# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2009

data_global
_journal_name_full               'New J.Chem.'

_journal_coden_Cambridge         0440

_publ_contact_author_name        'Li-Zhu Wu'
_publ_contact_author_email       LZWU@MAIL.IPC.AC.CN

_publ_section_title              
;
Tetrathiafulvalene derivatives bearing crown ether
with ICT properties: synthesis and cations binding studies
;
loop_
_publ_author_name
'Li-Zhu Wu'
'Yan Liu'
'Gang Si'
'Chen-Ho Tung'
'Xiao-Jun Wang'
;
Yao-Peng Zhao
;

# Attachment 'TBC.cif'

data_TBC
_database_code_depnum_ccdc_archive 'CCDC 644421'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H22 O5 S4'
_chemical_formula_weight         494.64

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.120(4)
_cell_length_b                   8.8777(16)
_cell_length_c                   28.301(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4804.0(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    3224
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      23.60

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8758
_exptl_absorpt_correction_T_max  0.9428
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            23120
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4243
_reflns_number_gt                2312
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4243
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

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
S1 S 0.12727(5) 1.08017(9) 1.14058(3) 0.0517(3) Uani 1 1 d . . .
S2 S -0.00544(4) 0.91163(9) 1.13881(3) 0.0529(3) Uani 1 1 d . . .
S3 S 0.07865(4) 0.61573(9) 1.09782(3) 0.0517(3) Uani 1 1 d . . .
S4 S 0.20958(5) 0.79101(10) 1.09966(4) 0.0584(3) Uani 1 1 d . . .
O1 O 0.13959(11) -0.2488(2) 0.91742(8) 0.0475(6) Uani 1 1 d . . .
O2 O 0.07077(12) -0.4398(2) 0.85353(8) 0.0534(6) Uani 1 1 d . . .
O3 O 0.11892(12) -0.3097(3) 0.76937(9) 0.0669(7) Uani 1 1 d . . .
O4 O 0.15187(13) -0.0019(3) 0.78802(8) 0.0646(7) Uani 1 1 d . . .
O5 O 0.20234(11) -0.0150(2) 0.88174(9) 0.0508(6) Uani 1 1 d . . .
C1 C 0.0498(2) 1.1809(4) 1.14688(12) 0.0558(10) Uani 1 1 d . . .
H1 H 0.0502 1.2851 1.1504 0.067 Uiso 1 1 calc R . .
C2 C -0.00946(19) 1.1056(4) 1.14653(12) 0.0526(10) Uani 1 1 d . . .
H2 H -0.0521 1.1545 1.1503 0.063 Uiso 1 1 calc R . .
C3 C 0.08480(16) 0.9092(3) 1.12800(11) 0.0385(8) Uani 1 1 d . . .
C4 C 0.11938(15) 0.7884(3) 1.11097(11) 0.0386(8) Uani 1 1 d . . .
C5 C 0.20759(18) 0.6306(3) 1.06547(12) 0.0510(9) Uani 1 1 d . . .
H5 H 0.2468 0.6019 1.0483 0.061 Uiso 1 1 calc R . .
C6 C 0.14952(18) 0.5479(3) 1.06377(11) 0.0426(9) Uani 1 1 d . . .
