Pseudocryptand-type [3]pseudorotaxane and "hook-ring" polypseudo[2]catenane based on a bis(m-phenylene)-32-crown-10 derivative and bisparaquat derivatives.
Niu, Zhenbin; Slebodnick, Carla; Gibson, Harry W.; Organic letters 13 (2011) 4616–4619; doi:10.1021/ol201837x

data_1502410
_publ_section_title
;
 Pseudocryptand-type [3]pseudorotaxane and &quot;hook-ring&quot;
 polypseudo[2]catenane based on a bis(m-phenylene)-32-crown-10 derivative
 and bisparaquat derivatives.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4616
_journal_page_last               4619
_journal_paper_doi               10.1021/ol201837x
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety
'C42 H50 N2 O14, C36 H32 N4, 5(C2 H3 N), 4(F6 P), 0.36 (H2 O)'
_chemical_formula_sum            'C88 H97.72 F24 N11 O14.37 P4'
_chemical_formula_weight         2119.22
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2011-05-26
_audit_creation_method
;
  Olex2 1.1
  (compiled Feb 15 2011 20:38:53, GUI svn.r3494)
;
_cell_angle_alpha                92.123(3)
_cell_angle_beta                 99.809(4)
_cell_angle_gamma                98.463(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4807(6)
_cell_length_b                   13.8068(5)
_cell_length_c                   26.5793(10)
_cell_measurement_reflns_used    13181
_cell_measurement_temperature    99.9
_cell_measurement_theta_max      74.5851
_cell_measurement_theta_min      3.2400
_cell_volume                     4811.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      99.9
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3174
_diffrn_detector_type            'Oxford Diffraction Onyx CCD'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
  1 omega  -97.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9419  125.0000  -30.0000 95

  2 omega   26.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419   37.0000  -30.0000 73

  3 omega   17.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419   77.0000 -150.0000 100

  4 omega  -34.00   70.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419  -37.0000   90.0000 104

  5 omega   51.00  141.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  179.0000  -60.0000 90

  6 omega   81.00  176.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   45.0000   60.0000 95

  7 omega   44.00  117.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -148.0000  -44.0000 73

  8 omega   79.00  171.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   45.0000  120.0000 92

  9 omega   84.00  111.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000   60.0000 27

 10 omega   49.00  141.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000    0.0000 92

 11 omega   33.00   70.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  -60.0000 37

 12 omega   37.00   64.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000   60.0000 27

 13 omega   30.00  104.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -123.0000  -20.0000 74

 14 omega   73.00  173.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   77.0000  150.0000 100

 15 omega -120.00   -8.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9419  -77.0000  -60.0000 112

 16 omega  -34.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419  -37.0000  150.0000 105

 17 omega   12.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419   37.0000   90.0000 105

 18 omega    8.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419   77.0000  120.0000 112

 19 omega -169.00  -56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -77.0000    0.0000 113

 20 omega   73.00  178.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   77.0000 -180.0000 105

 21 omega   59.00  178.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000  -60.0000 119
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Nova'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0202877000
_diffrn_orient_matrix_UB_12      -0.0091221000
_diffrn_orient_matrix_UB_13      -0.0551613000
_diffrn_orient_matrix_UB_21      -0.1040141000
_diffrn_orient_matrix_UB_22      0.0309713000
_diffrn_orient_matrix_UB_23      -0.0201467000
_diffrn_orient_matrix_UB_31      0.0505406000
_diffrn_orient_matrix_UB_32      0.1083290000
_diffrn_orient_matrix_UB_33      0.0050348000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52909
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.76
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'Nova Micro-focus X-ray Source (Cu)'
_diffrn_source_target            Cu
_diffrn_source_type              'Nova Micro-focus X-ray Source (Cu)'
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2187
_exptl_crystal_recrystallization_method
'Crystals grown from CH3CN / diisopropyl ether'
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.1375
_exptl_crystal_size_min          0.0404
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         18823
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.1054
_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^)+(0.1114P)^2^+15.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2556
_refine_ls_wR_factor_ref         0.2857
_reflns_number_gt                11849
_reflns_number_total             18823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201837x_si_003.cif
_cod_data_source_block           cs1679
_cod_database_code               1502410
_chemical_oxdiff_usercomment     'Zhenbin/Gibson NiuC51-3'