#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:32:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180226 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/12/7111261.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111261
loop_
_publ_author_name
'Purse, Byron W.'
'Shivanyuk, Alexander'
'Rebek, Julius'
_publ_section_title
;
 Resorcin[6]arene as a building block for tubular crystalline state
 architectures
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2612
_journal_paper_doi               10.1039/b208189j
_journal_year                    2002
_chemical_formula_sum            'C36 H44 O8 S0.44'
_chemical_formula_weight         618.96
_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            9
_cell_length_a                   28.453(5)
_cell_length_b                   28.453(5)
_cell_length_c                   10.024(3)
_cell_measurement_temperature    293(2)
_cell_volume                     7028(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1108
_diffrn_reflns_av_sigmaI/netI    0.1198
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21034
_diffrn_reflns_theta_full        28.13
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.120
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2980
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.494
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.494
_refine_ls_R_factor_all          0.2173
_refine_ls_R_factor_gt           0.1632
_refine_ls_shift/su_max          0.428
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4352
_refine_ls_wR_factor_ref         0.4641
_reflns_number_gt                2279
_reflns_number_total             3794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208189jsup1.cif
_cod_data_source_block           bpas1
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7111261
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
C6 C 0.1214(2) 0.1203(2) 0.5012(6) 0.0389(14) Uani 1 1 d .
H6 H 0.0997 0.0854 0.5345 0.047 Uiso 1 1 calc .
C1 C 0.1179(3) 0.1616(3) 0.5621(6) 0.0408(15) Uani 1 1 d .
C5 C 0.1549(2) 0.1264(3) 0.3933(7) 0.0411(15) Uani 1 1 d .
C8 C 0.0574(3) 0.1011(3) 0.7513(7) 0.0450(16) Uani 1 1 d .
H8A H 0.0377 0.0703 0.6922 0.054 Uiso 1 1 calc R
H8B H 0.0885 0.0997 0.7857 0.054 Uiso 1 1 calc R
C2 C 0.1549(3) 0.2152(3) 0.5146(7) 0.0415(15) Uani 1 1 d .
C4 C 0.1864(3) 0.1790(3) 0.3439(7) 0.0449(16) Uani 1 1 d .
C3 C 0.1865(3) 0.2217(3) 0.4058(8) 0.0486(17) Uani 1 1 d .
H3 H 0.2089 0.2565 0.3729 0.058 Uiso 1 1 calc .
C9 C 0.0208(4) 0.0968(4) 0.8667(9) 0.063(2) Uani 1 1 d .
H9A H 0.0394 0.1283 0.9225 0.095 Uiso 1 1 calc R
H9B H 0.0117 0.0649 0.9179 0.095 Uiso 1 1 calc R
H9C H -0.0117 0.0946 0.8325 0.095 Uiso 1 1 calc R
C7 C 0.0770(2) 0.1534(3) 0.6723(7) 0.0415(15) Uani 1 1 d .
CZ3 C 0.1024(2) 0.3100(2) 0.1476(7) 0.0380(14) Uani 1 1 d .
HZ3A H 0.0910 0.2883 0.0680 0.057 Uiso 1 1 calc R
HZ3B H 0.1353 0.3434 0.1302 0.057 Uiso 1 1 calc R
HZ3C H 0.0746 0.3177 0.1750 0.057 Uiso 1 1 calc R
CZ4 C 0.0689(4) 0.2746(5) 0.3871(12) 0.091(3) Uani 1 1 d .
HZ4A H 0.0875 0.3055 0.4446 0.136 Uiso 1 1 calc R
HZ4B H 0.0586 0.2421 0.4371 0.136 Uiso 1 1 calc R
HZ4C H 0.0371 0.2734 0.3514 0.136 Uiso 1 1 calc R
O1 O 0.1532(2) 0.25625(18) 0.5800(6) 0.0530(14) Uani 1 1 d .
H1 H 0.1832 0.2837 0.5765 0.080 Uiso 1 1 calc R
O2 O 0.2184(2) 0.1860(2) 0.2340(6) 0.0579(14) Uani 1 1 d .
H2 H 0.2249 0.2139 0.1948 0.087 Uiso 1 1 calc R
S1 S 0.11198(8) 0.27955(7) 0.2561(2) 0.0630(8) Uani 1 1 d .
OZ3 O 0.2291(3) 0.2722(3) 0.1015(8) 0.093(2) Uani 1 1 d .
S2A S 0.22381(17) 0.26764(12) -0.0534(3) 0.0896(14) Uani 0.862(8) 1 d P
S2 S 0.2192(6) 0.3054(6) 0.0027(14) 0.056(5) Uani 0.138(8) 1 d P
OZ5 O 0.0792(4) 0.2097(3) 0.2058(13) 0.141(6) Uani 0.97(3) 1 d P
CT1 C 0.2868(8) 0.3145(6) -0.1213(16) 0.136(6) Uani 1 1 d .
CT2 C 0.1905(8) 0.3056(7) -0.0953(16) 0.134(6) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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_3
C1 C6 C5 125.2(6) .
C6 C1 C2 115.7(6) .
C6 C1 C7 124.3(6) .
C2 C1 C7 119.9(6) .
C6 C5 C4 116.2(6) .
C6 C5 C7 120.8(6) 11_556
C4 C5 C7 122.9(6) 11_556
C9 C8 C7 112.1(6) .
O1 C2 C3 124.8(6) .
O1 C2 C1 115.5(6) .
C3 C2 C1 119.6(6) .
C3 C4 O2 121.9(6) .
C3 C4 C5 120.6(6) .
O2 C4 C5 117.5(6) .
C4 C3 C2 122.3(6) .
C8 C7 C1 113.8(5) .
C8 C7 C5 110.5(5) 12_556
C1 C7 C5 108.0(5) 12_556
CZ3 S1 CZ4 105.6(5) .
CZ3 S1 OZ5 107.0(4) .
CZ4 S1 OZ5 99.6(6) .
S2 OZ3 S2A 49.4(6) .
S2 S2A OZ3 62.4(7) .
S2 S2A CT1 91.5(9) .
OZ3 S2A CT1 107.7(7) .
S2 S2A CT2 45.1(8) .
OZ3 S2A CT2 103.8(6) .
CT1 S2A CT2 95.6(8) .
S2A S2 CT2 90.0(11) .
S2A S2 OZ3 68.1(8) .
CT2 S2 OZ3 146.8(14) .
S2A S2 CT1 52.9(7) .
CT2 S2 CT1 95.0(12) .
OZ3 S2 CT1 91.1(9) .
S2A CT1 S2 35.6(5) .
S2 CT2 S2A 44.9(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C6 C1 1.371(9) .
C6 C5 1.394(9) .
C1 C2 1.433(9) .
C1 C7 1.535(9) .
C5 C4 1.394(9) .
C5 C7 1.550(9) 11_556
C8 C9 1.519(11) .
C8 C7 1.524(9) .
C2 O1 1.361(8) .
C2 C3 1.366(10) .
C4 C3 1.363(10) .
C4 O2 1.380(9) .
C7 C5 1.550(9) 12_556
CZ3 S1 1.498(6) .
CZ4 S1 1.753(11) .
S1 OZ5 1.795(9) .
OZ3 S2 1.489(15) .
OZ3 S2A 1.559(9) .
S2A S2 1.277(16) .
S2A CT1 1.750(16) .
S2A CT2 1.807(16) .
S2 CT2 1.28(2) .
S2 CT1 2.19(2) .
