# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dr Braja Gopal Hazra'
_publ_contact_author_address     
;
Organic Chemistry Synthesis Division
National Chemical Laboratory
Dr. Homi Bhabha Road
Pashan, Pune
Pune
Maharashtra State, India
411 008
INDIA
;

_publ_contact_author_email       HAZRA@EMS.NCL.RES.IN

_publ_section_title              
;
Ionic hydrogenation of C-20, 22-ketene dithioacetal
: stereoselective synthesis of steroidal C (20R) aldehydes
;
loop_
_publ_author_name
'Braja Gopal Hazra'
'Mohan M. Bhadbhade'
'Rajesh G. Gonnade'
'Vandana S. Pore'
'Bapurao Shingate'

data_13
_database_code_depnum_ccdc_archive 'CCDC 240193'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'3-beta-acetoxy-pregna-5-ene-20-dithiane'
;
_chemical_name_common            3-beta-acetoxy-pregna-5-ene-20-dithiane
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H42 O2 S2.(C6 H12)0.25'
_chemical_formula_sum            'C27 H42 O2 S2.(C6 H12)0.25'
_chemical_formula_weight         473.13

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   8.1143(12)
_cell_length_b                   9.7663(15)
_cell_length_c                   19.215(3)
_cell_angle_alpha                99.467(2)
_cell_angle_beta                 99.538(2)
_cell_angle_gamma                90.654(2)
_cell_volume                     1480.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5107
_cell_measurement_theta_min      2.181
_cell_measurement_theta_max      23.954

