Fluorenyl Based Macrocyclic Polyradicaloids.
Lu, Xuefeng; Lee, Sangsu; Hong, Yongseok; Phan, Hoa; Gopalakrishna, Tullimilli Y.; Herng, Tun Seng; Tanaka, Takayuki; Sandoval-Salinas, María Eugenia; Zeng, Wangdong; Ding, Jun; Casanova, David; Osuka, Atsuhiro; Kim, Dongho; Wu, Jishan; Journal of the American Chemical Society 139 (2017) 13173–13183; doi:10.1021/jacs.7b07335

data_4131598
_publ_section_title
;
 Fluorenyl Based Macrocyclic Polyradicaloids.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13173
_journal_page_last               13183
_journal_paper_doi               10.1021/jacs.7b07335
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C41 H35, (C2 N)'
_chemical_formula_sum            'C44 H35 N1.5'
_chemical_formula_weight         584.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   21.096(6)
_cell_length_b                   36.965(10)
_cell_length_c                   44.576(13)
_cell_measurement_reflns_used    3053
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      31.3
_cell_volume                     34761(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            99479
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        61.994
_diffrn_reflns_theta_max         61.994
_diffrn_reflns_theta_min         7.012
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.894
_exptl_crystal_description       prism
_exptl_crystal_F_000             9904
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1837P)^2^+35.5883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.2760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4542
_reflns_number_total             6711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07335_si_002.cif
_cod_data_source_block           160203ta
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C44 H35 N1.50'
_cod_database_code               4131598
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              56880
_shelx_hkl_checksum              8303