# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_STHF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            
thiophene-bridged_molecular_gyroscope_with_3THF
_chemical_melting_point          ?
_chemical_formula_moiety         '(C52 H122 O3 S Si14), 3(C4H8O)'
_chemical_formula_sum            'C64 H146 O6 S Si14'
_chemical_formula_weight         1437.13

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'
Si Si 0.0817 0.0704 '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           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   26.247(4)
_cell_length_b                   26.247(4)
_cell_length_c                   22.735(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13564(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3571
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      1.55

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4740
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9029
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_process_details   'SADABS  Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 8.333
_diffrn_reflns_number            24388
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         28.51
_reflns_number_total             3571
_reflns_number_gt                2431
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 Bruker'
_computing_cell_refinement       'APEX 2 Bruker'
_computing_data_reduction        'APEX 2 Bruker'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^+87.8373P] 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         3571
_refine_ls_number_parameters     145
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1666
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Si01 Si 0.0000 0.0000 0.11234(6) 0.0220(3) Uani 1 3 d S . .
Si02 Si 0.12962(4) 0.19716(4) 0.08603(4) 0.0295(2) Uani 1 1 d . . .
Si03 Si 0.06931(4) 0.23626(4) 0.26159(4) 0.0297(2) Uani 1 1 d . . .
S01 S 0.0000 -0.03116(11) 0.2500 0.0249(7) Uani 0.33 2 d SPD . .
C01 C 0.0032(14) 0.0143(5) 0.1942(3) 0.030(4) Uani 0.33 1 d PD . .
C02 C 0.0002(5) 0.0606(4) 0.2186(4) 0.035(2) Uani 0.33 1 d PD . .
H02 H -0.0014 0.0901 0.1958 0.042 Uiso 0.33 1 calc PR . .
C03 C 0.03149(13) 0.07747(13) 0.08622(15) 0.0289(7) Uani 1 1 d . . .
H03A H 0.0240 0.0771 0.0435 0.035 Uiso 1 1 calc R . .
H03B H 0.0109 0.0955 0.1063 0.035 Uiso 1 1 calc R . .
C04 C 0.09815(13) 0.11600(13) 0.09732(16) 0.0296(7) Uani 1 1 d . . .
H04A H 0.1190 0.1025 0.0709 0.036 Uiso 1 1 calc R . .
H04B H 0.1064 0.1095 0.1383 0.036 Uiso 1 1 calc R . .
C05 C 0.09620(15) 0.22455(14) 0.14132(14) 0.0309(7) Uani 1 1 d . . .
H05A H 0.1143 0.2677 0.1367 0.037 Uiso 1 1 calc R . .
H05B H 0.0537 0.2067 0.1327 0.037 Uiso 1 1 calc R . .
C06 C 0.10350(18) 0.21092(18) 0.20612(15) 0.0434(9) Uani 1 1 d . . .
H06A H 0.1460 0.2294 0.2149 0.052 Uiso 1 1 calc R . .
H06B H 0.0862 0.1679 0.2103 0.052 Uiso 1 1 calc R . .
C07 C 0.11302(19) 0.21224(17) 0.01062(16) 0.0478(10) Uani 1 1 d . . .
H07A H 0.1305 0.1978 -0.0184 0.072 Uiso 1 1 calc R . .
H07B H 0.1295 0.2547 0.0055 0.072 Uiso 1 1 calc R . .
H07C H 0.0703 0.1921 0.0049 0.072 Uiso 1 1 calc R . .
C08 C 0.21126(16) 0.23469(17) 0.0972(2) 0.0497(10) Uani 1 1 d . . .
H08A H 0.2285 0.2201 0.0682 0.075 Uiso 1 1 calc R . .
H08B H 0.2197 0.2264 0.1370 0.075 Uiso 1 1 calc R . .
H08C H 0.2283 0.2772 0.0923 0.075 Uiso 1 1 calc R . .
C09 C 0.0993(3) 0.31597(19) 0.2553(2) 0.089(2) Uani 1 1 d . . .
H09A H 0.0806 0.3287 0.2846 0.134 Uiso 1 1 calc R . .
