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_7047989
_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         'C45 H50 O10, C33 H45 N4, I'
_chemical_formula_sum            'C81 H98 Cl3 I2 N4 O10'
_chemical_formula_weight         1647.78
_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             2017-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.067(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3045(5)
_cell_length_b                   12.8881(3)
_cell_length_c                   20.4913(5)
_cell_measurement_reflns_used    28483
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.5120
_cell_measurement_theta_min      4.0700
_cell_volume                     4116.3(2)
_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 0.999
_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    -33.00  33.00   1.00   10.00    --    0.00 -82.00-180.00   66
  2  \w    -46.00  31.00   1.00   10.00    --    0.00 -77.00  90.00   77
  3  \w    -33.00  33.00   1.00   10.00    --    0.00 -82.00  30.00   66
  4  \w    -33.00  33.00   1.00   10.00    --    0.00 -82.00 -90.00   66
  5  \w     12.00  77.00   1.00   40.00    --  101.10 -45.00 -30.00   65
  6  \w     12.00 134.00   1.00   40.00    --  101.10 -82.00   0.00  122
  7  \w     12.00  69.00   1.00   40.00    --  101.10 -30.00 150.00   57
  8  \w     12.00 132.00   1.00   40.00    --  101.10 -77.00-120.00  120
  9  \w     88.00 190.00   1.00   40.00    --  101.10  82.00  30.00  102
 10  \w     77.00 190.00   1.00   40.00    --  101.10  30.00   0.00  113
 11  \w     12.00 132.00   1.00   40.00    --  101.10 -77.00 -90.00  120
 12  \w     12.00  69.00   1.00   40.00    --  101.10 -30.00 120.00   57
 13  \w     12.00  69.00   1.00   40.00    --  101.10 -30.00  90.00   57
 14  \w     12.00  69.00   1.00   40.00    --  101.10 -30.00  30.00   57
 15  \w     12.00  69.00   1.00   40.00    --  101.10 -30.00   0.00   57
 16  \w     12.00 132.00   1.00   40.00    --  101.10 -77.00 -60.00  120
 17  \w     12.00  69.00   1.00   40.00    --  101.10 -30.00 -90.00   57
 18  \w    -23.00  89.00   1.00   10.00    --    0.00  38.00  30.00  112
 19  \w    -46.00  31.00   1.00   10.00    --    0.00 -77.00-120.00   77
 20  \w    -23.00  89.00   1.00   10.00    --    0.00  38.00-150.00  112
 21  \w     12.00 134.00   1.00   40.00    --  101.10 -82.00 120.00  122
 22  \w     64.00 190.00   1.00   40.00    --  101.10  15.00 -90.00  126
 23  \w     77.00 190.00   1.00   40.00    --  101.10  30.00  60.00  113
 24  \w     78.00 103.00   1.00   40.00    --  101.10  45.00-180.00   25
 25  \w     64.00 190.00   1.00   40.00    --  101.10  15.00 150.00  126
;
_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      0.0151795000
_diffrn_orient_matrix_UB_12      -0.1061666000
_diffrn_orient_matrix_UB_13      0.0360988000
_diffrn_orient_matrix_UB_21      0.0974952000
_diffrn_orient_matrix_UB_22      0.0192507000
_diffrn_orient_matrix_UB_23      0.0212786000
_diffrn_orient_matrix_UB_31      -0.0051369000
_diffrn_orient_matrix_UB_32      0.0515089000
_diffrn_orient_matrix_UB_33      0.0665621000
_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_reflns_av_R_equivalents  0.3012
_diffrn_reflns_av_unetI/netI     0.1382
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         4.106
_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    7.346
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.176