_exptl_crystal_description       'Thick plate'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_absorpt_coefficient_mu    0.1995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9208
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_process_details   bruker-sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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_device       'Bruker Smart APEX'
_diffrn_measurement_method       'phi and Omega Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14181
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10151
_reflns_number_gt                8833
_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    'SHELXTL, ORTEP32'
_computing_publication_material  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^)+(0.0888P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(7)
_refine_ls_number_reflns         10151
_refine_ls_number_parameters     602
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1385
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.175
_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
S1 S 0.09742(14) 0.21314(10) 1.20909(6) 0.0712(3) Uani 1 1 d . . .
S2 S 0.13635(13) 0.48509(12) 1.31191(5) 0.0695(3) Uani 1 1 d . . .
O1 O 0.1812(4) 0.2009(3) 0.62417(15) 0.0714(8) Uani 1 1 d . . .
O2 O 0.2374(6) -0.0234(4) 0.6225(2) 0.1035(12) Uani 1 1 d . . .
C1 C 0.2362(4) 0.2594(4) 0.82582(19) 0.0516(8) Uani 1 1 d . . .
H1A H 0.3353 0.2859 0.8617 0.062 Uiso 1 1 calc R . .
H1B H 0.1958 0.1692 0.8322 0.062 Uiso 1 1 calc R . .
C2 C 0.2862(5) 0.2451(4) 0.7522(2) 0.0620(9) Uani 1 1 d . . .
H2A H 0.3401 0.3312 0.7471 0.074 Uiso 1 1 calc R . .
H2B H 0.3652 0.1719 0.7469 0.074 Uiso 1 1 calc R . .
C3 C 0.1335(5) 0.2111(4) 0.6948(2) 0.0595(9) Uani 1 1 d . . .
H3 H 0.0808 0.1228 0.6991 0.071 Uiso 1 1 calc R . .
C4 C 0.0101(5) 0.3247(4) 0.7015(2) 0.0601(9) Uani 1 1 d . . .
H4A H -0.0883 0.3004 0.6650 0.072 Uiso 1 1 calc R . .
H4B H 0.0599 0.4106 0.6939 0.072 Uiso 1 1 calc R . .
C5 C -0.0418(4) 0.3465(3) 0.77572(19) 0.0502(8) Uani 1 1 d . . .
C6 C -0.2024(4) 0.3521(4) 0.7826(2) 0.0560(9) Uani 1 1 d . . .
H6 H -0.2811 0.3427 0.7408 0.067 Uiso 1 1 calc R . .
C7 C -0.2660(4) 0.3719(4) 0.8514(2) 0.0554(9) Uani 1 1 d . . .
H7A H -0.3185 0.2852 0.8564 0.066 Uiso 1 1 calc R . .
H7B H -0.3513 0.4407 0.8500 0.066 Uiso 1 1 calc R . .
C8 C -0.1301(4) 0.4191(3) 0.91782(18) 0.0447(7) Uani 1 1 d . . .
H8 H -0.1079 0.5193 0.9225 0.054 Uiso 1 1 calc R . .
C9 C 0.0337(4) 0.3436(3) 0.90818(18) 0.0454(7) Uani 1 1 d . . .
H9 H 0.0042 0.2442 0.9012 0.054 Uiso 1 1 calc R . .
C10 C 0.0999(4) 0.3666(3) 0.84009(18) 0.0444(7) Uani 1 1 d . . .
C11 C 0.1630(4) 0.3735(4) 0.97718(18) 0.0520(8) Uani 1 1 d . . .
H11A H 0.2584 0.3165 0.9711 0.062 Uiso 1 1 calc R . .
H11B H 0.2018 0.4699 0.9846 0.062 Uiso 1 1 calc R . .
C12 C 0.0981(4) 0.3462(4) 1.04396(18) 0.0518(8) Uani 1 1 d . . .
H12A H 0.1851 0.3724 1.0855 0.062 Uiso 1 1 calc R . .
H12B H 0.0718 0.2477 1.0394 0.062 Uiso 1 1 calc R . .
C13 C -0.0585(4) 0.4279(3) 1.05542(18) 0.0471(7) Uani 1 1 d . . .
C14 C -0.1864(4) 0.3899(3) 0.9858(2) 0.0475(8) Uani 1 1 d . . .
H14 H -0.2041 0.2888 0.9789 0.057 Uiso 1 1 calc R . .
C15 C -0.3500(4) 0.4499(4) 1.0052(2) 0.0608(9) Uani 1 1 d . . .
H15A H -0.3550 0.5475 1.0011 0.073 Uiso 1 1 calc R . .
H15B H -0.4462 0.3999 0.9744 0.073 Uiso 1 1 calc R . .
C16 C -0.3435(5) 0.4301(4) 1.0827(2) 0.0615(10) Uani 1 1 d . . .
H16A H -0.4266 0.3600 1.0856 0.074 Uiso 1 1 calc R . .
H16B H -0.3657 0.5164 1.1120 0.074 Uiso 1 1 calc R . .
C17 C -0.1648(4) 0.3832(4) 1.10924(19) 0.0511(8) Uani 1 1 d . . .
H17 H -0.1696 0.2815 1.1017 0.061 Uiso 1 1 calc R . .
C18 C -0.0148(5) 0.5852(4) 1.0741(2) 0.0605(9) Uani 1 1 d . . .
H18A H 0.0738 0.6031 1.1146 0.091 Uiso 1 1 calc R . .
H18B H -0.1116 0.6339 1.0853 0.091 Uiso 1 1 calc R . .
H18C H 0.0206 0.6165 1.0339 0.091 Uiso 1 1 calc R . .
C19 C 0.1817(5) 0.5143(4) 0.8486(2) 0.0594(9) Uani 1 1 d . . .
H19A H 0.2128 0.5275 0.8040 0.089 Uiso 1 1 calc R . .
H19B H 0.2794 0.5240 0.8850 0.089 Uiso 1 1 calc R . .
H19C H 0.1033 0.5825 0.8619 0.089 Uiso 1 1 calc R . .
C20 C -0.1088(5) 0.4350(4) 1.19116(19) 0.0541(8) Uani 1 1 d . . .
H20 H -0.1119 0.5366 1.1986 0.065 Uiso 1 1 calc R . .
C21 C -0.2337(6) 0.3844(6) 1.2343(2) 0.0804(13) Uani 1 1 d . . .
H21A H -0.2421 0.2847 1.2252 0.121 Uiso 1 1 calc R . .
H21B H -0.3414 0.4205 1.2202 0.121 Uiso 1 1 calc R . .
H21C H -0.1956 0.4164 1.2844 0.121 Uiso 1 1 calc R . .
C22 C 0.0711(5) 0.3997(4) 1.21966(19) 0.0550(8) Uani 1 1 d . . .
H22 H 0.1439 0.4370 1.1908 0.066 Uiso 1 1 calc R . .
C23 C 0.3256(7) 0.2173(6) 1.2368(3) 0.0858(14) Uani 1 1 d . . .
H23A H 0.3624 0.1226 1.2324 0.103 Uiso 1 1 calc R . .
H23B H 0.3772 0.2630 1.2041 0.103 Uiso 1 1 calc R . .
C24 C 0.3873(7) 0.2909(6) 1.3125(3) 0.0846(14) Uani 1 1 d . . .
H24A H 0.5060 0.2768 1.3249 0.102 Uiso 1 1 calc R . .
H24B H 0.3304 0.2496 1.3450 0.102 Uiso 1 1 calc R . .
C25 C 0.3588(6) 0.4461(5) 1.3227(2) 0.0757(12) Uani 1 1 d . . .
H25A H 0.4098 0.4867 1.2883 0.091 Uiso 1 1 calc R . .
H25B H 0.4136 0.4888 1.3703 0.091 Uiso 1 1 calc R . .
C26 C 0.2358(7) 0.0783(5) 0.5959(3) 0.0809(13) Uani 1 1 d . . .
C27 C 0.3010(12) 0.0907(7) 0.5275(3) 0.132(3) Uani 1 1 d . . .
H27A H 0.3923 0.1583 0.5379 0.198 Uiso 1 1 calc R . .
H27C H 0.2129 0.1194 0.4936 0.198 Uiso 1 1 calc R . .
H27B H 0.3388 0.0024 0.5076 0.198 Uiso 1 1 calc R . .
S1' S 0.50622(14) 0.51507(10) 0.61156(6) 0.0697(3) Uani 1 1 d . . .
S2' S 0.48906(12) 0.71566(10) 0.50710(5) 0.0639(3) Uani 1 1 d . . .
O1' O 0.4721(4) 0.8931(3) 1.20088(15) 0.0748(8) Uani 1 1 d . . .
O2' O 0.4182(8) 0.6681(5) 1.2019(3) 0.1389(19) Uani 1 1 d . . .
C1' C 0.4010(4) 0.8182(4) 0.9987(2) 0.0539(8) Uani 1 1 d . . .
H1'A H 0.3002 0.8189 0.9636 0.065 Uiso 1 1 calc R . .
H1'B H 0.4406 0.7244 0.9929 0.065 Uiso 1 1 calc R . .
C2' C 0.3560(5) 0.8549(4) 1.0734(2) 0.0630(10) Uani 1 1 d . . .
H2'A H 0.3059 0.9450 1.0787 0.076 Uiso 1 1 calc R . .
