Helically Locked Tethered Twistacenes.
Bedi, Anjan; Shimon, Linda J. W.; Gidron, Ori; Journal of the American Chemical Society 140 (2018) 8086–8090; doi:10.1021/jacs.8b04447

data_4132504
_publ_section_title
;
 Helically Locked Tethered Twistacenes.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8086
_journal_page_last               8090
_journal_paper_doi               10.1021/jacs.8b04447
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C47 H30 F12 O2'
_chemical_formula_sum            'C47 H30 F12 O2'
_chemical_formula_weight         854.71
_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-2016/4
_cell_angle_alpha                73.1970(10)
_cell_angle_beta                 88.8510(10)
_cell_angle_gamma                78.1490(10)
_cell_formula_units_Z            4
_cell_length_a                   15.2965(2)
_cell_length_b                   15.9067(3)
_cell_length_c                   16.5026(3)
_cell_measurement_reflns_used    20938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.1390
_cell_measurement_theta_min      4.2210
_cell_volume                     3758.68(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51273
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.071
_diffrn_reflns_theta_min         4.156
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1155
_refine_ls_number_reflns         14216
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.4395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11479
_reflns_number_total             14216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04447_si_004.cif
_cod_data_source_block           C5tether
_cod_database_code               4132504
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.985
_oxdiff_exptl_absorpt_empirical_full_min 0.827
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              79730
_shelx_hkl_checksum              23243