Synthesis, Structure, and Chiroptical Properties of a Double [7]Heterohelicene.
Wang, Xiao-Ye; Wang, Xin-Chang; Narita, Akimitsu; Wagner, Manfred; Cao, Xiao-Yu; Feng, Xinliang; Müllen, Klaus; Journal of the American Chemical Society 138 (2016) 12783–12786; doi:10.1021/jacs.6b08664

data_4131009
_publ_section_title
;
 Synthesis, Structure, and Chiroptical Properties of a Double
 [7]Heterohelicene.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12783
_journal_page_last               12786
_journal_paper_doi               10.1021/jacs.6b08664
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C50 H37 Br O4'
_chemical_formula_sum            'C50 H37 Br O4'
_chemical_formula_weight         781.70
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   32.9726(10)
_cell_length_b                   32.9726(10)
_cell_length_c                   10.6792(3)
_cell_measurement_reflns_used    15691
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      2.14
_cell_volume                     10054.9(5)
_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
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 210 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  0.0452
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.505
_diffrn_reflns_theta_min         2.140
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.9343
_exptl_absorpt_correction_T_min  0.6286
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             3636
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
TITL w160      R -3 :h      R = 0.10
CELL   32.9610   32.9610   10.6960     90.00     90.00    120.00
SPGR R-3
Q101 0.085 0.836 0.146 !       1.04 eA-3
Q102 0.015 0.698 0.123 !       0.73 eA-3
Q103 0.377 0.982 0.202 !       0.52 eA-3
;
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0020(4)
_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   1.525
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.532
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0932
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3353
_reflns_number_total             5631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b08664_si_002.cif
_cod_data_source_block           w160
_cod_original_cell_volume        10054.8(7)
_cod_database_code               4131009
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              22760
_shelx_hkl_checksum              5403
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              46434