.00  186
 54  \w    153.00 178.00   0.50    1.20    --  107.76 117.00 -18.00   50
 55  \w    115.00 140.00   0.50    1.20    --  107.76 161.00 132.00   50
 56  \w     71.00  97.00   0.50    0.30    --   43.22 161.00 132.00   52
 57  \w     69.00  99.00   0.50    1.20    --  107.76 161.00 132.00   60
 58  \w     97.00 127.00   0.50    1.20    --  107.76 117.00 -18.00   60
 59  \w     84.00 164.00   0.50    1.20    --  107.76  61.00  30.00  160
 60  \w     82.00 177.00   0.50    1.20    --  107.76  77.00 -30.00  190
 61  \w     87.00 173.00   0.50    1.20    --  107.76  45.00 120.00  172
 62  \w     87.00 178.00   0.50    1.20    --  107.76  45.00 -60.00  182
 63  \w     80.00 178.00   0.50    1.20    --  107.76  30.00-120.00  196
 64  \w    -70.00 -45.00   0.50    0.30    --  -43.22 161.00 132.00   50
 65  \w   -111.00 -73.00   0.50    1.20    --  -90.25 161.00 132.00   76
 66  \w   -116.00 -78.00   0.50    0.30    --  -43.22 161.00 132.00   76
 67  \w    -86.00 -19.00   0.50    0.30    --  -43.22 117.00 -18.00  134
 68  \w   -106.00 -58.00   0.50    1.20    --  -90.25 -79.00 -81.47   96
 69  \w   -118.00 -12.00   0.50    0.30    --  -43.22 -77.00-180.00  212
 70  \w   -118.00 -12.00   0.50    0.30    --  -43.22 -77.00 -60.00  212
 71  \w   -116.00 -15.00   0.50    0.30    --  -43.22 -77.00-120.00  202
 72  \w   -116.00 -18.00   0.50    0.30    --  -43.22 -38.00   0.00  196
 73  \w   -125.00 -99.00   0.50    1.20    --  -90.25 -77.00 -33.50   52
 74  \w   -142.00-116.00   0.50    1.20    --  -90.25 -77.00   0.00   52
 75  \w   -142.00-116.00   0.50    1.20    --  -90.25 -82.00  29.12   52
 76  \w   -136.00-101.00   0.50    1.20    --  -90.25 -74.00  81.24   70
 77  \w   -149.00-124.00   0.50    1.20    --  -90.25 -83.00 171.68   50
 78  \w   -149.00 -58.00   0.50    1.20    --  -90.25 -79.00 126.75  182
 79  \w   -162.00-117.00   0.50    1.20    --  -90.25 -74.00 -79.27   90
 80  \w   -143.00 -99.00   0.50    1.20    --  -90.25 -81.00-137.83   88
 81  \w   -152.00 -98.00   0.50    1.20    --  -90.25 -82.00-150.41  108
 82  \w   -151.00 -58.00   0.50    1.20    --  -90.25 -80.00-165.16  186
 83  \w   -152.00 -57.00   0.50    1.20    --  -90.25 -82.00 -87.61  190
 84  \w   -165.00 -96.00   0.50    1.20    --  -90.25 -74.00 -11.36  138
 85  \w   -155.00-129.00   0.50    1.20    --  -90.25 -81.00 -17.67   52
 86  \w   -158.00-112.00   0.50    1.20    --  -90.25 -81.00 -45.40   92
 87  \w   -165.00-118.00   0.50    1.20    --  -90.25 -83.00  66.97   94
 88  \w   -164.00-138.00   0.50    1.20    --  -90.25 -83.00 149.36   52
 89  \w   -164.00-120.00   0.50    1.20    --  -90.25 -82.00 111.22   88
 90  \w   -164.00-124.00   0.50    1.20    --  -90.25 -81.00 178.53   80
 91  \w   -154.00-129.00   0.50    1.20    --  -90.25 -81.00  53.73   50
 92  \w   -165.00-130.00   0.50    1.20    --  -90.25 -77.00 -33.50   70
 93  \w   -164.00-138.00   0.50    1.20    --  -90.25 -82.00-114.13   52
 94  \w   -160.00-134.00   0.50    1.20    --  -90.25 -82.00-124.99   52
 95  \w    -75.00 -50.00   0.50    1.20    --  -90.25 117.00 -18.00   50
;
_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      0.0878425000
_diffrn_orient_matrix_UB_12      0.0519945000
_diffrn_orient_matrix_UB_13      -0.0341089000
_diffrn_orient_matrix_UB_21      0.0105353000
_diffrn_orient_matrix_UB_22      0.0097785000
_diffrn_orient_matrix_UB_23      0.0654760000
_diffrn_orient_matrix_UB_31      0.0742143000
_diffrn_orient_matrix_UB_32      -0.0654406000
_diffrn_orient_matrix_UB_33      0.0107752000
_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  0.0809
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            141603
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.446
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         21272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0536P)^2^+44.3227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18700
_reflns_number_total             21272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00134a2.cif
_cod_data_source_block           exp_2130
_cod_database_code               7709627
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.308
_shelx_estimated_absorpt_t_min   0.091
_reflns_odcompleteness_completeness 99.92
_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) groups
2.a Aromatic/amide H refined with riding coordinates:
 N21(H21), N15(H15), C10(H10), C17(H17), C19(H19), N12(H12a), N25(H25),
 C14(H14), C9(H9), C16(H16), C13(H13), N28(H28), C2(H2), N9(H9a), C23(H23),
 C5(H5), C6(H6), C15(H15a), C20(H20), C22(H22), C8(H8), C21(H21a), C7(H7),
 C18(H18), C12(H12), N3(H3), C11(H11), C4(H4), C1(H1), C24(H24), N6(H6a),
 C3(H3a)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72045
_shelx_fab_checksum              84709
_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 1.992
_oxdiff_exptl_absorpt_empirical_full_min 0.380