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_7130871
_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
'2(O40 P V3 W9), Al28.667 O94 V3.133 W0.2, 52[H2O], 3[H2O]'
_chemical_formula_sum            'Al28.75 O174 P2 V9.11 W18.14'
_chemical_formula_weight         7421.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-07 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                   29.9847(5)
_cell_length_b                   27.7701(5)
_cell_length_c                   23.4604(5)
_cell_measurement_reflns_used    19787
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      29.9640
_cell_measurement_theta_min      2.7880
_cell_volume                     19535.0(6)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70791
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.054
_diffrn_reflns_theta_min         2.461
_exptl_absorpt_coefficient_mu    11.302
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.71016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.523
_exptl_crystal_description       block
_exptl_crystal_F_000             13391
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         13290
_refine_ls_number_restraints     1897
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+217.2995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9340
_reflns_number_total             13290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03545f2.cif
_cod_data_source_block           shelxl_sq
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7130871
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.344
_shelx_estimated_absorpt_t_min   0.282
_olex2_refinement_description
;
1. Shared sites
{W7, V7}
{W8, V8}
{W3, V3}
{W4, V4}
{W5, V5}
{W6, V6}
{W1, V1}
{Al2, V2}
2. Restrained distances
 Al10-O29 \\sim Al10-O29A
 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(W7) = Uanis(V7)
Uanis(W8) = Uanis(V8)
Uanis(W3) = Uanis(V3)
Uanis(W4) = Uanis(V4)
Uanis(W5) = Uanis(V5)
Uanis(W6) = Uanis(V6)
Uanis(W1) = Uanis(V1)
Uanis(Al2) = Uanis(V2)
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(W7)+Sof(V3)]+1*[Sof(W8)+Sof(V4)]+1*[Sof(W3)+Sof(V5)]+1*[Sof(W4)+
 Sof(V6)]+1*[Sof(W5)+Sof(V7)]+1*[Sof(W6)+Sof(V8)]=4.5 with esd of 0.0001
 Sof(V3)=1-FVAR(1)
 Sof(W7)=FVAR(1)
 Sof(V4)=1-FVAR(2)
 Sof(W8)=FVAR(2)
 Sof(V5)=1-FVAR(3)
 Sof(W3)=FVAR(3)
 Sof(V6)=1-FVAR(4)
 Sof(W4)=FVAR(4)
 Sof(V7)=1-FVAR(5)
 Sof(W5)=FVAR(5)
 Sof(V8)=1-FVAR(6)
 Sof(W6)=FVAR(6)
 Sof(W1)=0.5*(1-FVAR(8))
 Sof(V1)=0.5*FVAR(8)
 Sof(Al2)=0.5*(1-FVAR(9))
 Sof(V2)=0.5*FVAR(9)
 Sof(O29A)=1-FVAR(9)
 Sof(O29)=FVAR(9)
;
_shelx_res_checksum              49781
_shelx_hkl_checksum              23880
_shelx_fab_checksum              55710
_platon_squeeze_special_details
;
The number of water molecules given here is that found in this crystal, according 
to the number of electrons foundin the solvent mask. This number is somewhat higher 
than that determined by DSC.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'