Handcuff-like metallo-pseudorotaxanes consisting of tiara[5]arene wheels and dimeric silver trifluoroacetate axles.
Yang, Weiwei; Wang, Haiying; Chang, Rong; Feng, Zhitao; Zhu, Yumei; Sue, Andrew C.-H.; Chemical communications (Cambridge, England) 59 (2023) 2457–2460; doi:10.1039/d2cc06951b

data_7131323
_publ_section_title
;
 Handcuff-like metallo-pseudorotaxanes consisting of tiara[5]arene wheels
 and dimeric silver trifluoroacetate axles.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2457
_journal_page_last               2460
_journal_paper_doi               10.1039/d2cc06951b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety
'Ag C2 F3 O2, Ag1.82 C4 F6 O4, C40 H40 O5, 0.18(Ag)'
_chemical_formula_sum            'C46 H40 Ag3 F9 O11'
_chemical_formula_weight         1263.39
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-15 deposited with the CCDC.	2023-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.34190(10)
_cell_length_b                   20.96220(10)
_cell_length_c                   18.15160(10)
_cell_measurement_reflns_used    44836
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      74.5940
_cell_measurement_theta_min      2.0810
_cell_volume                     4656.22(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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    -56.00 -24.00   0.50    0.05    --  -45.87  66.00-115.00   64
  2  \w    -20.00   7.00   0.50    0.05    --  -45.87  66.00-115.00   54
  3  \w   -118.00 -35.00   0.50    0.05    --  -45.87 -66.00 110.00  166
  4  \w     32.00  65.00   0.50    0.05    --   45.87 -66.00 110.00   66
  5  \w    -85.00 -34.00   0.50    0.22    -- -100.00  66.00-115.00  102
  6  \w   -151.00-125.00   0.50    0.22    -- -100.00 -66.00 110.00   52
  7  \w    129.00 175.00   0.50    0.22    --  101.75  66.00-115.00   92
  8  \w     39.00  76.00   0.50    0.22    --  101.75 -66.00 110.00   74
  9  \w   -118.00 -75.00   0.50    0.05    --  -45.87-125.00 -90.00   86
 10  \w    -44.00  28.00   0.50    0.05    --  -45.87  38.00 120.00  144
 11  \w    -29.00   3.00   0.50    0.05    --   45.87 -19.00 120.00   64
 12  \w    -24.00  59.00   0.50    0.05    --   45.87 -57.00 -90.00  166
 13  \w     49.00  74.00   0.50    0.05    --   45.87  66.00-115.00   50
 14  \w     31.00 116.00   0.50    0.05    --   45.87  38.00   0.00  170
 15  \w     12.00  61.00   0.50    0.05    --   45.87 -19.00 120.00   98
 16  \w   -128.00-102.00   0.50    0.22    -- -100.00 -15.00   0.00   52
 17  \w   -114.00 -65.00   0.50    0.22    -- -100.00  45.00   0.00   98
 18  \w   -118.00 -25.00   0.50    0.22    -- -100.00  15.00   0.00  186
 19  \w   -117.00 -50.00   0.50    0.22    -- -100.00 125.00  90.00  134
 20  \w   -172.00 -82.00   0.50    0.22    -- -100.00 -61.00  30.00  180
 21  \w   -115.00 -88.00   0.50    0.22    -- -100.00  30.00  90.00   54
 22  \w   -172.00 -85.00   0.50    0.22    -- -100.00 -45.00 -30.00  174
 23  \w   -145.00 -86.00   0.50    0.22    -- -100.00 -45.00 -60.00  118
 24  \w   -137.00 -92.00   0.50    0.22    -- -100.00 -45.00   0.00   90
 25  \w   -171.00 -83.00   0.50    0.22    -- -100.00 -61.00-180.00  176
 26  \w   -170.00-142.00   0.50    0.22    -- -100.00 -45.00   0.00   56
 27  \w    -60.00 -35.00   0.50    0.22    -- -100.00  45.00   0.00   50
 28  \w    -57.00 -25.00   0.50    0.22    -- -100.00  30.00  90.00   64
 29  \w     85.00 110.00   0.50    0.22    --  101.75  61.00   0.00   50
 30  \w     88.00 163.00   0.50    0.22    --  101.75  45.00 -90.00  150
 31  \w     29.00  98.00   0.50    0.22    --  101.75 -94.00 -60.00  138
 32  \w     30.00 116.00   0.50    0.22    --  101.75 -45.00 120.00  172
 33  \w     79.00 106.00   0.50    0.22    --  101.75 -94.00-150.00   54
 34  \w     36.00  61.00   0.50    0.22    --  101.75 -94.00-150.00   50
 35  \w    146.00 172.00   0.50    0.22    --  101.75  30.00  30.00   52
 36  \w     87.00 125.00   0.50    0.22    --  101.75  30.00  30.00   76
 37  \w     43.00  94.00   0.50    0.22    --  101.75 -94.00 120.00  102
 38  \w     61.00 109.00   0.50    0.22    --  101.75 -94.00 -30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0460748000
_diffrn_orient_matrix_UB_12      0.0558997000
_diffrn_orient_matrix_UB_13      -0.0495980000
_diffrn_orient_matrix_UB_21      -0.1066547000
_diffrn_orient_matrix_UB_22      -0.0025311000
_diffrn_orient_matrix_UB_23      0.0355783000
_diffrn_orient_matrix_UB_31      0.0484664000
_diffrn_orient_matrix_UB_32      0.0476489000
_diffrn_orient_matrix_UB_33      0.0600094000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62012
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.711
_diffrn_reflns_theta_min         3.236
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.875
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.846
_refine_diff_density_min         -1.694
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9339
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0731P)^2^+19.4677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8517
_reflns_number_total             9339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06951b2.cif
_cod_data_source_block           yww-161-ag
_cod_database_code               7131323
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Ag3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 1*[Sof(Ag2A)]+1*[Sof(Ag2B)]+1*[Sof(Ag3)]=1 with esd of 0.001
 Sof(Ag1B)=1-FVAR(1)
 Sof(Ag1A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b), C40(H40a,H40b), C24(H24a,H24b), C16(H16a,H16b), C8(H8a,H8b)
4.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C21(H21), C30(H30), C14(H14), C2(H2), C13(H13), C26(H26), C18(H18),
 C27(H27), C38(H38), C6(H6), C37(H37), C10(H10), C5(H5), C22(H22)
4.c Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C23(H23a,H23b,H23c), C7(H7a,H7b,H7c), C15(H15a,H15b,
 H15c), C39(H39a,H39b,H39c)
;
_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 2.530
_oxdiff_exptl_absorpt_empirical_full_min 0.432