The first [2]pseudorotaxane and the first pseudocryptand-type poly[2]pseudorotaxane based on bis(meta-phenylene)-32-crown-10 and paraquat derivatives.
Niu, Zhenbin; Slebodnick, Carla; Bonrad, Klaus; Huang, Feihe; Gibson, Harry W.; Organic letters 13 (2011) 2872–2875; doi:10.1021/ol200862b

data_1502195
_publ_section_title
;
 The first [2]pseudorotaxane and the first pseudocryptand-type
 poly[2]pseudorotaxane based on bis(meta-phenylene)-32-crown-10 and
 paraquat derivatives.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2872
_journal_page_last               2875
_journal_paper_doi               10.1021/ol200862b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C54 H58 N2 O10'
_chemical_formula_sum            'C54 H58 N2 O10'
_chemical_formula_weight         895.02
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.540(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2786(13)
_cell_length_b                   13.2257(5)
_cell_length_c                   17.1649(11)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.9818
_cell_measurement_theta_min      4.0303
_cell_volume                     4443.1(5)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_publication_material
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_solution
'SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.0122
_diffrn_detector_type            'Oxford Diffraction Eos'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0753352569
_diffrn_orient_matrix_UB_12      0.0232163357
_diffrn_orient_matrix_UB_13      0.0294334334
_diffrn_orient_matrix_UB_21      0.0067732897
_diffrn_orient_matrix_UB_22      0.0503363876
_diffrn_orient_matrix_UB_23      0.0848076001
_diffrn_orient_matrix_UB_31      0.0208011180
_diffrn_orient_matrix_UB_32      -0.1017580186
_diffrn_orient_matrix_UB_33      0.0489089632
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21340
_diffrn_reflns_theta_full        71.29
_diffrn_reflns_theta_max         71.29
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'Nova (Cu) X-ray Source'
_diffrn_source_current           1
_diffrn_source_voltage           50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
 (compiled May  6 2009,17:20:42)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4273
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+2.6047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                3411
_reflns_number_total             4273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol200862b_si_002.cif
_cod_data_source_block           cs1349
_cod_original_cell_volume        4443.1(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1502195