1,2-Bis(4,4′-dipyridinium)ethane: a versatile dication for the formation of [2]rotaxanes with dibenzo-24-crown-8 ether
Loeb, Stephen J.; Wisner, James A.; Chemical Communications  (1998) 2757–; doi:10.1039/a807449f

data_7110374
_publ_section_title
;
 1,2-Bis(4,4&#x2032;-dipyridinium)ethane: a versatile dication for the
 formation of [2]rotaxanes with dibenzo-24-crown-8 ether
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2757
_journal_paper_doi               10.1039/a807449f
_journal_year                    1998
_chemical_formula_sum            'C86 H86 B4 F16 N4 O8 Pd2 S4'
_chemical_formula_weight         1991.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 116.800(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.8929(3)
_cell_length_b                   14.3181(2)
_cell_length_c                   19.4361(3)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.5
_cell_volume                     4444.52(13)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       '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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19889
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.15256
_exptl_absorpt_correction_T_min  0.09923
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.974
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         11599
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_obs          0.0569
_refine_ls_shift/esd_max         -0.768
_refine_ls_shift/esd_mean        0.079
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1431
_refine_ls_wR_factor_obs         0.1198
_reflns_number_observed          7492
_reflns_number_total             11604
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807449fsup1.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4444.5(1)
_cod_original_sg_symbol_H-M      Pc
_cod_database_code               7110374