Stable 3,6-Linked Fluorenyl Radical Oligomers with Intramolecular Antiferromagnetic Coupling and Polyradical Characters.
Lu, Xuefeng; Lee, Sangsu; Kim, Jun Oh; Gopalakrishna, Tullimilli Y.; Phan, Hoa; Herng, Tun Seng; Lim, Zhenglong; Zeng, Zebing; Ding, Jun; Kim, Dongho; Wu, Jishan; Journal of the American Chemical Society 138 (2016) 13048–13058; doi:10.1021/jacs.6b08138

data_4130963
_publ_section_title
;
 Stable 3,6-Linked Fluorenyl Radical Oligomers with Intramolecular
 Antiferromagnetic Coupling and Polyradical Characters.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13048
_journal_page_last               13058
_journal_paper_doi               10.1021/jacs.6b08138
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C91.50 H91.50 N0'
_chemical_formula_sum            'C91.5 H91.5 N0'
_chemical_formula_weight         1191.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 97.306(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.8736(15)
_cell_length_b                   19.1675(6)
_cell_length_c                   16.5421(5)
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.229
_cell_measurement_theta_min      2.486
_cell_volume                     15056.1(8)
_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 0.923
_diffrn_measured_fraction_theta_max 0.976
_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  0.0636
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42041
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.229
_diffrn_reflns_theta_min         2.486
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             5124
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.000005(17)
_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   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         12573
_refine_ls_number_restraints     425
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1515P)^2^+48.2120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2720
_refine_ls_wR_factor_ref         0.2901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9297
_reflns_number_total             12573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b08138_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C91.50 H91.50 N0'
_cod_database_code               4130963
_shelx_estimated_absorpt_t_min   0.795
_shelx_estimated_absorpt_t_max   0.939
_shelxl_version_number           2014/6
_shelx_res_checksum              20054
_shelx_hkl_checksum              4694