Encapsulation of the vanadium substituted Keggin polyoxometalates [α-PVW<sub>11</sub>O<sub>40</sub>]<sup>4-</sup> and [α-PV<sub>2</sub>W<sub>10</sub>O<sub>40</sub>]<sup>5-</sup> in HKUST-1.
Orozco, José C; Shuaib, Damola T.; Swenson, LaSalle; Chen, Ying-Pin; Chen, Yu-Sheng; Khan, M. Ishaque; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15913–15919; doi:10.1039/d4dt01705f

data_7716986
_publ_section_title
;
 Encapsulation of the vanadium substituted Keggin polyoxometalates
 [&#x3b1;-PVW<sub>11</sub>O<sub>40</sub>]<sup>4-</sup> and
 [&#x3b1;-PV<sub>2</sub>W<sub>10</sub>O<sub>40</sub>]<sup>5-</sup> in
 HKUST-1.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15913
_journal_page_last               15919
_journal_paper_doi               10.1039/d4dt01705f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'(C72 H24 Cu12 O48) (O40 P V W11)4- 2*(C4 H12 N+) 12*(H2O)@Cu 10(H2O) 2(H3O+)'
_chemical_formula_sum            'C80 H98 Cu12 N2 O112 P V W11'
_chemical_formula_weight         5746.34
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-15 deposited with the CCDC.	2024-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.2682(12)
_cell_length_b                   26.2682(12)
_cell_length_c                   26.2682(12)
_cell_measurement_reflns_used    4079
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      10.61
_cell_measurement_theta_min      2.21
_cell_volume                     18125.5(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'huber 3-circle'
_diffrn_measurement_method       '\phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1620
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            99252
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        13.896
_diffrn_reflns_theta_max         13.896
_diffrn_reflns_theta_min         0.901
_diffrn_source                   'synchrotron at Advanced Photo Source'
_diffrn_source_current           103.0
_diffrn_source_power             103.0
_diffrn_source_voltage           1000.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1482 before and 0.1047 after correction.
The Ratio of minimum to maximum transmission is 0.9067.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_meas      ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             10752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.585
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         812
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+54.9215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                631
_reflns_number_total             812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01705f2.cif
_cod_data_source_block           w11_final
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716986--7716987.cif.
;
_cod_original_cell_volume        18126(2)
_cod_database_code               7716986
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.822
_olex2_refinement_description
;
1. Shared sites
{W1, V1}
{O2W, O2U}
2. Restrained distances
 N1S-C1S
 1.5 with sigma of 0.01
 O2U-H2UA = O2U-H2UB = O2U-H2UC
 0.95 with sigma of 0.05
 H2UC-H2UA = H2UC-H2UB
 1.52 with sigma of 0.05
 H2UC-H2UA \\sim H2UC-H2UB \\sim H2UA-H2UB
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(V1)
Uanis(O2W) = Uanis(O2U)
4. Others
 Fixed Sof: W1(0.229175) V1(0.020825) O4(0.083333) H1SA(0.08335) H1SB(0.08335)
 H1SC(0.08335) O1W(0.25) H1WA(0.125) H1WB(0.25) O2W(0.20835) H(0.2083)
 HA(0.10415) O2U(0.04165) H2UA(0.0417) H2UB(0.04165) H2UC(0.0417)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H,HA)
5.b Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_checksum              37650
_olex2_submission_special_instructions 'No special instructions were received'