A Biradical Balancing Act: Redox Amphoterism in a Diindenoanthracene Derivative Results from Quinoidal Acceptor and Aromatic Donor Motifs.
Rudebusch, Gabriel E.; Espejo, Guzmán L; Zafra, José L; Peña-Alvarez, Miriam; Spisak, Sarah N.; Fukuda, Kotaro; Wei, Zheng; Nakano, Masayoshi; Petrukhina, Marina A.; Casado, Juan; Haley, Michael M.; Journal of the American Chemical Society 138 (2016) 12648–12654; doi:10.1021/jacs.6b07882

data_4130904
_publ_section_title
;
 A Biradical Balancing Act: Redox Amphoterism in a Diindenoanthracene
 Derivative Results from Quinoidal Acceptor and Aromatic Donor Motifs.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12648
_journal_page_last               12654
_journal_paper_doi               10.1021/jacs.6b07882
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C68 H76 Si2, C20 H40 K O8'
_chemical_formula_sum            'C88 H116 K O8 Si2'
_chemical_formula_weight         1397.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                78.478(2)
_cell_angle_beta                 82.510(2)
_cell_angle_gamma                72.2570(10)
_cell_formula_units_Z            1
_cell_length_a                   11.5995(3)
_cell_length_b                   12.1738(3)
_cell_length_c                   17.0652(4)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.51
_cell_measurement_theta_min      2.65
_cell_volume                     2242.66(10)
_computing_cell_refinement       'SAINT V.8.34 (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 v.2014.11-0 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V.8.34 (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_source         'INCOATEC ImuS micro-focus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38215
_diffrn_reflns_theta_full        73.77
_diffrn_reflns_theta_max         73.77
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.149
_exptl_absorpt_correction_T_max  0.8745
_exptl_absorpt_correction_T_min  0.8557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             755
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The solvent molecules in the voids are highly disordered which could not be modelled as discrete atomic sites.

The SQUEEZE routine of the program PLATON was used in order 
to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure was obtained.

The SQUEEZE routine suggested that a total potential solvent area volume of 300 Ang^3^[10.6% of cell volume],and a void electron population of 80 per cell. Considering the synthesis process and solvents employed, 2 THF molecules were assigned per unit cell.
;
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         8603
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0929P)^2^+0.2278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                6086
_reflns_number_total             8603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b07882_si_002.cif
_cod_data_source_block           sad_a_sqd
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4130904
_platon_squeeze_void_probe_radius 1.20