#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:11:47 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180380 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/49/7204951.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_7204951
loop_
_publ_author_name
'Caira, Mino R.'
'Nassimbeni, Luigi R.'
'Vujovic, Dejana'
'Weber, Edwin'
_publ_section_title
;
 Guest exchange and competition in inclusion compounds
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              861
_journal_paper_doi               10.1039/b009446n
_journal_year                    2001
_chemical_formula_sum            'C34.42 H28 O3 S0.58'
_chemical_formula_weight         508.24
_chemical_name_systematic
;3  
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                109.155(2)
_cell_angle_beta                 93.853(3)
_cell_angle_gamma                104.6010(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5652(2)
_cell_length_b                   12.4265(3)
_cell_length_c                   13.8868(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1332.83(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7226
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.155
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.864
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0903P)²+2.1607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                3937
_reflns_number_total             4794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009446n.txt
_cod_data_source_block           c:\dejana\struct~1\3
_cod_original_cell_volume        1332.83(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204951
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
O9A O 0.7646(2) 0.89227(18) 0.74121(15) 0.0310(5) Uani 1 1 d D . .
C4AA C 0.6315(3) 0.6359(2) 0.7980(2) 0.0259(6) Uani 1 1 d . . .
C10A C 0.8800(3) 0.9261(2) 0.91312(19) 0.0214(6) Uani 1 1 d . . .
C11A C 0.8950(3) 0.8974(2) 1.0016(2) 0.0289(6) Uani 1 1 d . . .
H11A H 0.8245 0.8278 1.0032 0.035 Uiso 1 1 calc R . .
C5A C 0.3584(3) 0.6598(3) 0.8603(2) 0.0351(7) Uani 1 1 d . . .
H5A H 0.3157 0.5805 0.8535 0.042 Uiso 1 1 calc R . .
C5AA C 0.5130(3) 0.7005(3) 0.8372(2) 0.0267(6) Uani 1 1 d . . .
C9A C 0.7495(3) 0.8421(2) 0.8199(2) 0.0241(6) Uani 1 1 d . . .
C3A C 0.7548(4) 0.4801(3) 0.7371(2) 0.0387(7) Uani 1 1 d . . .
H3A H 0.7517 0.4007 0.7209 0.046 Uiso 1 1 calc R . .
C8AA C 0.5780(3) 0.8196(2) 0.8486(2) 0.0249(6) Uani 1 1 d . . .
C4A C 0.6233(4) 0.5172(3) 0.7734(2) 0.0333(7) Uani 1 1 d . . .
H4A H 0.5317 0.4636 0.7810 0.040 Uiso 1 1 calc R . .
C1AA C 0.7684(3) 0.7167(2) 0.78577(19) 0.0244(6) Uani 1 1 d . . .
C2A C 0.8900(4) 0.5589(3) 0.7247(2) 0.0398(8) Uani 1 1 d . . .
H2A H 0.9766 0.5320 0.6998 0.048 Uiso 1 1 calc R . .
C12A C 0.9873(3) 1.0296(2) 0.9127(2) 0.0276(6) Uani 1 1 d . . .
H12A H 0.9806 1.0506 0.8544 0.033 Uiso 1 1 calc R . .
C1A C 0.8985(4) 0.6790(3) 0.7489(2) 0.0327(7) Uani 1 1 d . . .
H1A H 0.9897 0.7322 0.7404 0.039 Uiso 1 1 calc R . .
C6A C 0.2697(4) 0.7404(3) 0.8937(2) 0.0425(8) Uani 1 1 d . . .
H6A H 0.1669 0.7152 0.9106 0.051 Uiso 1 1 calc R . .
C8A C 0.4874(4) 0.8987(3) 0.8798(2) 0.0347(7) Uani 1 1 d . . .
H8A H 0.5292 0.9777 0.8857 0.042 Uiso 1 1 calc R . .
C7A C 0.3319(4) 0.8577(3) 0.9023(2) 0.0424(8) Uani 1 1 d . . .
H7A H 0.2695 0.9100 0.9234 0.051 Uiso 1 1 calc R . .
O9B O 0.2837(3) 0.30766(17) 0.59315(15) 0.0312(5) Uani 1 1 d D . .
C9B C 0.2462(3) 0.2181(2) 0.6383(2) 0.0244(6) Uani 1 1 d . . .
C8BB C 0.1972(3) 0.2764(2) 0.7422(2) 0.0249(6) Uani 1 1 d . . .
C10B C 0.1157(3) 0.1061(2) 0.5663(2) 0.0226(6) Uani 1 1 d . . .
C5BB C 0.3119(3) 0.2871(2) 0.8237(2) 0.0257(6) Uani 1 1 d . . .
C11B C 0.0671(3) 0.0899(3) 0.4643(2) 0.0279(6) Uani 1 1 d . . .
H11B H 0.1110 0.1498 0.4391 0.034 Uiso 1 1 calc R . .
C4BB C 0.4350(3) 0.2296(2) 0.7807(2) 0.0267(6) Uani 1 1 d . . .
C5B C 0.2987(4) 0.3465(3) 0.9255(2) 0.0330(7) Uani 1 1 d . . .
