Synthesis of sexithiophene-bridged cage compound: a new class of three-dimensionally expanded oligothiophenes.
Adachi, Kazuhiko; Hirao, Yasukazu; Matsumoto, Kouzou; Kubo, Takashi; Kurata, Hiroyuki; Organic letters 16 (2014) 5870–5873; doi:10.1021/ol5027816

data_1518156
_publ_section_title
;
 Synthesis of sexithiophene-bridged cage compound: a new class of
 three-dimensionally expanded oligothiophenes.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5870
_journal_page_last               5873
_journal_paper_doi               10.1021/ol5027816
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C154 H192 S18'
_chemical_formula_weight         2620.14
_chemical_name_common
;
Beta-ethano-linked tris(sexithienyl) cage 
;
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                77.272(3)
_cell_angle_beta                 88.520(3)
_cell_angle_gamma                86.926(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3862(17)
_cell_length_b                   23.118(3)
_cell_length_c                   26.137(3)
_cell_measurement_reflns_used    22115
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      55.07
_cell_measurement_theta_min      6.02
_cell_volume                     7877.5(17)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
;
Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku/Varimax Rapid/007HF'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1385
_diffrn_reflns_av_unetI/netI     0.3540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            79157
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.011
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.9971
_exptl_absorpt_correction_T_min  0.9177
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
Cage6T comprises a large pore voids in the structure filling
with the disordered ethanol solvent molecules. Attempts to model 
disordered solvent molecules were unsuccessful. 
We therefore employed PLATON/SQUEEZE to make the solvent-free 
diffraction intensities. SQUEEZE estimated a potential 
solvent volume of 1014.9 \%A^3^, 12.9 % of the total 
unit-cell volume.168.2 electrons per unit cell worth 
of scattering were located in the void. 
The reported structure is based on the PLATON/SQUEEZE corrected data.

Ref: Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1488
_refine_ls_number_reflns         35982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.1950
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10574
_reflns_number_total             35982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5027816_si_004.cif
_cod_data_source_block           Cage6T
_cod_depositor_comments
'Adding full bibliography for 1518156--1518157.cif.'
_cod_original_cell_volume        7877.3(17)
_cod_database_code               1518156
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014-3
_shelx_res_checksum              83240
_shelx_hkl_checksum              36088