C7 C 0.14123(17) 0.4113(4) 1.03860(12) 0.0469(9) Uani 1 1 d . . .
C8 C 0.13627(17) 0.2960(4) 1.01726(12) 0.0505(9) Uani 1 1 d . . .
C9 C 0.13384(18) 0.1555(3) 0.99139(12) 0.0454(9) Uani 1 1 d . . .
C10 C 0.17086(17) 0.1409(3) 0.94908(12) 0.0454(9) Uani 1 1 d . . .
H10 H 0.1958 0.2226 0.9372 0.054 Uiso 1 1 calc R . .
C11 C 0.17069(17) 0.0062(3) 0.92469(12) 0.0413(8) Uani 1 1 d . . .
C12 C 0.13531(17) -0.1192(3) 0.94339(12) 0.0411(8) Uani 1 1 d . . .
C13 C 0.09881(18) -0.1049(3) 0.98533(12) 0.0508(9) Uani 1 1 d . . .
H13 H 0.0754 -0.1875 0.9979 0.061 Uiso 1 1 calc R . .
C14 C 0.09709(19) 0.0330(4) 1.00876(12) 0.0551(10) Uani 1 1 d . . .
H14 H 0.0710 0.0429 1.0363 0.066 Uiso 1 1 calc R . .
C15 C 0.09752(18) -0.3752(3) 0.93170(12) 0.0527(10) Uani 1 1 d . . .
H15A H 0.0490 -0.3449 0.9351 0.063 Uiso 1 1 calc R . .
H15B H 0.1137 -0.4139 0.9618 0.063 Uiso 1 1 calc R . .
C16 C 0.10409(17) -0.4933(3) 0.89447(13) 0.0504(9) Uani 1 1 d . . .
H16A H 0.1530 -0.5135 0.8880 0.060 Uiso 1 1 calc R . .
H16B H 0.0822 -0.5860 0.9050 0.060 Uiso 1 1 calc R . .
C17 C 0.08404(19) -0.5242(3) 0.81227(13) 0.0580(10) Uani 1 1 d . . .
H17A H 0.0547 -0.6133 0.8117 0.070 Uiso 1 1 calc R . .
H17B H 0.1326 -0.5559 0.8116 0.070 Uiso 1 1 calc R . .
C18 C 0.0684(2) -0.4267(4) 0.77061(13) 0.0641(11) Uani 1 1 d . . .
H18A H 0.0706 -0.4855 0.7418 0.077 Uiso 1 1 calc R . .
H18B H 0.0218 -0.3844 0.7734 0.077 Uiso 1 1 calc R . .
C19 C 0.1009(2) -0.1888(4) 0.73993(14) 0.0754(13) Uani 1 1 d . . .
H19A H 0.0563 -0.1472 0.7497 0.090 Uiso 1 1 calc R . .
H19B H 0.0963 -0.2238 0.7076 0.090 Uiso 1 1 calc R . .
C20 C 0.1556(2) -0.0705(4) 0.74255(13) 0.0771(13) Uani 1 1 d . . .
H20A H 0.2015 -0.1149 0.7378 0.093 Uiso 1 1 calc R . .
H20B H 0.1480 0.0043 0.7181 0.093 Uiso 1 1 calc R . .
C21 C 0.21513(19) 0.0626(4) 0.80215(13) 0.0639(11) Uani 1 1 d . . .
H21A H 0.2263 0.1470 0.7817 0.077 Uiso 1 1 calc R . .
H21B H 0.2524 -0.0110 0.7995 0.077 Uiso 1 1 calc R . .
C22 C 0.20945(18) 0.1152(4) 0.85185(12) 0.0533(10) Uani 1 1 d . . .
H22A H 0.2509 0.1717 0.8606 0.064 Uiso 1 1 calc R . .
H22B H 0.1691 0.1804 0.8554 0.064 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0509(6) 0.0402(5) 0.0641(7) -0.0077(5) 0.0056(5) -0.0039(4)
S2 0.0397(5) 0.0471(5) 0.0719(7) -0.0009(5) 0.0037(5) 0.0035(4)
S3 0.0458(5) 0.0402(5) 0.0690(7) -0.0082(5) 0.0082(5) -0.0060(4)
S4 0.0395(5) 0.0432(5) 0.0926(8) -0.0147(5) 0.0086(5) -0.0022(4)
O1 0.0586(16) 0.0337(13) 0.0504(15) -0.0034(11) -0.0010(13) -0.0044(11)
O2 0.0591(16) 0.0484(14) 0.0528(17) -0.0055(13) -0.0131(13) 0.0119(11)
O3 0.0709(18) 0.0586(16) 0.0711(19) 0.0076(14) -0.0078(15) -0.0030(14)
