[2]pseudorotaxane formation with N-benzylanilinium axles and 24-crown-8 ether wheels.
Loeb, Stephen J.; Tiburcio, Jorge; Vella, Sarah J.; Organic letters 7 (2005) 4923–4926; doi:10.1021/ol051786e

data_1506712
_publ_contact_author
;
 Stephen J. Loeb
 Department of Chemistry and Biochemistry
 University of Windsor
 Windsor, Ontario, Canada
 N9B 3P4
 
;
_publ_section_title
;
 [2]pseudorotaxane formation with N-benzylanilinium axles and 24-crown-8
 ether wheels.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              4923
_journal_page_last               4926
_journal_paper_doi               10.1021/ol051786e
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C52 H60 F9 N O15 S'
_chemical_formula_weight         1142.07
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.5410(10)
_cell_angle_beta                 77.1870(10)
_cell_angle_gamma                66.6440(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4607(9)
_cell_length_b                   14.0815(9)
_cell_length_c                   16.0914(11)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     2724.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'hemisphere scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%
;
;
_diffrn_standards_number         50
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.875219
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas
;
;
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.30
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_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1528P)^2^+3.5621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2848
_reflns_number_gt                6051
_reflns_number_total             9556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol051786esi20050728_035829.cif
_cod_data_source_block           (2]pseudorotaxane
_cod_original_cell_volume        2724.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1506712