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_7709626
_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'
_chemical_formula_sum            'C16 H20 Mo12 N24 O28'
_chemical_formula_weight         2147.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8003(2)
_cell_length_b                   20.8003(2)
_cell_length_c                   26.7130(5)
_cell_measurement_reflns_used    10554
_cell_measurement_temperature    99.9(8)
_cell_measurement_theta_max      78.9700
_cell_measurement_theta_min      4.4380
_cell_volume                     11557.4(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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   -113.00 -73.00   0.50    1.20    --  -41.49-121.00 -94.00   80
  2  \w      0.00  53.00   0.50    1.20    --   41.49 -47.00 133.00  106
  3  \w    -34.00  -8.00   0.50    1.20    --   41.49 -47.00 133.00   52
  4  \w    -85.00 -60.00   0.50    5.00    --  -98.00  75.00 105.00   50
  5  \w     95.00 163.00   0.50    5.00    --  119.50  47.00 -77.00  136
  6  \w    123.00 164.00   0.50    5.00    --  119.50 153.00 147.00   82
  7  \w     93.00 121.00   0.50    5.00    --  119.50 153.00 147.00   56
  8  \w    -30.00  18.00   0.50    1.20    --   41.49 -19.00-120.00   96
  9  \w     83.00 123.00   0.50    1.20    --   41.49 178.00  90.00   80
 10  \w    -52.00 -27.00   0.50    5.00    --  -98.00  47.00 -77.00   50
 11  \w   -147.00-122.00   0.50    5.00    --  -98.00 -47.00 133.00   50
 12  \w     50.00 109.00   0.50    5.00    --  119.50-111.00 -30.00  118
 13  \w    143.00 175.00   0.50    5.00    --  119.50  61.00  90.00   64
 14  \w     66.00  93.00   0.50    5.00    --  119.50 -77.00 -90.00   54
 15  \w    101.00 147.00   0.50    5.00    --  119.50 111.00-180.00   92
 16  \w     41.00  75.00   0.50    5.00    --  119.50-111.00  90.00   68
 17  \w     75.00 104.00   0.50    5.00    --  119.50 -94.00 -30.00   58
 18  \w     45.00  85.00   0.50    5.00    --  119.50 -94.00-150.00   80
 19  \w     94.00 123.00   0.50    5.00    --  119.50  61.00  90.00   58
 20  \w     77.00 104.00   0.50    5.00    --  119.50 -77.00 -60.00   54
 21  \w     43.00  94.00   0.50    5.00    --  119.50-111.00-150.00  102
 22  \w     44.00  70.00   0.50    5.00    --  119.50 -94.00 -30.00   52
 23  \w     53.00  94.00   0.50    5.00    --  119.50 -77.00 120.00   82
;
_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      0.0380394000
_diffrn_orient_matrix_UB_12      0.0458114000
_diffrn_orient_matrix_UB_13      -0.0343853000
_diffrn_orient_matrix_UB_21      0.0200218000
_diffrn_orient_matrix_UB_22      0.0400354000
_diffrn_orient_matrix_UB_23      0.0458972000
_diffrn_orient_matrix_UB_31      0.0602792000
_diffrn_orient_matrix_UB_32      -0.0422167000
_diffrn_orient_matrix_UB_33      0.0063657000
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20237
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.497
_diffrn_reflns_theta_max         67.497
_diffrn_reflns_theta_min         2.692
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.705
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31521
_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 dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         5123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+30.1857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4200
_reflns_number_total             5123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00134a2.cif
_cod_data_source_block           exp_7272_auto_reduction_1
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7709626
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.414
_shelx_estimated_absorpt_t_min   0.100
_reflns_odcompleteness_completeness 94.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C4(H4), C3(H3a)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96853
_shelx_fab_checksum              9927
_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 2.326
_oxdiff_exptl_absorpt_empirical_full_min 0.534