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_7047988
_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         'C42 H52 I4 N6 Pd2, C45 H50 O10'
_chemical_formula_sum            'C87 H102 I4 N6 O10 Pd2'
_chemical_formula_weight         2112.14
_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             2017-02-08
_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                 92.453(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2495(7)
_cell_length_b                   12.2253(6)
_cell_length_c                   21.1205(7)
_cell_measurement_reflns_used    6651
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2120
_cell_measurement_theta_min      3.3280
_cell_volume                     4191.8(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                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.945
_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    -93.00  -3.00   1.00   17.50    --  -38.50 125.00-180.00   90
  2  \w   -111.00 -21.00   1.00   17.50    --  -38.50 -38.00  30.00   90
  3  \w    -19.00  14.00   1.00   17.50    --  -38.50  38.00 -30.00   33
  4  \w     98.00 176.00   1.00   70.00    --  106.13  45.00 -30.00   78
  5  \w     35.00  81.00   1.00   70.00    --  106.13 -30.00 -60.00   46
  6  \w     48.00  98.00   1.00   70.00    --  106.13 -45.00-120.00   50
  7  \w     61.00  88.00   1.00   70.00    --  106.13 -30.00  90.00   27
  8  \w     51.00  87.00   1.00   70.00    --  106.13 -30.00   0.00   36
  9  \w     29.00 107.00   1.00   70.00    --  106.13 -95.00 120.00   78
 10  \w     37.00 109.00   1.00   70.00    --  106.13-125.00  90.00   72
 11  \w     42.00 132.00   1.00   70.00    --  106.13 -77.00-180.00   90
;
_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      0.0171348000
_diffrn_orient_matrix_UB_12      0.0291036000
_diffrn_orient_matrix_UB_13      0.0703128000
_diffrn_orient_matrix_UB_21      0.0414822000
_diffrn_orient_matrix_UB_22      -0.1121017000
_diffrn_orient_matrix_UB_23      0.0110131000
_diffrn_orient_matrix_UB_31      0.0836048000
_diffrn_orient_matrix_UB_32      0.0496052000
_diffrn_orient_matrix_UB_33      -0.0163431000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17866
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.444
_diffrn_reflns_theta_min         3.363
_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    15.514
_exptl_absorpt_correction_T_max  0.313
_exptl_absorpt_correction_T_min  0.065
_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    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.064
_refine_diff_density_max         2.154
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         12242
_refine_ls_number_restraints     1796
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1502P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1897
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                8031
_reflns_number_total             12242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           pdpeld_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_database_code               7047988
_nottingham_internal_coll_name   PDPELD
_nottingham_internal_coll_number 16340