O4 0.0623(18) 0.0767(18) 0.0547(18) -0.0114(14) 0.0018(14) -0.0125(14)
O5 0.0643(16) 0.0349(13) 0.0532(16) -0.0026(12) 0.0060(13) -0.0012(11)
C1 0.072(3) 0.039(2) 0.057(3) -0.0016(18) 0.004(2) 0.0132(19)
C2 0.056(2) 0.048(2) 0.054(3) -0.0024(18) -0.003(2) 0.0182(19)
C3 0.040(2) 0.0331(17) 0.043(2) 0.0053(15) -0.0003(16) 0.0001(15)
C4 0.0356(19) 0.0381(18) 0.042(2) -0.0008(16) -0.0007(17) 0.0019(14)
C5 0.049(2) 0.042(2) 0.063(3) -0.0029(18) 0.012(2) 0.0088(17)
C6 0.050(2) 0.0331(18) 0.045(2) 0.0021(16) 0.0003(18) 0.0053(16)
C7 0.057(2) 0.039(2) 0.044(2) 0.0012(18) -0.0074(18) 0.0068(17)
C8 0.061(2) 0.047(2) 0.044(2) -0.0003(19) -0.0106(19) 0.0108(18)
C9 0.054(2) 0.039(2) 0.043(2) -0.0046(17) -0.018(2) 0.0079(17)
C10 0.049(2) 0.037(2) 0.050(2) -0.0012(18) -0.011(2) -0.0013(15)
C11 0.042(2) 0.042(2) 0.040(2) 0.0009(18) -0.0090(18) 0.0045(16)
C12 0.046(2) 0.037(2) 0.040(2) -0.0002(17) -0.0142(18) 0.0029(16)
C13 0.069(3) 0.042(2) 0.042(2) 0.0040(18) -0.006(2) -0.0031(18)
C14 0.072(3) 0.052(2) 0.041(2) -0.0009(19) -0.005(2) 0.004(2)
C15 0.071(3) 0.037(2) 0.050(2) 0.0118(18) -0.009(2) -0.0068(18)
C16 0.053(2) 0.0298(18) 0.068(3) 0.0029(18) -0.006(2) 0.0006(16)
C17 0.065(3) 0.043(2) 0.065(3) -0.012(2) -0.002(2) -0.0053(18)
C18 0.077(3) 0.059(2) 0.056(3) -0.011(2) -0.006(2) -0.016(2)
C19 0.111(4) 0.065(3) 0.050(3) -0.005(2) -0.017(3) -0.010(3)
C20 0.118(4) 0.075(3) 0.038(3) -0.002(2) 0.003(2) -0.022(3)
C21 0.065(3) 0.063(3) 0.064(3) 0.003(2) 0.009(2) -0.014(2)
C22 0.055(2) 0.045(2) 0.060(3) 0.0020(19) -0.001(2) -0.0121(17)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
S1 C1 1.740(4) . ?
S1 C3 1.758(3) . ?
S2 C2 1.737(3) . ?
S2 C3 1.753(3) . ?
S3 C4 1.759(3) . ?
S3 C6 1.768(3) . ?
S4 C5 1.722(3) . ?
S4 C4 1.754(3) . ?
O1 C12 1.367(3) . ?
O1 C15 1.439(3) . ?
O2 C16 1.405(4) . ?
O2 C17 1.410(4) . ?
O3 C19 1.402(4) . ?
O3 C18 1.419(4) . ?
O4 C21 1.397(4) . ?
O4 C20 1.426(4) . ?
O5 C11 1.371(4) . ?
O5 C22 1.439(4) . ?
C1 C2 1.316(4) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.349(4) . ?
C5 C6 1.332(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.415(4) . ?
C7 C8 1.192(4) . ?
C8 C9 1.447(4) . ?
C9 C14 1.385(4) . ?
C9 C10 1.397(4) . ?
C10 C11 1.381(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.406(4) . ?
C12 C13 1.383(4) . ?
C13 C14 1.392(4) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.491(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.493(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.484(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.486(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?

