Open-Shell Nonbenzenoid Nanographenes Containing Two Pairs of Pentagonal and Heptagonal Rings.
Liu, Junzhi; Mishra, Shantanu; Pignedoli, Carlo A.; Passerone, Daniele; Urgel, José I; Fabrizio, Alberto; Lohr, Thorsten G.; Ma, Ji; Komber, Hartmut; Baumgarten, Martin; Corminboeuf, Clémence; Berger, Reinhard; Ruffieux, Pascal; Müllen, Klaus; Fasel, Roman; Feng, Xinliang; Journal of the American Chemical Society 141 (2019) 12011–12020; doi:10.1021/jacs.9b04718

data_4128592
_publ_section_title
;
 Open-Shell Nonbenzenoid Nanographenes Containing Two Pairs of Pentagonal
 and Heptagonal Rings.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12011
_journal_page_last               12020
_journal_paper_doi               10.1021/jacs.9b04718
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C56 H42 O2, C H2 Cl2'
_chemical_formula_sum            'C57 H44 Cl2 O2'
_chemical_formula_weight         831.82
_chemical_name_systematic
;
5,14-Bis(4-(tert-butyl)phenyl)dibenzo[a,m]rubicene-9,18-dicarbaldehyde
;
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                95.063(5)
_cell_angle_beta                 97.091(5)
_cell_angle_gamma                91.364(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1700(7)
_cell_length_b                   12.9671(9)
_cell_length_c                   15.7532(10)
_cell_measurement_reflns_used    22424
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.58
_cell_measurement_theta_min      2.84
_cell_volume                     2254.1(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details      ' 1178 frames, detector distance = 40 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29043
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.043
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'Incoatec microSource Cu'
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.9501
_exptl_absorpt_correction_T_min  0.8356
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0038(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7808
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0669
_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^)+(0.1226P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4081
_reflns_number_total             7808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04718_si_001.cif
_cod_data_source_block           15a
_cod_database_code               4128592
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              8525
_shelx_hkl_checksum              94430