Docking rings in a solid: reversible assembling of pseudorotaxanes inside a zirconium metal–organic framework
Li, Xia; Xie, Jialin; Du, Zhenglin; Jiang, Long; Li, Guangqin; Ling, Sanliang; Zhu, Kelong; Chemical Science  (2022) –; doi:10.1039/D2SC01497A

data_1566953
_publ_section_title
;
 Docking rings in a solid: reversible assembling of pseudorotaxanes inside
 a zirconium metal--organic framework
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01497A
_journal_year                    2022
_chemical_formula_moiety         'C210 H128 N12 O32 Zr6, 35[H2O], 13[C3H7NO]'
_chemical_formula_sum            'C249 H289 N25 O80 Zr6'
_chemical_formula_weight         5459.35
_space_group_crystal_system      cubic
_space_group_IT_number           202
_space_group_name_Hall           '-F 2 2 3'
_space_group_name_H-M_alt        'F m -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-19 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.4865(7)
_cell_length_b                   38.4865(7)
_cell_length_c                   38.4865(7)
_cell_measurement_reflns_used    3597
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      43.6230
_cell_measurement_theta_min      4.9840
_cell_volume                     57006.6(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.00(10)
_diffrn_detector_area_resol_mean 10.5826
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9487
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        43.845
_diffrn_reflns_theta_max         43.845
_diffrn_reflns_theta_min         3.809
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36110
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.636
_exptl_crystal_description       block
_exptl_crystal_F_000             11352
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.679
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         1886
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      1.713
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.1352
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3408
_refine_ls_wR_factor_ref         0.3661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1442
_reflns_number_total             1886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01497a2.cif
_cod_data_source_block           fm-3_sq
_cod_original_cell_volume        57007(3)
_cod_database_code               1566953
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.909
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.528(14)
 0.472(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C3-C1 = C12-C10 = C19-C18 = C26-C15 = C35-C33
 1.5 with sigma of 0.02
 C1-O2 = C1-O3 = C35-O4 = C35-O5
 1.25 with sigma of 0.02
 N1-C17 = N1-C18 = N2-C18 = N2-C16
 1.35 with sigma of 0.02
 C16-C18 = C18-C17 = C17-N2 = N2-N1 = N1-C16
 2.35 with sigma of 0.02
 C1-C2 \\sim C1-C4 \\sim C10-C17 \\sim C10-C13 \\sim C12-C9 \\sim C12-C11 \\sim
C18-C20 \\sim C18-C24 ~
 C15-C25 \\sim C15-C27 \\sim C26-C14 \\sim C26-C16 \\sim C35-C32 \\sim C35-C34
 with sigma of 0.02
 O2-C3 \\sim O3-C3 \\sim O4-C33 \\sim O5-C33
 with sigma of 0.01
 N1-C19 \\sim N2-C19
 with sigma of 0.01
4. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12
 with sigma of 0.1
 C15, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35
 with sigma of 0.1
 O2, O3, C1, C3
 with sigma of 0.01
 O4, O5, C33, C35
 with sigma of 0.01
 N1, N2, C10, C12, C13, C14, C15, C16, C17, C18, C19, C26
 with sigma of 0.1
 C18, C19, C20, C21, C22, C23, C24
 with sigma of 0.1
5. Rigid bond restraints
 Zr1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim O4 \\sim O5 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3
\\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C24 \\sim
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C25 \\sim C26 \\sim C27 \\sim
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
7. Others
 Fixed Sof: H1A(0.33333) O2(0.25) O3(0.25) O4(0.25) O5(0.25) N1(0.25)
 H1(0.125) N2(0.25) H2(0.125) C1(0.25) C2(0.25) H2A(0.25) C3(0.25) C4(0.25)
 H4(0.25) C5(0.25) H5(0.25) C6(0.25) C7(0.25) C8(0.25) H8(0.25) C9(0.25)
 H9(0.25) C10(0.25) C11(0.25) H11(0.25) C12(0.25) C13(0.25) H13(0.25) C14(0.25)
 H14(0.25) C15(0.25) C16(0.25) C17(0.25) C18(0.25) C24(0.25) H24(0.25)
 C19(0.25) C20(0.25) H20(0.25) C21(0.25) H21(0.25) C22(0.25) H22(0.25)
 C23(0.25) H23(0.25) C25(0.25) H25(0.25) C26(0.25) C27(0.25) H27(0.25)
 C28(0.25) H28(0.25) C29(0.25) C30(0.25) C31(0.25) H31(0.25) C32(0.25)
 H32(0.25) C33(0.25) C34(0.25) H34(0.25) C35(0.25)
8.a Riding coordinates:
 O1(H1A)
8.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C13(H13),
 C14(H14), C24(H24), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C27(H27),
  C28(H28), C31(H31), C32(H32), C34(H34)
8.c Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C24(C19,C20,C21,C22,C23)
8.d Naphthalene refined as free rotating group:
 C2(C3,C4,C5,C6,C7,C8,C9,C10,C11), C25(C26,C27,C28,C29,C30,C31,C32,C33,C34)
;
_shelx_res_checksum              71504
_shelx_fab_checksum              49555
_platon_squeeze_special_details
;
A solvent mask was calculated and 3397 electrons were 
found in a volume of 31033\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
35[H2O], 13[C3H7NO] per Formula Unit 
which account for 3480 electrons 
per unit cell.

The solvent data was based on TG result.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'