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_7047995
_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         'C30 H39 Cl1.09 I1.91 N4 Pd, C45 H50 O10'
_chemical_formula_sum            'C79.25 H93.25 Cl13.84 I1.91 N4 O10 Pd'
_chemical_formula_weight         2101.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-08-06 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.023(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.515(2)
_cell_length_b                   22.309(3)
_cell_length_c                   24.313(2)
_cell_measurement_reflns_used    930
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      38.9410
_cell_measurement_theta_min      2.6790
_cell_volume                     8952.1(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_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    -56.00 -27.00   1.00   50.00    --  -42.81  19.00-120.00   29
  2  \w    -46.00  28.00   1.00   50.00    --  -42.81  38.00   0.00   74
  3  \w    -42.00  26.00   1.00   50.00    --  -42.81  38.00-120.00   68
  4  \w    -41.00  25.00   1.00   50.00    --  -42.81  38.00 120.00   66
  5  \w     35.00  97.00   1.00  200.00    --  102.38 -45.00  90.00   62
  6  \w     47.00  93.00   1.00  200.00    --  102.38 -45.00 -90.00   46
  7  \w     30.00  81.00   1.00  200.00    --  102.38 -30.00  30.00   51
  8  \w    118.00 173.00   1.00  200.00    --  102.38  30.00 120.00   55
  9  \w     32.00  87.00   1.00  200.00    --  102.38 -30.00 -30.00   55
 10  \w     88.00 120.00   1.00  200.00    --  102.38  45.00-150.00   32
;
_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      0.0135260000
_diffrn_orient_matrix_UB_12      -0.0454368000
_diffrn_orient_matrix_UB_13      -0.0464720000
_diffrn_orient_matrix_UB_21      0.0884001000
_diffrn_orient_matrix_UB_22      0.0212921000
_diffrn_orient_matrix_UB_23      -0.0034318000
_diffrn_orient_matrix_UB_31      0.0265471000
_diffrn_orient_matrix_UB_32      -0.0474458000
_diffrn_orient_matrix_UB_33      0.0430477000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2595
_diffrn_reflns_av_unetI/netI     0.3588
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25705
_diffrn_reflns_point_group_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.689
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    11.106
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.559
_exptl_crystal_description       plate
_exptl_crystal_F_000             4237
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00092(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         14455
_refine_ls_number_restraints     2231
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.4321
_refine_ls_R_factor_gt           0.2550
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5236
_refine_ls_wR_factor_ref         0.6260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1851
_reflns_number_total             14455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           pdpelf_sq
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_original_cell_volume        8952.2(18)
_cod_database_code               7047995
_nottingham_internal_coll_name   PDPELF
_nottingham_internal_coll_number 17593
_nottingham_internal_coll_client PEL/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '200.00, 50.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   20/03/2018
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 30/05/2018