H2'B H 0.2756 0.7863 1.0804 0.076 Uiso 1 1 calc R . .
C3' C 0.5142(5) 0.8582(4) 1.1289(2) 0.0619(9) Uani 1 1 d . . .
H3' H 0.5650 0.7674 1.1234 0.074 Uiso 1 1 calc R . .
C4' C 0.6373(5) 0.9690(4) 1.1204(2) 0.0626(10) Uani 1 1 d . . .
H4'A H 0.7377 0.9702 1.1558 0.075 Uiso 1 1 calc R . .
H4'B H 0.5886 1.0594 1.1282 0.075 Uiso 1 1 calc R . .
C5' C 0.6821(4) 0.9405(3) 1.04542(19) 0.0516(8) Uani 1 1 d . . .
C6' C 0.8429(4) 0.9387(4) 1.0368(2) 0.0576(9) Uani 1 1 d . . .
H6' H 0.9235 0.9569 1.0780 0.069 Uiso 1 1 calc R . .
C7' C 0.9030(4) 0.9102(4) 0.9673(2) 0.0583(9) Uani 1 1 d . . .
H7'A H 0.9509 0.8192 0.9624 0.070 Uiso 1 1 calc R . .
H7'B H 0.9913 0.9781 0.9674 0.070 Uiso 1 1 calc R . .
C8' C 0.7655(4) 0.9143(3) 0.90205(19) 0.0487(8) Uani 1 1 d . . .
H8' H 0.7473 1.0113 0.8967 0.058 Uiso 1 1 calc R . .
C9' C 0.6007(4) 0.8474(3) 0.91282(18) 0.0442(7) Uani 1 1 d . . .
H9' H 0.6260 0.7521 0.9196 0.053 Uiso 1 1 calc R . .
C10' C 0.5368(4) 0.9174(3) 0.98205(18) 0.0446(7) Uani 1 1 d . . .
C11' C 0.4682(4) 0.8345(4) 0.8454(2) 0.0547(9) Uani 1 1 d . . .
H11D H 0.4346 0.9268 0.8381 0.066 Uiso 1 1 calc R . .
H11C H 0.3706 0.7840 0.8527 0.066 Uiso 1 1 calc R . .
C12' C 0.5276(4) 0.7594(4) 0.77667(19) 0.0526(8) Uani 1 1 d . . .
H12D H 0.5480 0.6633 0.7811 0.063 Uiso 1 1 calc R . .
H12C H 0.4400 0.7602 0.7357 0.063 Uiso 1 1 calc R . .
C13' C 0.6878(4) 0.8292(3) 0.76397(19) 0.0475(7) Uani 1 1 d . . .
C14' C 0.8170(4) 0.8365(3) 0.83376(19) 0.0471(8) Uani 1 1 d . . .
H14' H 0.8295 0.7401 0.8414 0.056 Uiso 1 1 calc R . .
C15' C 0.9812(4) 0.8787(5) 0.8125(2) 0.0656(10) Uani 1 1 d . . .
H15D H 0.9912 0.9786 0.8153 0.079 Uiso 1 1 calc R . .
H15C H 1.0763 0.8490 0.8433 0.079 Uiso 1 1 calc R . .
C16' C 0.9710(5) 0.8048(5) 0.7357(2) 0.0663(10) Uani 1 1 d . . .
H16C H 1.0492 0.7304 0.7336 0.080 Uiso 1 1 calc R . .
H16D H 0.9981 0.8693 0.7056 0.080 Uiso 1 1 calc R . .
C17' C 0.7872(4) 0.7447(4) 0.7100(2) 0.0529(8) Uani 1 1 d . . .
H17' H 0.7856 0.6482 0.7181 0.064 Uiso 1 1 calc R . .
C18' C 0.6547(5) 0.9751(4) 0.7444(2) 0.0618(9) Uani 1 1 d . . .
H18E H 0.5680 0.9676 0.7032 0.093 Uiso 1 1 calc R . .
H18D H 0.7552 1.0137 0.7338 0.093 Uiso 1 1 calc R . .
H18F H 0.6204 1.0345 0.7840 0.093 Uiso 1 1 calc R . .
C19' C 0.4602(5) 1.0586(4) 0.9737(2) 0.0593(9) Uani 1 1 d . . .
H19F H 0.4498 1.1089 1.0200 0.089 Uiso 1 1 calc R . .
H19E H 0.3518 1.0437 0.9442 0.089 Uiso 1 1 calc R . .
H19D H 0.5314 1.1112 0.9517 0.089 Uiso 1 1 calc R . .
C20' C 0.7312(5) 0.7419(4) 0.6280(2) 0.0583(9) Uani 1 1 d . . .
H20' H 0.7424 0.8375 0.6194 0.070 Uiso 1 1 calc R . .
C21' C 0.8512(6) 0.6549(6) 0.5863(3) 0.0894(15) Uani 1 1 d . . .
H21F H 0.8619 0.5660 0.6013 0.134 Uiso 1 1 calc R . .
H21D H 0.9588 0.7023 0.5955 0.134 Uiso 1 1 calc R . .
H21E H 0.8076 0.6421 0.5359 0.134 Uiso 1 1 calc R . .
C22' C 0.5482(5) 0.6929(4) 0.60046(19) 0.0528(8) Uani 1 1 d . . .
H22' H 0.4789 0.7531 0.6287 0.063 Uiso 1 1 calc R . .
C23' C 0.2823(6) 0.5105(5) 0.5846(2) 0.0769(13) Uani 1 1 d . . .
H23C H 0.2377 0.4208 0.5898 0.092 Uiso 1 1 calc R . .
H23D H 0.2366 0.5807 0.6172 0.092 Uiso 1 1 calc R . .
C24' C 0.2211(6) 0.5340(5) 0.5088(2) 0.0742(12) Uani 1 1 d . . .
H24C H 0.2683 0.4654 0.4759 0.089 Uiso 1 1 calc R . .
H24D H 0.1004 0.5196 0.4982 0.089 Uiso 1 1 calc R . .
C25' C 0.2660(5) 0.6775(5) 0.4959(2) 0.0689(11) Uani 1 1 d . . .
H25D H 0.2185 0.7459 0.5288 0.083 Uiso 1 1 calc R . .
H25C H 0.2152 0.6870 0.4477 0.083 Uiso 1 1 calc R . .
C26' C 0.4313(10) 0.7899(6) 1.2313(3) 0.106(2) Uani 1 1 d . . .
C27' C 0.3861(12) 0.8396(7) 1.3042(3) 0.142(3) Uani 1 1 d . . .
H27E H 0.4037 0.7672 1.3326 0.213 Uiso 1 1 calc R . .
H27D H 0.2707 0.8633 1.2988 0.213 Uiso 1 1 calc R . .
H27F H 0.4551 0.9200 1.3275 0.213 Uiso 1 1 calc R . .
C28 C 0.8082(14) 0.1654(10) 0.4578(4) 0.13(2) Uiso 0.13 1 d PRD A 1
H28A H 0.6988 0.2053 0.4528 0.152 Uiso 0.13 1 calc PR B 1
H28B H 0.8833 0.2226 0.4965 0.152 Uiso 0.13 1 calc PR C 1
C29 C 0.8772(14) 0.1473(11) 0.3878(4) 0.046(6) Uiso 0.13 1 d PRD A 1
H29A H 0.8030 0.1965 0.3564 0.056 Uiso 0.13 1 calc PR D 1
H29B H 0.9833 0.1997 0.3989 0.056 Uiso 0.13 1 calc PR E 1
C30 C 0.9088(16) 0.0131(7) 0.3423(4) 0.058(7) Uiso 0.13 1 d PRD A 1
H30A H 0.8352 0.0138 0.2971 0.069 Uiso 0.13 1 calc PR F 1
H30B H 1.0210 0.0267 0.3328 0.069 Uiso 0.13 1 calc PR G 1
C31 C 0.9012(17) -0.1340(7) 0.3525(4) 0.086(11) Uiso 0.13 1 d PRD A 1
H31A H 1.0090 -0.1760 0.3530 0.104 Uiso 0.13 1 calc PR H 1
H31B H 0.8182 -0.1893 0.3163 0.104 Uiso 0.13 1 calc PR I 1
C32 C 0.8499(17) -0.1133(7) 0.4251(4) 0.070(9) Uiso 0.13 1 d PRD A 1
H32A H 0.7580 -0.1805 0.4202 0.084 Uiso 0.13 1 calc PR J 1
H32B H 0.9423 -0.1467 0.4558 0.084 Uiso 0.13 1 calc PR K 1
C33 C 0.7984(16) 0.0134(7) 0.4697(4) 0.062(8) Uiso 0.13 1 d PRD A 1
H33A H 0.8601 0.0136 0.5175 0.074 Uiso 0.13 1 calc PR L 1
H33B H 0.6821 -0.0050 0.4724 0.074 Uiso 0.13 1 calc PR M 1
C28' C 0.787(6) 0.198(3) 0.4758(19) 0.103(14) Uiso 0.13 1 d PD N 2
H28D H 0.8373 0.2671 0.5160 0.124 Uiso 0.13 1 calc PR N 2
H28C H 0.6694 0.2186 0.4648 0.124 Uiso 0.13 1 calc PR N 2
C29' C 0.861(4) 0.215(2) 0.4163(15) 0.070(8) Uiso 0.13 1 d PD N 2
H29D H 0.9700 0.2617 0.4347 0.084 Uiso 0.13 1 calc PR N 2
H29C H 0.7941 0.2783 0.3905 0.084 Uiso 0.13 1 calc PR N 2
C30' C 0.886(3) 0.095(2) 0.3651(12) 0.043(5) Uiso 0.13 1 d PD N 2
H30D H 0.8001 0.0929 0.3233 0.051 Uiso 0.13 1 calc PR N 2
H30C H 0.9926 0.1089 0.3503 0.051 Uiso 0.13 1 calc PR N 2
C31' C 0.884(7) -0.038(3) 0.3857(18) 0.112(15) Uiso 0.13 1 d PD N 2
H31D H 0.9958 -0.0719 0.3871 0.134 Uiso 0.13 1 calc PR N 2
H31C H 0.8112 -0.0989 0.3479 0.134 Uiso 0.13 1 calc PR N 2
C32' C 0.832(4) -0.052(2) 0.4521(13) 0.056(7) Uiso 0.13 1 d PD N 2
H32D H 0.7337 -0.1135 0.4412 0.067 Uiso 0.13 1 calc PR N 2
H32C H 0.9200 -0.0975 0.4793 0.067 Uiso 0.13 1 calc PR N 2
C33' C 0.795(5) 0.071(3) 0.4974(16) 0.082(10) Uiso 0.13 1 d PD N 2
H33D H 0.6884 0.0529 0.5112 0.098 Uiso 0.13 1 calc PR N 2
H33C H 0.8782 0.0817 0.5407 0.098 Uiso 0.13 1 calc PR N 2

