Rigid π-Extended Triptycenes via a Hexaketone Precursor.
Kohl, Bernd; Rominger, Frank; Mastalerz, Michael; Organic letters 16 (2014) 704–707; doi:10.1021/ol403383y

data_1513494
_publ_section_title
;
 Rigid \p-Extended Triptycenes via a Hexaketone Precursor.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              704
_journal_page_last               707
_journal_paper_doi               10.1021/ol403383y
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C135 H100 Cl13 N6 O6'
_chemical_formula_weight         2363.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0785(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.1444(4)
_cell_length_b                   37.2740(8)
_cell_length_c                   27.7739(5)
_cell_measurement_reflns_used    23110
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      72.6709
_cell_measurement_theta_min      3.0999
_cell_volume                     22866.8(8)
_computing_cell_refinement
; 
'Sun Jan 20 17:46:26 2013' 
;
_computing_data_collection
; 
'Sun Jan 20 17:46:26 2013' 
;
_computing_data_reduction
; 
'Sun Jan 20 17:46:26 2013' 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 10.3385
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            89560
_diffrn_reflns_theta_full        72.82
_diffrn_reflns_theta_max         72.82
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    3.365
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Analytical numeric absorption correction using a multifaceted crystal 
   model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9768
_exptl_crystal_size_max          0.3403
_exptl_crystal_size_mid          0.2587
_exptl_crystal_size_min          0.2053
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.565
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2874
_refine_ls_number_reflns         44202
_refine_ls_number_restraints     11828
_refine_ls_restrained_S_all      1.549
_refine_ls_R_factor_all          0.1785
_refine_ls_R_factor_gt           0.1376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3801
_refine_ls_wR_factor_ref         0.4208
_reflns_number_gt                28048
_reflns_number_total             44202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol403383y_si_002.cif
_cod_data_source_block           bek4
_cod_original_cell_volume        22866.7(8)
_cod_database_code               1513494
_shelxl_version_number           2008/4