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_7710673
_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         'C16 H48 N40 O32 S8 V8, 38[H2O]'
_chemical_formula_sum            'C16 H124 N40 O70 S8 V8'
_chemical_formula_weight         2661.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-06-26 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.54950(10)
_cell_length_b                   17.54950(10)
_cell_length_c                   15.90610(10)
_cell_measurement_reflns_used    37475
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9300
_cell_measurement_theta_min      3.5290
_cell_volume                     4898.84(5)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -85.00 -13.00   0.50    0.30    --  -47.87 113.00  66.00  144
  2  \w     28.00  54.00   0.50    0.30    --   47.87-113.00 -25.00   52
  3  \w   -102.00 -49.00   0.50    1.30    --  -99.00 113.00  66.00  106
  4  \w   -129.00-103.00   0.50    1.30    --  -99.00-113.00 -25.00   52
  5  \w    107.00 132.00   0.50    1.30    --  105.19 113.00  66.00   50
  6  \w     36.00 109.00   0.50    1.30    --  105.19-113.00 -25.00  146
  7  \w     -8.00  26.00   0.50    0.30    --  -47.87  19.00  60.00   68
  8  \w   -113.00 -76.00   0.50    0.30    --  -47.87-125.00-150.00   74
  9  \w    -22.00  22.00   0.50    0.30    --  -47.87  19.00 -30.00   88
 10  \w   -120.00 -92.00   0.50    0.30    --  -47.87-125.00  90.00   56
 11  \w     26.00 120.00   0.50    0.30    --   47.87  77.00-180.00  188
 12  \w     17.00  43.00   0.50    0.30    --   47.87 -38.00  60.00   52
 13  \w    -12.00  13.00   0.50    0.30    --   47.87 -38.00  60.00   50
 14  \w    -15.00  69.00   0.50    0.30    --   47.87 -77.00  60.00  168
 15  \w    -66.00 -40.00   0.50    1.30    --  -99.00  61.00 150.00   52
 16  \w    -58.00 -27.00   0.50    1.30    --  -99.00  61.00  60.00   62
 17  \w   -107.00 -29.00   0.50    1.30    --  -99.00 108.00 115.76  156
 18  \w   -166.00-139.00   0.50    1.30    --  -99.00 -95.00  30.00   54
 19  \w    -90.00 -38.00   0.50    1.30    --  -99.00  77.00  30.00  104
 20  \w   -170.00 -92.00   0.50    1.30    --  -99.00 -45.00-180.00  156
 21  \w    -57.00 -29.00   0.50    1.30    --  -99.00 112.00 153.94   56
 22  \w   -126.00 -74.00   0.50    1.30    --  -99.00 144.00 -33.66  104
 23  \w   -122.00 -96.00   0.50    1.30    --  -99.00 -61.00  60.00   52
 24  \w   -126.00 -99.00   0.50    1.30    --  -99.00 -95.00  30.00   54
 25  \w   -165.00-129.00   0.50    1.30    --  -99.00 -61.00  60.00   72
 26  \w    -67.00 -27.00   0.50    1.30    --  -99.00  61.00  90.00   80
 27  \w   -120.00 -27.00   0.50    1.30    --  -99.00 142.00   9.43  186
 28  \w   -108.00 -70.00   0.50    1.30    --  -99.00 112.00 153.94   76
 29  \w     67.00 101.00   0.50    1.30    --  105.19 -95.00-150.00   68
 30  \w     33.00  68.00   0.50    1.30    --  105.19 -61.00-120.00   70
 31  \w     57.00  82.00   0.50    1.30    --  105.19-125.00-180.00   50
 32  \w     46.00 111.00   0.50    1.30    --  105.19-125.00 -30.00  130
 33  \w     95.00 176.00   0.50    1.30    --  105.19  45.00   0.00  162
 34  \w    112.00 177.00   0.50    1.30    --  105.19  30.00-120.00  130
 35  \w     38.00  99.00   0.50    1.30    --  105.19 -95.00   0.00  122
 36  \w     34.00  64.00   0.50    1.30    --  105.19 -61.00 -60.00   60
 37  \w     45.00  71.00   0.50    1.30    --  105.19 -61.00-150.00   52
 38  \w     38.00  64.00   0.50    1.30    --  105.19 -61.00  90.00   52
 39  \w     47.00  72.00   0.50    1.30    --  105.19 -61.00  60.00   50
 40  \w     33.00  73.00   0.50    1.30    --  105.19 -61.00-180.00   80
 41  \w     41.00  91.00   0.50    1.30    --  105.19 -95.00-180.00  100
 42  \w     40.00  65.00   0.50    1.30    --  105.19-125.00  30.00   50
 43  \w     94.00 177.00   0.50    1.30    --  105.19  45.00  90.00  166
 44  \w     65.00 112.00   0.50    1.30    --  105.19-125.00-120.00   94
 45  \w     67.00 112.00   0.50    1.30    --  105.19-125.00 -60.00   90
 46  \w    120.00 173.00   0.50    1.30    --  105.19  45.00 -90.00  106
 47  \w     54.00  80.00   0.50    1.30    --  105.19 -95.00-120.00   52
;
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            69024
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.116
_diffrn_reflns_theta_min         3.562
_exptl_absorpt_coefficient_mu    8.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65219
_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    1.804
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.109(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5037
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0708P)^2^+11.8394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                4951
_reflns_number_total             5037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01360f2.cif
_cod_data_source_block           exp_243_auto
_cod_original_cell_volume        4898.84(6)
_cod_database_code               7710673
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.470
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.891(10)
 0.109(10)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
3. Restrained distances
 O2-H2
 0.85 with sigma of 0.02
 O1-H1
 0.85 with sigma of 0.02
 V1-H1
 2.5 with sigma of 0.02
 V2_$2-H1
 2.5 with sigma of 0.02
 V1-H1 \\sim V2_$2-H1
 with sigma of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
4.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N10(H10A,H10B), N4(H4A,H4B), N9(H9A,H9B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65236
_shelx_hkl_checksum              31975
_shelx_fab_checksum              71542
_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
;