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_7047987
_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, C30 H40 N4, 3(C H Cl3), 0.72(Br), 1.28(Cl)'
_chemical_formula_sum            'C78 H93 Br0.72 Cl10.28 N4 O10'
_chemical_formula_weight         1668.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-07
_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                 102.619(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.652(3)
_cell_length_b                   12.0617(4)
_cell_length_c                   27.909(2)
_cell_measurement_reflns_used    12908
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3170
_cell_measurement_theta_min      3.6630
_cell_volume                     16310.6(17)
_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 Titan S2 detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -111.00 -16.00   1.00   30.00    --  -38.50 -38.00-120.00   95
  2  \w   -111.00 -16.00   1.00   81.43    --  -38.50 -38.00 -30.00   95
  3  \w    -50.00  34.00   1.00   81.43    --  -38.50  38.00   0.00   84
  4  \w     33.00 122.00   1.00   81.43    --  104.50-125.00-150.00   89
  5  \w     30.00  91.00   1.00   81.43    --  104.50 -30.00-120.00   61
  6  \w     30.00  91.00   1.00   81.43    --  104.50 -30.00  90.00   61
  7  \w     31.00 136.00   1.00   81.43    --  104.50 -77.00-150.00  105
  8  \w     81.00 178.00   1.00   81.43    --  104.50  30.00 -90.00   97
  9  \w     30.00  91.00   1.00   81.43    --  104.50 -30.00 150.00   61
 10  \w     33.00  98.00   1.00   81.43    --  104.50 -45.00   0.00   65
 11  \w     16.00 113.00   1.00   81.43    --   43.08  57.00 120.00   97
 12  \w      2.00  98.00   1.00   81.43    --   43.08-125.00-150.00   96
 13  \w     16.00 113.00   1.00   81.43    --   43.08  57.00-150.00   97
 14  \w     77.00 102.00   1.00   81.43    --  104.50  61.00 150.00   25
;
_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      -0.0250346000
_diffrn_orient_matrix_UB_12      0.0329989000
_diffrn_orient_matrix_UB_13      0.0210256000
_diffrn_orient_matrix_UB_21      0.0174408000
_diffrn_orient_matrix_UB_22      -0.0150349000
_diffrn_orient_matrix_UB_23      0.0525177000
_diffrn_orient_matrix_UB_31      0.0089955000
_diffrn_orient_matrix_UB_32      0.1224098000
_diffrn_orient_matrix_UB_33      0.0008209000
_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  0.1578
_diffrn_reflns_av_unetI/netI     0.1099
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50074
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.088
_diffrn_reflns_theta_max         65.088
_diffrn_reflns_theta_min         3.358
_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    4.092
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.506
_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    1.359
_exptl_crystal_description       plank
_exptl_crystal_F_000             6951
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         13868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.291
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0963
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2450
_refine_ls_wR_factor_ref         0.2799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9058
_reflns_number_total             13868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04096f2.cif
_cod_data_source_block           opellg
_cod_depositor_comments
'Adding full bibliography for 7047987--7047996.cif.'
_cod_original_cell_volume        16310.8(16)
_cod_database_code               7047987
_nottingham_internal_coll_name   OPELLG
_nottingham_internal_coll_number 16853
_nottingham_internal_coll_client PEL/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '30.00, 81.43'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxpl
_nottingham_internal_coll_date   03/02/2017
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 07/02/2017
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 07/02/2017
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 07/02/2017
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 07/02/2017
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C78H90N4O10Br2Cl9
_chemical_oxdiff_usercomment
'OPELLG #16853 GVB-1294 in fomblin on a micromount for PEL/NRC'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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. Others
 1*[Sof(Br1)]+1*[Sof(Br2)]+1*[Sof(Cl1)]=1.5 with esd of 0.001
3.a Ternary CH refined with riding coordinates:
 C1C(H1C), C2C(H2C), C3C(H3C)
3.b Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C14A(H14A,H14B), C21A(H21A,H21B), C28A(H28A,H28B), C35A(H35A,
 H35B), C10B(H10A,H10B), C14B(H14C,H14D), C15B(H15A,H15B), C16B(H16B,H16C),
 C17B(H17A,H17B), C21B(H21C,H21D)
3.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C5A(H5A), C9A(H9A), C12A(H12A), C16A(H16A), C19A(H19A), C23A(H23A),
 C26A(H26A), C30A(H30A), C33A(H33A), C3B(H3B), C5B(H5B), C11B(H11B), C12B(H12B),
  C13B(H13B), C18B(H18B), C19B(H19B), C20B(H20B), C24B(H24B), C26B(H26B)
3.d Idealised Me refined as rotating group:
 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), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C28B(H28C,H28D,H28E),
 C29B(H29A,H29B,H29C), C30B(H30B,H30C,H30D)
;
_shelx_res_checksum              40094
_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 1.671
_oxdiff_exptl_absorpt_empirical_full_min 0.596