[3]Rotaxanes employing multiple 1,2-bis(pyridinium) ethane binding sites and dibenzo-24-crown-8 ethers
Loeb, Stephen J.; Wisner, James A.; Chemical Communications  (2000) 845–; doi:10.1039/b001018i

data_7110888
_publ_section_title
;
 [3]Rotaxanes employing multiple 1,2-bis(pyridinium) ethane binding sites
 and dibenzo-24-crown-8 ethers
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              845
_journal_paper_doi               10.1039/b001018i
_journal_year                    2000
_chemical_formula_sum            'C110 H126 F18 N6 O34 S6'
_chemical_formula_weight         2610.53
_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
_cell_angle_beta                 107.94(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.892(4)
_cell_length_b                   14.926(7)
_cell_length_c                   25.494(13)
_cell_measurement_reflns_used    'reflections form 60 data frames'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.60
_cell_volume                     6115(5)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL XPREP'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'hemisphere scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24910
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and finish'
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.262891
_exptl_absorpt_correction_T_min  0.119497
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         8401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.2204
_refine_ls_R_factor_gt           0.1368
_refine_ls_shift/su_max          0.170
_refine_ls_shift/su_mean         0.011
_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          0.3516
_refine_ls_wR_factor_ref         0.3959
_reflns_number_gt                3770
_reflns_number_total             8401
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            b001018isup1.cif
_cod_data_source_block           symmetrical[3]rotaxane
_cod_original_cell_volume        6115(4)
_cod_original_sg_symbol_H-M      'P21/n (14)'
_cod_database_code               7110888