Spin-coupling in dimers of 2,3-dicyano-5,6-dichlorosemiquinone radical anions in the crystalline state
Molčanov, Krešimir; Babić, Darko; Kojić-Prodić, Biserka; Stare, Jernej; Maltar-Strmečki, Nadica; Androš, Lidija; Acta Crystallographica Section B 70 (2014) 181–190; doi:10.1107/S2052520613027170

data_2105743
_publ_section_title
;
 Spin-coupling in dimers of 2,3-dicyano-5,6-dichlorosemiquinone radical
 anions in the crystalline state
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              181
_journal_page_last               190
_journal_paper_doi               10.1107/S2052520613027170
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C8 H4 Cl2 N2 O4 Rb'
_chemical_formula_sum            'C8 H4 Cl2 N2 O4 Rb'
_chemical_formula_weight         348.50
_chemical_name_common            RbDDQx2H2O
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4217(2)
_cell_length_b                   18.0295(6)
_cell_length_c                   9.5740(2)
_cell_measurement_reflns_used    3496
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      75.94
_cell_measurement_theta_min      4.61
_cell_volume                     1108.48(6)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Agilent, 2012)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012) & Mercury (Macrae et al., 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) & PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5137
_diffrn_reflns_theta_full        76.13
_diffrn_reflns_theta_max         76.13
_diffrn_reflns_theta_min         4.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.668
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro (Agilent, 2012)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.715
_refine_ls_abs_structure_details
;
 Refined as an inversion twin (TWIN + BASF)
 The refined BASF value indicates that this model represents the *minor*
 component. However, this model is retained since it has the same handedness
 as all other structures in this paper (it can be overlaid directly with the
 other structures and the DFT-optimized structures.
;
_refine_ls_abs_structure_Flack   0.64(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.3657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                2103
_reflns_number_total             2194
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi5007sup1.cif
_cod_data_source_block           RbDDQx2H2O_120K
_cod_original_sg_symbol_Hall     ' P 2 2ab'
_cod_database_code               2105743