_nottingham_internal_coll_client PEL/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '70.00, 17.50'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   27/07/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017-09'
_nottingham_internal_process_date 27/01/2017
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 08/02/2017
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 08/02/2017
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 08/02/2017
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C87H99I4N6O10Pd2
_chemical_oxdiff_usercomment
'PDPELD#16340 SN-1004 IN FOMBLIN FILM ON A MICROMOUNT FOR PEL/NRC'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(2) 0.49(2)
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
 N5B-C33B = C34B-C33B = C35B-C34B = C37B-C36B = C36B-C35B = N5B-C37B = N6B-
 C42B = N6B-C38B = C39B-C38B = C40B-C39B = C41B-C40B = C42B-C41B
 1.34914 with sigma of 0.02
 C3B-C2B = C2B-C1B = C6B-C1B = C6B-C5B = C5B-C4B = C4B-C3B = C29B-C28B = C28B-
 C27B = C27B-C26B = C26B-C25B = C25B-C24B = C29B-C24B
 1.38226 with sigma of 0.02
 C34A-C29A = C34A-C33A = C33A-C32A = C32A-C31A = C31A-C30A = C30A-C29A = C2A-
 C1A = C6A-C1A = C5A-C4A = C6A-C5A = C4A-C3A = C3A-C2A = C9A-C8A = C8A-C13A =
 C13A-C12A = C12A-C11A = C9A-C10A = C11A-C10A = C20A-C15A = C19A-C18A = C20A-
 C19A = C17A-C16A = C18A-C17A = C16A-C15A = C27A-C22A = C27A-C26A = C26A-C25A =
 C25A-C24A = C23A-C22A = C24A-C23A
 1.38075 with sigma of 0.02
 C8A-C7A = C7A-C4A = C15A-C14A = C14A-C11A = C21A-C18A = C22A-C21A = C28A-C25A
 = C29A-C28A = C35A-C32A = C35A-C1A
 1.5281 with sigma of 0.02
 N5B-C34B
 2.33549 with sigma of 0.04
 C33B-C35B
 2.33549 with sigma of 0.04
 C34B-C36B
 2.33549 with sigma of 0.04
 C35B-C37B
 2.33549 with sigma of 0.04
 C36B-N5B
 2.33549 with sigma of 0.04
 C37B-C33B
 2.33549 with sigma of 0.04
 N6B-C39B
 2.33549 with sigma of 0.04
 C38B-C40B
 2.33549 with sigma of 0.04
 C39B-C41B
 2.33549 with sigma of 0.04
 C40B-C42B
 2.33549 with sigma of 0.04
 C41B-N6B
 2.33549 with sigma of 0.04
 C42B-C38B
 2.33549 with sigma of 0.04
 C5B-C3B
 2.39289 with sigma of 0.04
 C4B-C2B
 2.39289 with sigma of 0.04
 C3B-C1B
 2.39289 with sigma of 0.04
 C2B-C6B
 2.39289 with sigma of 0.04
 C1B-C5B
 2.39289 with sigma of 0.04
 C6B-C4B
 2.39289 with sigma of 0.04
 C28B-C24B
 2.39289 with sigma of 0.04
 C28B-C26B
 2.39289 with sigma of 0.04
 C27B-C25B
 2.39289 with sigma of 0.04
 C26B-C24B
 2.39289 with sigma of 0.04
 C25B-C29B
 2.39289 with sigma of 0.04
 C29B-C27B
 2.39289 with sigma of 0.04
 C29A-C33A
 2.38882 with sigma of 0.04
 C34A-C32A
 2.38882 with sigma of 0.04
 C33A-C31A
 2.38882 with sigma of 0.04
 C32A-C30A
 2.38882 with sigma of 0.04
 C31A-C29A
 2.38882 with sigma of 0.04
 C30A-C34A
 2.38882 with sigma of 0.04
 C1A-C5A
 2.38882 with sigma of 0.04
 C6A-C4A
 2.38882 with sigma of 0.04
 C5A-C3A
 2.38882 with sigma of 0.04
 C4A-C2A
 2.38882 with sigma of 0.04
 C3A-C1A
 2.38882 with sigma of 0.04
 C2A-C6A
 2.38882 with sigma of 0.04
 C8A-C12A
 2.38882 with sigma of 0.04
 C13A-C11A
 2.38882 with sigma of 0.04
 C12A-C10A
 2.38882 with sigma of 0.04
 C11A-C9A
 2.38882 with sigma of 0.04
 C10A-C8A
 2.38882 with sigma of 0.04
 C9A-C13A
 2.38882 with sigma of 0.04
 C15A-C19A
 2.38882 with sigma of 0.04
 C20A-C18A
 2.38882 with sigma of 0.04
 C19A-C17A
 2.38882 with sigma of 0.04
 C18A-C16A
 2.38882 with sigma of 0.04
 C17A-C15A
