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_1502310
_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
'C50 H54 N2 O14, C12 H14 N2, 2(F6 P), 2.78(C2 H3 N)'
_chemical_formula_sum            'C67.56 H76.33 F12 N6.78 O14 P2'
_chemical_formula_weight         1497.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.495(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6770(2)
_cell_length_b                   31.7992(7)
_cell_length_c                   21.0198(5)
_cell_measurement_reflns_used    28015
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4243
_cell_measurement_theta_min      3.6141
_cell_volume                     7075.7(3)
_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_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0109674000
_diffrn_orient_matrix_UB_12      -0.0208116000
_diffrn_orient_matrix_UB_13      0.0115244000
_diffrn_orient_matrix_UB_21      -0.0025150000
_diffrn_orient_matrix_UB_22      -0.0073668000
_diffrn_orient_matrix_UB_23      -0.0319925000
_diffrn_orient_matrix_UB_31      0.0660672000
_diffrn_orient_matrix_UB_32      0.0031768000
_diffrn_orient_matrix_UB_33      0.0014023000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89157
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         15978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0798P)^2^+6.8820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                11528
_reflns_number_total             15978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201502r_si_005.cif
_cod_data_source_block           cs1675
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1502310