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 0.0863(7) 0.0555(6) 0.0701(6) 0.0076(5) 0.0116(5) 0.0043(5)
S2 0.0691(6) 0.0860(7) 0.0478(5) -0.0086(5) 0.0133(4) 0.0028(5)
O1 0.098(2) 0.0651(17) 0.0555(16) 0.0091(13) 0.0274(15) 0.0128(15)
O2 0.166(4) 0.066(2) 0.086(2) 0.0073(18) 0.049(2) 0.029(2)
C1 0.0486(19) 0.053(2) 0.055(2) 0.0104(16) 0.0110(15) 0.0113(15)
C2 0.061(2) 0.067(2) 0.062(2) 0.0134(18) 0.0177(18) 0.0163(18)
C3 0.075(2) 0.051(2) 0.055(2) 0.0089(17) 0.0217(18) 0.0061(17)
C4 0.061(2) 0.068(2) 0.051(2) 0.0128(17) 0.0039(17) 0.0051(17)
C5 0.053(2) 0.0472(18) 0.0497(19) 0.0112(15) 0.0041(15) 0.0067(14)
C6 0.0489(19) 0.065(2) 0.049(2) 0.0089(16) -0.0053(15) 0.0076(16)
C7 0.0397(17) 0.063(2) 0.061(2) 0.0094(17) 0.0017(15) 0.0059(15)
C8 0.0392(16) 0.0415(17) 0.0526(18) 0.0084(14) 0.0052(14) 0.0020(13)
C9 0.0388(16) 0.0401(17) 0.056(2) 0.0080(14) 0.0045(14) 0.0022(12)
C10 0.0413(16) 0.0412(17) 0.0495(18) 0.0066(14) 0.0051(14) 0.0016(13)
C11 0.0366(16) 0.070(2) 0.049(2) 0.0103(17) 0.0051(14) 0.0076(15)
C12 0.0421(17) 0.063(2) 0.0492(19) 0.0091(16) 0.0059(14) 0.0078(15)
C13 0.0418(17) 0.0487(18) 0.0497(19) 0.0055(14) 0.0073(14) 0.0005(13)
C14 0.0398(17) 0.0417(17) 0.060(2) 0.0062(14) 0.0078(15) 0.0010(13)
C15 0.0415(18) 0.072(2) 0.068(2) 0.0085(19) 0.0080(16) 0.0112(16)
C16 0.049(2) 0.070(2) 0.066(2) 0.0021(19) 0.0219(18) 0.0049(17)
C17 0.0473(18) 0.0483(19) 0.058(2) 0.0017(15) 0.0168(15) -0.0019(14)
C18 0.066(2) 0.053(2) 0.061(2) 0.0053(17) 0.0111(18) -0.0074(17)
C19 0.067(2) 0.049(2) 0.064(2) 0.0100(17) 0.0172(18) -0.0072(17)
C20 0.054(2) 0.060(2) 0.0474(19) -0.0009(16) 0.0150(16) 0.0012(16)
C21 0.068(3) 0.112(4) 0.063(3) 0.011(2) 0.021(2) 0.000(2)
C22 0.065(2) 0.054(2) 0.0460(19) -0.0011(15) 0.0173(16) -0.0039(16)
C23 0.091(3) 0.087(3) 0.081(3) 0.013(3) 0.018(3) 0.029(3)
C24 0.076(3) 0.115(4) 0.068(3) 0.029(3) 0.012(2) 0.022(3)
C25 0.069(3) 0.102(4) 0.056(2) 0.005(2) 0.0161(19) -0.001(2)
C26 0.109(4) 0.070(3) 0.068(3) 0.008(2) 0.033(3) 0.014(3)
C27 0.216(8) 0.114(5) 0.087(4) 0.019(3) 0.080(5) 0.048(5)
S1' 0.0885(7) 0.0551(5) 0.0704(6) 0.0164(5) 0.0220(5) 0.0023(5)
S2' 0.0749(6) 0.0711(6) 0.0490(5) 0.0127(4) 0.0176(4) -0.0007(5)
O1' 0.104(2) 0.0655(17) 0.0597(16) 0.0087(13) 0.0288(15) 0.0022(15)
O2' 0.245(6) 0.079(3) 0.116(3) 0.024(2) 0.090(4) 0.006(3)
C1' 0.0458(18) 0.054(2) 0.058(2) -0.0011(16) 0.0091(16) -0.0051(15)
C2' 0.065(2) 0.060(2) 0.065(2) 0.0022(18) 0.0224(19) -0.0050(18)
C3' 0.082(3) 0.053(2) 0.054(2) 0.0092(17) 0.0208(19) 0.0052(19)
C4' 0.064(2) 0.063(2) 0.055(2) 0.0029(18) 0.0005(18) -0.0055(18)
C5' 0.052(2) 0.0445(18) 0.054(2) 0.0026(15) 0.0012(15) -0.0020(14)
C6' 0.0423(19) 0.064(2) 0.059(2) 0.0043(17) -0.0050(16) -0.0033(16)
C7' 0.0366(17) 0.068(2) 0.065(2) 0.0068(18) -0.0009(16) -0.0022(15)
C8' 0.0385(16) 0.0434(17) 0.062(2) 0.0079(15) 0.0036(15) 0.0003(13)
C9' 0.0382(16) 0.0391(16) 0.0542(19) 0.0076(14) 0.0053(14) 0.0011(12)
C10' 0.0390(16) 0.0379(16) 0.0546(19) 0.0042(14) 0.0053(14) -0.0009(12)
C11' 0.0411(18) 0.061(2) 0.061(2) 0.0034(17) 0.0110(16) 0.0009(15)
C12' 0.0393(17) 0.065(2) 0.052(2) 0.0050(16) 0.0073(14) -0.0057(15)
C13' 0.0431(17) 0.0467(18) 0.0532(19) 0.0093(15) 0.0085(15) 0.0035(14)
C14' 0.0361(16) 0.0478(18) 0.059(2) 0.0148(15) 0.0061(14) 0.0032(13)
C15' 0.0400(18) 0.083(3) 0.073(3) 0.013(2) 0.0078(17) -0.0044(18)
C16' 0.043(2) 0.081(3) 0.078(3) 0.020(2) 0.0148(19) 0.0022(18)
C17' 0.0448(18) 0.057(2) 0.061(2) 0.0164(17) 0.0138(16) 0.0078(15)
C18' 0.067(2) 0.055(2) 0.067(2) 0.0166(18) 0.0131(19) 0.0127(17)
C19' 0.063(2) 0.052(2) 0.064(2) 0.0109(17) 0.0128(18) 0.0134(17)
C20' 0.057(2) 0.062(2) 0.061(2) 0.0166(17) 0.0217(18) 0.0076(17)
C21' 0.067(3) 0.133(5) 0.072(3) 0.009(3) 0.031(2) 0.018(3)
C22' 0.058(2) 0.053(2) 0.0494(19) 0.0089(15) 0.0155(16) 0.0036(15)
C23' 0.094(3) 0.073(3) 0.065(3) 0.002(2) 0.028(2) -0.019(2)
C24' 0.077(3) 0.084(3) 0.058(2) -0.009(2) 0.022(2) -0.014(2)
C25' 0.071(3) 0.078(3) 0.051(2) -0.0026(19) 0.0043(19) 0.004(2)
C26' 0.178(6) 0.075(3) 0.076(3) 0.011(3) 0.054(4) 0.015(4)
C27' 0.245(10) 0.107(5) 0.096(5) 0.018(4) 0.093(6) -0.003(5)