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plate
_exptl_crystal_F_000             1698
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.148
_platon_squeeze_details
;
TITL opellf    P 1 21 1     R = 0.28
CELL   16.3045   12.8881   20.4913     90.00    107.07     90.00
SPGR P21
C101 0.061 0.264 0.454 !      15.62 eA-3
C102 0.094 0.191 0.045 !      14.40 eA-3
C103 0.850 0.940 0.591 !       9.67 eA-3
C104 0.995 0.890 0.700 !       8.70 eA-3
C105 0.861 0.528 0.124 !       6.65 eA-3
C106 0.064 0.044 0.986 !       5.49 eA-3
C107 0.075 0.988 0.048 !       4.98 eA-3
C108 0.873 0.347 0.050 !       4.71 eA-3
C109 0.955 0.888 0.609 !       3.76 eA-3
C110 0.976 0.977 0.874 !       3.69 eA-3
C111 0.015 0.392 0.156 !       3.59 eA-3
C112 0.988 0.340 0.078 !       3.49 eA-3
C113 0.978 0.941 0.858 !       3.46 eA-3
C114 0.966 0.841 0.873 !       3.01 eA-3
C115 0.988 0.772 0.656 !       2.91 eA-3
C116 0.013 0.765 0.891 !       2.89 eA-3
C117 0.046 0.654 0.047 !       2.74 eA-3
C118 1.006 0.467 0.064 !       2.51 eA-3
C119 0.923 0.404 0.076 !       2.45 eA-3
C120 0.922 0.451 0.079 !       2.34 eA-3
C121 0.073 0.321 0.093 !       2.34 eA-3
Q122 0.061 0.697 0.878 !       2.29 eA-3
C123 0.040 0.749 0.663 !       2.25 eA-3
C124 0.904 0.490 0.058 !       2.17 eA-3
C125 0.997 0.564 0.043 !       2.13 eA-3
C126 0.857 0.479 0.047 !       1.97 eA-3
C127 0.888 0.871 0.532 !       1.91 eA-3
C128 0.846 0.760 0.495 !       1.90 eA-3
C129 0.161 0.064 0.009 !       1.89 eA-3
Q130 0.968 0.947 0.532 !       1.86 eA-3
C131 0.074 0.858 0.894 !       1.85 eA-3
C132 0.780 0.730 0.031 !       1.81 eA-3
C133 0.904 0.981 0.559 !       1.80 eA-3
C134 0.926 1.001 0.542 !       1.74 eA-3
C135 0.093 0.401 0.200 !       1.74 eA-3
C136 0.837 0.569 0.961 !       1.73 eA-3
C137 0.878 0.560 0.042 !       1.71 eA-3
C138 0.127 0.296 0.456 !       1.68 eA-3
Q139 0.093 0.604 0.019 !       1.68 eA-3
C140 0.834 0.545 0.018 !       1.65 eA-3
Q141 0.830 0.554 0.921 !       1.63 eA-3
Q142 0.813 1.013 0.532 !       1.59 eA-3
Q143 0.845 0.503 0.185 !       1.53 eA-3
C144 0.028 0.195 0.889 !       1.52 eA-3
C145 1.004 0.477 0.262 !       1.51 eA-3
Q146 0.891 0.036 0.690 !       1.46 eA-3
Q147 0.049 0.784 0.717 !       1.36 eA-3
C148 0.015 0.462 0.229 !       1.31 eA-3
Q149 0.857 0.178 0.875 !       1.29 eA-3
Q150 0.853 0.528 0.218 !       1.26 eA-3
C151 0.947 0.260-0.002 !       1.25 eA-3
Q152 0.906 0.967 0.501 !       1.24 eA-3
Q153 0.098 0.702 0.973 !       1.20 eA-3
Q154 0.043 0.021 0.722 !       1.18 eA-3
Q155 0.960 0.520 0.223 !       1.16 eA-3
Q156 0.343 0.861 0.657 !       1.15 eA-3
Q157 0.342 0.387 0.139 !       1.15 eA-3
Q158 0.856 0.127 0.876 !       1.14 eA-3
C159 0.032 0.484 0.372 !       1.14 eA-3
Q160 0.211 0.115 0.031 !       1.13 eA-3
Q161 0.149 0.671 0.013 !       1.13 eA-3
C162 0.928 0.151 0.893 !       1.12 eA-3
Q163 0.204 0.775 0.989 !       1.11 eA-3
Q164 0.743 0.813 0.893 !       1.09 eA-3
C165 0.987 0.163 0.890 !       1.08 eA-3
Q166 0.180 0.345 0.123 !       1.04 eA-3
Q167 1.002 0.588 0.871 !       1.03 eA-3
Q168 0.399 0.729 0.127 !       1.02 eA-3
C169 0.124 0.942 0.836 !       1.01 eA-3
Q170 0.702 0.876 0.871 !       1.01 eA-3
Q171 0.390 0.885 0.687 !       1.00 eA-3
Q172 0.889 0.122 0.918 !       0.99 eA-3
Q173 0.129 0.129 0.536 !       0.99 eA-3
Q174 0.377 0.209 0.360 !       0.97 eA-3
Q175 0.115 0.060 0.798 !       0.96 eA-3
Q176 0.822 0.376 0.753 !       0.95 eA-3
Q177 0.529 0.066 0.291 !       0.95 eA-3