H5B H 0.3771 0.3563 0.9798 0.040 Uiso 1 1 calc R . .
C6B C 0.1664(4) 0.3910(3) 0.9442(2) 0.0382(7) Uani 1 1 d . . .
H6B H 0.1554 0.4305 1.0118 0.046 Uiso 1 1 calc R . .
C12B C 0.0464(4) 0.0146(3) 0.6012(2) 0.0303(6) Uani 1 1 d . . .
H12B H 0.0768 0.0236 0.6696 0.036 Uiso 1 1 calc R . .
C1BB C 0.3988(3) 0.1885(2) 0.6730(2) 0.0245(6) Uani 1 1 d . . .
C8B C 0.0653(4) 0.3204(3) 0.7615(2) 0.0346(7) Uani 1 1 d . . .
H8B H -0.0123 0.3121 0.7074 0.042 Uiso 1 1 calc R . .
C1B C 0.4953(4) 0.1296(3) 0.6127(2) 0.0334(7) Uani 1 1 d . . .
H1B H 0.4678 0.1003 0.5411 0.040 Uiso 1 1 calc R . .
C4B C 0.5685(4) 0.2118(3) 0.8291(3) 0.0366(7) Uani 1 1 d . . .
H4B H 0.5931 0.2393 0.9008 0.044 Uiso 1 1 calc R . .
C7B C 0.0506(4) 0.3773(3) 0.8637(3) 0.0396(8) Uani 1 1 d . . .
H7B H -0.0385 0.4066 0.8778 0.048 Uiso 1 1 calc R . .
C3B C 0.6646(4) 0.1522(3) 0.7683(3) 0.0440(8) Uani 1 1 d . . .
H3B H 0.7515 0.1369 0.7998 0.053 Uiso 1 1 calc R . .
C2B C 0.63230(11) 0.11426(9) 0.65850(7) 0.0431(8) Uani 1 1 d . . .
H2B H 0.7019 0.0798 0.6185 0.052 Uiso 1 1 calc R . .
S1G S 0.35664(11) 0.68716(9) 0.52504(7) 0.0428(4) Uani 0.742(3) 1 d PR . .
O1G O 0.53394(11) 0.73795(9) 0.56754(7) 0.0508(7) Uani 1 1 d R . .
S2G S 0.37055(11) 0.71536(9) 0.61624(7) 0.0557(14) Uani 0.258(3) 1 d PR . .
C1G C 0.2927(6) 0.5522(5) 0.5521(4) 0.0855(17) Uani 1 1 d . . .
C3G C 0.2732(7) 0.7850(7) 0.6190(5) 0.087(3) Uani 0.796(12) 1 d P . .
C2G C 0.2132(19) 0.7306(16) 0.5266(15) 0.045(6) Uani 0.204(12) 1 d P . .
H9A H 0.679(4) 0.842(3) 0.688(2) 0.054(11) Uiso 1 1 d D . .
H9B H 0.352(4) 0.287(4) 0.545(3) 0.061(12) Uiso 1 1 d 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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4A C4AA C1AA 120.9(3) . . ?
C4A C4AA C5AA 130.7(3) . . ?
C1AA C4AA C5AA 108.3(2) . . ?
C12A C10A C11A 117.9(2) . . ?
C12A C10A C9A 122.4(2) . . ?
C11A C10A C9A 119.6(2) . . ?
C12A C11A C10A 121.5(3) 2_777 . ?
C6A C5A C5AA 118.3(3) . . ?
C5A C5AA C8AA 120.9(3) . . ?
C5A C5AA C4AA 130.4(3) . . ?
C8AA C5AA C4AA 108.7(2) . . ?
O9A C9A C1AA 113.1(2) . . ?
O9A C9A C8AA 113.1(2) . . ?
C1AA C9A C8AA 101.0(2) . . ?
O9A C9A C10A 107.3(2) . . ?
C1AA C9A C10A 110.4(2) . . ?
C8AA C9A C10A 111.9(2) . . ?
C2A C3A C4A 121.0(3) . . ?
C8A C8AA C5AA 120.4(3) . . ?
C8A C8AA C9A 128.7(3) . . ?
C5AA C8AA C9A 110.8(2) . . ?
C4AA C4A C3A 118.4(3) . . ?
C1A C1AA C4AA 120.4(3) . . ?
C1A C1AA C9A 128.6(3) . . ?
C4AA C1AA C9A 111.0(2) . . ?
C3A C2A C1A 120.8(3) . . ?
C10A C12A C11A 120.6(3) . 2_777 ?
C1AA C1A C2A 118.5(3) . . ?
C7A C6A C5A 120.9(3) . . ?
C8AA C8A C7A 118.6(3) . . ?
C6A C7A C8A 120.8(3) . . ?
O9B C9B C8BB 106.0(2) . . ?
O9B C9B C10B 111.5(2) . . ?
C8BB C9B C10B 114.0(2) . . ?
O9B C9B C1BB 112.5(2) . . ?
C8BB C9B C1BB 101.1(2) . . ?
C10B C9B C1BB 111.3(2) . . ?
C8B C8BB C5BB 120.5(3) . . ?
