Crystallographic Distinction between "Contact" and "Separated" Ion Pairs: Structural Effects on Electronic/ESR Spectra of Alkali-Metal Nitrobenzenides
Milya G. Davlieva; Jian-Ming Lü; Sergey V. Lindeman; Jay K. Kochi; Journal of the American Chemical Society 126 (2004) 4557–4565; doi:10.1021/ja049856k

data_4112435
_publ_section_title
;
 Crystallographic Distinction between "Contact" and "Separated" Ion Pairs:
 Structural Effects on Electronic/ESR Spectra of Alkali-Metal
 Nitrobenzenides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4557
_journal_page_last               4565
_journal_paper_doi               10.1021/ja049856k
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'chemical synthesis'
_chemical_formula_sum            'C44 H74 Cs2 N2 O18'
_chemical_formula_weight         1184.88
_chemical_name_systematic
; 
 Bis(cesium 18-crown-6 nitrobenzenide) tetrahydrofurane disolvate
;
_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                99.0780(10)
_cell_angle_beta                 93.0020(10)
_cell_angle_gamma                102.6190(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5177(5)
_cell_length_b                   12.4319(7)
_cell_length_c                   26.1918(14)
_cell_measurement_reflns_used    5828
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     2661.7(3)
_computing_cell_refinement       'SAINT V6.28 (BrukerAXS, 1997-2001)'
_computing_data_collection       'SMART V5.625 (BrukerAXS, 1997-2001)'
_computing_data_reduction        'SAINT & SADABS V2.06 (Sheldrick, 2000)'
_computing_molecular_graphics    'XP V5.06 (BrukerAXS, 1997-99)'
_computing_publication_material  'SHELXL-93, XCIF V5.05 (BrukerAXS, 1997-99)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method
;
\w-scan, frame range 0.3 deg, hemisphere
;
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28877
_diffrn_reflns_theta_max         31.76
_diffrn_reflns_theta_min         0.79
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment
;
Riding model wit Uiso=1.2Uiso/eq of an adjacent atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         16458
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_obs          0.0399
_refine_ls_shift/esd_max         0.109
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+1.4134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1053
_refine_ls_wR_factor_obs         0.0960
_reflns_number_observed          12953
_reflns_number_total             16475
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja049856krom20040109_111815.cif
_cod_data_source_block           milmsx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+1.4134P] 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^)+(0.0512P)^2^+1.4134P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4112435