_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 C22 1.819(4) . ?
S1 C23 1.838(5) . ?
S2 C22 1.819(4) . ?
S2 C25 1.834(5) . ?
O1 C26 1.342(6) . ?
O1 C3 1.460(4) . ?
O2 C26 1.189(6) . ?
C1 C2 1.521(5) . ?
C1 C10 1.558(5) . ?
C2 C3 1.509(6) . ?
C3 C4 1.507(6) . ?
C4 C5 1.534(5) . ?
C5 C6 1.333(5) . ?
C5 C10 1.527(5) . ?
C6 C7 1.481(5) . ?
C7 C8 1.544(5) . ?
C8 C14 1.521(5) . ?
C8 C9 1.550(4) . ?
C9 C11 1.532(5) . ?
C9 C10 1.542(5) . ?
C10 C19 1.553(5) . ?
C11 C12 1.525(5) . ?
C12 C13 1.536(5) . ?
C13 C14 1.540(5) . ?
C13 C18 1.542(5) . ?
C13 C17 1.562(5) . ?
C14 C15 1.534(5) . ?
C15 C16 1.526(6) . ?
C16 C17 1.555(5) . ?
C17 C20 1.561(5) . ?
C20 C22 1.536(5) . ?
C20 C21 1.536(6) . ?
C23 C24 1.514(7) . ?
C24 C25 1.521(7) . ?
C26 C27 1.519(7) . ?
S1' C23' 1.803(5) . ?
S1' C22' 1.820(4) . ?
S2' C25' 1.814(4) . ?
S2' C22' 1.829(4) . ?
O1' C26' 1.310(6) . ?
O1' C3' 1.466(5) . ?
O2' C26' 1.226(7) . ?
C1' C2' 1.527(5) . ?
C1' C10' 1.565(5) . ?
C2' C3' 1.523(6) . ?
C3' C4' 1.511(6) . ?
C4' C5' 1.526(5) . ?
C5' C6' 1.342(5) . ?
C5' C10' 1.533(5) . ?
C6' C7' 1.483(5) . ?
C7' C8' 1.540(5) . ?
C8' C14' 1.528(5) . ?
C8' C9' 1.541(4) . ?
C9' C11' 1.527(5) . ?
C9' C10' 1.563(5) . ?
C10' C19' 1.540(5) . ?
C11' C12' 1.553(5) . ?
C12' C13' 1.534(5) . ?
C13' C18' 1.547(5) . ?
C13' C14' 1.550(5) . ?
C13' C17' 1.555(5) . ?
C14' C15' 1.528(5) . ?
C15' C16' 1.520(6) . ?
C16' C17' 1.567(5) . ?
C17' C20' 1.561(5) . ?
C20' C22' 1.534(5) . ?
C20' C21' 1.538(6) . ?
C23' C24' 1.515(7) . ?
C24' C25' 1.513(6) . ?
C26' C27' 1.512(7) . ?
C28 C29 1.5259 . ?
C28 C33 1.542(5) . ?
C29 C30 1.501(3) . ?
C30 C31 1.483(2) . ?
C31 C32 1.5039 . ?
C32 C33 1.4906(12) . ?
C28' C33' 1.37(4) . ?
C28' C29' 1.41(2) . ?
C29' C30' 1.44(2) . ?
C30' C31' 1.42(2) . ?
C31' C32' 1.43(2) . ?
C32' C33' 1.43(2) . ?

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
C22 S1 C23 97.8(2) . . ?
C22 S2 C25 99.08(19) . . ?
C26 O1 C3 117.1(3) . . ?
C2 C1 C10 115.5(3) . . ?
C3 C2 C1 110.0(3) . . ?
O1 C3 C4 107.6(3) . . ?
O1 C3 C2 109.9(3) . . ?
C4 C3 C2 110.4(3) . . ?
C3 C4 C5 111.1(3) . . ?
C6 C5 C10 122.5(3) . . ?
C6 C5 C4 121.0(3) . . ?
C10 C5 C4 116.5(3) . . ?
C5 C6 C7 125.3(3) . . ?
C6 C7 C8 114.1(3) . . ?
C14 C8 C7 111.4(3) . . ?
C14 C8 C9 109.6(3) . . ?
C7 C8 C9 109.9(3) . . ?
C11 C9 C10 114.7(3) . . ?
C11 C9 C8 110.9(3) . . ?
C10 C9 C8 113.3(3) . . ?
C5 C10 C9 110.5(3) . . ?
C5 C10 C19 108.7(3) . . ?
C9 C10 C19 111.8(3) . . ?
C5 C10 C1 109.3(3) . . ?
C9 C10 C1 108.7(3) . . ?
C19 C10 C1 107.7(3) . . ?
C12 C11 C9 114.4(3) . . ?
C11 C12 C13 111.8(3) . . ?
C12 C13 C14 106.6(3) . . ?
C12 C13 C18 110.6(3) . . ?
C14 C13 C18 112.2(3) . . ?
C12 C13 C17 117.5(3) . . ?
C14 C13 C17 99.1(3) . . ?
C18 C13 C17 110.3(3) . . ?
C8 C14 C15 119.0(3) . . ?
C8 C14 C13 116.1(3) . . ?
C15 C14 C13 104.3(3) . . ?
C16 C15 C14 103.9(3) . . ?
C15 C16 C17 107.0(3) . . ?
C16 C17 C20 111.3(3) . . ?
C16 C17 C13 103.9(3) . . ?
C20 C17 C13 119.4(3) . . ?
C22 C20 C21 111.6(3) . . ?
C22 C20 C17 113.8(3) . . ?
C21 C20 C17 111.1(3) . . ?
C20 C22 S1 111.9(2) . . ?
C20 C22 S2 110.8(2) . . ?
S1 C22 S2 112.1(2) . . ?
C24 C23 S1 114.4(3) . . ?
C23 C24 C25 113.2(4) . . ?
C24 C25 S2 112.7(3) . . ?
O2 C26 O1 124.2(4) . . ?
O2 C26 C27 125.5(5) . . ?
O1 C26 C27 110.3(4) . . ?
C23' S1' C22' 97.69(19) . . ?
C25' S2' C22' 98.94(18) . . ?
C26' O1' C3' 117.3(4) . . ?
C2' C1' C10' 114.9(3) . . ?
C3' C2' C1' 109.0(3) . . ?
O1' C3' C4' 107.7(3) . . ?
O1' C3' C2' 109.4(3) . . ?
C4' C3' C2' 110.2(3) . . ?
C3' C4' C5' 110.1(3) . . ?
C6' C5' C4' 120.2(3) . . ?
C6' C5' C10' 122.6(3) . . ?
C4' C5' C10' 117.2(3) . . ?
C5' C6' C7' 125.5(3) . . ?
C6' C7' C8' 113.8(3) . . ?
C14' C8' C7' 110.8(3) . . ?
C14' C8' C9' 108.9(3) . . ?
C7' C8' C9' 110.3(3) . . ?
C11' C9' C8' 111.3(3) . . ?
C11' C9' C10' 113.4(3) . . ?
C8' C9' C10' 113.5(3) . . ?
C5' C10' C19' 108.4(3) . . ?
C5' C10' C9' 109.8(3) . . ?
C19' C10' C9' 112.0(3) . . ?
C5' C10' C1' 108.7(3) . . ?
C19' C10' C1' 109.0(3) . . ?
C9' C10' C1' 108.7(2) . . ?
C9' C11' C12' 113.9(3) . . ?
C13' C12' C11' 111.6(3) . . ?
C12' C13' C18' 111.4(3) . . ?
C12' C13' C14' 106.6(3) . . ?
C18' C13' C14' 111.6(3) . . ?
C12' C13' C17' 117.0(3) . . ?
C18' C13' C17' 110.0(3) . . ?
C14' C13' C17' 99.6(3) . . ?
C8' C14' C15' 119.4(3) . . ?
C8' C14' C13' 116.3(3) . . ?
C15' C14' C13' 103.7(3) . . ?
C16' C15' C14' 104.4(3) . . ?
C15' C16' C17' 106.9(3) . . ?
C13' C17' C20' 119.6(3) . . ?
C13' C17' C16' 103.6(3) . . ?
C20' C17' C16' 111.3(3) . . ?
C22' C20' C21' 111.7(4) . . ?
C22' C20' C17' 113.7(3) . . ?
C21' C20' C17' 109.7(3) . . ?
C20' C22' S1' 112.8(3) . . ?
C20' C22' S2' 109.8(2) . . ?
S1' C22' S2' 111.46(19) . . ?
C24' C23' S1' 115.6(3) . . ?
C25' C24' C23' 113.7(4) . . ?
C24' C25' S2' 114.2(3) . . ?
O2' C26' O1' 124.0(5) . . ?
O2' C26' C27' 123.6(5) . . ?
O1' C26' C27' 112.1(5) . . ?
C29 C28 C33 100.8 . . ?
C30 C29 C28 127.19(18) . . ?
C31 C30 C29 132.94(15) . . ?
C30 C31 C32 99.1 . . ?
C33 C32 C31 131.00(6) . . ?
C32 C33 C28 128.3 . . ?
C33' C28' C29' 118.0(13) . . ?
C28' C29' C30' 119.3(11) . . ?
C31' C30' C29' 118.8(12) . . ?
C30' C31' C32' 119.4(9) . . ?
C33' C32' C31' 118.2(13) . . ?
C28' C33' C32' 122.2(15) . . ?

