"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_4111454
_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, 2(C12 H24 K1 O6)'
_chemical_formula_sum            'C30 H52 K2 N2 O16'
_chemical_formula_weight         774.94
_chemical_name_systematic
; 
 Bis(18-crown-6 potassium) dinitrobenzene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.938(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.411(3)
_cell_length_b                   8.3205(12)
_cell_length_c                   22.718(4)
_cell_measurement_reflns_used    73
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      19.26
_cell_measurement_theta_min      2.62
_cell_volume                     3744.6(10)
_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 0.950
_diffrn_measured_fraction_theta_max 0.912
_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    0.0885
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8459
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.006
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         8441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.9770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1513
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                5576
_reflns_number_total             8459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja043998xsi20041001_031038.cif
_cod_data_source_block           mil-zsx
_cod_database_code               4111454