H09B H 0.0915 0.3254 0.2158 0.134 Uiso 1 1 calc R . .
H09C H 0.1419 0.3364 0.2622 0.134 Uiso 1 1 calc R . .
C10 C 0.0821(2) 0.2171(2) 0.33645(18) 0.0592(12) Uani 1 1 d . . .
H10A H 0.0656 0.1744 0.3392 0.089 Uiso 1 1 calc R . .
H10B H 0.0631 0.2297 0.3655 0.089 Uiso 1 1 calc R . .
H10C H 0.1245 0.2369 0.3442 0.089 Uiso 1 1 calc R . .
O01 O 0.0000 0.2040(2) 0.2500 0.0767(17) Uani 1 2 d S . .
O02 O 0.2762(3) 0.2762(3) 0.2500 0.122(3) Uani 1 2 d S . .
C11 C 0.2857(4) 0.3328(3) 0.2336(4) 0.133(3) Uani 1 1 d . . .
H11A H 0.2574 0.3409 0.2544 0.160 Uiso 1 1 calc R . .
H11B H 0.2796 0.3339 0.1908 0.160 Uiso 1 1 calc R . .
C12 C 0.3449(3) 0.3767(3) 0.2488(6) 0.175(5) Uani 1 1 d . . .
H12A H 0.3460 0.3946 0.2875 0.210 Uiso 1 1 calc R . .
H12B H 0.3619 0.4081 0.2187 0.210 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
Si01 0.0208(4) 0.0208(4) 0.0243(7) 0.000 0.000 0.0104(2)
Si02 0.0233(5) 0.0219(4) 0.0376(5) -0.0021(4) 0.0053(4) 0.0071(4)
Si03 0.0308(5) 0.0241(5) 0.0321(5) -0.0026(4) -0.0019(4) 0.0121(4)
S01 0.0352(17) 0.0209(11) 0.0234(16) -0.0007(6) -0.0013(13) 0.0176(9)
C01 0.028(5) 0.023(8) 0.027(4) -0.002(3) -0.004(8) 0.004(8)
C02 0.064(7) 0.029(5) 0.022(5) 0.000(4) -0.006(5) 0.031(5)
C03 0.0210(15) 0.0246(16) 0.0413(19) 0.0002(13) 0.0008(13) 0.0116(13)
C04 0.0237(15) 0.0239(15) 0.0409(19) -0.0032(13) 0.0037(13) 0.0116(13)
C05 0.0306(17) 0.0229(15) 0.0370(18) -0.0005(13) 0.0003(14) 0.0117(14)
C06 0.052(2) 0.055(2) 0.0370(19) -0.0083(17) -0.0070(17) 0.037(2)
C07 0.058(3) 0.036(2) 0.039(2) 0.0021(16) 0.0080(19) 0.0163(19)
C08 0.0284(19) 0.037(2) 0.073(3) -0.0128(19) 0.0046(18) 0.0081(16)
C09 0.153(6) 0.034(2) 0.073(4) 0.005(2) 0.050(4) 0.041(3)
C10 0.069(3) 0.079(3) 0.041(2) -0.010(2) -0.014(2) 0.045(3)
O01 0.026(2) 0.135(4) 0.032(2) -0.0018(8) -0.0035(16) 0.0131(10)
O02 0.109(4) 0.109(4) 0.118(6) 0.025(3) -0.025(3) 0.032(5)
C11 0.182(9) 0.090(5) 0.147(7) -0.049(5) -0.084(6) 0.082(6)
C12 0.109(6) 0.063(4) 0.325(15) -0.025(7) 0.051(9) 0.022(4)

_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
Si01 C03 1.868(3) 3 ?
Si01 C03 1.868(3) 2 ?
Si01 C03 1.868(3) . ?
Si01 C01 1.892(8) . ?
Si01 C01 1.892(8) 3 ?
Si01 C01 1.891(8) 2 ?
Si02 C07 1.859(4) . ?
Si02 C05 1.870(3) . ?
Si02 C08 1.875(4) . ?