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
C10 C1 C2 C3 -55.3(4) . . . . ?
C26 O1 C3 C4 -155.1(4) . . . . ?
C26 O1 C3 C2 84.6(5) . . . . ?
C1 C2 C3 O1 178.6(3) . . . . ?
C1 C2 C3 C4 60.0(4) . . . . ?
O1 C3 C4 C5 -177.7(3) . . . . ?
C2 C3 C4 C5 -57.8(4) . . . . ?
C3 C4 C5 C6 -130.9(4) . . . . ?
C3 C4 C5 C10 51.2(4) . . . . ?
C10 C5 C6 C7 -2.6(6) . . . . ?
C4 C5 C6 C7 179.7(3) . . . . ?
C5 C6 C7 C8 13.0(6) . . . . ?
C6 C7 C8 C14 -160.3(3) . . . . ?
C6 C7 C8 C9 -38.6(4) . . . . ?
C14 C8 C9 C11 -49.7(4) . . . . ?
C7 C8 C9 C11 -172.4(3) . . . . ?
C14 C8 C9 C10 179.6(3) . . . . ?
C7 C8 C9 C10 56.9(4) . . . . ?
C6 C5 C10 C9 19.1(5) . . . . ?
C4 C5 C10 C9 -163.1(3) . . . . ?
C6 C5 C10 C19 -104.0(4) . . . . ?
C4 C5 C10 C19 73.8(4) . . . . ?
C6 C5 C10 C1 138.7(4) . . . . ?
C4 C5 C10 C1 -43.5(4) . . . . ?
C11 C9 C10 C5 -175.0(3) . . . . ?
C8 C9 C10 C5 -46.3(4) . . . . ?
C11 C9 C10 C19 -53.8(4) . . . . ?
C8 C9 C10 C19 75.0(4) . . . . ?
C11 C9 C10 C1 65.0(4) . . . . ?
C8 C9 C10 C1 -166.2(3) . . . . ?
C2 C1 C10 C5 45.8(4) . . . . ?
C2 C1 C10 C9 166.5(3) . . . . ?
C2 C1 C10 C19 -72.1(4) . . . . ?
C10 C9 C11 C12 -178.2(3) . . . . ?
C8 C9 C11 C12 51.9(4) . . . . ?
C9 C11 C12 C13 -55.8(4) . . . . ?
C11 C12 C13 C14 54.9(4) . . . . ?
C11 C12 C13 C18 -67.4(4) . . . . ?
C11 C12 C13 C17 164.8(3) . . . . ?
C7 C8 C14 C15 -56.1(4) . . . . ?
C9 C8 C14 C15 -177.9(3) . . . . ?
C7 C8 C14 C13 177.9(3) . . . . ?
C9 C8 C14 C13 56.1(4) . . . . ?
C12 C13 C14 C8 -57.9(4) . . . . ?
C18 C13 C14 C8 63.3(4) . . . . ?
C17 C13 C14 C8 179.7(3) . . . . ?
C12 C13 C14 C15 169.0(3) . . . . ?
C18 C13 C14 C15 -69.8(4) . . . . ?
C17 C13 C14 C15 46.6(3) . . . . ?
C8 C14 C15 C16 -166.9(3) . . . . ?
C13 C14 C15 C16 -35.5(4) . . . . ?
C14 C15 C16 C17 9.5(4) . . . . ?
C15 C16 C17 C20 149.0(3) . . . . ?
C15 C16 C17 C13 19.3(4) . . . . ?
C12 C13 C17 C16 -153.9(3) . . . . ?
C14 C13 C17 C16 -39.7(3) . . . . ?
C18 C13 C17 C16 78.2(3) . . . . ?
C12 C13 C17 C20 81.4(4) . . . . ?
C14 C13 C17 C20 -164.4(3) . . . . ?
C18 C13 C17 C20 -46.5(4) . . . . ?
C16 C17 C20 C22 -176.4(3) . . . . ?
C13 C17 C20 C22 -55.4(4) . . . . ?
C16 C17 C20 C21 56.6(4) . . . . ?
C13 C17 C20 C21 177.7(3) . . . . ?
C21 C20 C22 S1 64.3(4) . . . . ?
C17 C20 C22 S1 -62.5(4) . . . . ?
C21 C20 C22 S2 -61.6(4) . . . . ?
C17 C20 C22 S2 171.6(3) . . . . ?
C23 S1 C22 C20 172.7(3) . . . . ?
C23 S1 C22 S2 -62.1(3) . . . . ?
C25 S2 C22 C20 -171.0(3) . . . . ?
C25 S2 C22 S1 63.2(3) . . . . ?
C22 S1 C23 C24 60.6(4) . . . . ?
S1 C23 C24 C25 -66.8(5) . . . . ?
C23 C24 C25 S2 66.0(5) . . . . ?
C22 S2 C25 C24 -60.7(3) . . . . ?
C3 O1 C26 O2 5.0(8) . . . . ?
C3 O1 C26 C27 -172.7(5) . . . . ?
C10' C1' C2' C3' -56.7(4) . . . . ?
C26' O1' C3' C4' -150.7(5) . . . . ?
C26' O1' C3' C2' 89.5(5) . . . . ?
C1' C2' C3' O1' -179.9(3) . . . . ?
C1' C2' C3' C4' 61.9(4) . . . . ?
O1' C3' C4' C5' -178.4(3) . . . . ?
C2' C3' C4' C5' -59.1(4) . . . . ?
C3' C4' C5' C6' -129.0(4) . . . . ?
C3' C4' C5' C10' 52.1(4) . . . . ?
C4' C5' C6' C7' 179.0(4) . . . . ?
C10' C5' C6' C7' -2.2(6) . . . . ?
C5' C6' C7' C8' 13.2(6) . . . . ?
C6' C7' C8' C14' -160.1(3) . . . . ?
C6' C7' C8' C9' -39.4(4) . . . . ?
C14' C8' C9' C11' -51.5(4) . . . . ?
C7' C8' C9' C11' -173.2(3) . . . . ?
C14' C8' C9' C10' 179.2(3) . . . . ?
C7' C8' C9' C10' 57.4(4) . . . . ?
C6' C5' C10' C19' -104.8(4) . . . . ?
C4' C5' C10' C19' 74.1(4) . . . . ?
C6' C5' C10' C9' 17.9(4) . . . . ?
C4' C5' C10' C9' -163.2(3) . . . . ?
C6' C5' C10' C1' 136.8(4) . . . . ?
C4' C5' C10' C1' -44.4(4) . . . . ?
C11' C9' C10' C5' -173.9(3) . . . . ?
C8' C9' C10' C5' -45.5(4) . . . . ?
C11' C9' C10' C19' -53.3(4) . . . . ?
C8' C9' C10' C19' 75.0(4) . . . . ?
C11' C9' C10' C1' 67.3(3) . . . . ?
C8' C9' C10' C1' -164.4(3) . . . . ?
C2' C1' C10' C5' 46.7(4) . . . . ?
C2' C1' C10' C19' -71.4(4) . . . . ?
C2' C1' C10' C9' 166.2(3) . . . . ?
C8' C9' C11' C12' 53.0(4) . . . . ?
C10' C9' C11' C12' -177.5(3) . . . . ?
C9' C11' C12' C13' -55.4(4) . . . . ?
C11' C12' C13' C18' -68.1(4) . . . . ?
C11' C12' C13' C14' 53.9(4) . . . . ?
C11' C12' C13' C17' 164.2(3) . . . . ?
C7' C8' C14' C15' -56.0(4) . . . . ?
C9' C8' C14' C15' -177.4(3) . . . . ?
C7' C8' C14' C13' 178.5(3) . . . . ?
C9' C8' C14' C13' 57.0(4) . . . . ?
C12' C13' C14' C8' -58.0(4) . . . . ?
C18' C13' C14' C8' 63.9(4) . . . . ?
C17' C13' C14' C8' 179.9(3) . . . . ?
C12' C13' C14' C15' 168.9(3) . . . . ?
C18' C13' C14' C15' -69.3(4) . . . . ?
C17' C13' C14' C15' 46.8(3) . . . . ?
C8' C14' C15' C16' -167.3(3) . . . . ?
C13' C14' C15' C16' -36.0(4) . . . . ?
C14' C15' C16' C17' 10.5(4) . . . . ?
C12' C13' C17' C20' 81.9(4) . . . . ?
C18' C13' C17' C20' -46.5(4) . . . . ?
C14' C13' C17' C20' -163.8(3) . . . . ?
C12' C13' C17' C16' -153.5(3) . . . . ?
C18' C13' C17' C16' 78.1(4) . . . . ?
C14' C13' C17' C16' -39.2(3) . . . . ?
C15' C16' C17' C13' 18.5(4) . . . . ?
C15' C16' C17' C20' 148.3(3) . . . . ?
C13' C17' C20' C22' -55.5(4) . . . . ?
C16' C17' C20' C22' -176.2(3) . . . . ?
C13' C17' C20' C21' 178.6(3) . . . . ?
C16' C17' C20' C21' 57.8(5) . . . . ?
C21' C20' C22' S1' 62.4(4) . . . . ?
C17' C20' C22' S1' -62.5(4) . . . . ?
C21' C20' C22' S2' -62.6(4) . . . . ?
C17' C20' C22' S2' 172.5(3) . . . . ?
C23' S1' C22' C20' 173.0(3) . . . . ?
C23' S1' C22' S2' -63.0(2) . . . . ?
C25' S2' C22' C20' -171.2(3) . . . . ?
C25' S2' C22' S1' 63.1(2) . . . . ?
C22' S1' C23' C24' 60.9(4) . . . . ?
S1' C23' C24' C25' -64.6(5) . . . . ?
C23' C24' C25' S2' 62.9(5) . . . . ?
C22' S2' C25' C24' -59.3(3) . . . . ?
C3' O1' C26' O2' -3.9(10) . . . . ?
C3' O1' C26' C27' -178.4(6) . . . . ?
C33 C28 C29 C30 5.0 . . . . ?
C28 C29 C30 C31 -6.86(15) . . . . ?
C29 C30 C31 C32 0.07(13) . . . . ?
C30 C31 C32 C33 7.6 . . . . ?
C31 C32 C33 C28 -9.80(8) . . . . ?
C29 C28 C33 C32 2.01(6) . . . . ?
C33' C28' C29' C30' 23(6) . . . . ?
C28' C29' C30' C31' -19(5) . . . . ?
C29' C30' C31' C32' 10(6) . . . . ?
C30' C31' C32' C33' -4(6) . . . . ?
C29' C28' C33' C32' -18(6) . . . . ?
C31' C32' C33' C28' 8(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.053


