Synthesis of Tetrachalcogenide-Substituted Phenalenyl Derivatives: Preparation and Solid-State Characterization of Bis(3,4,6,7-tetrathioalkyl-phenalenyl)boron Radicals
Pradip Bag; Sushanta K. Pal; Mikhail E. Itkis; Arindam Sarkar; Fook S. Tham; Bruno Donnadieu; Robert C. Haddon; Journal of the American Chemical Society 135 (2013) 12936–12939; doi:10.1021/ja405814f

data_4120713
_publ_section_title
;
 Synthesis of Tetrachalcogenide-Substituted Phenalenyl Derivatives:
 Preparation and Solid-State Characterization of
 Bis(3,4,6,7-tetrathioalkyl-phenalenyl)boron Radicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12936
_journal_page_last               12939
_journal_paper_doi               10.1021/ja405814f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C34 H30 B Cl0 O4 S8'
_chemical_formula_weight         769.87
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                106.125(8)
_cell_angle_beta                 102.415(8)
_cell_angle_gamma                94.755(9)
_cell_formula_units_Z            2
_cell_length_a                   8.296(6)
_cell_length_b                   14.369(10)
_cell_length_c                   15.486(11)
_cell_measurement_reflns_used    1704
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.94
_cell_measurement_theta_min      2.35
_cell_volume                     1712(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.1372
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10198
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.9460
_exptl_absorpt_correction_T_min  0.8321
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       'needle frag'
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0050(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3027
_reflns_number_total             5320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405814f_si_005.cif
_cod_data_source_block           shelxl
_cod_database_code               4120713