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_7047994
_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_absolute_configuration ad
_chemical_formula_moiety         'C32 H42 Ag2 Br2 N4, C45 H47 O10, 2(C H Cl3)'
_chemical_formula_sum            'C81 H93 Ag2 Br2 Cl12 N4 O10'
_chemical_formula_weight         2083.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.327(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1948(5)
_cell_length_b                   28.7424(6)
_cell_length_c                   12.6578(4)
_cell_measurement_reflns_used    10252
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.5530
_cell_measurement_theta_min      3.9750
_cell_volume                     4350.2(3)
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'PILATUS3 R 200K Hybrid Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.920
_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    -15.00  83.00   1.00    4.00    --    0.00  38.00  60.00   98
  2  \w    -45.00  17.00   1.00    4.00    --    0.00 -38.00 -90.00   62
  3  \w    155.00 187.00   1.00   16.00    --  101.10  30.00  30.00   32
  4  \w     34.00  69.00   1.00   16.00    --  101.10 -30.00  30.00   35
  5  \w     12.00  75.00   1.00   16.00    --  101.10 -45.00-150.00   63
  6  \w     13.00  52.00   1.00   16.00    --  101.10 -30.00  90.00   39
  7  \w     14.00  68.00   1.00   16.00    --  101.10 -30.00   0.00   54
  8  \w     27.00  64.00   1.00   16.00    --  101.10 -30.00 -30.00   37
  9  \w     12.00  57.00   1.00   16.00    --  101.10 -30.00  60.00   45
 10  \w     13.00  70.00   1.00   16.00    --  101.10 -45.00-180.00   57
 11  \w     47.00  77.00   1.00   16.00    --  101.10 -45.00   0.00   30
 12  \w     89.00 162.00   1.00   16.00    --  101.10  61.00 -60.00   73
 13  \w    108.00 134.00   1.00   16.00    --  101.10  82.00   0.00   26
 14  \w    159.00 190.00   1.00   16.00    --  101.10  82.00   0.00   31
 15  \w     29.00  55.00   1.00   16.00    --  101.10 -45.00-120.00   26
 16  \w     12.00 129.00   1.00   16.00    --  101.10 -75.00-173.00  117
 17  \w     15.00  62.00   1.00   16.00    --  101.10 -30.00-120.00   47
 18  \w     84.00 111.00   1.00   16.00    --  101.10  30.00  30.00   27
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'XtalLAB PRO MM007, PILATUS3 R 200K'
_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      0.1195083000
_diffrn_orient_matrix_UB_12      -0.0154260000
_diffrn_orient_matrix_UB_13      0.0518541000
_diffrn_orient_matrix_UB_21      -0.0479583000
_diffrn_orient_matrix_UB_22      -0.0415611000
_diffrn_orient_matrix_UB_23      0.0529195000
_diffrn_orient_matrix_UB_31      0.0051111000
_diffrn_orient_matrix_UB_32      -0.0301188000
_diffrn_orient_matrix_UB_33      -0.0995724000
_diffrn_radiation_collimation    'VariMax VHF mirror optic'
_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  0.0668
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20543
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.696
_diffrn_reflns_theta_min         3.697
_diffrn_source                   'rotating anode'
_diffrn_source_current           30
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'MicroMax 007 HF'
_diffrn_source_voltage           40
_exptl_absorpt_coefficient_mu    8.549
_exptl_absorpt_correction_T_max  0.433
_exptl_absorpt_correction_T_min  0.212
_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    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             2110
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.052
_platon_squeeze_details
;
TITL agpele6_a.res in P2(1)