data_9
_database_code_depnum_ccdc_archive 'CCDC 240194'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
3 beta-tert-butyldimethylsilyloxy-(20R)-20-hydroxy-pregna-5-en-dithiane
;
_chemical_name_common            
;3 beta-tert-butyldimethylsilyloxy-(20R)-20-hydroxy-pregna-5-
en-dithiane
;
_chemical_melting_point          502
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H54 O2 S2 Si'
_chemical_formula_weight         550.95

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   6.287(4)
_cell_length_b                   41.68(3)
_cell_length_c                   6.537(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.537(11)
_cell_angle_gamma                90.00
_cell_volume                     1604.2(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    629
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      17.15

_exptl_crystal_description       'very thin needle'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9473
_exptl_absorpt_correction_T_max  0.9955
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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_device       'Bruker Smart APEX'
_diffrn_measurement_method       'phi and Omega Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11540
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_sigmaI/netI    0.2117
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5556
_reflns_number_gt                2058
_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    SHELXTL
_computing_publication_material  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^)+(0.0666P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(18)
_refine_ls_number_reflns         5556
_refine_ls_number_parameters     344
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.2387
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.1958
_refine_ls_wR_factor_gt          0.1439
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.007

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
Si1 Si 0.1120(4) -0.03475(5) 1.0845(4) 0.0707(8) Uani 1 1 d . . .
O1 O 0.7146(12) 0.24355(14) 0.5469(13) 0.099(2) Uani 1 1 d . . .
H1 H 0.7498 0.2609 0.5091 0.148 Uiso 1 1 calc R . .
O2 O 0.3148(9) -0.01116(12) 1.0717(10) 0.0791(18) Uani 1 1 d . . .
C1 C 0.4656(14) 0.07690(17) 1.1400(12) 0.060(2) Uani 1 1 d . . .
H1A H 0.3285 0.0852 1.1571 0.072 Uiso 1 1 calc R . .
H1B H 0.5937 0.0879 1.2445 0.072 Uiso 1 1 calc R . .
C2 C 0.4849(14) 0.04112(18) 1.1945(13) 0.071(3) Uani 1 1 d . . .
H2A H 0.6274 0.0329 1.1900 0.085 Uiso 1 1 calc R . .
H2B H 0.4832 0.0379 1.3409 0.085 Uiso 1 1 calc R . .
C3 C 0.2878(15) 0.02301(17) 1.0311(16) 0.066(3) Uani 1 1 d . . .
H3 H 0.1458 0.0300 1.0477 0.079 Uiso 1 1 calc R . .
C4 C 0.2742(15) 0.02938(19) 0.8018(14) 0.066(2) Uani 1 1 d . . .
H4A H 0.1377 0.0195 0.7018 0.080 Uiso 1 1 calc R . .
H4B H 0.4036 0.0195 0.7785 0.080 Uiso 1 1 calc R . .
C5 C 0.2707(14) 0.06510(19) 0.7504(13) 0.060(2) Uani 1 1 d . . .
C6 C 0.1221(14) 0.07735(19) 0.5704(14) 0.070(2) Uani 1 1 d . . .
H6 H 0.0147 0.0634 0.4793 0.084 Uiso 1 1 calc R . .
C7 C 0.1120(12) 0.11110(18) 0.5019(12) 0.052(2) Uani 1 1 d . . .
H7A H -0.0149 0.1215 0.5268 0.062 Uiso 1 1 calc R . .
H7B H 0.0845 0.1119 0.3464 0.062 Uiso 1 1 calc R . .
C8 C 0.3294(12) 0.12968(17) 0.6234(12) 0.0477(19) Uani 1 1 d . . .
H8 H 0.4482 0.1230 0.5673 0.057 Uiso 1 1 calc R . .
C9 C 0.4072(12) 0.12160(16) 0.8691(12) 0.049(2) Uani 1 1 d . . .
H9 H 0.2751 0.1257 0.9117 0.058 Uiso 1 1 calc R . .
C10 C 0.4593(13) 0.08477(16) 0.9109(13) 0.051(2) Uani 1 1 d . . .
C11 C 0.5941(13) 0.14329(17) 1.0134(12) 0.062(2) Uani 1 1 d . . .
H11A H 0.7374 0.1368 1.0013 0.074 Uiso 1 1 calc R . .
H11B H 0.6062 0.1403 1.1643 0.074 Uiso 1 1 calc R . .
C12 C 0.5546(13) 0.17955(17) 0.9553(13) 0.059(2) Uani 1 1 d . . .
H12A H 0.4275 0.1872 0.9935 0.071 Uiso 1 1 calc R . .
H12B H 0.6882 0.1916 1.0408 0.071 Uiso 1 1 calc R . .
C13 C 0.5060(13) 0.18562(17) 0.7135(12) 0.051(2) Uani 1 1 d . . .
C14 C 0.2947(11) 0.16539(17) 0.5925(11) 0.0441(19) Uani 1 1 d . . .
H14 H 0.1772 0.1714 0.6520 0.053 Uiso 1 1 calc R . .
C15 C 0.2183(14) 0.17800(17) 0.3597(12) 0.063(2) Uani 1 1 d . . .
H15A H 0.0575 0.1741 0.2845 0.076 Uiso 1 1 calc R . .
H15B H 0.3030 0.1679 0.2785 0.076 Uiso 1 1 calc R . .
C16 C 0.2678(14) 0.21398(18) 0.3855(13) 0.071(3) Uani 1 1 d . . .
H16A H 0.1276 0.2261 0.3455 0.085 Uiso 1 1 calc R . .
H16B H 0.3518 0.2208 0.2937 0.085 Uiso 1 1 calc R . .
C17 C 0.4112(12) 0.21900(16) 0.6298(12) 0.052(2) Uani 1 1 d . . .
H17 H 0.3014 0.2238 0.7012 0.062 Uiso 1 1 calc R . .
C18 C 0.7078(13) 0.17677(19) 0.6547(13) 0.070(2) Uani 1 1 d . . .
H18A H 0.8367 0.1892 0.7410 0.105 Uiso 1 1 calc R . .
H18B H 0.6761 0.1811 0.5026 0.105 Uiso 1 1 calc R . .
H18C H 0.7402 0.1544 0.6826 0.105 Uiso 1 1 calc R . .
C19 C 0.6829(13) 0.07608(18) 0.8854(14) 0.073(3) Uani 1 1 d . . .
H19A H 0.8064 0.0833 1.0110 0.110 Uiso 1 1 calc R . .
H19B H 0.6918 0.0862 0.7566 0.110 Uiso 1 1 calc R . .
H19C H 0.6920 0.0532 0.8723 0.110 Uiso 1 1 calc R . .
C20 C 0.5660(16) 0.2486(2) 0.6686(14) 0.069(3) Uani 1 1 d . A .
C21 C 0.7087(18) 0.2531(2) 0.9015(16) 0.119(4) Uani 1 1 d . . .
H21A H 0.8162 0.2359 0.9476 0.179 Uiso 1 1 calc R . .
H21B H 0.6138 0.2532 0.9889 0.179 Uiso 1 1 calc R . .
H21C H 0.7884 0.2731 0.9187 0.179 Uiso 1 1 calc R . .
C22 C 0.4292(15) 0.2795(2) 0.5726(14) 0.087(3) Uiso 1 1 d D . .
C26 C 0.0461(19) -0.0252(3) 1.3274(15) 0.128(4) Uani 1 1 d . . .
H26A H 0.1816 -0.0267 1.4542 0.192 Uiso 1 1 calc R . .
H26B H -0.0653 -0.0400 1.3405 0.192 Uiso 1 1 calc R . .
H26C H -0.0128 -0.0037 1.3155 0.192 Uiso 1 1 calc R . .
C27 C -0.1519(13) -0.0302(2) 0.8415(14) 0.094(3) Uani 1 1 d . . .
H27A H -0.1882 -0.0079 0.8159 0.141 Uiso 1 1 calc R . .
H27B H -0.2746 -0.0411 0.8672 0.141 Uiso 1 1 calc R . .
H27C H -0.1289 -0.0393 0.7160 0.141 Uiso 1 1 calc R . .
C28 C 0.2315(17) -0.07606(19) 1.1025(17) 0.078(3) Uani 1 1 d . . .
C29 C 0.2813(18) -0.0839(2) 0.8941(18) 0.130(5) Uani 1 1 d . . .
H29C H 0.4189 -0.0962 0.9315 0.195 Uiso 1 1 calc R . .
H29B H 0.2985 -0.0643 0.8241 0.195 Uiso 1 1 calc R . .
H29A H 0.1577 -0.0961 0.7965 0.195 Uiso 1 1 calc R . .
C30 C 0.0675(19) -0.1007(2) 1.131(2) 0.126(4) Uani 1 1 d . . .
H30A H 0.1267 -0.1218 1.1278 0.189 Uiso 1 1 calc R . .
H30B H -0.0764 -0.0985 1.0147 0.189 Uiso 1 1 calc R . .
H30C H 0.0478 -0.0973 1.2685 0.189 Uiso 1 1 calc R . .
C31 C 0.4531(19) -0.0775(3) 1.3009(19) 0.137(4) Uani 1 1 d . . .
H31A H 0.4184 -0.0772 1.4327 0.206 Uiso 1 1 calc R . .
H31B H 0.5458 -0.0593 1.2989 0.206 Uiso 1 1 calc R . .
H31C H 0.5335 -0.0968 1.2950 0.206 Uiso 1 1 calc R . .
S1A S 0.259(2) 0.2880(3) 0.749(2) 0.102(6) Uiso 0.33 1 d PD A 1
C23A C 0.025(5) 0.3185(8) 0.543(5) 0.090(10) Uiso 0.33 1 d PD A 1
C24A C 0.094(8) 0.3406(12) 0.471(9) 0.14(2) Uiso 0.33 1 d PD A 1
C25A C 0.318(6) 0.3413(6) 0.392(5) 0.069(9) Uiso 0.33 1 d PD A 1
S2A S 0.5674(18) 0.3136(3) 0.523(2) 0.098(4) Uiso 0.33 1 d P A 1
S1B S 0.204(2) 0.2879(2) 0.695(2) 0.049(3) Uiso 0.33 1 d PD A 2
C23B C 0.221(5) 0.3316(5) 0.686(4) 0.084(9) Uiso 0.33 1 d PD A 2
C24B C 0.173(7) 0.3396(8) 0.369(5) 0.092(12) Uiso 0.33 1 d PD A 2
C25B C 0.306(6) 0.3280(7) 0.296(5) 0.095(11) Uiso 0.33 1 d PD A 2
S2B S 0.3687(12) 0.2884(2) 0.3261(12) 0.089(2) Uiso 0.33 1 d PD A 2
S1C S 0.1822(16) 0.2889(2) 0.5927(16) 0.085(4) Uiso 0.33 1 d P A 3
C23C C 0.045(5) 0.3174(7) 0.395(5) 0.073(8) Uiso 0.33 1 d P A 3
C24C C 0.186(8) 0.3474(8) 0.478(7) 0.078(11) Uiso 0.33 1 d P A 3
C25C C 0.449(6) 0.3395(7) 0.384(5) 0.082(10) Uiso 0.33 1 d P A 3
S2C S 0.6112(16) 0.3149(2) 0.6186(17) 0.079(3) Uiso 0.33 1 d P A 3

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
Si1 0.0822(19) 0.0569(16) 0.0745(18) -0.0091(15) 0.0295(15) -0.0141(15)
O1 0.099(5) 0.081(5) 0.150(7) 0.003(5) 0.084(5) -0.015(4)
O2 0.061(4) 0.057(4) 0.103(5) 0.009(3) 0.008(3) -0.007(3)
C1 0.067(6) 0.043(5) 0.056(6) 0.001(4) 0.003(4) -0.007(4)
C2 0.084(7) 0.057(6) 0.054(5) 0.006(5) 0.002(5) 0.004(5)
C3 0.063(6) 0.030(5) 0.102(8) -0.003(5) 0.027(6) -0.008(4)
C4 0.065(6) 0.060(6) 0.063(6) -0.014(5) 0.009(5) -0.002(5)
C5 0.060(6) 0.056(6) 0.047(5) -0.011(4) -0.004(5) 0.005(5)
C6 0.053(6) 0.059(6) 0.072(6) -0.009(5) -0.011(5) -0.021(5)
C7 0.049(5) 0.055(5) 0.044(5) -0.003(4) 0.007(4) 0.002(4)
C8 0.036(5) 0.047(5) 0.053(5) -0.010(4) 0.008(4) -0.008(4)
C9 0.040(5) 0.039(5) 0.069(6) -0.018(4) 0.022(4) 0.000(4)
C10 0.052(6) 0.047(5) 0.048(5) -0.006(4) 0.009(4) 0.001(4)
C11 0.062(6) 0.041(5) 0.070(6) -0.005(4) 0.007(5) -0.001(4)
C12 0.054(5) 0.053(5) 0.066(6) -0.013(4) 0.015(4) 0.003(4)
C13 0.052(6) 0.052(5) 0.054(5) -0.005(4) 0.024(5) 0.005(4)
C14 0.022(4) 0.057(5) 0.050(5) -0.007(4) 0.007(4) 0.000(4)
C15 0.068(6) 0.052(5) 0.048(5) -0.006(4) -0.005(4) -0.010(4)
C16 0.084(7) 0.059(6) 0.066(6) 0.002(5) 0.021(5) 0.010(5)
C17 0.051(5) 0.036(5) 0.063(6) 0.007(4) 0.014(4) 0.004(4)
C18 0.054(6) 0.071(6) 0.091(6) -0.018(5) 0.032(5) 0.002(5)
C19 0.065(6) 0.042(5) 0.111(7) -0.013(5) 0.029(6) 0.005(5)
C20 0.073(7) 0.068(7) 0.069(7) 0.006(5) 0.029(6) -0.005(5)
C21 0.125(9) 0.091(8) 0.110(9) -0.014(7) 0.003(8) -0.060(7)
C26 0.180(12) 0.125(9) 0.091(8) -0.031(7) 0.063(8) -0.026(9)
C27 0.063(6) 0.114(8) 0.099(7) 0.002(7) 0.020(5) -0.012(6)
C28 0.086(7) 0.038(5) 0.108(8) -0.002(5) 0.031(7) -0.008(5)
C29 0.167(12) 0.090(9) 0.171(13) -0.023(8) 0.106(11) 0.003(8)
C30 0.145(10) 0.041(6) 0.199(13) -0.002(6) 0.070(10) -0.025(7)
C31 0.140(10) 0.085(9) 0.156(11) 0.035(8) 0.015(10) 0.017(8)

_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
Si1 O2 1.635(6) . ?
Si1 C26 1.820(9) . ?
Si1 C27 1.861(8) . ?
Si1 C28 1.866(9) . ?
O1 C20 1.439(9) . ?
O2 C3 1.448(8) . ?
C1 C10 1.520(9) . ?
C1 C2 1.528(9) . ?
C2 C3 1.522(10) . ?
C3 C4 1.495(10) . ?
C4 C5 1.525(10) . ?
C5 C6 1.321(9) . ?
C5 C10 1.519(10) . ?
C6 C7 1.471(10) . ?
C7 C8 1.528(9) . ?
C8 C14 1.508(9) . ?
C8 C9 1.543(9) . ?
C9 C11 1.520(9) . ?
C9 C10 1.573(9) . ?
C10 C19 1.516(9) . ?
C11 C12 1.557(10) . ?
C12 C13 1.522(9) . ?
C13 C18 1.495(9) . ?
C13 C17 1.537(9) . ?
C13 C14 1.538(9) . ?
C14 C15 1.520(9) . ?
C15 C16 1.529(10) . ?
C16 C17 1.548(9) . ?
C17 C20 1.537(10) . ?
C20 C21 1.483(11) . ?
C20 C22 1.555(11) . ?
C22 S2B 1.564(10) . ?
C22 S1C 1.650(12) . ?
C22 S2A 1.754(14) . ?
C22 S2C 1.825(13) . ?
C22 S1B 1.885(14) . ?
C22 S1A 1.859(15) . ?
C28 C30 1.511(11) . ?
C28 C29 1.536(11) . ?
C28 C31 1.536(11) . ?
S1A C23A 2.05(3) . ?
C23A C24A 1.18(4) . ?
C24A C25A 1.66(3) . ?
C25A S2A 1.89(3) . ?
S1B C23B 1.82(2) . ?
C23B C24B 2.02(3) . ?
C24B C25B 1.20(4) . ?
C25B S2B 1.70(3) . ?
S1C C23C 1.74(3) . ?
C23C C24C 1.52(5) . ?
C24C C25C 1.98(6) . ?
C25C S2C 1.83(3) . ?

