The first [2]pseudorotaxane and the first pseudocryptand-type poly[2]pseudorotaxane based on bis(meta-phenylene)-32-crown-10 and paraquat derivatives.
Niu, Zhenbin; Slebodnick, Carla; Bonrad, Klaus; Huang, Feihe; Gibson, Harry W.; Organic letters 13 (2011) 2872–2875; doi:10.1021/ol200862b

data_1502196
_publ_section_title
;
 The first [2]pseudorotaxane and the first pseudocryptand-type
 poly[2]pseudorotaxane based on bis(meta-phenylene)-32-crown-10 and
 paraquat derivatives.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2872
_journal_page_last               2875
_journal_paper_doi               10.1021/ol200862b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety
'C54 H58 N2 O10, 2(C12 H14 N2), 4(F6 P), 3(C3 H6 O), 1.501(H2 O)'
_chemical_formula_sum            'C87 H107 F24 N6 O14.5 P4'
_chemical_formula_weight         2048.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                69.100(4)
_cell_angle_beta                 79.470(3)
_cell_angle_gamma                77.127(4)
_cell_formula_units_Z            2
_cell_length_a                   15.8655(6)
_cell_length_b                   16.8640(7)
_cell_length_c                   19.0778(7)
_cell_measurement_reflns_used    14285
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8232
_cell_measurement_theta_min      2.8732
_cell_volume                     4618.7(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_area_resol_mean 8.3174
_diffrn_detector_type            'Oxford Diffraction Onyx CCD'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_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      0.0266351000
_diffrn_orient_matrix_UB_12      0.0897460000
_diffrn_orient_matrix_UB_13      -0.0326351000
_diffrn_orient_matrix_UB_21      -0.0933202000
_diffrn_orient_matrix_UB_22      0.0408455000
_diffrn_orient_matrix_UB_23      -0.0197819000
_diffrn_orient_matrix_UB_31      -0.0251431000
_diffrn_orient_matrix_UB_32      0.0113772000
_diffrn_orient_matrix_UB_33      0.0781835000
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35283
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         75.00
_diffrn_reflns_theta_min         2.88
_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    1.767
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66
 (release 28-04-2010 CrysAlis171 .NET)(compiled Apr 28 2010,14:27:37)
 Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2126
_exptl_crystal_size_max          0.4895
_exptl_crystal_size_mid          0.0846
_exptl_crystal_size_min          0.0374
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         18424
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1207P)^2^+1.4689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2036
_reflns_number_gt                13572
_reflns_number_total             18424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol200862b_si_003.cif
_cod_data_source_block           cs1583
_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_formula_sum        'C87 H107 F24 N6 O14.50 P4'
_cod_database_code               1502196