Vanadium-substituted polycationic Al-oxo cluster in a porous ionic crystal exhibiting Lewis acidity
Zhou, Wei; Ogiwara, Naoki; Weng, Zhewei; Zhao, Congcong; Yan, Likai; Kikukawa, Yuji; Uchida, Sayaka; Chemical Communications  (2022) –; doi:10.1039/D2CC03545F

data_7130870
_publ_section_title
;
 Vanadium-substituted polycationic Al-oxo cluster in a porous ionic
 crystal exhibiting Lewis acidity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03545F
_journal_year                    2022
_chemical_formula_moiety         'O40 P V3 W9, Al13 O40, 24[H2O]'
_chemical_formula_sum            'Al13 H48 O104 P V3 W9'
_chemical_formula_weight         3901.56
_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_primary     dual
_audit_creation_date             2022-08-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-29 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.8523(4)
_cell_length_b                   13.8253(2)
_cell_length_c                   25.2206(4)
_cell_measurement_reflns_used    29669
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      30.3510
_cell_measurement_theta_min      2.3050
_cell_volume                     9711.6(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  (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 0.889
_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    -61.00 -35.00   0.50   36.44    --    5.00  45.00   0.00   52
  2  \w      0.00  38.00   0.50   36.44    --  -14.60  45.00  60.00   76
  3  \w    -90.00 -43.00   0.50   36.44    --  -14.60  45.00 150.00   94
  4  \w     44.00  70.00   0.50   36.44    --  -14.60  45.00 150.00   52
  5  \w   -104.00  26.00   0.50   36.44    --  -14.60  45.00  30.00  260
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            63808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.449
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Ultrax 18'
_exptl_absorpt_coefficient_mu    11.154
_exptl_absorpt_correction_T_max  0.02784
_exptl_absorpt_correction_T_min  0.00867
_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 orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.668
_exptl_crystal_description       block
_exptl_crystal_F_000             7196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         2.621
_refine_diff_density_min         -3.527
_refine_diff_density_rms         0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         13610
_refine_ls_number_restraints     2031
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0860
_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^)+(0.0395P)^2^+578.6611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.1991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11985
_reflns_number_total             13610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03545f2.cif
_cod_data_source_block           exp_182_sq
_cod_database_code               7130870
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.402
_shelx_estimated_absorpt_t_min   0.285
_olex2_refinement_description
;
1. Shared sites
{W1, V1}
{W2, V2}
{W3, V3}
{W4, V4}
{W5, V5}
{W6, V6}
{W7, V7}
2. Restrained distances
 W6-O26 \\sim W6-O25
 with sigma of 0.02
 V6-O26 \\sim V6-O25
 with sigma of 0.02
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(V1)
Uanis(W2) = Uanis(V2)
Uanis(W3) = Uanis(V3)
Uanis(W4) = Uanis(V4)
Uanis(W5) = Uanis(V5)
Uanis(W6) = Uanis(V6)
Uanis(W7) = Uanis(V7)
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
 1*[Sof(W1)+Sof(V1)]+1*[Sof(W2)+Sof(V2)]+1*[Sof(W3)+Sof(V3)]+0.5*[Sof(W4)+
 Sof(V4)]+1*[Sof(W5)+Sof(V5)]+0.5*[Sof(W6)+Sof(V6)]+1*[Sof(W7)+Sof(V7)]=4.5
 with esd of 0.0001
 Sof(V1)=1-FVAR(1)
 Sof(W1)=FVAR(1)
 Sof(V2)=1-FVAR(2)
 Sof(W2)=FVAR(2)
 Sof(V3)=1-FVAR(3)
 Sof(W3)=FVAR(3)
 Sof(V4)=0.5*(1-FVAR(5))
 Sof(W4)=0.5*FVAR(5)
 Sof(V5)=1-FVAR(5)
 Sof(W5)=FVAR(5)
 Sof(V6)=0.5*(1-FVAR(7))
 Sof(W6)=0.5*FVAR(7)
 Sof(V7)=1-FVAR(7)
 Sof(W7)=FVAR(7)
 Sof(O25)=0.5*(1-FVAR(9))
 Sof(O26)=0.5*FVAR(9)
;
_shelx_res_checksum              48957
_shelx_hkl_checksum              53507
_shelx_fab_checksum              65301
_platon_squeeze_special_details
'Precise number of lattice water molecules is calculated by TG analysis.'
_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
;