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_7131325
_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                   12.1518(3)
_cell_length_b                   20.0181(5)
_cell_length_c                   21.6563(7)
_cell_measurement_reflns_used    12513
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      75.1010
_cell_measurement_theta_min      3.0070
_cell_volume                     5268.0(3)
_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      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_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     35.00  93.00   0.50    0.63    --   47.12-121.00 147.00  116
  2  \w    -96.00 -50.00   0.50    2.51    -- -100.00 108.00 -30.00   92
  3  \w    146.00 178.00   0.50    2.51    --  107.75  20.00 157.00   64
  4  \w    100.00 126.00   0.50    2.51    --  107.75  20.00 157.00   52
  5  \w     32.00  60.00   0.50    0.63    --   47.12 -37.00 -90.00   56
  6  \w     89.00 119.00   0.50    0.63    --   47.12 125.00-180.00   60
  7  \w    -27.00   8.00   0.50    0.63    --   47.12 -37.00 -90.00   70
  8  \w     32.00 117.00   0.50    0.63    --   47.12  57.00-120.00  170
  9  \w   -115.00 -89.00   0.50    2.51    -- -100.00  30.00 -90.00   52
 10  \w   -114.00 -41.00   0.50    2.51    -- -100.00  45.00-180.00  146
 11  \w   -117.00 -55.00   0.50    2.51    -- -100.00  61.00-180.00  124
 12  \w    -78.00 -25.00   0.50    2.51    -- -100.00  30.00 -90.00  106
 13  \w   -106.00 -29.00   0.50    2.51    -- -100.00  45.00 -90.00  154
 14  \w    112.00 173.00   0.50    2.51    --  107.75  45.00-150.00  122
 15  \w     60.00  99.00   0.50    2.51    --  107.75 -94.00 -90.00   78
 16  \w     73.00 106.00   0.50    2.51    --  107.75 -94.00-150.00   66
 17  \w     89.00 114.00   0.50    2.51    --  107.75-121.00 147.00   50
 18  \w     40.00  65.00   0.50    2.51    --  107.75-121.00 147.00   50
;
_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      -0.0226507000
_diffrn_orient_matrix_UB_12      -0.0755150000
_diffrn_orient_matrix_UB_13      -0.0048333000
_diffrn_orient_matrix_UB_21      0.1211169000
_diffrn_orient_matrix_UB_22      -0.0120560000
_diffrn_orient_matrix_UB_23      -0.0177658000
_diffrn_orient_matrix_UB_31      0.0296050000
_diffrn_orient_matrix_UB_32      -0.0084028000
_diffrn_orient_matrix_UB_33      0.0687698000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29117
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.434
_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    8.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84604
_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 colourless'
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 2415 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         10518
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1215P)^2^+1.8506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2272
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                7527
_reflns_number_total             10518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06951b2.cif
_cod_data_source_block           20220710-yww-p5-ag
_cod_database_code               7131325
_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
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Others
 Sof(Ag3)=1-FVAR(1)
 Sof(Ag2)=FVAR(1)
 Fixed Sof: Ag1(0.76) Ag4(0.12) Ag5(0.12)
4.a Ternary CH refined with riding coordinates:
 C48(H48)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C22(H22A,H22B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C11(H11), C13(H13), C20(H20), C21(H21), C27(H27), C28(H28),
 C31(H31), C34(H34)
4.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), 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 2.996
_oxdiff_exptl_absorpt_empirical_full_min 0.345