Si02 C04 1.878(3) . ?
Si03 O01 1.599(4) . ?
Si03 C09 1.836(4) . ?
Si03 C10 1.853(4) . ?
Si03 C06 1.853(4) . ?
S01 C01 1.715(8) . ?
S01 C01 1.715(8) 5 ?
C01 C02 1.373(9) . ?
C02 C02 1.428(18) 5 ?
C02 H02 0.9500 . ?
C03 C04 1.542(4) . ?
C03 H03A 0.9900 . ?
C03 H03B 0.9900 . ?
C04 H04A 0.9900 . ?
C04 H04B 0.9900 . ?
C05 C06 1.550(5) . ?
C05 H05A 0.9900 . ?
C05 H05B 0.9900 . ?
C06 H06A 0.9900 . ?
C06 H06B 0.9900 . ?
C07 H07A 0.9800 . ?
C07 H07B 0.9800 . ?
C07 H07C 0.9800 . ?
C08 H08A 0.9800 . ?
C08 H08B 0.9800 . ?
C08 H08C 0.9800 . ?
C09 H09A 0.9800 . ?
C09 H09B 0.9800 . ?
C09 H09C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O01 Si03 1.599(4) 5 ?
O02 C11 1.429(8) 6 ?
O02 C11 1.429(8) . ?
C11 C12 1.439(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.445(16) 6 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

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
C03 Si01 C03 110.39(11) 3 2 ?
C03 Si01 C03 110.39(11) 3 . ?
C03 Si01 C03 110.39(11) 2 . ?
C03 Si01 C01 115.2(8) 3 . ?
C03 Si01 C01 111.5(9) 2 . ?
C03 Si01 C01 115.2(8) 2 3 ?
C03 Si01 C01 111.5(9) . 3 ?
C03 Si01 C01 111.5(9) 3 2 ?
C03 Si01 C01 115.2(8) . 2 ?
C07 Si02 C05 109.46(17) . . ?
C07 Si02 C08 109.9(2) . . ?
C05 Si02 C08 109.84(17) . . ?
C07 Si02 C04 110.52(17) . . ?
C05 Si02 C04 108.62(15) . . ?
C08 Si02 C04 108.44(17) . . ?
O01 Si03 C09 108.5(3) . . ?
O01 Si03 C10 108.70(18) . . ?
C09 Si03 C10 110.4(2) . . ?
O01 Si03 C06 108.9(2) . . ?
C09 Si03 C06 110.3(2) . . ?
C10 Si03 C06 109.94(19) . . ?
C02 C01 S01 108.2(7) . . ?
C02 C01 Si01 123.8(8) . . ?
S01 C01 Si01 127.5(5) . . ?
C01 C02 C02 113.9(5) . 5 ?
C01 C02 H02 123.1 . . ?
C02 C02 H02 123.1 5 . ?
C04 C03 Si01 113.7(2) . . ?
C04 C03 H03A 108.8 . . ?
Si01 C03 H03A 108.8 . . ?
C04 C03 H03B 108.8 . . ?
Si01 C03 H03B 108.8 . . ?
H03A C03 H03B 107.7 . . ?
C03 C04 Si02 115.6(2) . . ?
C03 C04 H04A 108.4 . . ?
Si02 C04 H04A 108.4 . . ?
C03 C04 H04B 108.4 . . ?
Si02 C04 H04B 108.4 . . ?
H04A C04 H04B 107.4 . . ?
C06 C05 Si02 114.5(2) . . ?
C06 C05 H05A 108.6 . . ?
Si02 C05 H05A 108.6 . . ?
C06 C05 H05B 108.6 . . ?
Si02 C05 H05B 108.6 . . ?
H05A C05 H05B 107.6 . . ?
C05 C06 Si03 115.2(2) . . ?
C05 C06 H06A 108.5 . . ?
Si03 C06 H06A 108.5 . . ?
C05 C06 H06B 108.5 . . ?
Si03 C06 H06B 108.5 . . ?
H06A C06 H06B 107.5 . . ?
Si02 C07 H07A 109.5 . . ?
