Pseudo-polyrotaxanes based on a protonated version of the 1,2-bis(4,4′-bipyridinium)ethane‒24-crown-8 ether motif
Tiburcio, Jorge; Davidson, Gregory J. E.; Loeb, Stephen J.; Chemical Communications  (2002) 1282–; doi:10.1039/b201664h

data_7114299
_publ_section_title
;
 Pseudo-polyrotaxanes based on a protonated version of the
 1,2-bis(4,4&#x2032;-bipyridinium)ethane--24-crown-8 ether motif
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1282
_journal_paper_doi               10.1039/b201664h
_journal_year                    2002
_chemical_formula_sum            'C98 H126 F12 N4 O40 S4'
_chemical_formula_weight         2356.3
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                98.355(7)
_cell_angle_beta                 93.107(6)
_cell_angle_gamma                110.818(7)
_cell_formula_units_Z            1
_cell_length_a                   11.653(4)
_cell_length_b                   14.953(5)
_cell_length_c                   17.266(6)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     2764.0(16)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12412
_diffrn_reflns_theta_full        23.35
_diffrn_reflns_theta_max         23.35
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.1452
_exptl_absorpt_correction_T_min  0.1045
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1234
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         7890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.361
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1803P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.2867
_reflns_number_gt                4361
_reflns_number_total             7890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201664h.txt
_cod_data_source_block           pi-stacked_pseudo-polyrotaxane
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2764.2(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114299