Preparation and Structure of a Tubular Addition Polymer: A True Synthetic Nanotube
Te-Jung Hsu; Frank W. Fowler; Joseph W. Lauher; Journal of the American Chemical Society 134 (2012) 142–145; doi:10.1021/ja209792f

data_4117251
_publ_contact_author_address
;Joseph W. Lauher
Department of Chemistry
State University of New York
Stony Brook, NY 11720
;
_publ_contact_author_email       joseph.lauher@stonybrook.edu
_publ_contact_author_name        'Joseph W. Lauher'
_publ_contact_author_phone       631-632-7925
_publ_section_title
;
 Preparation and Structure of a Tubular Addition Polymer: A True Synthetic
 Nanotube
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              142
_journal_page_last               145
_journal_paper_doi               10.1021/ja209792f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C36 H24 O4'
_chemical_formula_sum            'C36 H24 O4'
_chemical_formula_weight         520.55
_chemical_name_common            Monomer
_chemical_name_systematic
;5,12,24,31-Tetraoxa-tricyclo[33.3.1.16.20]tetracontra-1(39),16,18, 
20(40),35,37-hexaene-2,7,9,14,21,26,28,33-octayne
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_cell_angle_alpha                85.317(4)
_cell_angle_beta                 86.918(4)
_cell_angle_gamma                80.569(5)
_cell_formula_units_Z            1.00000
_cell_length_a                   4.8389(3)
_cell_length_b                   9.1349(5)
_cell_length_c                   15.9935(8)
_cell_measurement_reflns_used    3661
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.1135
_cell_measurement_theta_min      4.9120
_cell_volume                     694.49(7)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_computing_data_collection
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_chemical_name_systematic     'Monomer'
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) 
(compiled Jan 27 2009,14:17:37) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
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_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4962
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_diffrn_measurement_details
; 
  1 omega -109.00  -24.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543  -37.0000  300.0000 85 
  
  2 omega -109.00   -9.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543  -37.0000   30.0000 100 
  
  3 omega -119.00  -48.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543  179.0000   60.0000 71 
  
  4 omega  -76.00  -45.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543  179.0000  150.0000 31 
  
  5 omega   21.00   77.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -       32.9543   37.0000  240.0000 56 
  
  6 omega   57.00  123.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -       32.9543  179.0000   30.0000 66 
  
  7 omega   82.00  112.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -       32.9543  179.0000  150.0000 30 
  
  8 omega -139.00  -99.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      -68.5000  -77.0000  330.0000 40 
  
  9 omega  -82.00  -53.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      -68.5000  -77.0000  330.0000 29 
  
 10 omega -131.00 -103.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      -68.5000  -45.0000   30.0000 28 
  
 11 omega  -76.00  -47.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      -68.5000  -45.0000   30.0000 29 
  
 12 omega   41.00   72.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -45.0000  120.0000 31 
  
 13 omega  122.00  178.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000   15.0000  270.0000 56 
  
 14 omega   88.00  136.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -45.0000  120.0000 48 
  
 15 omega  110.00  143.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -45.0000  180.0000 33 
  
 16 omega   59.00   89.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -45.0000  180.0000 30 
  
 17 omega   91.00  178.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000   45.0000  300.0000 87 
  
 18 omega   36.00  149.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -77.0000  150.0000 113 
  
 19 omega   87.00  178.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000   45.0000  210.0000 91 
  
 20 omega  100.00  163.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  111.0000  150.0000 63 
  
 21 omega  123.00  150.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  179.0000  240.0000 27 
  
 22 omega  132.00  178.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  111.0000  240.0000 46 
  
 23 omega   47.00  143.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -45.0000    0.0000 96 
  
 24 omega   56.00  142.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  -77.0000  300.0000 86 
  
 25 omega   86.00  145.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  179.0000   60.0000 59 
  
 26 omega   85.00  123.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000 -128.0000  140.0000 38 
  
 27 omega  100.00  167.00   1.0000   14.9900 
omega____ theta____ kappa____ phi______ frames 
    -      115.0000  111.0000  120.0000 67 
  
 28 omega -112.00  -48.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543  -77.0000   30.0000 64 
  
 29 omega -112.00    1.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543  -77.0000  150.0000 113 
  
 30 omega -122.00   56.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -      -32.9543    0.0000  120.0000 178 
  
 31 omega   56.00  123.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -       32.9543  179.0000  180.0000 67 
  
 32 omega   -1.00  112.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -       32.9543   77.0000  300.0000 113 
  
 33 omega   29.00  100.00   1.0000    5.0000 
omega____ theta____ kappa____ phi______ frames 
    -       32.9543 -142.0000  329.0000 71 
  
;
_diffrn_measurement_device_type  'Gon Xcalibur, detector: Atlas (Gemini Cu)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0277050783
_diffrn_orient_matrix_UB_12      -0.0201655838
_diffrn_orient_matrix_UB_13      0.0967615456
_diffrn_orient_matrix_UB_21      -0.0611353964
_diffrn_orient_matrix_UB_22      0.1705559775
_diffrn_orient_matrix_UB_23      0.0041560434
_diffrn_orient_matrix_UB_31      -0.3172734648
_diffrn_orient_matrix_UB_32      -0.0029874599
_diffrn_orient_matrix_UB_33      -0.0050761908
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7311
_diffrn_reflns_theta_full        77.1
_diffrn_reflns_theta_max         77.1135
_diffrn_reflns_theta_min         4.9120
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       needle
_exptl_crystal_F_000             272
_exptl_crystal_recrystallization_method '1:1 dichloromethane hexane'
_exptl_crystal_size_max          1.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+0.1082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                2146
_reflns_number_total             2871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja209792f_si_003.cif
_cod_data_source_block           monomer_triclinic
_cod_database_code               4117251