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_1502409
_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
'2(C42 H50 N2 O14), C30 H30 N4, 2(C3 H6 O), 4(F6 P), 0.6(H2 O)'
_chemical_formula_sum            'C120 H143.2 F24 N8 O30.6 P4'
_chemical_formula_weight         2767.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-05-24
_audit_creation_method
;
  Olex2 1.1
  (compiled Feb 15 2011 20:38:53, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.028(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.050(3)
_cell_length_b                   11.6489(7)
_cell_length_c                   26.955(3)
_cell_measurement_reflns_used    3829
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.1326
_cell_measurement_theta_min      3.7915
_cell_volume                     6583.7(13)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_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      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            'Oxford Diffraction Atlas'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -100.00  -23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4802  -37.0000  150.0000 77

  2 omega  -78.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4802  125.0000 -150.0000 72

  3 omega -116.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4802  -37.0000   60.0000 102

  4 omega   38.00   76.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 38

  5 omega   39.00   77.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 38

  6 omega  100.00  177.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000 -180.0000 77

  7 omega   43.00   77.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 34

  8 omega   41.00   77.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 36

  9 omega   39.00   75.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   90.0000 36

 10 omega   38.00   77.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   60.0000 39

 11 omega   32.00  178.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000    0.0000 146

 12 omega -119.00   -7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4802  -77.0000   30.0000 112

 13 omega -119.00   -7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.4802  -77.0000  -60.0000 112

 14 omega   23.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.4802 -125.0000  150.0000 75

 15 omega   52.00  178.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000 -120.0000 126

 16 omega   52.00  178.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  120.0000 126

 17 omega   33.00  110.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -105.0000  140.0000 77

 18 omega   34.00  118.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000 -120.0000 84

 19 omega   85.00  178.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000    0.0000 93

 20 omega   38.00   77.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -180.0000 39
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0253540000
_diffrn_orient_matrix_UB_12      0.0408139000
_diffrn_orient_matrix_UB_13      0.0570708000
_diffrn_orient_matrix_UB_21      0.0543757000
_diffrn_orient_matrix_UB_22      -0.0884847000
_diffrn_orient_matrix_UB_23      0.0106299000
_diffrn_orient_matrix_UB_31      0.0424069000
_diffrn_orient_matrix_UB_32      0.0894963000
_diffrn_orient_matrix_UB_33      -0.0155012000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1220
_diffrn_reflns_av_unetI/netI     0.1366
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40113
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         4.17
_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    1.490
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_recrystallization_method 'Crystallized from acetone/pentane'
_exptl_crystal_size_max          0.2757
_exptl_crystal_size_mid          0.1308
_exptl_crystal_size_min          0.0135
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         12019
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.2203
_refine_ls_R_factor_gt           0.1357
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3536
_refine_ls_wR_factor_ref         0.4209
_reflns_number_gt                6215
_reflns_number_total             12019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201837x_si_002.cif
_cod_data_source_block           cs1677
_cod_original_cell_volume        6583.9(12)
_cod_original_formula_sum        'C120 H143.20 F24 N8 O30.60 P4'
_cod_database_code               1502409
_chemical_oxdiff_usercomment     'Zhenbin Niu/Gibson (NiuC50-1)'