Restricting shuttling in bis(imidazolium)…pillar[5]arene rotaxanes using metal coordination.
Langer, Philipp; Yang, Lixu; Pfeiffer, Constance R.; Lewis, William; Champness, Neil R.; Dalton transactions (Cambridge, England : 2003) 48 (2018) 58–64; doi:10.1039/c8dt04096f

data_7047993
_publ_section_title
;
 Restricting shuttling in bis(imidazolium)&#x2026;pillar[5]arene rotaxanes
 using metal coordination.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              58
_journal_page_last               64
_journal_paper_doi               10.1039/c8dt04096f
_journal_volume                  48
_journal_year                    2018
_chemical_formula_moiety         'C45 H50 O10, C30 H38 Ag2 Cl2 N4, 2(C H Cl3)'
_chemical_formula_sum            'C77 H90 Ag2 Cl8 N4 O10'
_chemical_formula_weight         1730.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                77.554(2)
_cell_angle_beta                 80.633(2)
_cell_angle_gamma                80.930(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4582(3)
_cell_length_b                   16.8795(4)
_cell_length_c                   19.1895(5)
_cell_measurement_reflns_used    23147
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8900
_cell_measurement_theta_min      2.3540
_cell_volume                     3856.36(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      2.00  96.00   1.00   25.00    --   43.31-125.00   0.00   94
  2  \w     15.00 119.00   1.00   25.00    --   43.31  19.00 -90.00  104
  3  \w    -27.00  66.00   1.00   25.00    --   43.31 -38.00  30.00   93
  4  \w    -27.00  66.00   1.00   25.00    --   43.31 -38.00  90.00   93
  5  \w     32.00 122.00   1.00  100.00    --  103.63-125.00-120.00   90
  6  \w     35.00  98.00   1.00  100.00    --  103.63 -45.00  90.00   63
  7  \w     23.00 109.00   1.00  100.00    --  103.63 -94.00  60.00   86
  8  \w     35.00  98.00   1.00  100.00    --  103.63 -45.00  30.00   63
  9  \w     35.00  98.00   1.00  100.00    --  103.63 -45.00 -90.00   63
 10  \w     23.00 109.00   1.00  100.00    --  103.63 -94.00 -60.00   86
 11  \w     32.00 122.00   1.00  100.00    --  103.63-125.00  60.00   90
 12  \w     32.00 122.00   1.00  100.00    --  103.63-125.00-180.00   90
 13  \w     78.00 173.00   1.00  100.00    --  103.63  61.00  30.00   95
 14  \w     35.00  98.00   1.00  100.00    --  103.63 -45.00-180.00   63
 15  \w     23.00 109.00   1.00  100.00    --  103.63 -94.00-120.00   86
 16  \w     29.00 178.00   1.00  100.00    --  103.63   0.00   0.00  149
 17  \w     13.00 115.00   1.00   25.00    --   43.31  77.00 -30.00  102
 18  \w     13.00 115.00   1.00   25.00    --   43.31  77.00-180.00  102
 19  \w     13.00  61.00   1.00   25.00    --   43.31  77.00-120.00   48
 20  \w     13.00 115.00   1.00   25.00    --   43.31  77.00  90.00  102
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0645395000
_diffrn_orient_matrix_UB_12      0.0388284000
_diffrn_orient_matrix_UB_13      -0.0635848000
_diffrn_orient_matrix_UB_21      0.0908627000
_diffrn_orient_matrix_UB_22      0.0544221000
_diffrn_orient_matrix_UB_23      -0.0333381000
_diffrn_orient_matrix_UB_31      0.0595358000
_diffrn_orient_matrix_UB_32      -0.0664069000
_diffrn_orient_matrix_UB_33      -0.0415613000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42843
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         2.379
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.107
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.953
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.354
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         13599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.354
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0547
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12072
_reflns_number_total             13599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           agpelb
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_original_cell_volume        3856.37(17)
_cod_database_code               7047993
_nottingham_internal_coll_name   AGPELB
_nottingham_internal_coll_number 16469
_nottingham_internal_coll_client PEL/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 25.00, 100.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   09/09/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 12/09/2016
_nottingham_internal_process_user pcxpl
_nottingham_internal_solution_date 24/01/2017
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 25/01/2017
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 25/01/2017
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C75H88N4O10Ag2I2
_chemical_oxdiff_usercomment
'AGPELB #16469 GVA-1060 in fomblin film on a micromount for PEL/NRC'
_reflns_odcompleteness_completeness 99.99
_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.a Ternary CH refined with riding coordinates:
 C2C(H2C), C1C(H1C)
2.b Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C14A(H14A,H14B), C21A(H21A,H21B), C28A(H28A,H28B), C35A(H35A,
 H35B), C10B(H10B,H10C), C14B(H14C,H14D), C15B(H15A,H15B), C16B(H16A,H16B),
 C17B(H17B,H17C), C21B(H21C,H21D)
2.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C6A(H6A), C10A(H10A), C13A(H13A), C17A(H17A), C20A(H20A),
 C24A(H24A), C27A(H27A), C31A(H31A), C34A(H34A), C2B(H2B), C6B(H6B), C12B(H12B),
  C13B(H13B), C19B(H19B), C20B(H20B), C24B(H24B), C26B(H26B)
2.d Idealised Me refined as rotating group:
 C36A(H36A,H36B,H36C), C37A(H37A,H37B,H37C), C38A(H38A,H38B,H38C), C39A(H39A,
 H39B,H39C), C40A(H40A,H40B,H40C), C41A(H41A,H41B,H41C), C42A(H42A,H42B,H42C),
 C43A(H43A,H43B,H43C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C), C7B(H7BA,
 H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C28B(H28C,H28D,H28E),
 C29B(H29A,H29B,H29C), C30B(H30A,H30B,H30C)
;
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 1.949
_oxdiff_exptl_absorpt_empirical_full_min 0.504