Si02 C07 H07B 109.5 . . ?
H07A C07 H07B 109.5 . . ?
Si02 C07 H07C 109.5 . . ?
H07A C07 H07C 109.5 . . ?
H07B C07 H07C 109.5 . . ?
Si02 C08 H08A 109.5 . . ?
Si02 C08 H08B 109.5 . . ?
H08A C08 H08B 109.5 . . ?
Si02 C08 H08C 109.5 . . ?
H08A C08 H08C 109.5 . . ?
H08B C08 H08C 109.5 . . ?
Si03 C09 H09A 109.5 . . ?
Si03 C09 H09B 109.5 . . ?
H09A C09 H09B 109.5 . . ?
Si03 C09 H09C 109.5 . . ?
H09A C09 H09C 109.5 . . ?
H09B C09 H09C 109.5 . . ?
Si03 C10 H10A 109.5 . . ?
Si03 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si03 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si03 O01 Si03 175.5(5) . 5 ?
C11 O02 C11 105.1(8) 6 . ?
O02 C11 C12 109.1(7) . . ?
O02 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
O02 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C11 C12 C12 104.6(5) . 6 ?
C11 C12 H12A 110.8 . . ?
C12 C12 H12A 110.8 6 . ?
C11 C12 H12B 110.8 . . ?
C12 C12 H12B 110.8 6 . ?
H12A C12 H12B 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.930
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.077
_database_code_depnum_ccdc_archive 'CCDC 968219'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_SO2THF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            SO2-bridged_molecular_gyroscope_with_3THF
_chemical_melting_point          ?
_chemical_formula_moiety         '(C52 H122 O5 S Si14), 3(C4H8O)'
_chemical_formula_sum            'C64 H146 O8 S Si14'
_chemical_formula_weight         1469.13

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'
Si Si 0.0817 0.0704 '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           trigonal
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   26.249(2)
_cell_length_b                   26.249(2)
_cell_length_c                   22.827(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13621(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3629
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      27.95

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4836
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9023
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_process_details   'SADABS  Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 8.333
_diffrn_reflns_number            25260
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         27.95
_reflns_number_total             3629
_reflns_number_gt                3049
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 Bruker'
_computing_cell_refinement       'APEX 2 Bruker'
_computing_data_reduction        'APEX 2 Bruker'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0874P)^2^+31.5013P] 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         3629
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1594
_refine_ls_wR_factor_gt          0.1490
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.69442(7) 0.3333 0.0833 0.0246(4) Uani 0.33 2 d SP . .
Si1 Si 0.6667 0.3333 0.22244(4) 0.0230(2) Uani 1 3 d S . .
Si2 Si 0.86445(2) 0.40348(3) 0.24829(3) 0.03228(19) Uani 1 1 d . . .
Si3 Si 0.90387(3) 0.50077(3) 0.07272(3) 0.03369(19) Uani 1 1 d . . .
O1 O 0.7493(2) 0.3874(2) 0.0808(3) 0.0455(13) Uani 0.33 1 d P . .
O2 O 0.86638(16) 0.53305(16) 0.0833 0.0702(10) Uani 1 2 d S . .
C1 C 0.6852(3) 0.3491(4) 0.1414(2) 0.0236(12) Uani 0.33 1 d P . .
C2 C 0.7301(3) 0.3960(3) 0.1158(2) 0.0301(13) Uani 0.33 1 d P . .
H2 H 0.7606 0.4268 0.1379 0.036 Uiso 0.33 1 calc PR . .
C3 C 0.74449(9) 0.38089(9) 0.24663(11) 0.0342(5) Uani 1 1 d . . .
H3A H 0.7617 0.4188 0.2253 0.041 Uiso 1 1 calc R . .
H3B H 0.7448 0.3895 0.2889 0.041 Uiso 1 1 calc R . .
C4 C 0.78353(9) 0.35317(9) 0.23640(10) 0.0330(4) Uani 1 1 d . . .
H4A H 0.7775 0.3383 0.1957 0.040 Uiso 1 1 calc R . .
H4B H 0.7700 0.3189 0.2629 0.040 Uiso 1 1 calc R . .
