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_7047996
_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         'C45 H50 O10, C32 H44 N4, 2(C H2 Cl2), 2(I)'
_chemical_formula_sum            'C79 H98 Cl4 I2 N4 O10'
_chemical_formula_weight         1659.21
_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                 102.9695(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0828(3)
_cell_length_b                   12.8444(2)
_cell_length_c                   31.5223(5)
_cell_measurement_reflns_used    48424
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6940
_cell_measurement_theta_min      3.4810
_cell_volume                     7923.8(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                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            'Agilent Diffraction Atlas S2 detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     16.00 113.00   1.00    5.00    --   42.83  57.00 -30.00   97
  2  \w    -20.00  83.00   1.00    5.00    --   42.83 -99.00-180.00  103
  3  \w     20.00 115.00   1.00    5.00    --   42.83  38.00  60.00   95
  4  \w     30.00  91.00   1.00   20.00    --  104.50 -30.00  90.00   61
  5  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00 -30.00   86
  6  \w     30.00  91.00   1.00   20.00    --  104.50 -30.00-180.00   61
  7  \w     33.00  98.00   1.00   20.00    --  104.50 -45.00-150.00   65
  8  \w     24.00 150.00   1.00   20.00    --  104.50 -15.00-150.00  126
  9  \w     33.00  98.00   1.00   20.00    --  104.50 -45.00 -60.00   65
 10  \w     30.00  91.00   1.00   20.00    --  104.50 -30.00 150.00   61
 11  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00  60.00   86
 12  \w    -30.00  65.00   1.00    5.00    --   42.83 -38.00  30.00   95
 13  \w     16.00 113.00   1.00    5.00    --   42.83  57.00 120.00   97
 14  \w     11.00 117.00   1.00    5.00    --   42.83  77.00-180.00  106
 15  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00 150.00   86
 16  \w     59.00 178.00   1.00   20.00    --  104.50  15.00   0.00  119
 17  \w     77.00 175.00   1.00   20.00    --  104.50  61.00  60.00   98
 18  \w     77.00 175.00   1.00   20.00    --  104.50  61.00-180.00   98
 19  \w     77.00 175.00   1.00   20.00    --  104.50  61.00 120.00   98
 20  \w     80.00 176.00   1.00   20.00    --  104.50  45.00-120.00   96
 21  \w    -94.00  -2.00   1.00    5.00    --  -38.50 125.00-120.00   92
 22  \w     11.00 117.00   1.00    5.00    --   42.83  77.00  30.00  106
 23  \w     11.00 117.00   1.00    5.00    --   42.83  77.00 -90.00  106
 24  \w     73.00 102.00   1.00   20.00    --  104.50  77.00   0.00   29
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_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      0.0765759000
_diffrn_orient_matrix_UB_12      0.0213931000
_diffrn_orient_matrix_UB_13      0.0181832000
_diffrn_orient_matrix_UB_21      0.0115005000
_diffrn_orient_matrix_UB_22      0.0026708000
_diffrn_orient_matrix_UB_23      -0.0467088000
_diffrn_orient_matrix_UB_31      -0.0141361000
_diffrn_orient_matrix_UB_32      0.1179446000
_diffrn_orient_matrix_UB_33      -0.0022148000
_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  0.0850
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            95903
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.730
_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    7.939
_exptl_absorpt_correction_T_max  0.196
_exptl_absorpt_correction_T_min  0.011
_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    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.105
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.950
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         14000
_refine_ls_number_restraints     1350
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.1494
_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^)+(0.0526P)^2^+234.3887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3317
_refine_ls_wR_factor_ref         0.3323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13416
_reflns_number_total             14000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           opelld
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_database_code               7047996
_nottingham_internal_coll_name   OPELLD
_nottingham_internal_coll_number 16277
_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,, 5.00, 20.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   12/07/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 21/07/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 21/07/2016
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 21/07/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 21/07/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C77H94N4O10I2
_chemical_oxdiff_usercomment
'OPELLD #16277 GVB-1105 FOMBLIN ON MICROMOUNT FOR PEL/NRC'
_reflns_odcompleteness_completeness 99.96
_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. 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
3. 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
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C35(H35A,H35B),
 C55(H55A,H55B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B), C68(H68A,H68B), C1C(H1CA,H1CB), C2C(H2CA,H2CB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C30(H30), C33(H33), C47(H47), C51(H51), C56(H56), C57(H57), C58(H58), C65(H65),
  C66(H66), C67(H67), C71(H71), C73(H73)
4.c Idealised Me refined as rotating group:
 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), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C75(H75A,H75B,H75C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C)
;
_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 2.405
_oxdiff_exptl_absorpt_empirical_full_min 0.438