C8B C8BB C9B 128.6(3) . . ?
C5BB C8BB C9B 110.8(2) . . ?
C11B C10B C12B 117.8(2) . . ?
C11B C10B C9B 121.8(2) . . ?
C12B C10B C9B 120.4(2) . . ?
C5B C5BB C8BB 120.5(3) . . ?
C5B C5BB C4BB 130.8(3) . . ?
C8BB C5BB C4BB 108.7(2) . . ?
C10B C11B C12B 120.9(3) . 2_556 ?
C4B C4BB C1BB 120.5(3) . . ?
C4B C4BB C5BB 130.9(3) . . ?
C1BB C4BB C5BB 108.6(2) . . ?
C6B C5B C5BB 118.6(3) . . ?
C7B C6B C5B 120.8(3) . . ?
C11B C12B C10B 121.3(3) 2_556 . ?
C1B C1BB C4BB 120.6(3) . . ?
C1B C1BB C9B 128.6(3) . . ?
C4BB C1BB C9B 110.7(2) . . ?
C8BB C8B C7B 118.7(3) . . ?
C2B C1B C1BB 120.3(3) . . ?
C3B C4B C4BB 118.7(3) . . ?
C6B C7B C8B 120.8(3) . . ?
C4B C3B C2B 121.1(3) . . ?
C1B C2B C3B 118.60(19) . . ?
S2G S1G C2G 88.7(8) . . ?
S2G S1G O1G 72.4 . . ?
C2G S1G O1G 137.0(7) . . ?
S2G S1G C3G 48.3(2) . . ?
C2G S1G C3G 43.3(7) . . ?
O1G S1G C3G 101.0(2) . . ?
S2G S1G C1G 73.15(18) . . ?
C2G S1G C1G 105.3(7) . . ?
O1G S1G C1G 105.41(16) . . ?
C3G S1G C1G 101.8(3) . . ?
S1G O1G S2G 45.1 . . ?
S1G S2G C3G 90.2(3) . . ?
S1G S2G O1G 62.5 . . ?
C3G S2G O1G 119.4(3) . . ?
S1G S2G C1G 68.84(15) . . ?
C3G S2G C1G 121.3(4) . . ?
O1G S2G C1G 98.81(19) . . ?
S1G S2G C2G 51.7(6) . . ?
C3G S2G C2G 41.7(6) . . ?
O1G S2G C2G 104.6(6) . . ?
C1G S2G C2G 89.0(6) . . ?
S1G C1G S2G 38.02(10) . . ?
C2G C3G S2G 92.3(9) . . ?
C2G C3G S1G 53.9(8) . . ?
S2G C3G S1G 41.45(18) . . ?
C3G C2G S1G 82.8(10) . . ?
C3G C2G S2G 46.0(6) . . ?
S1G C2G S2G 39.6(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O9A C9A 1.423(3) . ?
C4AA C4A 1.383(4) . ?
C4AA C1AA 1.399(4) . ?
C4AA C5AA 1.472(4) . ?
C10A C12A 1.382(4) . ?
C10A C11A 1.394(4) . ?
C10A C9A 1.532(4) . ?
C11A C12A 1.387(4) 2_777 ?
C5A C6A 1.386(5) . ?
C5A C5AA 1.393(4) . ?
C5AA C8AA 1.394(4) . ?
C9A C1AA 1.527(4) . ?
C9A C8AA 1.530(4) . ?
C3A C2A 1.377(5) . ?
C3A C4A 1.386(5) . ?
C8AA C8A 1.381(4) . ?
C1AA C1A 1.380(4) . ?
C2A C1A 1.399(5) . ?
C12A C11A 1.387(4) 2_777 ?
C6A C7A 1.381(5) . ?
C8A C7A 1.397(5) . ?
O9B C9B 1.428(3) . ?
C9B C8BB 1.527(4) . ?
C9B C10B 1.529(4) . ?
C9B C1BB 1.533(4) . ?
C8BB C8B 1.379(4) . ?
C8BB C5BB 1.396(4) . ?
C10B C11B 1.383(4) . ?
C10B C12B 1.393(4) . ?
C5BB C5B 1.390(4) . ?
C5BB C4BB 1.471(4) . ?
C11B C12B 1.388(4) 2_556 ?
C4BB C4B 1.389(4) . ?
C4BB C1BB 1.397(4) . ?
C5B C6B 1.385(5) . ?
C6B C7B 1.380(5) . ?
C12B C11B 1.388(4) 2_556 ?
C1BB C1B 1.384(4) . ?
C8B C7B 1.393(4) . ?
C1B C2B 1.383(3) . ?
C4B C3B 1.388(5) . ?
C3B C2B 1.425(4) . ?
S1G S2G 1.1868 . ?
S1G C2G 1.460(17) . ?
S1G O1G 1.4848 . ?
S1G C3G 1.793(6) . ?
S1G C1G 1.797(5) . ?
O1G S2G 1.5964 . ?
S2G C3G 1.339(7) . ?
S2G C1G 1.844(5) . ?
S2G C2G 1.860(17) . ?
C3G C2G 1.239(19) . ?
