Pseudocryptand-type [2]pseudorotaxanes based on bis(meta-phenylene)-32-crown-10 derivatives and paraquats with remarkably improved association constants.
Niu, Zhenbin; Slebodnick, Carla; Schoonover, Daniel; Azurmendi, Hugo; Harich, Kim; Gibson, Harry W.; Organic letters 13 (2011) 3992–3995; doi:10.1021/ol201502r

data_1502309
_publ_section_title
;
 Pseudocryptand-type [2]pseudorotaxanes based on
 bis(meta-phenylene)-32-crown-10 derivatives and paraquats with remarkably
 improved association constants.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3992
_journal_page_last               3995
_journal_paper_doi               10.1021/ol201502r
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C48 H52 N4 O14, C12 H14 N2, 2(F6 P)'
_chemical_formula_sum            'C60 H66 F12 N6 O14 P2'
_chemical_formula_weight         1385.13
_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             2011-05-11
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.224(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4472(3)
_cell_length_b                   31.1654(17)
_cell_length_c                   21.6799(9)
_cell_measurement_reflns_used    9401
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      77.7409
_cell_measurement_theta_min      3.5025
_cell_volume                     6986.2(5)
_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      100.1
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            'Oxford Diffraction Atlas'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega -110.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -37.0000  -90.0000 94

  2 omega  -68.00   28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552   37.0000   90.0000 96

  3 omega   24.00   99.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3552 -125.0000  -90.0000 75

  4 omega   53.00   80.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3552 -125.0000   90.0000 27

  5 omega  101.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000  -90.0000 75

  6 omega   39.00   77.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 38

  7 omega   38.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -119.0000  158.0000 67

  8 omega   86.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000    0.0000 92

  9 omega   42.00  117.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -122.0000  -83.0000 75

 10 omega  101.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000 -150.0000 77

 11 omega   94.00  167.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   30.0000 73

 12 omega   52.00  114.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -108.0000  -49.0000 62

 13 omega   39.00   68.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 29

 14 omega -120.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000 -150.0000 112

 15 omega -120.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000  120.0000 112

 16 omega -120.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000   30.0000 112

 17 omega   52.00  100.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  -60.0000 48

 18 omega   79.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 99

 19 omega   52.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000 -180.0000 126
;
_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      -0.0039799000
_diffrn_orient_matrix_UB_12      0.0456848000
_diffrn_orient_matrix_UB_13      0.0268109000
_diffrn_orient_matrix_UB_21      0.0402617000
_diffrn_orient_matrix_UB_22      -0.0177327000
_diffrn_orient_matrix_UB_23      0.0662450000
_diffrn_orient_matrix_UB_31      0.1434246000
_diffrn_orient_matrix_UB_32      0.0064158000
_diffrn_orient_matrix_UB_33      -0.0070614000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            56783
_diffrn_reflns_theta_full        77.96
_diffrn_reflns_theta_max         77.96
_diffrn_reflns_theta_min         3.51
_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    1.401
_exptl_absorpt_correction_T_max  1.285
_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    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.5948
_exptl_crystal_size_mid          0.0763
_exptl_crystal_size_min          0.0477
_platon_squeeze_details
;
;
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         14427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1531P)^2^+4.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2604
_refine_ls_wR_factor_ref         0.2844
_reflns_number_gt                8996
_reflns_number_total             14427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201502r_si_004.cif
_cod_data_source_block           cs1719
_cod_database_code               1502309
_chemical_oxdiff_formula         'C48 H52 N4 O14 C12 H14 F12 N2 P2'
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33