CELL   12.1948   28.7424   12.6578     90.00    101.33     90.00
SPGR P21
C101 0.843 0.844 0.300 !       8.06 eA-3
C102 0.219 0.285 0.537 !       6.82 eA-3
C103 0.090 0.243 0.678 !       4.98 eA-3
C104 0.017 0.280 0.580 !       4.37 eA-3
C105 0.733 0.757 0.348 !       3.16 eA-3
Q106 0.737 0.258 0.553 !       2.78 eA-3
Q107 0.750 0.255 0.490 !       2.72 eA-3
Q108 0.207 0.771 0.484 !       2.56 eA-3
Q109 0.291 0.780 0.494 !       2.35 eA-3
C110 0.863 0.791 0.343 !       2.22 eA-3
Q111 0.876 0.243 0.633 !       1.93 eA-3
C112 0.752 0.744 0.258 !       1.61 eA-3
C113 0.876 0.793 0.253 !       1.38 eA-3
C114 0.966 0.236 0.517 !       1.37 eA-3
C115 0.798 0.785 0.289 !       1.36 eA-3
Q116 0.234 0.770 0.596 !       1.33 eA-3
Q117 0.357 0.298 0.384 !       1.29 eA-3
C118 1.001 0.259 0.511 !       1.22 eA-3
C119 0.129 0.283 0.809 !       1.18 eA-3
Q120 0.579 0.848 0.202 !       1.17 eA-3
Q121 0.378 0.288 0.301 !       1.17 eA-3
C122 0.987 0.848 0.350 !       1.17 eA-3
Q123 0.942 0.338 0.623 !       1.16 eA-3
Q124 0.297 0.779 0.377 !       1.14 eA-3
C125 0.782 0.792 0.374 !       1.08 eA-3
Q126 0.654 0.816 0.168 !       1.06 eA-3
Q127 0.632 0.852 0.128 !       1.06 eA-3
Q128 0.965 0.337 0.565 !       1.06 eA-3
Q129 0.916 0.273 0.470 !       1.03 eA-3
Q130 0.204 0.293 0.419 !       1.01 eA-3
C131 0.704 0.740 0.483 !       0.95 eA-3
Q132 0.394 0.413 0.826 !       0.95 eA-3
C133 0.032 0.236 0.523 !       0.94 eA-3
Q134 0.612 0.929 0.106 !       0.93 eA-3
Q135 0.596 0.769 0.644 !       0.93 eA-3
C136 0.286 0.348 0.495 !       0.93 eA-3
C137 0.810 0.722 0.316 !       0.90 eA-3
Q138 0.888 0.322 0.546 !       0.89 eA-3
Q139 0.557 0.828 0.114 !       0.87 eA-3
Q140 0.981 0.195 0.710 !       0.87 eA-3
C141 0.765 0.746 0.424 !       0.86 eA-3
Q142 0.336 0.389 0.912 !       0.86 eA-3
Q143 0.222 0.366 0.548 !       0.86 eA-3
C144 0.769 0.854 0.415 !       0.85 eA-3
Q145 0.816 0.226 0.409 !       0.84 eA-3
Q146 0.926 0.281 0.636 !       0.84 eA-3
C147 1.001 0.228 0.705 !       0.84 eA-3
Q148 0.342 0.731 0.751 !       0.84 eA-3
C149 0.934 0.851 0.568 !       0.83 eA-3
Q150 0.935 0.300 0.685 !       0.83 eA-3
Q151 0.422 0.312 0.179 !       0.83 eA-3
Q152 0.473 0.819 0.739 !       0.82 eA-3
Q153 0.330 0.326 0.500 !       0.80 eA-3
Q154 0.644 0.241 0.532 !       0.80 eA-3
Q155 0.061 0.721 0.254 !       0.80 eA-3
Q156 0.195 0.236 0.831 !       0.79 eA-3
Q157 0.917 0.341 0.490 !       0.78 eA-3
Q158 0.560 0.235 0.450 !       0.78 eA-3
Q159 0.865 0.296 0.506 !       0.76 eA-3
Q160 0.664 0.779 0.912 !       0.75 eA-3
Q161 0.015 0.215 0.766 !       0.74 eA-3
Q162 0.218 0.697 0.438 !       0.73 eA-3
C163 0.206 0.224 0.616 !       0.73 eA-3
C164 0.840 0.834 0.585 !       0.73 eA-3
Q165 0.201 0.712 0.364 !       0.72 eA-3
Q166 0.566 0.832 0.566 !       0.72 eA-3
Q167 0.935 0.787 0.574 !       0.72 eA-3
Q168 0.129 0.366 0.455 !       0.72 eA-3
Q169 0.457 0.279 0.248 !       0.71 eA-3
Q170 0.335 0.352 0.738 !       0.71 eA-3
Q171 0.977 0.183 0.794 !       0.71 eA-3
Q172 0.276 0.322 0.038 !       0.71 eA-3
Q173 0.120 0.667 0.833 !       0.70 eA-3
Q174 0.904 0.247 0.567 !       0.70 eA-3
Q175 0.348 0.773 0.594 !       0.69 eA-3
Q176 0.704 0.268 0.271 !       0.69 eA-3
Q177 0.915 0.220 0.390 !       0.69 eA-3
Q178 0.655 0.304 0.542 !       0.68 eA-3
Q179 0.435 0.658 0.910 !       0.68 eA-3
Q180 0.949 0.920 0.673 !       0.68 eA-3
C181 0.020 0.380 0.377 !       0.68 eA-3
Q182 0.915 0.195 0.455 !       0.67 eA-3
Q183 0.825 0.302 0.557 !       0.67 eA-3
Q184 0.629 0.757 0.730 !       0.67 eA-3
Q185 0.729 0.554 0.734 !       0.66 eA-3