 2.38882 with sigma of 0.04
 C22A-C26A
 2.38882 with sigma of 0.04
 C27A-C25A
 2.38882 with sigma of 0.04
 C26A-C24A
 2.38882 with sigma of 0.04
 C25A-C23A
 2.38882 with sigma of 0.04
 C24A-C22A
 2.38882 with sigma of 0.04
 C23A-C27A
 2.38882 with sigma of 0.04
 C9A-C38A
 2.43992 with sigma of 0.04
 C2A-C36A
 2.43992 with sigma of 0.04
 C37A-C5A
 2.43992 with sigma of 0.04
 C44A-C30A
 2.43992 with sigma of 0.04
 C33A-C45A
 2.43992 with sigma of 0.04
 C26A-C43A
 2.43992 with sigma of 0.04
 C23A-C42A
 2.43992 with sigma of 0.04
 C1A-C32A
 2.52469 with sigma of 0.04
 C29A-C25A
 2.59259 with sigma of 0.04
 C22A-C18A
 2.59259 with sigma of 0.04
 C15A-C11A
 2.59259 with sigma of 0.04
 C8A-C4A
 2.59259 with sigma of 0.04
 C16A-C40A
 2.43992 with sigma of 0.04
 O2A-C5A \\sim O4A-C12A \\sim O3A-C9A \\sim O5A-C16A \\sim O1A-C2A \\sim
O10A-C33A \\sim O9A-C30A ~
 O8A-C26A \\sim O6A-C19A \\sim O7A-C23A
 with sigma of 0.02
 O6A-C41A \\sim O5A-C40A \\sim O7A-C42A \\sim O4A-C39A \\sim O8A-C43A \\sim
O9A-C44A \\sim O10A-C45A ~
 O1A-C36A \\sim O2A-C37A \\sim O3A-C38A
 with sigma of 0.02
 C8B-C4B \\sim C7B-C2B \\sim C9B-C6B
 with sigma of 0.02
 N4B-C20B \\sim N3B-C20B \\sim N1B-C11B \\sim N2B-C11B
 with sigma of 0.02
 N2B-C13B \\sim N1B-C12B \\sim N3B-C21B \\sim N4B-C22B
 with sigma of 0.02
 C22B-C21B \\sim C13B-C12B
 with sigma of 0.02
4. Restrained planarity
 C1B, C2B, C3B, C4B, C5B, C6B
 with sigma of 0.1
 C24B, C25B, C26B, C27B, C28B, C29B
 with sigma of 0.1
5. 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
6. 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
7. Others
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=
 1(DANG)=1(DANG)=1(DANG)=FVAR(2)
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=
 1(DANG)=1(DANG)=1(DANG)=FVAR(4)
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=
 1(DANG)=1(DANG)=FVAR(6)
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=1(DANG)=FVAR(8)
 1(DANG)=1(DANG)=1(DANG)=1(DANG)=FVAR(9)
8.a Secondary CH2 refined with riding coordinates:
 C10B(H10a,H10b), C14B(H14a,H14b), C15B(H15a,H15b), C16B(H16a,H16b), C17B(H17a,
 H17b), C18B(H18a,H18b), C19B(H19a,H19b), C23B(H23a,H23b), C7A(H7Aa,H7Ab),
 C14A(H14c,H14d), C21A(H21a,H21c), C28A(H28a,H28c), C35A(H35a,H35c)
8.b Me refined with riding coordinates:
 C30B(H30a,H30b,H30c), C31B(H31a,H31b,H31c), C32B(H32a,H32b,H32c), C7B(H7Ba,
 H7Bb,H7Bc), C8B(H8Ba,H8Bb,H8Bc), C9B(H9Ba,H9Bb,H9Bc), C37A(H37a,H37c,H37d),
 C39A(H39a,H39c,H39d), C40A(H40a,H40c,H40d), C41A(H41a,H41c,H41d), C42A(H42a,
 H42c,H42d), C43A(H43a,H43b,H43c), C44A(H44a,H44b,H44c), C45A(H45a,H45b,H45c)
8.c Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C5B(H5B), C12B(H12B), C13B(H13B), C21B(H21B), C22B(H22B),
 C26B(H26B), C28B(H28B), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B),
 C37B(H37B), C38B(H38B), C39B(H39B), C40B(H40B), C41B(H41B), C42B(H42B),
 C3A(H3A), C6A(H6A), C10A(H10c), C13A(H13A), C17A(H17c), C20A(H20A), C24A(H24A),
  C27A(H27A), C31A(H31d), C34A(H34A)
8.d Idealised Me refined as rotating group:
 C36A(H36a,H36c,H36d), C38A(H38a,H38c,H38d)
;
_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 2.997
_oxdiff_exptl_absorpt_empirical_full_min 0.253
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 173.8682\% 
 around [0.10 0.01 0.99] (reciprocal) or [0.22 0.04 0.98] (direct)
;