Benzobis(imidazolium) salts as templates for the self-assembly of starburst [24]pseudorotaxanes and their corresponding carbene-based classic [22]pseudorotaxanes
Foster, Mathew W.; Mehl, Benjamin T.; Treadwell, Ed; Semeniuc, Radu F.; Wheeler, Kraig A.; Chemical Communications  (2019) –; doi:10.1039/C8CC09936G

data_7122848
_publ_section_title
;
 Benzobis(imidazolium) salts as templates for the self-assembly of
 starburst [24]pseudorotaxanes and their corresponding carbene-based
 classic [22]pseudorotaxanes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09936G
_journal_year                    2019
_chemical_formula_moiety         'C36 H44 O10, C12 H16 N4, 2(F6 P)'
_chemical_formula_sum            'C48 H60 F12 N4 O10 P2'
_chemical_formula_weight         1142.94
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-07 deposited with the CCDC.
2019-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7748(2)
_cell_length_b                   22.7748(2)
_cell_length_c                   22.9902(3)
_cell_measurement_reflns_used    8167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.417
_cell_measurement_theta_min      2.731
_cell_volume                     11924.8(2)
_computing_cell_refinement       APEX2
_computing_data_reduction
;
SAINT (Bruker, 2009) and XPREP (Bruker, 2009)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1089
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
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_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.961
_diffrn_reflns_theta_min         2.731
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            colorless
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_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 1820 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.511(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1866
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4530
_reflns_number_total             5414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09936g2.cif
_cod_data_source_block           10rfs09_squeezed
_cod_original_cell_volume        11924.8(3)
_cod_database_code               7122848
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              24433
_shelx_hkl_checksum              73665