Q186 0.788 0.882 0.204 !       0.66 eA-3
Q187 0.749 0.320 0.521 !       0.66 eA-3
Q188 0.427 0.772 0.620 !       0.66 eA-3
Q189 0.594 0.227 0.093 !       0.66 eA-3
Q190 0.342 0.247 0.397 !       0.65 eA-3
Q191 0.421 0.734 0.825 !       0.65 eA-3
Q192 0.152 0.810 0.470 !       0.65 eA-3
Q193 0.326 0.381 0.114 !       0.64 eA-3
Q194 0.767 0.853 0.122 !       0.64 eA-3
Q195 0.045 0.387 0.641 !       0.64 eA-3
Q196 0.328 0.769 0.676 !       0.63 eA-3
Q197 0.614 0.819 0.266 !       0.63 eA-3
Q198 0.577 0.337 0.246 !       0.63 eA-3
Q199 0.516 0.345 0.248 !       0.63 eA-3
;
_refine_diff_density_max         2.781
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.197(17)
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         11419
_refine_ls_number_restraints     1500
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2766
_refine_ls_wR_factor_ref         0.3002
_reflns_Friedel_coverage         0.967
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                7820
_reflns_number_total             11419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           agpele6_sq
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_database_code               7047994
_nottingham_internal_coll_name   AGPELE
_nottingham_internal_coll_number 16816
_nottingham_internal_coll_client PL/NRC
_nottingham_internal_coll_type   custom
_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_user   pczcrp
_nottingham_internal_coll_date   30/01/2017
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_process_date 17/02/2017
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 17/02/201
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 17/02/201
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 17/02/201
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C80H95O10N4Ag2Br2Cl9
_chemical_oxdiff_usercomment
'AGPELE #16816 MM-400 FOMBLIN ON MICROMOUNT FOR PL/NRC'
_reflns_odcompleteness_completeness 96.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.803(17) 0.197(17)
2. 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
3. Restrained distances
 Cl1C-C1C \\sim Cl2C-C1C \\sim Cl3C-C1C \\sim Cl4C-C2C \\sim Cl6C-C2C \\sim
Cl5C-C2C
 with sigma of 0.02
 C29B-C28B \\sim C29B-C24B \\sim C25B-C24B \\sim C26B-C25B \\sim C27B-C26B
\\sim C27B-C28B \\sim C1B-
 C2B \\sim C2B-C3B \\sim C4B-C3B \\sim C4B-C5B \\sim C6B-C5B \\sim C6B-C1B
 with sigma of 0.02
4. 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
5. 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
6.a Ternary CH refined with riding coordinates:
 C1C(H1C), C2C(H2C)
6.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), C18B(H18A,H18B), C19B(H19A,H19B),
 C21A(H21A,H21B), C23B(H23A,H23B), C28A(H28A,H28B), C35A(H35A,H35B)
6.c Me refined with riding coordinates:
 C43A(H43A,H43B,H43C)
6.d Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C5B(H5B), C6A(H6A), C10A(H10A), C12B(H12B), C13A(H13A),
 C13B(H13B), C17A(H17A), C20A(H20A), C21B(H21C), C22B(H22B), C24A(H24A),
 C26B(H26B), C27A(H27A), C28B(H28C), C31A(H31A), C34A(H34A)
6.e Idealised Me refined as rotating group:
 C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C30B(H30A,H30B,
 H30C), C31B(H31B,H31C,H31D), C32B(H32A,H32B,H32C), C36A(H36A,H36B,H36C),
 C37A(H37A,H37B,H37C), C38A(H38A,H38B,H38C), C40A(H40A,H40B,H40C), C41A(H41A,
 H41B,H41C), C42A(H42A,H42B,H42C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C)
;
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   6514
_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 2.950
_oxdiff_exptl_absorpt_empirical_full_min 0.254