Fused Dibenzo[a,m]rubicene: A New Bowl-Shaped Subunit of C70 Containing Two Pentagons.
Liu, Junzhi; Osella, Silvio; Ma, Ji; Berger, Reinhard; Beljonne, David; Schollmeyer, Dieter; Feng, Xinliang; Müllen, Klaus; Journal of the American Chemical Society 138 (2016) 8364–8367; doi:10.1021/jacs.6b04426

data_4130550
_publ_section_title
;
 Fused Dibenzo[a,m]rubicene: A New Bowl-Shaped Subunit of C70 Containing
 Two Pentagons.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8364
_journal_page_last               8367
_journal_paper_doi               10.1021/jacs.6b04426
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C54 H40 Cl2'
_chemical_formula_sum            'C54 H40 Cl2'
_chemical_formula_weight         759.76
_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                107.388(4)
_cell_angle_beta                 93.328(5)
_cell_angle_gamma                96.709(4)
_cell_formula_units_Z            4
_cell_length_a                   11.7932(7)
_cell_length_b                   18.2962(10)
_cell_length_c                   20.0268(12)
_cell_measurement_reflns_used    33214
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      66.31
_cell_measurement_theta_min      2.88
_cell_volume                     4075.7(4)
_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
_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 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details      ' 1211 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  0.0668
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44034
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.673
_diffrn_reflns_theta_max         67.673
_diffrn_reflns_theta_min         3.950
_diffrn_source                   'Incoatec microSource Cu'
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.9654
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0034(2)
_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   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         13804
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1252P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5489
_reflns_number_total             13804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04426_si_002.cif
_cod_data_source_block           cl5bist
_cod_database_code               4130550
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              83590
_shelx_hkl_checksum              17118