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_7131324
_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         'Ag2 C4 F6 O4, C H Cl3, C45 H50 O10'
_chemical_formula_sum            'C50 H51 Ag2 Cl3 F6 O14'
_chemical_formula_weight         1311.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.10780(10)
_cell_length_b                   20.0062(2)
_cell_length_c                   21.6776(2)
_cell_measurement_reflns_used    19450
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      73.3070
_cell_measurement_theta_min      3.0160
_cell_volume                     5250.99(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.977
_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     25.00  84.00   0.50    0.05    --   35.61-102.00  80.00  118
  2  \w   -105.00 -40.00   0.50    0.15    -- -100.00 113.00 -88.00  130
  3  \w   -177.00-132.00   0.50    0.15    -- -100.00 -26.00 -95.00   90
  4  \w    -93.00 -54.00   0.50    0.15    -- -100.00 -26.00 -95.00   78
  5  \w     27.00 110.00   0.50    0.15    --  109.32-102.00  80.00  166
  6  \w    100.00 127.00   0.50    0.15    --  109.32 102.00-176.00   54
  7  \w    -37.00  82.00   0.50    0.05    --   35.61 -26.00 -95.00  238
  8  \w      7.00 112.00   0.50    0.05    --   35.61  77.00-180.00  210
  9  \w    -69.00 -19.00   0.50    0.15    -- -100.00 111.00  30.00  100
 10  \w   -137.00 -89.00   0.50    0.15    -- -100.00 179.00  60.00   96
 11  \w    -70.00 -45.00   0.50    0.15    -- -100.00 179.00  60.00   50
 12  \w     88.00 178.00   0.50    0.15    --  109.32 111.00 120.00  180
 13  \w     49.00  75.00   0.50    0.15    --  109.32 -94.00 120.00   52
 14  \w     36.00  73.00   0.50    0.15    --  109.32 -94.00 -30.00   74
 15  \w     29.00 112.00   0.50    0.15    --  109.32-111.00 -90.00  166
 16  \w     78.00 106.00   0.50    0.15    --  109.32 -94.00 -30.00   56
 17  \w     71.00 172.00   0.50    0.15    --  109.32  77.00-120.00  202
;
_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      -0.0813975000
_diffrn_orient_matrix_UB_12      -0.0532441000
_diffrn_orient_matrix_UB_13      -0.0239077000
_diffrn_orient_matrix_UB_21      0.0904305000
_diffrn_orient_matrix_UB_22      -0.0538106000
_diffrn_orient_matrix_UB_23      0.0060775000
_diffrn_orient_matrix_UB_31      -0.0375286000
_diffrn_orient_matrix_UB_32      -0.0140871000
_diffrn_orient_matrix_UB_33      0.0666024000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26674
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.742
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30233
_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            'clear light colourless'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 3911 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10225
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1033P)^2^+9.4501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                9688
_reflns_number_total             10225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06951b2.cif
_cod_data_source_block           20210907-yww-dmp5-ag-2
_cod_database_code               7131324
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.98
_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. Rigid bond restraints
 O13, Ag3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Ag2, O13
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O13: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Sof(Ag3)=1-FVAR(1)
 Sof(Ag2)=FVAR(1)
 Sof(Ag4)=1-FVAR(2)
 Sof(Ag1)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C13(H13A,H13B), C31(H31A,H31B), C39(H39A,H39B), C40(H40A,H40B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C16(H16), C17(H17), C19(H19), C21(H21), C23(H23), C25(H25),
 C32(H32), C35(H35)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_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 3.339
_oxdiff_exptl_absorpt_empirical_full_min 0.436