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_7134356
_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
'C55 H44 N Nb2 O66 P8 S2 V14, 4(C2 H8 N), 2(C2 H7 N), C2.1 H6.3 N, C3 H7 N O, C H3 O, C H4 O'
_chemical_formula_sum            'C80 H152 N11 Nb2 O70 P8 S2 V14'
_chemical_formula_weight         3598.98
_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             2025-03-12
_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                 90.2780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0624(3)
_cell_length_b                   25.9485(4)
_cell_length_c                   29.2392(5)
_cell_measurement_reflns_used    32956
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      31.2170
_cell_measurement_theta_min      3.2160
_cell_volume                     13704.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_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      150.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72059
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.217
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47289
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             7300
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.548
_refine_diff_density_min         -2.759
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1617
_refine_ls_number_reflns         23827
_refine_ls_number_restraints     6343
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1561P)^2^+125.9220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2470
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19236
_reflns_number_total             23827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01376c2.cif
_cod_data_source_block           1_a_sq
_cod_depositor_comments
'Adding full bibliography for 7134353--7134356.cif.'
_cod_database_code               7134356
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.731
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 P4, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 V4, O5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.05
 V4, O17
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.05
 V4, O18
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.05
 V7, O40
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.05
 V7, O52
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.02
 V7, O53
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
O61 \\sim O65 \\sim O66 \\sim O53 \\sim O17 \\sim O11 \\sim O34 \\sim O42 \\sim
O43 \\sim O37 \\sim O40 \\sim O15 \\sim O38 \\sim O21 \\sim O46 \\sim O50 \\sim
O19 \\sim O6 \\sim O36 \\sim O48 \\sim O39 \\sim O22 \\sim O28 \\sim O20 \\sim
O30 \\sim O65A \\sim O66A \\sim O32 \\sim O23 \\sim O14 \\sim O31 \\sim O24
\\sim O63 \\sim O18 \\sim O52 \\sim O10 \\sim O45 \\sim O55 \\sim O47 \\sim O9
\\sim O60 \\sim O56 \\sim O49 \\sim O33 \\sim O12 \\sim O29 \\sim O44 \\sim O26
\\sim O1 \\sim O58 \\sim O4 \\sim O8 \\sim O62 \\sim O54 \\sim O35 \\sim O5
\\sim O13 \\sim O16 \\sim O64 \\sim O3 \\sim O7 \\sim O2 \\sim O51 \\sim O59
\\sim O25 \\sim O57 \\sim O41 \\sim O27 \\sim O68 \\sim O69 \\sim O67 \\sim V1
\\sim V5 \\sim V4 \\sim V3 \\sim V2 \\sim V7 \\sim V8 \\sim V12 \\sim V9 \\sim
V11 \\sim V6 \\sim V13 \\sim V10 \\sim V14 \\sim Nb1 \\sim Nb2 \\sim P3 \\sim
P4 \\sim P6 \\sim P5 \\sim P1 \\sim P2 \\sim P8 \\sim P7 \\sim C7 \\sim C12
\\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C38 \\sim C37 \\sim C42 \\sim C41
\\sim C40 \\sim C39 \\sim C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31
\\sim C47 \\sim C46 \\sim C45 \\sim C44 \\sim C43 \\sim C48 \\sim C2 \\sim C1
\\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C15 \\sim C16 \\sim C17 \\sim C18
\\sim C13 \\sim C14 \\sim C27 \\sim C26 \\sim C25 \\sim C30 \\sim C29 \\sim C28
\\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C57 \\sim C56
\\sim C54 \\sim C52 \\sim C77 \\sim C66 \\sim C76 \\sim C69 \\sim C67 \\sim C68
\\sim C62 \\sim C65 \\sim C72 \\sim C73 \\sim C58 \\sim C59 \\sim C53A \\sim
C51A \\sim C55A \\sim C57A \\sim C56A \\sim C55 \\sim C51 \\sim C63 \\sim C64
\\sim C53 \\sim C70 \\sim C75 \\sim C74 \\sim C60 \\sim C71 \\sim C61 \\sim C86
\\sim N1 \\sim N2 \\sim N8 \\sim N9 \\sim N7 \\sim N6 \\sim N1A \\sim N5 \\sim
N3 \\sim N4: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
V7 \\sim O40: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
V7 \\sim O52: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.04 within 2A
V7 \\sim O53: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
V4 \\sim O5: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
V4 \\sim O17: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
V4 \\sim O18: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(N6) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C57(0.5) C56(0.5) C62(0.6) H62A(0.6) H62B(0.6) H62C(0.6) C65(0.5)
 H65A(0.5) H65B(0.5) H65C(0.5) C53A(0.5) H53A(0.5) C51A(0.5) H51A(0.5)
 C55A(0.5) H55A(0.5) C57A(0.5) C56A(0.5) C55(0.5) H55(0.5) C51(0.5) H51(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5)
 N1(0.5) N1A(0.5) C53(0.5) H53(0.5) O65(0.5) O66(0.5) O65A(0.5) O66A(0.5)
5.a Riding coordinates:
 N8(H8A)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), N2(H2A,H2B), N9(H9A,H9B), N5(H5A,H5B), N3(H3A,H3B), N4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C10(H10), C9(H9), C8(H8), C38(H38), C42(H42), C41(H41),
 C40(H40), C39(H39), C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C47(H47),
  C46(H46), C45(H45), C44(H44), C48(H48), C2(H2), C6(H6), C5(H5), C4(H4),
 C3(H3), C15(H15), C16(H16), C17(H17), C18(H18), C14(H14), C27(H27), C26(H26),
 C30(H30), C29(H29), C28(H28), C21(H21), C22(H22), C23(H23), C24(H24),
 C53A(H53A), C51A(H51A), C55A(H55A), C55(H55), C51(H51), C53(H53), C60(H60)
5.d Fitted hexagon refined as free rotating group:
 C7(C12,C11,C10,C9,C8), C38(C37,C42,C41,C40,C39), C36(C35,C34,C33,C32,C31),
 C47(C46,C45,C44,C43,C48), C2(C1,C6,C5,C4,C3), C15(C16,C17,C18,C13,C14),
 C27(C26,C25,C30,C29,C28), C19(C20,C21,C22,C23,C24)
5.e X=CH2 refined with riding coordinates:
 C72(H72A,H72B)
5.f Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C66(H66A,H66B,H66C), C76(H76A,H76B,H76C), C69(H69A,H69B,
 H69C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C62(H62A,H62B,H62C), C65(H65A,
 H65B,H65C), C73(H73A,H73B,H73C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C75(H75A,H75B,
 H75C), C74(H74A,H74B,H74C), C71(H71A,H71B,H71C), C61(H61A,H61B,H61C), C86(H86A,
 H86B,H86C)
5.g Idealised tetrahedral OH refined as rotating group:
 O67(H67)
;
_shelx_res_checksum              30657
_shelx_hkl_checksum              64745
_shelx_fab_checksum              45637
_olex2_submission_special_instructions 'No special instructions were received'