Basicity of Isostructural Porous Ionic Crystals Composed of Nb/Ta-Substituted Keggin-Type Polyoxotungstates
Weng, Zhewei; Ogiwara, Naoki; Yokogawa, Daisuke; Kitao, Takashi; Kikukawa, Yuji; Uchida, Sayaka; Dalton Transactions  (2022) –; doi:10.1039/D2DT00478J

data_7710102
_publ_section_title
;
 Basicity of Isostructural Porous Ionic Crystals Composed of
 Nb/Ta-Substituted Keggin-Type Polyoxotungstates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00478J
_journal_year                    2022
_chemical_formula_moiety         'C6 H6 Cr3 K4 O66 Si Ta1 W11'
_chemical_formula_sum            'C6 H6 Cr3 K4 O66 Si Ta W11'
_chemical_formula_weight         3677.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4565(4)
_cell_length_b                   16.0527(4)
_cell_length_c                   17.0555(4)
_cell_measurement_reflns_used    14901
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      30.4530
_cell_measurement_theta_min      2.4670
_cell_volume                     6695.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153.15
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Rigaku HyPix-6000 area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.896
_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   -104.00  66.00   0.50    4.11    --  -14.60  45.00  60.00  340
  2  \w    -17.00   8.00   0.50    4.11    --  -14.60  45.00 120.00   50
  3  \w     15.00  40.00   0.50    4.11    --  -14.60  45.00 120.00   50
  4  \w     -2.00  41.00   0.50    4.11    --  -14.60  45.00   0.00   86
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0184713000
_diffrn_orient_matrix_UB_12      0.0326678000
_diffrn_orient_matrix_UB_13      0.0089919000
_diffrn_orient_matrix_UB_21      -0.0138117000
_diffrn_orient_matrix_UB_22      -0.0264301000
_diffrn_orient_matrix_UB_23      0.0268042000
_diffrn_orient_matrix_UB_31      0.0175866000
_diffrn_orient_matrix_UB_32      0.0136191000
_diffrn_orient_matrix_UB_33      0.0305135000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1400
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41684
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.454
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Ultrax 18'
_exptl_absorpt_coefficient_mu    21.283
_exptl_absorpt_correction_T_max  0.01116
_exptl_absorpt_correction_T_min  0.00133
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.648
_exptl_crystal_description       block
_exptl_crystal_F_000             6476
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         9.382
_refine_diff_density_min         -3.224
_refine_diff_density_rms         0.900
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         9407
_refine_ls_number_restraints     1644
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.1052
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2644
_refine_ls_wR_factor_ref         0.2751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7365
_reflns_number_total             9407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00478j2.cif
_cod_data_source_block           cr-h-siw11ta_sq
_cod_database_code               7710102
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C4H4Cr3K4O61SiW11Ta
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.184
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{W1, Ta1}
{W2, Ta2}
{W3, Ta3}
{W4, Ta4}
{W5, Ta5}
{W6, Ta6}
{W7, Ta7}
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(W1) = Uanis(Ta1)
Uanis(W2) = Uanis(Ta2)
Uanis(W3) = Uanis(Ta3)
Uanis(W4) = Uanis(Ta4)
Uanis(W5) = Uanis(Ta5)
Uanis(W6) = Uanis(Ta6)
Uanis(W7) = Uanis(Ta7)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: W1(0.45833) W2(0.91667) W3(0.91667) W4(0.91667) W5(0.91667)
 W6(0.45833) W7(0.91667) Ta1(0.04167) Ta2(0.0833) Ta3(0.0833) Ta4(0.0833)
 Ta5(0.0833) Ta6(0.04167) Ta7(0.0833)
7.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C22(H22), C31(H31), C39(H39)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26382
_shelx_fab_checksum              16625
_platon_squeeze_void_probe_radius 1.20
_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 5.474
_oxdiff_exptl_absorpt_empirical_full_min 0.217