An open hollow polyoxovanadate cage based on {Nb(V5)} pentagons with size-selective encapsulation properties
Fang, Renbo; Zhang, Di; Dong, Jing; Feng, Yeqin; Liu, Chengpeng; Yao, Liaoyuan; Chi, Yingnan; Hu, Changwen; Chemical Communications 61 (2025) 6182–6185; doi:10.1039/D5CC01376C

data_7134354
_publ_section_title
;
 An open hollow polyoxovanadate cage based on {Nb(V5)} pentagons with
 size-selective encapsulation properties
;
_journal_issue                   33
_journal_name_full               'Chemical Communications'
_journal_page_first              6182
_journal_page_last               6185
_journal_paper_doi               10.1039/D5CC01376C
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C12.25 H11.75 Cs1.063 N0.125 Nb0.5 O18.25 P2 S V3.5, 0.125(O), 0.5(C2 H8 N), 0.25(C2 H6 O0.25)'
_chemical_formula_sum            'C72 H135 Cs4 N11 Nb2 O72 P8 S4 V14'
_chemical_formula_weight         4113.52
_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     iterative
_audit_creation_date             2025-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-12 deposited with the CCDC.	2025-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.0643(4)
_cell_length_b                   31.9841(7)
_cell_length_c                   16.5506(3)
_cell_measurement_reflns_used    27361
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      30.8770
_cell_measurement_theta_min      3.3030
_cell_volume                     13797.3(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku (Mo) X-ray Source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            69343
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.191
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31226
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    7.921
_exptl_crystal_description       block
_exptl_crystal_F_000             32448
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.168
_refine_diff_density_min         -5.516
_refine_diff_density_rms         0.341
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         12365
_refine_ls_number_restraints     2482
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.1161
_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^)+(0.2380P)^2^+395.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3388
_refine_ls_wR_factor_ref         0.3531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10147
_reflns_number_total             12365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01376c2.cif
_cod_data_source_block           aaa_a_sq
_cod_depositor_comments
'Adding full bibliography for 7134353--7134356.cif.'
_cod_database_code               7134354
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.333
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 S2-O35 = S2A-O35
 1.45 with sigma of 0.5
 Nb1-O35
 2.2 with sigma of 0.5
 C28-N1
 1.2 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O40 \\sim O37 \\sim O9 \\sim O16 \\sim O32 \\sim O10 \\sim O18 \\sim O8 \\sim
O31 \\sim O17 \\sim O25 \\sim O30 \\sim O28 \\sim O24 \\sim O27 \\sim O29 \\sim
O21 \\sim O19 \\sim O20 \\sim O23 \\sim O2 \\sim O33 \\sim O1 \\sim O3 \\sim O5
\\sim O39 \\sim O4 \\sim O13 \\sim O11 \\sim O7 \\sim O15 \\sim O26 \\sim O12
\\sim O6 \\sim O34 \\sim O22 \\sim O14 \\sim O42 \\sim O41 \\sim O43 \\sim O35
\\sim O36 \\sim O38 \\sim V3 \\sim V2 \\sim V4 \\sim V1 \\sim V5 \\sim V6 \\sim
V7 \\sim V9 \\sim V8 \\sim Nb1 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim
C15 \\sim C14 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C8 \\sim C7 \\sim C12 \\sim C11 \\sim C10 \\sim C9 \\sim C5 \\sim C4 \\sim C3
\\sim C2 \\sim C1 \\sim C6 \\sim C26 \\sim C25 \\sim C29 \\sim C27 \\sim C28
\\sim P3 \\sim P4 \\sim P1 \\sim P2 \\sim S1 \\sim S2 \\sim S2A: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cs2(0.25) O17(0.5) H33A(0.5) H33B(0.5) O34(0.25) Cs1(0.375)
 O43(0.125) C27(0.25) H27A(0.25) H27B(0.25) H27C(0.25) C28(0.25) H28A(0.25)
 H28B(0.25) H28C(0.25) N1(0.25) H1A(0.5) H1B(0.5) S2(0.5) O36(0.5) S2A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 O33(H33A,H33B), N2(H2A,H2B), N1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C8(H8), C12(H12), C11(H11), C10(H10), C9(H9),
 C5(H5), C4(H4), C3(H3), C2(H2), C6(H6)
5.c Fitted hexagon refined as free rotating group:
 C13(C18,C17,C16,C15,C14), C19(C20,C21,C22,C23,C24), C8(C7,C12,C11,C10,C9),
 C5(C4,C3,C2,C1,C6)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              55710
_shelx_hkl_checksum              75144
_shelx_fab_checksum              97437
_olex2_submission_special_instructions 'No special instructions were received'