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_7047991
_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
'C34 H46 Ag2 Br Cl N4, C45 H50 O10, 2(C H Cl3)'
_chemical_formula_sum            'C81 H98 Ag2 Br Cl7 N4 O10'
_chemical_formula_weight         1831.43
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-08
_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                 107.615(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.4695(4)
_cell_length_b                   12.8394(4)
_cell_length_c                   20.6024(6)
_cell_measurement_reflns_used    7574
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6370
_cell_measurement_theta_min      2.7880
_cell_volume                     4152.3(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    'ShelXS (Sheldrick, 2008)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.969
_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    -41.00  24.00   1.00   20.00    --  -43.31  38.00 120.00   65
  2  \w    -49.00  -9.00   1.00   20.00    --  -43.31  38.00-180.00   40
  3  \w    -43.00  33.00   1.00   20.00    --  -43.31  19.00  60.00   76
  4  \w     62.00 111.00   1.00   20.00    --   43.31 147.00  32.00   49
  5  \w     33.00  69.00   1.00   80.00    --  103.00 -30.00  90.00   36
  6  \w     57.00  94.00   1.00   80.00    --  103.00 -45.00  60.00   37
  7  \w     30.00  78.00   1.00   80.00    --  103.00 -30.00 150.00   48
  8  \w     56.00  86.00   1.00   80.00    --  103.00 -45.00  30.00   30
  9  \w     82.00 172.00   1.00   80.00    --  103.00  45.00 -30.00   90
 10  \w     42.00  91.00   1.00   80.00    --  103.00 -45.00-150.00   49
 11  \w     93.00 175.00   1.00   80.00    --  103.00  30.00 -90.00   82
 12  \w     33.00  81.00   1.00   80.00    --  103.00 -30.00   0.00   48
;
_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      0.0243444000
_diffrn_orient_matrix_UB_12      -0.0178450000
_diffrn_orient_matrix_UB_13      0.0775169000
_diffrn_orient_matrix_UB_21      0.0755631000
_diffrn_orient_matrix_UB_22      0.0755882000
_diffrn_orient_matrix_UB_23      0.0106621000
_diffrn_orient_matrix_UB_31      -0.0576825000
_diffrn_orient_matrix_UB_32      0.0913891000
_diffrn_orient_matrix_UB_33      0.0062741000
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18124
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.713
_diffrn_reflns_theta_min         2.815
_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    6.886
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.425
_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    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.424(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         10970
_refine_ls_number_restraints     1635
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0973P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                8910
_reflns_number_total             10970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           agpelc_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_database_code               7047991
_nottingham_internal_coll_name   AGPELC
_nottingham_internal_coll_number 16621
_nottingham_internal_coll_client PEL/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '20.00, 80.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   07/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 24/01/2017
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 25/01/2017
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 25/01/2017
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 08/02/2017
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C81H98N4O10Ag2Cl8
_chemical_oxdiff_usercomment
'AGPELC #16621 GVA-1107 IN FOMBLIN FILM ON MICROMOUNT FOR NRC'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.576(11) 0.424(11)
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
 Cl7-Cl8
 2.8 with sigma of 0.04
 C1B-C2B \\sim C1B-C6B \\sim C6B-C5B \\sim C5B-C4B \\sim C3B-C4B \\sim C2B-C3B
 with sigma of 0.02
 C7B-C1B \\sim C7-C1B
 with sigma of 0.02
 Cl00-C2C \\sim Cl8-C2C \\sim Cl7-C2C \\sim Cl06-C2C \\sim Cl14-C2C \\sim
Cl07-C2C
 with sigma of 0.02
 Cl6C-C1C \\sim Cl3C-C1C \\sim Cl4C-C1C \\sim Cl1C-C1C \\sim Cl5C-C1C \\sim
Cl2C-C1C
 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
Uanis(Cl1) = Uanis(Br1)
Uanis(Br2) = Uanis(Cl2)
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(H2CA)=Sof(Cl7)=Sof(Cl8)=Sof(Cl14)=1-FVAR(1)
 Sof(H2C)=Sof(Cl00)=Sof(Cl06)=Sof(Cl07)=FVAR(1)
 Sof(H1CA)=Sof(Cl4C)=Sof(Cl5C)=Sof(Cl6C)=1-FVAR(2)
 Sof(H1C)=Sof(Cl1C)=Sof(Cl2C)=Sof(Cl3C)=FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=1-FVAR(3)
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=FVAR(3)
 Sof(Cl1)=Sof(Br2)=1-FVAR(4)
 Sof(Cl2)=Sof(Br1)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C1C(H1C), C1C(H1CA), C2C(H2C), C2C(H2CA)
7.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),
 C20B(H20B,H20C), C21A(H21A,H21B), C21B(H21C,H21D), C25B(H25A,H25B), C28A(H28A,
 H28B), C35A(H35A,H35B)
7.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), C20A(H20A), C23B(H23B), C24A(H24A), C24B(H24B),
 C27A(H27A), C28B(H28C), C30B(H30B), C31A(H31A), C34A(H34A)
7.d Idealised Me refined as rotating group:
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C32B(H32A,H32B,H32C), C33B(H33A,
 H33B,H33C), C34B(H34B,H34C,H34D), 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), C7(H7A,H7B,H7C)
;
_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 3.133
_oxdiff_exptl_absorpt_empirical_full_min 0.433
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 2.8375\% 
 around [0.71 -0.57 -0.41] (reciprocal) or [0.58 -0.81 -0.09] (direct)
;