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_1502307
_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         'C42 H50 N2 O14'
_chemical_formula_sum            'C42 H50 N2 O14'
_chemical_formula_weight         806.84
_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                 93.7759(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.03389(14)
_cell_length_b                   8.73956(18)
_cell_length_c                   32.8330(7)
_cell_measurement_reflns_used    13224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3183
_cell_measurement_theta_min      4.0447
_cell_volume                     2013.97(7)
_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 8.3174
_diffrn_detector_type            'Oxford Diffraction Onyx CCD'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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      0.1277003000
_diffrn_orient_matrix_UB_12      0.0915429000
_diffrn_orient_matrix_UB_13      0.0312207000
_diffrn_orient_matrix_UB_21      -0.0239086000
_diffrn_orient_matrix_UB_22      -0.1257756000
_diffrn_orient_matrix_UB_23      0.0321642000
_diffrn_orient_matrix_UB_31      0.1769023000
_diffrn_orient_matrix_UB_32      -0.0828870000
_diffrn_orient_matrix_UB_33      -0.0142441000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            24093
_diffrn_reflns_theta_full        76.51
_diffrn_reflns_theta_max         76.51
_diffrn_reflns_theta_min         5.24
_diffrn_source                   'Nova Micro-focus X-ray Source (Cu)'
_diffrn_source_current           0.95
_diffrn_source_voltage           49.5
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd., V1.171.34.36 (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            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0549P)^2^+1.0130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                3761
_reflns_number_total             4172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201502r_si_002.cif
_cod_data_source_block           cs1613
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2013.96(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1502307