Successive constructions of regular tetra-, hexa- and octanuclear microporous polyoxovanadates(III) for gas adsorptions
Xie, Zhenlang; An, Dongli; Weng, Weizheng; Zhou, Zhao-Hui; Dalton Transactions  (2022) –; doi:10.1039/D2DT01360F

data_7710670
_publ_section_title
;
 Successive constructions of regular tetra-, hexa- and octanuclear
 microporous polyoxovanadates(III) for gas adsorptions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01360F
_journal_year                    2022
_chemical_formula_moiety         'C20 H16 K2 N8 O24 V4, 2(H4 N)'
_chemical_formula_sum            'C20 H34 K2 N10 O29 V4'
_chemical_formula_weight         1160.53
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-02-24 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.11633(10)
_cell_length_b                   18.11633(10)
_cell_length_c                   11.42819(6)
_cell_measurement_reflns_used    42550
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.9090
_cell_measurement_theta_min      2.7940
_cell_volume                     3248.24(3)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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     95.00 177.00   0.50    0.07    --  105.19  45.00-150.00  164
  2  \w    100.00 178.00   0.50    0.07    --  105.19  30.00 -60.00  156
  3  \w    -16.00  19.00   0.50    0.05    --   47.87 -19.00-120.00   70
  4  \w    -25.00  27.00   0.50    0.05    --   47.87 -19.00-150.00  104
  5  \w    -24.00  28.00   0.50    0.05    --   47.87 -19.00  90.00  104
  6  \w     92.00 177.00   0.50    0.07    --  105.19  61.00 150.00  170
  7  \w     33.00  69.00   0.50    0.07    --  105.19 -95.00-150.00   72
  8  \w     53.00  79.00   0.50    0.07    --  105.19-125.00 -90.00   52
  9  \w     71.00 119.00   0.50    0.07    --  105.19-135.00-129.00   96
 10  \w     37.00 105.00   0.50    0.07    --  105.19 -95.00-120.00  136
 11  \w     54.00  80.00   0.50    0.05    --   47.87-135.00-129.00   52
 12  \w     69.00 112.00   0.50    0.07    --  105.19-125.00 -60.00   86
 13  \w     35.00  63.00   0.50    0.05    --   47.87-134.00  49.00   56
 14  \w     72.00 119.00   0.50    0.07    --  105.19-134.00  49.00   94
 15  \w     33.00 100.00   0.50    0.07    --  105.19 -95.00  30.00  134
 16  \w     33.00  84.00   0.50    0.07    --  105.19 -77.00  30.00  102
 17  \w     36.00  61.00   0.50    0.07    --  105.19 -61.00  90.00   50
 18  \w     38.00  67.00   0.50    0.07    --  105.19 -61.00  60.00   58
 19  \w     47.00  73.00   0.50    0.07    --  105.19 -61.00 -60.00   52
 20  \w     38.00  73.00   0.50    0.07    --  105.19 -61.00 -90.00   70
 21  \w     72.00  97.00   0.50    0.05    --   47.87 135.00 -64.00   50
 22  \w    100.00 125.00   0.50    0.07    --  105.19 135.00 -64.00   50
 23  \w     93.00 122.00   0.50    0.07    --  105.19 134.00 116.00   58
 24  \w     73.00  98.00   0.50    0.05    --   47.87 134.00 116.00   50
 25  \w    -24.00  27.00   0.50    0.05    --  -47.87  19.00-120.00  102
 26  \w    -53.00 -27.00   0.50    0.07    --  -99.00  61.00 -90.00   52
 27  \w   -103.00 -27.00   0.50    0.07    --  -99.00  77.00 -30.00  152
 28  \w    -20.00  27.00   0.50    0.05    --  -47.87  19.00  90.00   94
 29  \w    -54.00 -29.00   0.50    0.07    --  -99.00 125.00  60.00   50
 30  \w   -116.00 -28.00   0.50    0.07    --  -99.00 134.00 116.00  176
 31  \w   -126.00 -83.00   0.50    0.07    --  -99.00 144.00  75.29   86
 32  \w   -118.00 -65.00   0.50    0.07    --  -99.00 135.00 -64.00  106
 33  \w    -97.00 -20.00   0.50    0.05    --  -47.87 135.00 -64.00  154
 34  \w   -109.00 -63.00   0.50    0.07    --  -99.00 125.00  60.00   92
 35  \w    -97.00 -48.00   0.50    0.05    --  -47.87 134.00 116.00   98
 36  \w   -114.00 -89.00   0.50    0.07    --  -99.00 -15.00 -90.00   50
 37  \w   -169.00-144.00   0.50    0.07    --  -99.00 -15.00 -90.00   50
 38  \w   -170.00 -88.00   0.50    0.07    --  -99.00 -45.00  60.00  164
 39  \w   -102.00 -77.00   0.50    0.07    --  -99.00 -77.00 120.00   50
 40  \w   -171.00 -78.00   0.50    0.07    --  -99.00 -77.00 150.00  186
 41  \w   -171.00-123.00   0.50    0.07    --  -99.00 -77.00 120.00   96
 42  \w   -119.00 -92.00   0.50    0.05    --  -47.87-125.00   0.00   54
 43  \w   -110.00 -70.00   0.50    0.05    --  -47.87-134.00  49.00   80
 44  \w   -110.00 -76.00   0.50    0.05    --  -47.87-125.00  90.00   68
 45  \w    -99.00 -74.00   0.50    0.05    --  -47.87-135.00-129.00   50
 46  \w   -123.00 -92.00   0.50    0.07    --  -99.00-135.00-129.00   62
 47  \w   -144.00-119.00   0.50    0.07    --  -99.00-134.00  49.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            48980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.981
_diffrn_reflns_theta_min         2.816
_exptl_absorpt_coefficient_mu    9.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17494
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       needle
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(11)
_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     263
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+7.3684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4419
_reflns_number_total             4498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01360f2.cif
_cod_data_source_block           exp_607_auto
_cod_original_cell_volume        3248.24(4)
_cod_database_code               7710670
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.443
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.982(11)
 0.018(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
3. Restrained distances
 O6-H6
 0.85 with sigma of 0.02
 O5-H5
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(C10) = Uanis(O8)
5.a Riding coordinates:
 N5(H5A,H5B,H5C), N5(H5D), O8(H6), O8(H5)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6A), C7(H7), C8(H8), C2(H2), C1(H1), C3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78601
_shelx_hkl_checksum              74728
_shelx_fab_checksum              14702
_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
;