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
C1 S1 C3 94.10(17) . . ?
C2 S2 C3 94.47(16) . . ?
C4 S3 C6 94.17(15) . . ?
C5 S4 C4 94.01(16) . . ?
C12 O1 C15 118.1(3) . . ?
C16 O2 C17 114.9(2) . . ?
C19 O3 C18 114.1(3) . . ?
C21 O4 C20 112.9(3) . . ?
C11 O5 C22 116.9(2) . . ?
C2 C1 S1 118.1(3) . . ?
C2 C1 H1 120.9 . . ?
S1 C1 H1 120.9 . . ?
C1 C2 S2 117.8(3) . . ?
C1 C2 H2 121.1 . . ?
S2 C2 H2 121.1 . . ?
C4 C3 S2 123.7(2) . . ?
C4 C3 S1 122.2(2) . . ?
S2 C3 S1 114.11(17) . . ?
C3 C4 S4 122.5(2) . . ?
C3 C4 S3 123.4(2) . . ?
S4 C4 S3 114.09(17) . . ?
C6 C5 S4 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
S4 C5 H5 120.2 . . ?
C5 C6 C7 125.7(3) . . ?
C5 C6 S3 115.6(2) . . ?
C7 C6 S3 118.7(3) . . ?
C8 C7 C6 178.1(4) . . ?
C7 C8 C9 177.3(4) . . ?
C14 C9 C10 119.3(3) . . ?
C14 C9 C8 120.9(3) . . ?
C10 C9 C8 119.8(3) . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O5 C11 C10 124.1(3) . . ?
O5 C11 C12 116.0(3) . . ?
C10 C11 C12 119.9(3) . . ?
O1 C12 C13 124.7(3) . . ?
O1 C12 C11 115.8(3) . . ?
C13 C12 C11 119.5(3) . . ?
C12 C13 C14 120.1(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C9 C14 C13 120.6(3) . . ?
C9 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
O1 C15 C16 107.6(3) . . ?
O1 C15 H15A 110.2 . . ?
C16 C15 H15A 110.2 . . ?
O1 C15 H15B 110.2 . . ?
C16 C15 H15B 110.2 . . ?
H15A C15 H15B 108.5 . . ?
O2 C16 C15 107.9(2) . . ?
O2 C16 H16A 110.1 . . ?
C15 C16 H16A 110.1 . . ?
O2 C16 H16B 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
O2 C17 C18 108.0(3) . . ?
O2 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
O2 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
O3 C18 C17 107.9(3) . . ?
O3 C18 H18A 110.1 . . ?
C17 C18 H18A 110.1 . . ?
O3 C18 H18B 110.1 . . ?
C17 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
O3 C19 C20 109.8(3) . . ?
O3 C19 H19A 109.7 . . ?
C20 C19 H19A 109.7 . . ?
O3 C19 H19B 109.7 . . ?
C20 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
O4 C20 C19 108.2(3) . . ?
O4 C20 H20A 110.1 . . ?
C19 C20 H20A 110.1 . . ?
O4 C20 H20B 110.1 . . ?
C19 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
O4 C21 C22 109.7(3) . . ?
O4 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
O4 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O5 C22 C21 108.1(3) . . ?
O5 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
O5 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 S1 C1 C2 7.7(3) . . . . ?
S1 C1 C2 S2 -1.1(4) . . . . ?
C3 S2 C2 C1 -6.2(3) . . . . ?
C2 S2 C3 C4 -168.0(3) . . . . ?
C2 S2 C3 S1 11.2(2) . . . . ?
C1 S1 C3 C4 167.7(3) . . . . ?
C1 S1 C3 S2 -11.6(2) . . . . ?
S2 C3 C4 S4 178.92(17) . . . . ?
S1 C3 C4 S4 -0.2(4) . . . . ?
S2 C3 C4 S3 -0.7(4) . . . . ?
S1 C3 C4 S3 -179.81(17) . . . . ?
C5 S4 C4 C3 -164.2(3) . . . . ?
C5 S4 C4 S3 15.5(2) . . . . ?
C6 S3 C4 C3 164.3(3) . . . . ?
C6 S3 C4 S4 -15.4(2) . . . . ?
C4 S4 C5 C6 -9.7(3) . . . . ?
S4 C5 C6 C7 -177.7(3) . . . . ?
S4 C5 C6 S3 0.3(4) . . . . ?
C4 S3 C6 C5 9.1(3) . . . . ?
C4 S3 C6 C7 -172.7(3) . . . . ?
C5 C6 C7 C8 14(11) . . . . ?
S3 C6 C7 C8 -164(11) . . . . ?
C6 C7 C8 C9 7(17) . . . . ?
C7 C8 C9 C14 122(8) . . . . ?
C7 C8 C9 C10 -56(8) . . . . ?
C14 C9 C10 C11 0.2(5) . . . . ?
C8 C9 C10 C11 178.1(3) . . . . ?
C22 O5 C11 C10 -27.2(4) . . . . ?
C22 O5 C11 C12 151.5(3) . . . . ?
C9 C10 C11 O5 176.2(3) . . . . ?
C9 C10 C11 C12 -2.5(5) . . . . ?
C15 O1 C12 C13 6.9(4) . . . . ?
C15 O1 C12 C11 -172.5(3) . . . . ?
O5 C11 C12 O1 2.9(4) . . . . ?
C10 C11 C12 O1 -178.3(3) . . . . ?
O5 C11 C12 C13 -176.5(3) . . . . ?
C10 C11 C12 C13 2.3(5) . . . . ?
O1 C12 C13 C14 -179.2(3) . . . . ?
C11 C12 C13 C14 0.1(5) . . . . ?
C10 C9 C14 C13 2.2(5) . . . . ?
C8 C9 C14 C13 -175.7(3) . . . . ?
C12 C13 C14 C9 -2.4(5) . . . . ?
C12 O1 C15 C16 172.4(3) . . . . ?
C17 O2 C16 C15 167.9(3) . . . . ?
O1 C15 C16 O2 -68.3(3) . . . . ?
C16 O2 C17 C18 -159.5(3) . . . . ?
C19 O3 C18 C17 -164.5(3) . . . . ?
O2 C17 C18 O3 67.9(4) . . . . ?
C18 O3 C19 C20 177.9(3) . . . . ?
C21 O4 C20 C19 155.1(3) . . . . ?
O3 C19 C20 O4 -70.2(4) . . . . ?
C20 O4 C21 C22 -173.3(3) . . . . ?
C11 O5 C22 C21 -155.9(3) . . . . ?
O4 C21 C22 O5 67.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.055