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_7134353
_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
'C48 H40 Nb2 O64 P8 S2 V14, C2 H8 N, C2 H7 N, 0.25[]'
_chemical_formula_sum            'C82 H161 N13 Nb2 O72 P8 S2 V14'
_chemical_formula_weight         3692.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-07
_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                 92.117(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4212(4)
_cell_length_b                   25.9376(5)
_cell_length_c                   29.3062(6)
_cell_measurement_reflns_used    31854
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.9050
_cell_measurement_theta_min      2.3310
_cell_volume                     13993.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.86a (Rigaku OD, 2023)'
_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      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.786
_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      2.00  29.00   0.50    5.00    --    3.55 -99.00  60.00   54
  2  \w     -7.00  70.00   0.50    5.00    --    3.55  57.00 120.00  154
  3  \w    -17.00  36.00   0.50    5.00    --    3.55 -99.00 -60.00  106
  4  \w    -62.00  -1.00   0.50    5.00    --   -6.91 -38.00-150.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0222533000
_diffrn_orient_matrix_UB_12      0.0219117000
_diffrn_orient_matrix_UB_13      0.0031888000
_diffrn_orient_matrix_UB_21      0.0299832000
_diffrn_orient_matrix_UB_22      0.0163331000
_diffrn_orient_matrix_UB_23      -0.0040414000
_diffrn_orient_matrix_UB_31      -0.0095552000
_diffrn_orient_matrix_UB_32      0.0001722000
_diffrn_orient_matrix_UB_33      -0.0236799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.786
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            105343
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.786
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.005
_diffrn_reflns_theta_min         2.029
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.86a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             7504
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.977
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         35067
_refine_ls_number_restraints     726
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0995P)^2^+41.2099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23624
_reflns_number_total             35067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01376c2.cif
_cod_data_source_block           phosphor_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7134353--7134356.cif.'
_cod_database_code               7134353
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'V O P'
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.777
_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
2. Uiso/Uaniso restraints and constraints
C7 \\sim C13 \\sim C31 \\sim C37 \\sim C1 \\sim C8 \\sim C43 \\sim C25 \\sim
C12 \\sim C10 \\sim C19 \\sim C14 \\sim C9 \\sim C11 \\sim C44 \\sim C38 \\sim
C30 \\sim C24 \\sim C20 \\sim C29 \\sim C6 \\sim C47 \\sim C27 \\sim C35 \\sim
C23 \\sim C4 \\sim C21 \\sim C42 \\sim C32 \\sim C36 \\sim C16 \\sim C18 \\sim
C48 \\sim C45 \\sim C15 \\sim C50 \\sim C33 \\sim C17 \\sim C39 \\sim C49 \\sim
C2 \\sim C28 \\sim C26 \\sim C22 \\sim C41 \\sim C40 \\sim C34 \\sim C46 \\sim
C3 \\sim C5: within 4A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 4A
3. Others
 Fixed Sof: H1B(0.5) H1A(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5)
 H52A(0.5) H52B(0.5) H52C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) H53C(0.5)
4.a Riding coordinates:
 N1(H1B), N1(H1A)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C8(H8), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C30(H30), C26(H26), C27(H27), C28(H28), C29(H29), C24(H24),
  C20(H20), C21(H21), C22(H22), C23(H23), C36(H36), C35(H35), C34(H34),
 C33(H33), C32(H32), C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C2(H2),
 C6(H6), C5(H5), C4(H4), C3(H3), C41(H41), C42(H42), C38(H38), C39(H39),
 C40(H40)
4.d Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C7,C8), C44(C45,C46,C47,C48,C43), C30(C25,C26,C27,C28,C29),
 C24(C19,C20,C21,C22,C23), C36(C35,C34,C33,C32,C31), C18(C17,C16,C15,C14,C13),
 C2(C1,C6,C5,C4,C3), C41(C42,C37,C38,C39,C40)
4.e Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              30820
_shelx_hkl_checksum              6285
_shelx_fab_checksum              9577
_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 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.856