Tris(thianthrene)(2+) bis(dodecamethylcarba-<i>closo</i>-dodecaborate) dichloromethane tetrasolvate: a crossed triple-decker π-trimer dication
Rosokha, Sergiy V.; Lu, Jianjiang; Rosokha, Tetyana Y.; Kochi, Jay K.; Acta Crystallographica Section C 63 (2007) o347–o349; doi:10.1107/S0108270107018136

data_2015991
_publ_section_title
;
 Tris(thianthrene)(2+) bis(dodecamethylcarba-<i>closo</i>-dodecaborate)
 dichloromethane tetrasolvate: a crossed triple-decker \p-trimer
 dication
;
_journal_coeditor_code           GG3084
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o347
_journal_page_last               o349
_journal_paper_doi               10.1107/S0108270107018136
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'3C12 H8 S2 0.67+ , 2C13 H36 B11 - , 4C H2 Cl2'
_chemical_formula_moiety         '3C12 H8 S2 2+ , 2C13 H36 B11 - , 4C H2 Cl2'
_chemical_formula_sum            'C66 H104 B22 Cl8 S6'
_chemical_formula_weight         1611.27
_chemical_name_systematic
;
Tris(thianthrenediium) bis(dodecamethylcarba-closo-dodecaborate)
dichloromethane tetrasolvate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.013(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.585(8)
_cell_length_b                   14.573(4)
_cell_length_c                   16.523(5)
_cell_measurement_reflns_used    578
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      1.52
_cell_volume                     4204(2)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT and SADABS (Bruker, 2003)'
_computing_molecular_graphics    'XP (Bruker, 1999)'
_computing_publication_material  'SHELXTL and XCIF (Bruker, 1999)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'Bruker SMART APEX'
_diffrn_measurement_method       'full-sphere \w'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29585
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.454
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0937P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                5156
_reflns_number_total             6546
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3084.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2015991
_cod_database_fobs_code          2015991