Bis-corannulenoanthracene: An Angularly Fused Pentacene as a Precursor for Barrelene-Tethered Receptors for Fullerenes.
Kumarasinghe, K G Upul R; Fronczek, Frank R.; Valle, Henry U.; Sygula, Andrzej; Organic letters 18 (2016) 3054–3057; doi:10.1021/acs.orglett.6b01049

data_1543785
_publ_section_title
;
 Bis-corannulenoanthracene: An Angularly Fused Pentacene as a Precursor
 for Barrelene-Tethered Receptors for Fullerenes.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3054
_journal_page_last               3057
_journal_paper_doi               10.1021/acs.orglett.6b01049
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C50 H22 O2'
_chemical_formula_sum            'C50 H22 O2'
_chemical_formula_weight         654.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.193(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0215(5)
_cell_length_b                   13.1109(6)
_cell_length_c                   15.1972(7)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      72.309
_cell_measurement_theta_min      4.595
_cell_volume                     2047.50(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35868
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         72.302
_diffrn_reflns_theta_min         4.595
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.9197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0545 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.9219.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       Thin-Plate
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The 277 electrons removed by SQUEEZE correspond to approximately
2.8 molecules of disordered solvent, assumed to be toluene, 
per molecule of 9b.
;
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.1111
_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^)+(0.1439P)^2^+8.2579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2901
_refine_ls_wR_factor_ref         0.2936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3704
_reflns_number_total             3994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01049_si_002.cif
_cod_data_source_block           msu0010d8
_cod_database_code               1543785
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9923(9) 0.0077(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19),
 C20(H20), C25(H25)
;
_shelx_res_checksum              87073
_shelx_hkl_checksum              76170
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'