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_7709625
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 98.7530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2669(2)
_cell_length_b                   20.0855(3)
_cell_length_c                   19.2031(3)
_cell_measurement_reflns_used    30264
_cell_measurement_temperature    99.8(8)
_cell_measurement_theta_max      78.7000
_cell_measurement_theta_min      2.3380
_cell_volume                     6582.35(16)
_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      99.8(8)
_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 0.979
_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     96.00 124.00   0.50    0.75    --  119.50  61.00  30.00   56
  2  \w    132.00 174.00   0.50    0.75    --  119.50  61.00  30.00   84
  3  \w     87.00 177.00   0.50    0.75    --  119.50  77.00  90.00  180
  4  \w     96.00 158.00   0.50    0.75    --  119.50  61.00 150.00  124
  5  \w     94.00 159.00   0.50    0.75    --  119.50  59.00  90.00  130
  6  \w    118.00 176.00   0.50    0.75    --  119.50  45.00-180.00  116
  7  \w    -29.00  30.00   0.50    0.19    --  -41.61  59.00  90.00  118
  8  \w    -25.00  41.00   0.50    0.19    --  -41.61  19.00  60.00  132
  9  \w    -63.00 -38.00   0.50    0.19    --  -41.61  59.00  90.00   50
 10  \w     45.00  70.00   0.50    0.75    --  119.50-111.00 150.00   50
 11  \w     74.00 112.00   0.50    0.75    --  119.50-111.00 150.00   76
 12  \w     63.00  96.00   0.50    0.75    --  119.50-111.00  90.00   66
 13  \w     85.00 110.00   0.50    0.75    --  119.50-111.00 -30.00   50
 14  \w     44.00  73.00   0.50    0.75    --  119.50-111.00 -30.00   58
 15  \w     53.00  95.00   0.50    0.75    --  119.50-111.00-120.00   84
 16  \w     46.00  94.00   0.50    0.75    --  119.50 -77.00 -30.00   96
 17  \w     48.00 101.00   0.50    0.75    --  119.50 -77.00   0.00  106
 18  \w     68.00 103.00   0.50    0.75    --  119.50 -77.00  30.00   70
 19  \w     46.00 104.00   0.50    0.75    --  119.50 -77.00 -90.00  116
 20  \w     62.00  89.00   0.50    0.75    --  119.50 -77.00-150.00   54
 21  \w     -6.00  19.00   0.50    0.19    --   41.61 -59.00 -49.00   50
 22  \w    -40.00  26.00   0.50    0.19    --   41.61 -19.00 150.00  132
 23  \w    101.00 126.00   0.50    0.75    --  119.50 111.00 -30.00   50
 24  \w    134.00 168.00   0.50    0.75    --  119.50 111.00 -30.00   68
 25  \w     67.00  94.00   0.50    0.19    --   41.61 178.00-150.00   54
 26  \w    142.00 174.00   0.50    0.75    --  119.50 111.00   0.00   64
 27  \w    101.00 177.00   0.50    0.75    --  119.50 111.00  30.00  152
 28  \w    100.00 130.00   0.50    0.75    --  119.50 111.00   0.00   60
 29  \w   -114.00 -27.00   0.50    0.19    --  -41.61 -59.00 -49.00  174
 30  \w   -171.00-126.00   0.50    0.75    --  -98.00 -59.00 -49.00   90
 31  \w    -50.00 -23.00   0.50    0.75    --  -98.00  45.00-150.00   54
 32  \w    -51.00 -24.00   0.50    0.75    --  -98.00  45.00-120.00   54
 33  \w    -47.00 -21.00   0.50    0.75    --  -98.00  45.00 -90.00   52
 34  \w    -50.00 -21.00   0.50    0.75    --  -98.00  45.00 -60.00   58
 35  \w    -47.00 -22.00   0.50    0.75    --  -98.00  45.00  30.00   50
 36  \w    -68.00 -28.00   0.50    0.75    --  -98.00  59.00  90.00   80
;
_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      0.0678877000
_diffrn_orient_matrix_UB_12      0.0504801000
_diffrn_orient_matrix_UB_13      0.0117050000
_diffrn_orient_matrix_UB_21      -0.0221986000
_diffrn_orient_matrix_UB_22      0.0181703000
_diffrn_orient_matrix_UB_23      0.0723320000
_diffrn_orient_matrix_UB_31      0.0552244000
_diffrn_orient_matrix_UB_32      -0.0548339000
_diffrn_orient_matrix_UB_33      0.0348605000
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50482
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.852
_diffrn_reflns_theta_min         3.204
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30011
_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    2.167
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0572P)^2^+18.5673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12550
_reflns_number_total             14046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00134a2.cif
_cod_data_source_block           exp_5668_auto
_cod_database_code               7709625
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.255
_shelx_estimated_absorpt_t_min   0.071
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 N22(H22), N4(H4), N16(H16), C3(H3), C1(H1), C9(H9), C11(H11), C15(H15),
 N7(H7), C7(H7a), C5(H5), C12(H12), C13(H13), C10(H10), C16(H16a), C14(H14),
 C8(H8), C4(H4a), C6(H6), C2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83946
_shelx_fab_checksum              11018
_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 2.989
_oxdiff_exptl_absorpt_empirical_full_min 0.590