Q178 0.937 0.149 0.847 !       0.95 eA-3
Q179 0.451 0.083 0.202 !       0.94 eA-3
Q180 0.189 0.578 0.277 !       0.93 eA-3
Q181 0.954 0.806 0.750 !       0.89 eA-3
Q182 0.838 0.812 0.330 !       0.89 eA-3
Q183 0.580 0.055 0.278 !       0.89 eA-3
Q184 0.910 0.597 0.503 !       0.89 eA-3
Q185 0.175 0.213 0.266 !       0.88 eA-3
Q186 0.127 0.052 0.528 !       0.88 eA-3
Q187 0.562 0.397 0.287 !       0.88 eA-3
Q188 0.442 0.876 0.500 !       0.87 eA-3
Q189 0.064 0.453 0.874 !       0.85 eA-3
Q190 0.844 0.580 0.251 !       0.85 eA-3
Q191 0.889 0.835 0.064 !       0.84 eA-3
Q192 0.950 0.029 0.700 !       0.84 eA-3
Q193 0.028 0.539 0.863 !       0.84 eA-3
Q194 0.555 0.699 0.589 !       0.83 eA-3
Q195 0.500 0.530 0.754 !       0.83 eA-3
Q196 0.849 0.060 0.030 !       0.83 eA-3
Q197 0.623 0.556 0.843 !       0.82 eA-3
Q198 0.957 0.476 0.516 !       0.82 eA-3
Q199 0.849 0.651 0.562 !       0.82 eA-3
;
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.470(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.535
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         14052
_refine_ls_number_restraints     1355
_refine_ls_restrained_S_all      1.469
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.1536
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3790
_refine_ls_wR_factor_ref         0.4041
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10940
_reflns_number_total             14052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           opellf_sq
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_original_cell_volume        4116.31(19)
_cod_database_code               7047989
_nottingham_internal_coll_name   OPELLF
_nottingham_internal_coll_number 16314
_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,, 10.00, 40.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   21/07/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_process_date 22/07/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 23/01/2017
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 23/01/2017
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 23/01/2017
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C79H98N4O10I3
_chemical_oxdiff_usercomment
'OPELLF 16314 MM-264 Fomblim on micromount for PEL/NRC'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.530(17) 0.470(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
 N3-C65 \\sim N4-C65 \\sim N1-C54 \\sim N2-C54
 with sigma of 0.02
 N4-C67 \\sim N3-C66 \\sim N2-C55 \\sim N1-C56
 with sigma of 0.02
 C67-C66 \\sim C55-C56
 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. Others
 Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C48(H48)
7.b Secondary CH2 refined with riding coordinates:
 C6BA(H6BA,H6BB), C3BA(H3BA,H3BB), C21(H21A,H21B), C28(H28A,H28B), C35(H35A,
 H35B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C68(H68A,H68B)
7.c Aromatic/amide H refined with riding coordinates:
 C6AA(H6AA), C5BA(H5BA), C0BA(H0BA), C1AA(H1AA), C16(H16), C5AA(H5AA),
 C23(H23), C26(H26), C30(H30), C33(H33), C46(H46), C50(H50), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58), C65(H65), C66(H66), C67(H67), C71(H71), C73(H73)
7.d Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C43(H43A,H43B,H43C), C43A(H43D,H43E,H43F)
;
_shelx_res_checksum              71588
_shelx_fab_checksum              40112
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.776
_oxdiff_exptl_absorpt_empirical_full_min 0.147