C5 C 0.89216(9) 0.46382(9) 0.19299(9) 0.0332(4) Uani 1 1 d . . .
H5A H 0.8719 0.4867 0.1990 0.040 Uiso 1 1 calc R . .
H5B H 0.9347 0.4907 0.1998 0.040 Uiso 1 1 calc R . .
C6 C 0.88310(13) 0.44246(11) 0.12873(11) 0.0472(6) Uani 1 1 d . . .
H6A H 0.8411 0.4126 0.1232 0.057 Uiso 1 1 calc R . .
H6B H 0.9064 0.4228 0.1218 0.057 Uiso 1 1 calc R . .
C7 C 0.87888(12) 0.43492(15) 0.32329(11) 0.0538(7) Uani 1 1 d . . .
H7A H 0.8642 0.4030 0.3521 0.081 Uiso 1 1 calc R . .
H7B H 0.8588 0.4575 0.3287 0.081 Uiso 1 1 calc R . .
H7C H 0.9213 0.4608 0.3287 0.081 Uiso 1 1 calc R . .
C8 C 0.90239(12) 0.35968(13) 0.23810(14) 0.0543(7) Uani 1 1 d . . .
H8A H 0.8946 0.3430 0.1985 0.081 Uiso 1 1 calc R . .
H8B H 0.8875 0.3278 0.2670 0.081 Uiso 1 1 calc R . .
H8C H 0.9449 0.3854 0.2434 0.081 Uiso 1 1 calc R . .
C9 C 0.98249(13) 0.5553(2) 0.07897(17) 0.0931(15) Uani 1 1 d . . .
H9A H 0.9931 0.5861 0.0494 0.140 Uiso 1 1 calc R . .
H9B H 1.0057 0.5360 0.0727 0.140 Uiso 1 1 calc R . .
H9C H 0.9906 0.5729 0.1181 0.140 Uiso 1 1 calc R . .
C10 C 0.88616(17) 0.46728(15) -0.00159(12) 0.0637(8) Uani 1 1 d . . .
H10A H 0.8440 0.4388 -0.0041 0.096 Uiso 1 1 calc R . .
H10B H 0.9085 0.4472 -0.0089 0.096 Uiso 1 1 calc R . .
H10C H 0.8966 0.4982 -0.0310 0.096 Uiso 1 1 calc R . .
O3 O 0.9443(3) 0.3333 0.0833 0.178(3) Uani 1 2 d S . .
C11 C 1.0020(3) 0.3790(3) 0.1023(4) 0.168(4) Uani 1 1 d . . .
H11A H 1.0107 0.4173 0.0854 0.202 Uiso 1 1 calc R . .
H11B H 1.0028 0.3825 0.1455 0.202 Uiso 1 1 calc R . .
C12 C 1.0460(3) 0.3647(3) 0.0834(5) 0.200(5) Uani 1 1 d . . .
H12A H 1.0608 0.3805 0.0437 0.240 Uiso 1 1 calc R . .
