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_4130903
_publ_section_title
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 A Biradical Balancing Act: Redox Amphoterism in a Diindenoanthracene
 Derivative Results from Quinoidal Acceptor and Aromatic Donor Motifs.
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_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_sum            'C88 H120 K2 O8 Si2'
_chemical_formula_weight         1440.22
_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                66.240(2)
_cell_angle_beta                 84.5840(10)
_cell_angle_gamma                81.803(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1690(4)
_cell_length_b                   15.4719(7)
_cell_length_c                   17.6353(7)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.49
_cell_measurement_theta_min      2.74
_cell_volume                     2264.45(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51467
_diffrn_reflns_theta_full        74.73
_diffrn_reflns_theta_max         74.73
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_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 237 Ang^3^[10.4% of cell volume],and a void electron population of 86 per cell. Considering the synthesis process and solvents employed, 2 THF molecules were assigned per unit cell.
;
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         9027
_refine_ls_number_restraints     1528
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1072P)^2^+0.8659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1927
_refine_ls_wR_factor_ref         0.2048
_reflns_number_gt                6705
_reflns_number_total             9027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b07882_si_004.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               4130903
_platon_squeeze_void_probe_radius 1.20