Toward Tetraradicaloid: The Effect of Fusion Mode on Radical Character and Chemical Reactivity.
Hu, Pan; Lee, Sangsu; Herng, Tun Seng; Aratani, Naoki; Gonçalves, Théo P; Qi, Qingbiao; Shi, Xueliang; Yamada, Hiroko; Huang, Kuo-Wei; Ding, Jun; Kim, Dongho; Wu, Jishan; Journal of the American Chemical Society 138 (2016) 1065–1077; doi:10.1021/jacs.5b12532

data_4129985
_publ_section_title
;
 Toward Tetraradicaloid: The Effect of Fusion Mode on Radical Character
 and Chemical Reactivity.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1065
_journal_page_last               1077
_journal_paper_doi               10.1021/jacs.5b12532
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C55 H54 O'
_chemical_formula_sum            'C55 H54 O'
_chemical_formula_weight         730.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 101.364(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9865(5)
_cell_length_b                   7.9786(3)
_cell_length_c                   34.6321(12)
_cell_measurement_reflns_used    1092
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.544
_cell_measurement_theta_min      2.603
_cell_volume                     4059.8(2)
_computing_cell_refinement
'SHELXTL, Acta Cryst., Sect. A 2008, 64, 112-122.'
_computing_data_collection       'APEX3 v2015.5.2'
_computing_data_reduction        'Saint, APEX v2014.11.0.'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'APEX3 v2015.5.2'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT, Acta Cryst., Sect. A 2015, A71, 3-8.'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            35607
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.544
_diffrn_reflns_theta_min         2.603
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+2.2813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6325
_reflns_number_total             8160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12532_si_007.cif
_cod_data_source_block           PF-M
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4129985
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2014/6
_shelx_res_checksum              73973
_shelx_hkl_checksum              99389