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_7710671
_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         'C24 H24 N8 Na2 O21 V4, 2(H2 N)'
_chemical_formula_sum            'C24 H40 N10 Na2 O27 V4'
_chemical_formula_weight         1150.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_formula_units_Z            4
_cell_length_a                   12.6075(5)
_cell_length_b                   19.6716(6)
_cell_length_c                   19.2268(6)
_cell_measurement_reflns_used    4521
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.9670
_cell_measurement_theta_min      4.1390
_cell_volume                     4768.4(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    '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 0.995
_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     39.00  71.00   0.50    2.00    --  105.19 -61.00-150.00   64
  2  \w     44.00  71.00   0.50    2.00    --  105.19 -61.00 -90.00   54
  3  \w     33.00  58.00   0.50    2.00    --  105.19 -61.00 -30.00   50
  4  \w     33.00  58.00   0.50    2.00    --  105.19 -61.00  30.00   50
  5  \w    -25.00  27.00   0.50    0.50    --   47.87 -19.00 -30.00  104
  6  \w     42.00  68.00   0.50    2.00    --  105.19 -61.00 120.00   52
  7  \w    104.00 168.00   0.50    2.00    --  105.19  45.00  30.00  128
  8  \w   -155.00-107.00   0.50    2.00    --  -99.00 -47.00 143.00   96
  9  \w   -119.00 -46.00   0.50    0.50    --  -47.87 -47.00 143.00  146
 10  \w   -105.00 -74.00   0.50    0.50    --  -47.87-125.00  90.00   62
 11  \w   -108.00 -75.00   0.50    0.50    --  -47.87-125.00 -60.00   66
 12  \w   -104.00 -29.00   0.50    2.00    --  -99.00 120.00 159.00  150
 13  \w    -68.00 -42.00   0.50    2.00    --  -99.00  61.00 150.00   52
 14  \w    -88.00 -27.00   0.50    2.00    --  -99.00  74.00  87.00  122
;
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9530
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        66.989
_diffrn_reflns_theta_max         66.989
_diffrn_reflns_theta_min         4.165
_exptl_absorpt_coefficient_mu    7.416
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57359
_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    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.719
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.092(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4005
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1590P)^2^+3.4443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2087
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.873
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                3577
_reflns_number_total             4005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01360f2.cif
_cod_data_source_block           exp_246_auto
_cod_database_code               7710671
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.524
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.908(19)
 0.092(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O10-H10
 0.85 with sigma of 0.02
 H5-O5
 0.85 with sigma of 0.02
 H5-V1
 2.45 with sigma of 0.02
 V2-H5
 2.45 with sigma of 0.02
 H10-H10_$3
 3.1 with sigma of 0.02
 H5_$3-H5
 3.1 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O1W(0.5)
6.a Riding coordinates:
 N5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C1(H1), C2(H2), C9(H9)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C4(H4A,H4B,H4C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32737
_shelx_hkl_checksum              93712
_shelx_fab_checksum              90897
_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
;