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_1566952
_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         '2(C2 H6 O S), C35 H22 N2 O4'
_chemical_formula_sum            'C39 H34 N2 O6 S2'
_chemical_formula_weight         690.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-19 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                93.222(2)
_cell_angle_beta                 99.421(2)
_cell_angle_gamma                100.5780(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9015(3)
_cell_length_b                   11.8523(4)
_cell_length_c                   14.5872(4)
_cell_measurement_reflns_used    9163
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.267
_cell_measurement_theta_min      2.682
_cell_volume                     1653.52(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26660
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         59.368
_diffrn_reflns_theta_min         2.682
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1027 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8817.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7157
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0700P)^2^+2.1042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5454
_reflns_number_total             7157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01497a2.cif
_cod_data_source_block           b20122905a1526_0m
_cod_database_code               1566952
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.930
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O002-H002
 1 with sigma of 0.02
 S1-C3 = S1A-C3A
 1.7 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.04
 O2-C3 \\sim O2A-C3A
 with sigma of 0.04
 O2-C4 \\sim O2A-C4A
 with sigma of 0.04
 S1-C3 \\sim S1A-C3A
 with sigma of 0.02
 S1-C4 \\sim S1A-C4A
 with sigma of 0.02
 S1-O2 \\sim S1A-O2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim S1 \\sim C3 \\sim C4: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
O2A \\sim S1A \\sim C3A \\sim C4A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O2A)=Sof(S1A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(S1)=Sof(O2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N006(H006), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K),
 C00L(H00L), C00M(H00M), C00R(H00R), C00T(H00T), C00U(H00U), C00Z(H00Z),
 C010(H010), C012(H012), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C01A(H01A)
5.b Idealised Me refined as rotating group:
 C019(H01B,H01C,H01D), C01B(H01E,H01F,H01G), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC)
;
_olex2_submission_special_instructions 'No special instructions were received'