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_7047990
_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         'C30 H38 Ag2 Br2 N4, C45 H50 O10, 2(C H Cl3)'
_chemical_formula_sum            'C77 H90 Ag2 Br2 Cl6 N4 O10'
_chemical_formula_weight         1819.78
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                77.409(4)
_cell_angle_beta                 80.515(5)
_cell_angle_gamma                80.739(5)
_cell_formula_units_Z            2
_cell_length_a                   12.5204(10)
_cell_length_b                   16.9379(8)
_cell_length_c                   19.2586(7)
_cell_measurement_reflns_used    8371
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1390
_cell_measurement_theta_min      3.9480
_cell_volume                     3898.2(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.899
_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    -23.00  89.00   1.00    4.00    --    0.00  38.00 150.00  112
  2  \w    -33.00  33.00   1.00    4.00    --    0.00 -82.00   0.00   66
  3  \w    -33.00  33.00   1.00    4.00    --    0.00 -82.00-120.00   66
  4  \w    -46.00  31.00   1.00    4.00    --    0.00 -77.00-180.00   77
  5  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00   0.00  122
  6  \w     12.00  69.00   1.00   16.00    --  101.10 -30.00 -30.00   57
  7  \w     12.00 128.00   1.00   16.00    --  101.10 -61.00-120.00  116
  8  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00 150.00  122
  9  \w     64.00 190.00   1.00   16.00    --  101.10  15.00-150.00  126
 10  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00 120.00  122
 11  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00  60.00  122
 12  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00  30.00  122
 13  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00-180.00  122
 14  \w     12.00 132.00   1.00   16.00    --  101.10 -77.00  60.00  120
 15  \w     12.00 132.00   1.00   16.00    --  101.10 -77.00 150.00  120
 16  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00-150.00  122
 17  \w     12.00  69.00   1.00   16.00    --  101.10 -30.00  30.00   57
 18  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00 -30.00  122
 19  \w     12.00  69.00   1.00   16.00    --  101.10 -30.00 -90.00   57
 20  \w     12.00  69.00   1.00   16.00    --  101.10 -30.00 -60.00   57
 21  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00 -60.00  122
 22  \w     12.00  69.00   1.00   16.00    --  101.10 -30.00  60.00   57
 23  \w     12.00 132.00   1.00   16.00    --  101.10 -77.00 -90.00  120
 24  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00  90.00  122
 25  \w     12.00 134.00   1.00   16.00    --  101.10 -82.00 -90.00  122
 26  \w     12.00  77.00   1.00   16.00    --  101.10 -45.00-180.00   65
 27  \w     12.00 132.00   1.00   16.00    --  101.10 -77.00   0.00  120
 28  \w     64.00 190.00   1.00   16.00    --  101.10  15.00 120.00  126
 29  \w    -33.00  33.00   1.00    4.00    --    0.00 -82.00 -60.00   66
 30  \w    -33.00  33.00   1.00    4.00    --    0.00 -82.00  60.00   66
 31  \w    -89.00  23.00   1.00    4.00    --    0.00 -38.00-150.00  112
 32  \w    -33.00  33.00   1.00    4.00    --    0.00 -82.00 120.00   66
 33  \w     75.00 190.00   1.00   16.00    --  101.10  61.00  90.00  115
 34  \w     78.00 190.00   1.00   16.00    --  101.10  45.00  30.00  112
 35  \w     77.00 190.00   1.00   16.00    --  101.10  30.00 -90.00  113
 36  \w     78.00 190.00   1.00   16.00    --  101.10  45.00-150.00  112
 37  \w     64.00 190.00   1.00   16.00    --  101.10  15.00   0.00  126
 38  \w     75.00 190.00   1.00   16.00    --  101.10  61.00 -90.00  115
 39  \w     75.00 190.00   1.00   16.00    --  101.10  61.00 -30.00  115
 40  \w     73.00 190.00   1.00   16.00    --  101.10  67.00 -13.00  117
 41  \w     75.00 190.00   1.00   16.00    --  101.10  61.00  60.00  115
 42  \w     78.00 190.00   1.00   16.00    --  101.10  45.00-180.00  112
 43  \w     75.00 190.00   1.00   16.00    --  101.10  61.00-150.00  115
 44  \w     75.00 190.00   1.00   16.00    --  101.10  61.00 -60.00  115
 45  \w     75.00 190.00   1.00   16.00    --  101.10  61.00  30.00  115
 46  \w     75.00 184.00   1.00   16.00    --  101.10  61.00-120.00  109
 47  \w     75.00 190.00   1.00   16.00    --  101.10  61.00 120.00  115
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0403000000
_diffrn_orient_matrix_UB_12      0.0725318000
_diffrn_orient_matrix_UB_13      -0.0572656000
_diffrn_orient_matrix_UB_21      0.0918108000
_diffrn_orient_matrix_UB_22      -0.0284220000
_diffrn_orient_matrix_UB_23      -0.0564528000
_diffrn_orient_matrix_UB_31      -0.0760001000
_diffrn_orient_matrix_UB_32      -0.0525891000
_diffrn_orient_matrix_UB_33      -0.0193920000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2027
_diffrn_reflns_av_unetI/netI     0.1838
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53950
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.746
_diffrn_reflns_theta_min         3.610
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.601
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.709
_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    1.550
_exptl_crystal_description       plate
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.032
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         15508
_refine_ls_number_restraints     1401
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.003
_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          0.2181
_refine_ls_wR_factor_ref         0.2767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6972
_reflns_number_total             15508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           agpeli
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_database_code               7047990
_chemical_oxdiff_formula         C79H94N4O10Ag2Br2
_chemical_oxdiff_usercomment
'AGPELI #16872 MM-410 FOMBLIN ON MICROMOUNT FOR PL/NRC'
_reflns_odcompleteness_completeness 96.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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. Restrained distances
 Cl5C-C2C \\sim Cl4C-C2C \\sim Cl6C-C2C \\sim Cl2C-C1C \\sim Cl1C-C1C \\sim
Cl3C-C1C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C2C(H2C), C1C(H1C)
5.b Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C10B(H10B,H10C), C14A(H14A,H14B), C14B(H14C,H14D), C15B(H15A,
 H15B), C16B(H16A,H16B), C17B(H17B,H17C), C21A(H21A,H21B), C21B(H21C,H21D),
 C28A(H28A,H28B), C35A(H35A,H35B)
5.c Aromatic/amide H refined with riding coordinates:
 C2B(H2B), C3A(H3A), C6A(H6A), C6B(H6B), C10A(H10A), C12B(H12B), C13A(H13A),
 C13B(H13B), C17A(H17A), C19B(H19B), C20A(H20A), C20B(H20B), C24A(H24A),
 C24B(H24B), C26B(H26B), C27A(H27A), C31A(H31A), C34A(H34A)
5.d Idealised Me refined as rotating group:
 C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C28B(H28C,H28D,
 H28E), C29B(H29A,H29B,H29C), C30B(H30A,H30B,H30C), 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)
;
_shelx_res_checksum              47555
_shelx_shelxl_version_number     2014/7
_nottingham_internal_coll_client PL/NRC
_nottingham_internal_coll_date   14/02/2017
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 4.00, 16.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_name   AGPELI
_nottingham_internal_coll_number 16872
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_process_date 16/02/2017
_nottingham_internal_process_user pczcrp
_nottingham_internal_refinement_date 16/02/2017
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 16/02/2017
_nottingham_internal_solution_date 16/02/2017
_nottingham_internal_solution_user pczcrp
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   79077
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.621
_oxdiff_exptl_absorpt_empirical_full_min 0.261