H12B H 1.0795 0.3804 0.1110 0.240 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 0.0220(6) 0.0372(11) 0.0195(9) 0.0043(7) 0.0021(4) 0.0186(5)
Si1 0.0253(3) 0.0253(3) 0.0184(4) 0.000 0.000 0.01266(14)
Si2 0.0254(3) 0.0381(3) 0.0347(3) 0.0091(2) 0.0027(2) 0.0169(2)
Si3 0.0329(3) 0.0386(3) 0.0291(3) 0.0033(2) 0.0043(2) 0.0176(3)
O1 0.022(2) 0.062(3) 0.029(3) 0.007(2) 0.000(2) 0.003(2)
O2 0.112(2) 0.112(2) 0.0389(15) -0.0003(5) 0.0003(5) 0.095(2)
C1 0.022(5) 0.026(6) 0.019(2) -0.002(2) 0.0011(17) 0.009(2)
C2 0.027(3) 0.029(3) 0.016(3) -0.003(2) -0.002(2) 0.000(2)
C3 0.0248(9) 0.0270(9) 0.0506(13) -0.0025(9) 0.0004(9) 0.0129(8)
C4 0.0265(9) 0.0283(10) 0.0451(12) 0.0050(8) 0.0043(8) 0.0143(8)
C5 0.0306(10) 0.0334(10) 0.0321(11) 0.0025(8) 0.0011(8) 0.0135(8)
C6 0.0695(18) 0.0373(12) 0.0349(12) 0.0023(10) 0.0068(11) 0.0269(12)
C7 0.0416(14) 0.077(2) 0.0341(13) 0.0023(12) -0.0014(10) 0.0234(14)
C8 0.0424(14) 0.0620(17) 0.0726(19) 0.0204(14) 0.0118(13) 0.0367(13)
C9 0.0381(15) 0.116(3) 0.075(2) 0.042(2) -0.0064(15) 0.0012(18)
C10 0.097(2) 0.0697(19) 0.0318(14) -0.0037(13) 0.0085(14) 0.0469(18)
O3 0.158(4) 0.214(8) 0.180(7) -0.088(6) -0.044(3) 0.107(4)
C11 0.118(5) 0.130(5) 0.176(7) -0.054(5) 0.063(5) 0.002(4)
C12 0.075(4) 0.175(8) 0.311(12) 0.073(9) 0.044(6) 0.035(4)

_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 S1 1.262(3) 2_655 ?
S1 S1 1.262(3) 3_665 ?
S1 O1 1.431(5) . ?
S1 O1 1.431(5) 16_554 ?
S1 C1 1.444(7) . ?
S1 C1 1.444(7) 16_554 ?
S1 C1 1.498(8) 18_544 ?
S1 C1 1.498(8) 3_665 ?
S1 C2 1.609(6) 16_554 ?
S1 C2 1.623(6) 18_544 ?
S1 C2 1.623(6) 3_665 ?
S1 C1 1.774(5) 17_654 ?
Si1 C3 1.867(2) 3_665 ?
Si1 C3 1.867(2) . ?
Si1 C3 1.867(2) 2_655 ?
Si1 C1 1.905(6) 3_665 ?
Si1 C1 1.905(6) . ?
Si1 C1 1.905(6) 2_655 ?
Si2 C7 1.856(3) . ?
Si2 C5 1.865(2) . ?
Si2 C8 1.874(3) . ?
Si2 C4 1.877(2) . ?
Si3 O2 1.606(4) . ?
Si3 C9 1.837(3) . ?
Si3 C6 1.855(3) . ?
Si3 C10 1.860(3) . ?
O1 C2 0.965(8) 18_544 ?
O1 O1 1.300(12) 18_544 ?
O1 S1 1.919(5) 2_655 ?
O2 Si3 1.606(4) 18_544 ?
C1 C1 0.786(8) 2_655 ?
C1 C1 0.786(8) 3_665 ?
C1 C2 1.340(8) . ?
C1 S1 1.498(8) 2_655 ?
C1 S1 1.774(5) 3_665 ?
C2 C2 1.483(11) 18_544 ?
C2 H2 0.9500 . ?
C3 C4 1.543(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.546(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O3 C11 1.451(8) . ?
O3 C11 1.451(8) 16_554 ?
C11 C12 1.447(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.428(14) 16_554 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?

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
O1 S1 O1 118.7(5) . 16_554 ?
O1 S1 C1 109.6(5) 16_554 . ?
O1 S1 C1 109.6(5) . 16_554 ?
C1 S1 C1 143.8(8) . 16_554 ?
O1 S1 C1 117.8(4) 16_554 18_544 ?
C1 S1 C1 128.8(2) . 18_544 ?
O1 S1 C1 117.8(4) . 3_665 ?
C1 S1 C1 128.8(2) 16_554 3_665 ?
C1 S1 C1 136.3(9) 18_544 3_665 ?
S1 S1 C2 120.3(3) 2_655 16_554 ?
O1 S1 C2 134.9(4) . 16_554 ?
C1 S1 C2 131.6(4) . 16_554 ?
C1 S1 C2 100.7(3) 3_665 16_554 ?