_nottingham_internal_process_user pczwl
_nottingham_internal_solution_date 21/3/2018
_nottingham_internal_solution_user pczwl
_nottingham_internal_refinement_date 30/5/2018
_nottingham_internal_refinement_user pczwl
_nottingham_internal_validation_date 30/5/2018
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 30/5/2018
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C75H89Br2ClN4O10Pd
_chemical_oxdiff_usercomment
'PDPELF #17593 GVA-1414 IN FOMBLIN FILM ON A MICROMOUNT FOR PEL/NRC'
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.328
_reflns_odcompleteness_completeness 91.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. 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
2. Restrained distances
 H83A-H90A
 -1.9 with sigma of 0.02
 C34B-C35B \\sim C30B-C35B \\sim C30B-C31B \\sim C31B-C32B \\sim C33B-C32B
\\sim C33B-C34B
 with sigma of 0.02
 C28B-C23B \\sim C23B-C25B
 with sigma of 0.02
 N24B-C23B \\sim N18B-C20B
 with sigma of 0.02
 C23B-C22B \\sim C21B-C22B \\sim C21B-C20B
 with sigma of 0.02
 C19B-C20B \\sim C20B-C17B
 with sigma of 0.02
 C23B-C21B \\sim C22B-C20B
 with sigma of 0.02
 C10B-C5B \\sim C6B-C5B \\sim C7B-C6B \\sim C8B-C7B \\sim C9B-C8B \\sim C10B-C9B
 with sigma of 0.02
 C5B-C7B \\sim C6B-C8B \\sim C7B-C9B \\sim C8B-C10B \\sim C9B-C5B \\sim
C10B-C6B \\sim C30B-C32B ~
 C31B-C33B \\sim C32B-C34B \\sim C33B-C35B \\sim C34B-C30B \\sim C35B-C31B
 with sigma of 0.02
 C6B-C14B \\sim C14B-C10B \\sim C31B-C29B \\sim C29B-C35B
 with sigma of 0.02
 C19B-C14B \\sim C14B-C16B
 with sigma of 0.02
 C26B-C25B \\sim C16B-C17B
 with sigma of 0.02
 N27B-C29B \\sim N15B-C14B \\sim N18B-C20B \\sim N24B-C23B
 with sigma of 0.02
 C19B-C20B \\sim C20B-C17B \\sim C23B-C25B \\sim C25B-C28B \\sim C26B-C29B
\\sim C29B-C28B \\sim C19B-
 C14B \\sim C14B-C16B
 with sigma of 0.02
 N15B-C14B \\sim N18B-C20B \\sim N24B-C23B \\sim N27B-C29B
 with sigma of 0.02
 C30B-C29B \\sim C14B-C5B
 with sigma of 0.02
 C10B-C5B \\sim C6B-C5B \\sim C10B-C9B \\sim C9B-C8B \\sim C8B-C7B \\sim
C7B-C6B \\sim C35B-C30B ~
 C31B-C30B \\sim C32B-C31B \\sim C35B-C34B \\sim C34B-C33B \\sim C33B-C32B
 with sigma of 0.02
 N15B-C14B \\sim C14B-C5B \\sim N18B-C20B \\sim C20B-C21B \\sim C21B-C22B \\sim
C22B-C23B \\sim N24B-
 C23B \\sim N27B-C29B \\sim C30B-C29B
 with sigma of 0.02
 C11B-C6B \\sim C13B-C10B \\sim C12B-C8B
 with sigma of 0.02
 H13B-H14B \\sim H14B-H13A
 with sigma of 0.02
 C38B-C35B \\sim C31B-C36B \\sim C33B-C37B
 with sigma of 0.02
 C5B-C11B \\sim C11B-C7B \\sim C7B-C12B \\sim C12B-C9B \\sim C9B-C13B \\sim
C13B-C5B \\sim C30B-C38B ~
 C38B-C34B \\sim C30B-C36B \\sim C36B-C32B \\sim C32B-C37B \\sim C37B-C34B
 with sigma of 0.02
 H36A-H29A \\sim H29A-H36B
 with sigma of 0.02
 I4B-Pd1B \\sim I3B-Pd1B \\sim I2B-Pd1B
 with sigma of 0.02
 Pd1B-Cl2B \\sim Pd1B-Cl4B \\sim Pd1B-Cl3B
 with sigma of 0.02
 C83A-C91A \\sim C91A-C81A
 with sigma of 0.02
 C84A-C71A \\sim C71A-C86A \\sim C63A-C71A \\sim C71A-C61A \\sim C64A-C51A
\\sim C51A-C66A \\sim C41A-
 C51A \\sim C51A-C43A \\sim C44A-C31A \\sim C31A-C46A \\sim C23A-C31A \\sim
C31A-C21A \\sim C24A-C11A ~
 C11A-C26A \\sim C3A-C11A \\sim C11A-C1A \\sim C4A-C91A \\sim C91A-C6A
 with sigma of 0.02
 C25A-C11A \\sim C2A-C11A \\sim C91A-C5A \\sim C91A-C82A \\sim C71A-C85A \\sim
C62A-C71A \\sim C65A-
 C51A \\sim C42A-C51A \\sim C22A-C31A \\sim C45A-C31A
 with sigma of 0.02
 O29A-C24A \\sim O9A-C4A \\sim O89A-C84A \\sim O69A-C64A \\sim O49A-C44A \\sim
