#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:53:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178922 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/51/4115119.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4115119
loop_
_publ_author_name
'Daniel B. Werz'
'Rolf Gleiter'
'Frank Rominger'
_publ_contact_author_address
;
        Organisch-Chemisches Institut
        Universität Heidelberg
        Im Neuenheimer Feld 270
        D-69120 Heidelberg
        Germany
;
_publ_contact_author_email       rolf.gleiter@urz.uni-heidelberg.de
_publ_contact_author_fax         '049 6221 54- 4205'
_publ_contact_author_name        'Gleiter, Rolf'
_publ_contact_author_phone       '049 6221 54- 8400'
_publ_section_title
;
 Nanotube Formation Favored by Chalcogen-Chalcogen Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10638
_journal_page_last               10639
_journal_paper_doi               10.1021/ja027146d
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C27 H30 S6'
_chemical_formula_weight         546.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.01340(10)
_cell_length_b                   24.01340(10)
_cell_length_c                   9.86980(10)
_cell_measurement_temperature    200(2)
_cell_volume                     4928.86(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17163
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .12
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0379
_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/[σ²(Fo²)+(0.0511P)²+2.1328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                1754
_reflns_number_total             2517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027146d_s2_3.cif
_cod_data_source_block           dwe53_(in_paper_2*hexane)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4115119
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S1 S 0.72297(2) 0.73897(2) 0.07029(5) 0.04689(17) Uani 1 1 d .
S2 S 0.97375(3) 0.76119(3) 0.49134(5) 0.05636(19) Uani 1 1 d .
C1 C 0.76363(10) 0.82139(10) 0.0069(2) 0.0513(5) Uani 1 1 d .
H1A H 0.7964 0.8259 -0.0599 0.062 Uiso 1 1 calc R
H1B H 0.7317 0.8284 -0.0421 0.062 Uiso 1 1 calc R
C3 C 0.78113(9) 0.73940(9) 0.16503(18) 0.0404(4) Uani 1 1 d .
C4 C 0.82301(9) 0.74171(9) 0.23554(18) 0.0397(4) Uani 1 1 d .
C5 C 0.87109(9) 0.74578(9) 0.31680(19) 0.0414(4) Uani 1 1 d .
C6 C 0.91467(10) 0.75186(9) 0.3866(2) 0.0447(5) Uani 1 1 d .
C8 C 1.03923(9) 0.78440(10) 0.3711(2) 0.0507(5) Uani 1 1 d .
H8A H 1.0765 0.7869 0.4194 0.061 Uiso 1 1 calc R
H8B H 1.0255 0.7504 0.3013 0.061 Uiso 1 1 calc R
C9 C 1.06022(9) 0.84748(9) 0.30196(19) 0.0422(5) Uani 1 1 d .
H9A H 1.0753 0.8818 0.3713 0.051 Uiso 1 1 calc R
H9B H 1.0228 0.8455 0.2554 0.051 Uiso 1 1 calc R
C10 C 1.11416(9) 0.86512(9) 0.19830(19) 0.0449(5) Uani 1 1 d .
H10A H 1.1543 0.8753 0.2467 0.054 Uiso 1 1 calc R
H10B H 1.1026 0.8277 0.1389 0.054 Uiso 1 1 calc R
C11 C 1.12597(10) 0.92221(9) 0.1119(2) 0.0487(5) Uani 1 1 d .
H11A H 1.0855 0.9117 0.0649 0.058 Uiso 1 1 calc R
H11B H 1.1372 0.9593 0.1723 0.058 Uiso 1 1 calc R
C21 C 1.0000 1.0000 0.064(5) 0.59(3) Uiso 1 3 d S
C22 C 0.973(2) 0.943(3) 0.198(5) 0.30(3) Uiso 0.23(2) 1 d P
C23 C 1.0000 1.0000 0.312(9) 0.504(19) Uiso 1 3 d S
C24 C 0.9586(8) 0.9393(9) 0.4268(16) 0.339(10) Uiso 0.80(2) 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C3 S1 C1 101.08(10) . .
C6 S2 C8 100.52(10) . .
C11 C1 S1 116.31(14) 3_675 .
C4 C3 S1 177.50(17) . .
C3 C4 C5 178.6(2) . .
C6 C5 C4 177.4(2) . .
C5 C6 S2 176.93(18) . .
C9 C8 S2 114.09(14) . .
C8 C9 C10 113.14(16) . .
C11 C10 C9 112.03(16) . .
C1 C11 C10 114.90(17) 2_765 .
C21 C21 C22 138(2) 10_775 3_675
C21 C21 C22 138(2) 10_775 .
C22 C21 C22 70(4) 3_675 .
C21 C21 C22 138(2) 10_775 2_765
C22 C21 C22 70(4) 3_675 2_765
C22 C21 C22 70(4) . 2_765
C23 C22 C21 92(5) . .
C22 C23 C22 78(4) 3_675 .
C22 C23 C22 78(4) 3_675 2_765
C22 C23 C22 78(4) . 2_765
C22 C23 C24 146.0(17) 3_675 2_765
C22 C23 C24 127.6(17) . 2_765
C22 C23 C24 85.7(16) 2_765 2_765
C22 C23 C24 127.6(17) 3_675 .
C22 C23 C24 85.7(16) . .
C22 C23 C24 146.0(17) 2_765 .
C24 C23 C24 81(3) 2_765 .
C22 C23 C24 85.7(16) 3_675 3_675
C22 C23 C24 146.0(17) . 3_675
C22 C23 C24 127.6(17) 2_765 3_675
C24 C23 C24 81(3) 2_765 3_675
C24 C23 C24 81(3) . 3_675
C23 C24 C24 104(2) . 11_566
C23 C24 C24 104(2) . 12_656
C24 C24 C24 70.4(14) 11_566 12_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 C3 1.676(2) .
S1 C1 1.825(2) .
S2 C6 1.677(2) .
S2 C8 1.821(2) .
C1 C11 1.515(3) 3_675
C3 C4 1.201(2) .
C4 C5 1.369(3) .
C5 C6 1.200(3) .
C8 C9 1.500(3) .
C9 C10 1.535(3) .
C10 C11 1.516(3) .
C11 C1 1.515(3) 2_765
C21 C21 1.26(9) 10_775
C21 C22 1.77(4) 3_675
C21 C22 1.77(4) .
C21 C22 1.77(4) 2_765
C22 C23 1.63(4) .
C23 C22 1.63(4) 3_675
C23 C22 1.63(4) 2_765
C23 C24 1.72(4) 2_765
C23 C24 1.72(4) .
C23 C24 1.72(4) 3_675
C24 C24 1.94(2) 11_566
C24 C24 1.94(2) 12_656
