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_7110373
_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            'C68 H82 B4 F16 N4 O8'
_chemical_formula_weight         1430.62
_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
_cell_angle_alpha                86.686(1)
_cell_angle_beta                 80.281(1)
_cell_angle_gamma                75.390(1)
_cell_formula_units_Z            2
_cell_length_a                   13.9669(3)
_cell_length_b                   17.0627(3)
_cell_length_c                   17.0640(3)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      1.21
_cell_volume                     3878.11(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      293(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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15271
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and finish'
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.49203
_exptl_absorpt_correction_T_min  0.26566
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.908
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         9509
_refine_ls_number_restraints     795
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.246
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_obs          0.1297
_refine_ls_shift/esd_max         -0.976
_refine_ls_shift/esd_mean        0.092
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4310
_refine_ls_wR_factor_obs         0.3690
_reflns_number_observed          4888
_reflns_number_total             9521
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807449fsup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.3628P)^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^)+(0.3628P)^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        3878.1(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110373