O47A-C41A \\sim O27A-
 C21A \\sim O7A-C1A \\sim O87A-C81A \\sim O67A-C61A
 with sigma of 0.02
 C82A-O87A \\sim O87A-C86A \\sim C62A-O67A \\sim O67A-C66A \\sim C42A-O47A
\\sim O47A-C46A \\sim C22A-
 O27A \\sim O27A-C26A \\sim C2A-O7A \\sim O7A-C6A \\sim C3A-O9A \\sim O9A-C5A
\\sim C83A-O89A \\sim O89A-
 C85A \\sim C63A-O69A \\sim O69A-C65A \\sim C43A-O49A \\sim O49A-C45A \\sim
C23A-O29A \\sim O29A-C25A
 with sigma of 0.02
 O69A-C70A \\sim O89A-C90A \\sim O9A-C10A \\sim O49A-C50A \\sim O29A-C30A \\sim
O27A-C28A \\sim O7A-
 C8A \\sim O87A-C88A \\sim O47A-C48A \\sim O67A-C68A
 with sigma of 0.02
 C4A-C10A \\sim C24A-C30A \\sim C44A-C50A \\sim C64A-C70A \\sim C84A-C90A \\sim
C81A-C88A \\sim C61A-
 C68A \\sim C41A-C48A \\sim C21A-C28A \\sim C1A-C8A
 with sigma of 0.02
 H90A-H11E_$1 \\sim H11E_$1-H90C
 with sigma of 0.04
3. Restrained planarity
 C51A, C61A, C62A, C63A, C64A, C65A, C66A, O67A, O69A, C71A
 with sigma of 0.1
 C31A, C41A, C42A, C43A, C44A, C45A, C46A, O47A, O49A, C51A
 with sigma of 0.1
 C11A, C21A, C22A, C23A, C24A, C25A, C26A, O27A, O29A, C31A
 with sigma of 0.1
 C1A, C2A, C3A, C4A, C5A, C6A, O7A, O9A, C11A, C91A
 with sigma of 0.1
 C23B, N24B, C25B, C26B, N27B, C28B, C29B
 with sigma of 0.1
 C5B, C6B, C7B, C8B, C9B, C10B, C11B, C12B, C13B, C14B
 with sigma of 0.1
 Pd1B, I2B, C14B, N15B, C16B, C17B, N18B, C19B, C20B
 with sigma of 0.1
 C30B, C31B, C32B, C33B, C34B, C35B, C36B, C37B, C38B
 with sigma of 0.1
 C71A, C81A, C82A, C83A, C84A, C85A, C86A, O87A, O89A, C91A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
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(I2B)=1-FVAR(1)
 Sof(Cl2B)=FVAR(1)
 Sof(Cl4B)=1-FVAR(2)
 Sof(I4B)=FVAR(2)
 Sof(Cl3B)=1-FVAR(3)
 Sof(I3B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C14B(H14A,H14B), C20B(H20A,H20B), C21B(H21A,H21B), C22B(H22A,H22B), C23B(H23B,
 H23C), C29B(H29A,H29B), C11A(H11A,H11B), C31A(H31A,H31B), C51A(H51A,H51B),
 C71A(H71A,H71B), C91A(H91A,H91B)
7.b Me refined with riding coordinates:
 C11B(H11C,H11D,H11E), C12B(H12A,H12B,H12C), C37B(H37A,H37B,H37C), C38B(H38A,
 H38B,H38C), C8A(H8AA,H8AB,H8AC), C10A(H10A,H10B,H10C), C28A(H28A,H28B,H28C),
 C30A(H30A,H30B,H30C), C48A(H48A,H48B,H48C), C50A(H50A,H50B,H50C), C68A(H68A,
 H68B,H68C), C70A(H70A,H70B,H70C), C88A(H88A,H88B,H88C)
7.c Aromatic/amide H refined with riding coordinates:
 C7B(H7B), C9B(H9B), C16B(H16B), C17B(H17B), C28B(H28D), C25B(H25B),
 C26B(H26B), C34B(H34B), C32B(H32B), C6A(H6A), C3A(H3A), C26A(H26A), C23A(H23A),
  C43A(H43A), C46A(H46A), C63A(H63A), C66A(H66A), C86A(H86A), C83A(H83A)
7.d Fitted pentagon refined as free rotating group:
 N15B(C16B,C17B,N18B,C19B), N27B(C28B,N24B,C25B,C26B)
7.e Fitted hexagon refined as free rotating group:
 C5B(C6B,C7B,C8B,C9B,C10B), C30B(C35B,C34B,C33B,C32B,C31B), C2A(C1A,C6A,C5A,
 C4A,C3A), C22A(C21A,C26A,C25A,C24A,C23A), C42A(C43A,C44A,C45A,C46A,C41A),
 C62A(C63A,C64A,C65A,C66A,C61A), C82A(C81A,C86A,C85A,C84A,C83A)
7.f Idealised Me refined as rotating group:
 C13B(H13A,H13B,H13C), C36B(H36A,H36B,H36C), C90A(H90A,H90B,H90C)
;
_shelx_res_checksum              38312
_shelx_fab_checksum              44787
_olex2_date_sample_data_collection 2018-03-20
_olex2_date_sample_submission    2018-03-12
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id PL411
_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 3.174
_oxdiff_exptl_absorpt_empirical_full_min 0.531