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_7047992
_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         'C44 H56 I4 N6 Pd2, C45 H50 O10'
_chemical_formula_sum            'C89 H106 I4 N6 O10 Pd2'
_chemical_formula_weight         2140.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.157(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0957(6)
_cell_length_b                   12.1538(3)
_cell_length_c                   37.0911(11)
_cell_measurement_reflns_used    58734
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.2990
_cell_measurement_theta_min      3.1630
_cell_volume                     8821.3(4)
_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 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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    -67.00 -29.00   1.00   50.00    --   -6.45 133.00 101.64   38
  2  \w    -15.00  80.00   1.00   50.00    --    7.23  38.00 -30.00   95
  3  \w    -19.00  77.00   1.00   50.00    --    7.23  57.00  30.00   96
  4  \w    -20.00  47.00   1.00   50.00    --    7.23 -99.00-150.00   67
  5  \w    -67.00  39.00   1.00   50.00    --    7.23 -77.00 -30.00  106
  6  \w    -65.00  30.00   1.00   50.00    --    7.23 -38.00 -30.00   95
  7  \w    -20.00  33.00   1.00   50.00    --   -6.45 -99.00  30.00   53
  8  \w    -33.00  64.00   1.00   50.00    --   -6.45  57.00  90.00   97
  9  \w    -20.00  33.00   1.00   50.00    --   -6.45 -99.00 150.00   53
 10  \w    -20.00  33.00   1.00   50.00    --   -6.45 -99.00  60.00   53
 11  \w    -63.00  34.00   1.00   50.00    --    7.23 -57.00-120.00   97
 12  \w    -20.00  47.00   1.00   50.00    --    7.23 -99.00  90.00   67
 13  \w    -67.00 -29.00   1.00   50.00    --   -6.45 133.00 144.59   38
 14  \w     -9.00  54.00   1.00   50.00    --    7.23-112.00 171.00   63
 15  \w    -11.00  53.00   1.00   50.00    --    7.23-109.00  24.50   64
 16  \w    -21.00  47.00   1.00   50.00    --    7.23 -98.00  56.88   68
 17  \w    -63.00  36.00   1.00   50.00    --    7.23 -65.00 118.58   99
 18  \w    -13.00  52.00   1.00   50.00    --    7.23-107.00 -74.82   65
 19  \w    -20.00  33.00   1.00   50.00    --   -6.45 -99.00 -30.00   53
 20  \w    -80.00  25.00   1.00   50.00    --   -6.45 -77.00  60.00  105
 21  \w    -80.00  25.00   1.00   50.00    --   -6.45 -77.00 -60.00  105
 22  \w     -9.00  41.00   1.00   50.00    --   -6.45-112.00 171.00   50
 23  \w    -21.00  47.00   1.00   50.00    --    7.23 -98.00 104.42   68
 24  \w    -65.00  30.00   1.00   50.00    --    7.23 -38.00  30.00   95
 25  \w    -46.00  26.00   1.00   50.00    --   -6.45 -80.00-106.00   72
 26  \w    -20.00  47.00   1.00   50.00    --    7.23 -99.00  30.00   67
 27  \w    -63.00  34.00   1.00   50.00    --    7.23 -57.00   0.00   97
 28  \w    -63.00  23.00   1.00   50.00    --    7.23 -57.00  60.00   86
 29  \w     24.00  86.00   1.00   50.00    --    7.23-164.00 -25.25   62
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_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      0.0132944000
_diffrn_orient_matrix_UB_12      0.0351796000
_diffrn_orient_matrix_UB_13      0.0151988000
_diffrn_orient_matrix_UB_21      -0.0133365000
_diffrn_orient_matrix_UB_22      -0.0353396000
_diffrn_orient_matrix_UB_23      0.0118531000
_diffrn_orient_matrix_UB_31      0.0309529000
_diffrn_orient_matrix_UB_32      -0.0303202000
_diffrn_orient_matrix_UB_33      0.0038093000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.2245
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            542213
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.905
