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_7710100
_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 B Cr3 K4 O66 W12'
_chemical_formula_sum            'C6 H6 B Cr3 K4 O66 W12'
_chemical_formula_weight         3663.52
_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             2022-03-31
_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                   24.3679(4)
_cell_length_b                   15.9691(2)
_cell_length_c                   16.9507(2)
_cell_measurement_reflns_used    22804
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      30.4930
_cell_measurement_theta_min      2.5430
_cell_volume                     6596.08(16)
_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  (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.895
_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     68.00  94.00   0.50   10.81    --    5.00  45.00 150.00   52
  2  \w     49.00  74.00   0.50   10.81    --  -14.60  45.00   0.00   50
  3  \w    -12.00  14.00   0.50   10.81    --  -14.60  45.00   0.00   52
  4  \w    -99.00  73.00   0.50   10.81    --  -14.60  45.00 120.00  344
;
_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      0.0199931000
_diffrn_orient_matrix_UB_12      -0.0307590000
_diffrn_orient_matrix_UB_13      0.0092721000
_diffrn_orient_matrix_UB_21      0.0147327000
_diffrn_orient_matrix_UB_22      0.0105489000
_diffrn_orient_matrix_UB_23      -0.0347101000
_diffrn_orient_matrix_UB_31      0.0151801000
_diffrn_orient_matrix_UB_32      0.0302564000
_diffrn_orient_matrix_UB_33      0.0214562000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.432
_diffrn_reflns_theta_min         2.422
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Ultrax 18'
_exptl_absorpt_coefficient_mu    21.671
_exptl_absorpt_correction_T_max  0.01092
_exptl_absorpt_correction_T_min  0.00128
_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    3.689
_exptl_crystal_description       needle
_exptl_crystal_F_000             6444
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         5.975
_refine_diff_density_min         -2.674
_refine_diff_density_rms         0.628
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         9251
_refine_ls_number_restraints     958
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1045P)^2^+59.4398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8524
_reflns_number_total             9251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00478j2.cif
_cod_data_source_block           exp_174_sq
_cod_original_cell_volume        6596.11(16)
_cod_database_code               7710100
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         Cr3C4H4K4BW12O65
_shelx_estimated_absorpt_t_max   0.312
_shelx_estimated_absorpt_t_min   0.059
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. 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
3. 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
4. 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
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              21945
_shelx_fab_checksum              52449
_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 2.708
_oxdiff_exptl_absorpt_empirical_full_min 0.560