DIBPillar[n]arenes (n = 5, 6): syntheses, X-ray crystal structures, and complexation with n-octyltriethyl ammonium hexafluorophosphate.
Han, Chengyou; Ma, Fengying; Zhang, Zibin; Xia, Binyuan; Yu, Yihua; Huang, Feihe; Organic letters 12 (2010) 4360–4363; doi:10.1021/ol1018344

data_1503218
_publ_section_title
;
 DIBPillar[n]arenes (n = 5, 6): syntheses, X-ray crystal structures, and
 complexation with n-octyltriethyl ammonium hexafluorophosphate.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              4360
_journal_page_last               4363
_journal_paper_doi               10.1021/ol1018344
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C75 H107 O10, C2 H3 N, C H2 Cl2 '
_chemical_formula_sum            'C78 H110 Cl2 N O10'
_chemical_formula_weight         1292.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   55.9475(11)
_cell_length_b                   44.3294(18)
_cell_length_c                   12.4822(2)
_cell_measurement_reflns_used    9128
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9172
_cell_measurement_theta_min      2.5449
_cell_volume                     30957.3(15)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17885
_diffrn_reflns_theta_full        67.17
_diffrn_reflns_theta_max         67.17
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.53 (release 17-11-2009 CrysAlis171 .NET)
(compiled Nov 17 2009,16:58:22)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11184
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         10172
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1956P)^2^+41.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2438
_refine_ls_wR_factor_ref         0.2582
_reflns_number_gt                8464
_reflns_number_total             10172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol1018344_si_002.cif
_cod_data_source_block           DIBpillar[5]arene
_cod_original_cell_volume        30957.4(15)
_cod_original_sg_symbol_H-M      'F d d 2 '
_cod_database_code               1503218