π-Extended Pyrene-Fused Double [7]Carbohelicene as a Chiral Polycyclic Aromatic Hydrocarbon.
Hu, Yunbin; Paternò, Giuseppe M; Wang, Xiao-Ye; Wang, Xin-Chang; Guizzardi, Michele; Chen, Qiang; Schollmeyer, Dieter; Cao, Xiao-Yu; Cerullo, Giulio; Scotognella, Francesco; Müllen, Klaus; Narita, Akimitsu; Journal of the American Chemical Society 141 (2019) 12797–12803; doi:10.1021/jacs.9b05610

data_4127754
_publ_section_title
;
 \p-Extended Pyrene-Fused Double [7]Carbohelicene as a Chiral Polycyclic
 Aromatic Hydrocarbon.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12797
_journal_page_last               12803
_journal_paper_doi               10.1021/jacs.9b05610
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C90 H54, C S2'
_chemical_formula_sum            'C91 H54 S2'
_chemical_formula_weight         1211.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                94.076(3)
_cell_angle_beta                 92.133(3)
_cell_angle_gamma                97.566(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8872(3)
_cell_length_b                   15.4283(6)
_cell_length_c                   24.3545(10)
_cell_measurement_reflns_used    17838
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.22
_cell_volume                     2927.1(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    SHELXT-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 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      ' 222 frames, detector distance = 70 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27526
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.318
_diffrn_reflns_theta_min         2.063
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         14493
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0887
_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^)+(0.0805P)^2^+6.9117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9129
_reflns_number_total             14493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05610_si_002.cif
_cod_data_source_block           2
_cod_database_code               4127754
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              33591
_shelx_hkl_checksum              78072