"Separated" versus "Contact" Ion-Pair Structures in Solution from Their Crystalline States: Dynamic Effects on Dinitrobenzenide as a Mixed-Valence Anion
Jian-Ming Lü; Sergiy V. Rosokha; Sergey V. Lindeman; Ivan S. Neretin; Jay K. Kochi; Journal of the American Chemical Society 127 (2005) 1797–1809; doi:10.1021/ja043998x

data_4111452
_publ_section_title
;
 "Separated" versus "Contact" Ion-Pair Structures in Solution from Their
 Crystalline States: Dynamic Effects on Dinitrobenzenide as a
 Mixed-Valence Anion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1797
_journal_page_last               1809
_journal_paper_doi               10.1021/ja043998x
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C6 H4 N2 O4, C28 H40 K O10'
_chemical_formula_sum            'C34 H44 K N2 O14'
_chemical_formula_weight         743.81
_chemical_name_common            (Benzo-15-crown)2K*DNB
_chemical_name_systematic
; 
 Bis(benzo-15-crown-5)potassium dinitrobenzene
;
_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                111.6820(10)
_cell_angle_beta                 91.8330(10)
_cell_angle_gamma                110.0570(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1156(6)
_cell_length_b                   12.8981(7)
_cell_length_c                   12.9427(7)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      20.14
_cell_measurement_theta_min      3.73
_cell_volume                     1736.03(16)
_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  'SHELXTL v. 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL v. 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.904
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10834
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.93
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       needle
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.038
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          -0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.3482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1240
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                8786
_reflns_number_total             10834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043998xsi20041001_031008.cif
_cod_data_source_block           lu-csx
_cod_original_cell_volume        1736.0(2)
_cod_database_code               4111452