_diffrn_reflns_theta_min         2.899
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Mo
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.646
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       plate
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.862
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1070
_refine_ls_number_reflns         22446
_refine_ls_number_restraints     1820
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1980
_refine_ls_R_factor_gt           0.1116
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1317P)^2^+127.6020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2940
_refine_ls_wR_factor_ref         0.3418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11385
_reflns_number_total             22446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           pdpele
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_database_code               7047992
_nottingham_internal_coll_name   PDPELE
_nottingham_internal_coll_number 16356
_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,, 50.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   05/08/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 10/08/2016
_nottingham_internal_process_user pcxpl
_nottingham_internal_solution_date 10/08/2016
_nottingham_internal_solution_user 'pcxpl, pczcrp'
_nottingham_internal_refinement_user 'pczcrp, pcxpl'
_nottingham_internal_self_archive_date 10/08/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C89 H106 I6 N6 O10 Pd2'
_chemical_oxdiff_usercomment
'PDPELE#16356 IN FOBLIN ON MICROMOUNT FOR PEL/NRC'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.10
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28C-C27B \\sim C28B-C27B
 with sigma of 0.02
 C16C-C15B \\sim C16B-C15B \\sim C17B-C16B \\sim C16C-C17C \\sim C18B-C17B
\\sim C18C-C17C \\sim C19C-
 C18C \\sim C19B-C18B \\sim C20B-C19B \\sim C19C-C20C \\sim C21B-C20C \\sim
C21B-C20B
 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. Others
 Sof(C28C)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(H15C)=Sof(H15D)=Sof(H21C)=Sof(H21D)=Sof(C16C)=Sof(H16C)=Sof(H16D)=
 Sof(C17C)=Sof(H17C)=Sof(H17D)=Sof(C18C)=Sof(H18C)=Sof(H18D)=Sof(C19C)=
 Sof(H19C)=Sof(H19D)=Sof(C20C)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(H15A)=Sof(H15B)=Sof(H21A)=Sof(H21B)=Sof(C16B)=Sof(H16A)=Sof(H16B)=
 Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(C19B)=
 Sof(H19A)=Sof(H19B)=Sof(C20B)=Sof(H20A)=Sof(H20B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C10B(H10A,H10B), C14A(H14C,H14D), C14B(H14A,H14B), C15B(H15A,
 H15B), C15B(H15C,H15D), C017(H01A,H01B), C21A(H21E,H21F), C21B(H21A,H21B),
 C21B(H21C,H21D), C25B(H25A,H25B), C28A(H28G,H28H), C16B(H16A,H16B), C17B(H17A,
 H17B), C18B(H18A,H18B), C19B(H19A,H19B), C20B(H20A,H20B), C16C(H16C,H16D),
 C17C(H17C,H17D), C18C(H18C,H18D), C19C(H19C,H19D), C20C(H20C,H20D)
6.b Me refined with riding coordinates:
 C36A(H36A,H36B,H36C), C28B(H28A,H28B,H28C), C28C(H28D,H28E,H28F)
6.c Aromatic/amide H refined with riding coordinates:
 C01P(H01P), C01R(H01R), C02G(H02G), C02L(H02L), C02M(H02M), C02N(H02N),
 C02V(H02V), C3A(H3A), C3B(H3B), C4B(H4B), C6A(H6A), C10A(H10C), C11B(H11B),
 C12B(H12B), C13A(H13A), C17A(H17E), C20A(H20E), C23B(H23B), C024(H024),
 C24A(H24A), C24B(H24B), C027(H027), C27A(H27A), C028(H028), C29B(H29B),
 C31A(H31D), C32B(H32B), C34A(H34D)
6.d Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC), C6B(H6BA,H6BB,H6BC), C8B(H8BA,H8BB,H8BC), C31B(H31A,H31B,
 H31C), C34B(H34A,H34B,H34C), C35A(H35A,H35B,H35C), 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)
;