S1 S1 C2 119.2(3) 3_665 18_544 ?
O1 S1 C2 139.1(4) 16_554 18_544 ?
C1 S1 C2 102.4(4) . 18_544 ?
C1 S1 C2 132.3(3) 3_665 18_544 ?
C2 S1 C2 124.9(4) 16_554 18_544 ?
O1 S1 C2 139.1(4) . 3_665 ?
C1 S1 C2 102.4(4) 16_554 3_665 ?
C1 S1 C2 132.3(3) 18_544 3_665 ?
O1 S1 C1 109.8(4) . 17_654 ?
O1 S1 C1 109.7(5) 16_554 17_654 ?
C1 S1 C1 119.2(6) . 17_654 ?
C1 S1 C1 113.8(6) 3_665 17_654 ?
C2 S1 C1 110.1(5) 3_665 17_654 ?
C3 Si1 C3 111.64(7) 3_665 . ?
C3 Si1 C3 111.64(7) 3_665 2_655 ?
C3 Si1 C3 111.64(7) . 2_655 ?
C3 Si1 C1 110.3(4) . 3_665 ?
C3 Si1 C1 116.6(3) 2_655 3_665 ?
C3 Si1 C1 116.6(3) 3_665 . ?
C3 Si1 C1 110.3(4) 2_655 . ?
C3 Si1 C1 110.3(4) 3_665 2_655 ?
C3 Si1 C1 116.6(3) . 2_655 ?
C7 Si2 C5 109.91(13) . . ?
C7 Si2 C8 109.53(15) . . ?
C5 Si2 C8 109.62(11) . . ?
C7 Si2 C4 110.72(11) . . ?
C5 Si2 C4 108.85(10) . . ?
C8 Si2 C4 108.17(12) . . ?
O2 Si3 C9 108.9(2) . . ?
O2 Si3 C6 109.07(13) . . ?
C9 Si3 C6 109.97(15) . . ?
O2 Si3 C10 108.23(13) . . ?
C9 Si3 C10 110.92(19) . . ?
C6 Si3 C10 109.74(14) . . ?
Si3 O2 Si3 175.1(3) 18_544 . ?
C1 C1 C2 133.5(19) 2_655 . ?
C1 C1 C2 147.8(14) 3_665 . ?
C1 C1 S1 101.3(4) 2_655 . ?
C2 C1 S1 105.7(4) . 3_665 ?
C1 C1 Si1 78.09(13) 2_655 . ?
C1 C1 Si1 78.09(13) 3_665 . ?
C2 C1 Si1 129.4(4) . . ?
S1 C1 Si1 152.9(8) . . ?
S1 C1 Si1 146.1(7) 2_655 . ?
S1 C1 Si1 124.6(3) 3_665 . ?
C1 C2 C2 115.9(3) . 18_544 ?
C1 C2 H2 122.1 . . ?
C2 C2 H2 122.1 18_544 . ?
C4 C3 Si1 113.74(14) . . ?
C4 C3 H3A 108.8 . . ?
Si1 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
Si1 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 Si2 115.54(14) . . ?
C3 C4 H4A 108.4 . . ?
Si2 C4 H4A 108.4 . . ?
C3 C4 H4B 108.4 . . ?
Si2 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C6 C5 Si2 114.22(16) . . ?
C6 C5 H5A 108.7 . . ?
Si2 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
Si2 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 Si3 115.24(17) . . ?
C5 C6 H6A 108.5 . . ?
Si3 C6 H6A 108.5 . . ?
C5 C6 H6B 108.5 . . ?
Si3 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 O3 C11 101.8(8) . 16_554 ?
C12 C11 O3 109.6(6) . . ?
C12 C11 H11A 109.8 . . ?
O3 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
O3 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
C12 C12 C11 103.0(4) 16_554 . ?
C12 C12 H12A 111.2 16_554 . ?
C11 C12 H12A 111.2 . . ?
C12 C12 H12B 111.2 16_554 . ?
C11 C12 H12B 111.2 . . ?
H12A C12 H12B 109.1 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 968220'