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_7710101
_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 Nb1 O66 Si W11'
_chemical_formula_sum            'C6 H6 Cr3 K4 Nb O66 Si W11'
_chemical_formula_weight         3589.86
_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                   24.4216(4)
_cell_length_b                   16.0494(2)
_cell_length_c                   17.0259(2)
_cell_measurement_reflns_used    20399
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      30.3550
_cell_measurement_theta_min      2.5500
_cell_volume                     6673.34(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 10.0000
_diffrn_detector_type            'Rigaku HyPix-6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_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    -70.00 -44.00   0.50   15.51    --  -14.60  45.00   0.00   52
  2  \w     -1.00  48.00   0.50   15.51    --  -14.60  45.00   0.00   98
  3  \w   -104.00  74.00   0.50   15.51    --  -14.60  45.00 120.00  356
  4  \w   -101.00 -76.00   0.50   15.51    --  -14.60  45.00   0.00   50
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0167457000
_diffrn_orient_matrix_UB_12      -0.0297689000
_diffrn_orient_matrix_UB_13      0.0192784000
_diffrn_orient_matrix_UB_21      -0.0152746000
_diffrn_orient_matrix_UB_22      0.0056409000
_diffrn_orient_matrix_UB_23      0.0350364000
_diffrn_orient_matrix_UB_31      -0.0181700000
_diffrn_orient_matrix_UB_32      -0.0321652000
_diffrn_orient_matrix_UB_33      -0.0116727000
_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  0.0530
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44291
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.481
_diffrn_reflns_theta_min         2.392
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.888
_exptl_absorpt_correction_T_max  0.01232
_exptl_absorpt_correction_T_min  0.00164
_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    3.573
_exptl_crystal_description       block
_exptl_crystal_F_000             6348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         4.416
_refine_diff_density_min         -1.964
_refine_diff_density_rms         0.601
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9507
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7984
_reflns_number_total             9507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00478j2.cif
_cod_data_source_block           exp_195_sq
_cod_original_cell_volume        6673.31(17)
_cod_database_code               7710101
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C6H6Cr3K4NbO6SiW11
_shelx_estimated_absorpt_t_max   0.199
_shelx_estimated_absorpt_t_min   0.109
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{W2, Nb2}
{W3, Nb3}
{W4, Nb4}
{W5, Nb5}
{W6, Nb6}
{W7, Nb7}
3. Uiso/Uaniso restraints and constraints
Uanis(W2) = Uanis(Nb2)
Uanis(W3) = Uanis(Nb3)
Uanis(W4) = Uanis(Nb4)
Uanis(W5) = Uanis(Nb5)
Uanis(W6) = Uanis(Nb6)
Uanis(W7) = Uanis(Nb7)
4. Others
 1*[Sof(W2)+Sof(Nb2)]+1*[Sof(W3)+Sof(Nb3)]+1*[Sof(W4)+Sof(Nb4)]+0.5*[Sof(W5)+
 Sof(Nb5)]+1*[Sof(W6)+Sof(Nb6)]+1*[Sof(W7)+Sof(Nb7)]=5 with esd of 0.001
 Sof(Nb2)=1-FVAR(1)
 Sof(W2)=FVAR(1)
 Sof(Nb3)=1-FVAR(2)
 Sof(W3)=FVAR(2)
 Sof(Nb4)=1-FVAR(3)
 Sof(W4)=FVAR(3)
 Sof(Nb5)=0.5*(1-FVAR(5))
 Sof(W5)=0.5*FVAR(5)
 Sof(Nb6)=1-FVAR(5)
 Sof(W6)=FVAR(5)
 Sof(Nb7)=1-FVAR(6)
 Sof(W7)=FVAR(6)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C16(H16), C17(H17)
;
_shelx_res_checksum              3455
_shelx_fab_checksum              50772
_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 18.390
_oxdiff_exptl_absorpt_empirical_full_min 0.391