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
O2 Si1 C26 109.5(4) . . ?
O2 Si1 C27 111.9(4) . . ?
C26 Si1 C27 108.3(5) . . ?
O2 Si1 C28 104.7(4) . . ?
C26 Si1 C28 111.0(5) . . ?
C27 Si1 C28 111.5(5) . . ?
C3 O2 Si1 123.9(5) . . ?
C10 C1 C2 114.4(6) . . ?
C3 C2 C1 110.0(6) . . ?
O2 C3 C4 108.7(7) . . ?
O2 C3 C2 110.2(7) . . ?
C4 C3 C2 111.2(7) . . ?
C3 C4 C5 112.7(6) . . ?
C6 C5 C10 122.9(7) . . ?
C6 C5 C4 121.6(7) . . ?
C10 C5 C4 115.3(7) . . ?
C5 C6 C7 125.6(7) . . ?
C6 C7 C8 113.0(6) . . ?
C14 C8 C7 111.7(6) . . ?
C14 C8 C9 109.5(6) . . ?
C7 C8 C9 109.2(6) . . ?
C11 C9 C8 114.2(6) . . ?
C11 C9 C10 113.8(6) . . ?
C8 C9 C10 111.4(6) . . ?
C19 C10 C1 110.6(6) . . ?
C19 C10 C5 108.9(6) . . ?
C1 C10 C5 108.0(6) . . ?
C19 C10 C9 111.0(6) . . ?
C1 C10 C9 108.3(6) . . ?
C5 C10 C9 110.0(6) . . ?
C9 C11 C12 113.8(6) . . ?
C13 C12 C11 111.8(6) . . ?
C18 C13 C12 110.3(6) . . ?
C18 C13 C17 113.0(6) . . ?
C12 C13 C17 115.6(6) . . ?
C18 C13 C14 113.0(6) . . ?
C12 C13 C14 105.4(6) . . ?
C17 C13 C14 99.0(6) . . ?
C8 C14 C15 117.1(6) . . ?
C8 C14 C13 114.5(6) . . ?
C15 C14 C13 103.8(6) . . ?
C14 C15 C16 104.4(6) . . ?
C15 C16 C17 105.6(6) . . ?
C20 C17 C13 121.6(6) . . ?
C20 C17 C16 112.6(6) . . ?
C13 C17 C16 104.9(6) . . ?
O1 C20 C21 108.0(8) . . ?
O1 C20 C17 106.7(7) . . ?
C21 C20 C17 113.0(7) . . ?
O1 C20 C22 105.8(7) . . ?
C21 C20 C22 111.1(8) . . ?
C17 C20 C22 111.8(7) . . ?
C20 C22 S2B 120.7(7) . . ?
C20 C22 S1C 124.6(8) . . ?
S2B C22 S1C 97.5(7) . . ?
C20 C22 S2A 120.5(7) . . ?
S2B C22 S2A 65.0(6) . . ?
S1C C22 S2A 111.2(7) . . ?
C20 C22 S2C 112.2(7) . . ?
S2B C22 S2C 83.8(6) . . ?
S1C C22 S2C 110.4(7) . . ?
S2A C22 S2C 18.8(4) . . ?
C20 C22 S1B 112.0(7) . . ?
S2B C22 S1B 116.4(7) . . ?
S1C C22 S1B 19.2(5) . . ?
S2A C22 S1B 114.9(7) . . ?
S2C C22 S1B 107.5(6) . . ?
C20 C22 S1A 105.3(7) . . ?
S2B C22 S1A 127.5(7) . . ?
S1C C22 S1A 31.2(5) . . ?
S2A C22 S1A 112.9(8) . . ?
S2C C22 S1A 102.0(7) . . ?
S1B C22 S1A 12.2(6) . . ?
C30 C28 C29 108.9(8) . . ?
C30 C28 C31 109.0(9) . . ?
C29 C28 C31 109.5(8) . . ?
C30 C28 Si1 110.9(7) . . ?
C29 C28 Si1 110.1(7) . . ?
C31 C28 Si1 108.3(7) . . ?
C22 S1A C23A 98.5(10) . . ?
C24A C23A S1A 118(3) . . ?
C25A C24A C23A 127(3) . . ?
C24A C25A S2A 120.4(19) . . ?
C22 S2A C25A 101.1(10) . . ?
C23B S1B C22 96.4(10) . . ?
S1B C23B C24B 102.0(14) . . ?
C25B C24B C23B 118(3) . . ?
C24B C25B S2B 121(3) . . ?
C22 S2B C25B 108.1(12) . . ?
C22 S1C C23C 109.8(12) . . ?
C24C C23C S1C 103(2) . . ?
C23C C24C C25C 102(3) . . ?
S2C C25C C24C 96.4(18) . . ?
C22 S2C C25C 100.5(12) . . ?

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
C26 Si1 O2 C3 -68.3(8) . . . . ?
C27 Si1 O2 C3 51.8(8) . . . . ?
C28 Si1 O2 C3 172.7(7) . . . . ?
C10 C1 C2 C3 -57.6(9) . . . . ?
Si1 O2 C3 C4 -105.4(8) . . . . ?
Si1 O2 C3 C2 132.6(6) . . . . ?
C1 C2 C3 O2 175.5(7) . . . . ?
C1 C2 C3 C4 55.0(9) . . . . ?
O2 C3 C4 C5 -173.9(7) . . . . ?
C2 C3 C4 C5 -52.5(9) . . . . ?
C3 C4 C5 C6 -132.7(9) . . . . ?
C3 C4 C5 C10 51.6(10) . . . . ?
C10 C5 C6 C7 -1.7(14) . . . . ?
C4 C5 C6 C7 -177.1(8) . . . . ?
C5 C6 C7 C8 16.2(12) . . . . ?
C6 C7 C8 C14 -165.8(7) . . . . ?
C6 C7 C8 C9 -44.6(8) . . . . ?
C14 C8 C9 C11 -46.1(8) . . . . ?
C7 C8 C9 C11 -168.6(6) . . . . ?
C14 C8 C9 C10 -176.7(6) . . . . ?
C7 C8 C9 C10 60.7(7) . . . . ?
C2 C1 C10 C19 -65.5(8) . . . . ?
C2 C1 C10 C5 53.6(9) . . . . ?
C2 C1 C10 C9 172.7(6) . . . . ?
C6 C5 C10 C19 -105.4(9) . . . . ?
C4 C5 C10 C19 70.2(8) . . . . ?
C6 C5 C10 C1 134.4(8) . . . . ?
C4 C5 C10 C1 -49.9(9) . . . . ?
C6 C5 C10 C9 16.4(11) . . . . ?
C4 C5 C10 C9 -167.9(6) . . . . ?
C11 C9 C10 C19 -55.9(8) . . . . ?
C8 C9 C10 C19 75.0(8) . . . . ?
C11 C9 C10 C1 65.7(7) . . . . ?
C8 C9 C10 C1 -163.4(6) . . . . ?
C11 C9 C10 C5 -176.5(6) . . . . ?
C8 C9 C10 C5 -45.6(8) . . . . ?
C8 C9 C11 C12 44.4(8) . . . . ?
C10 C9 C11 C12 173.8(6) . . . . ?
C9 C11 C12 C13 -51.8(8) . . . . ?
C11 C12 C13 C18 -63.9(8) . . . . ?
C11 C12 C13 C17 166.4(6) . . . . ?
C11 C12 C13 C14 58.3(8) . . . . ?
C7 C8 C14 C15 -59.2(9) . . . . ?
C9 C8 C14 C15 179.8(6) . . . . ?
C7 C8 C14 C13 179.1(6) . . . . ?
C9 C8 C14 C13 58.0(7) . . . . ?
C18 C13 C14 C8 56.1(9) . . . . ?
C12 C13 C14 C8 -64.4(7) . . . . ?
C17 C13 C14 C8 175.9(6) . . . . ?
C18 C13 C14 C15 -72.7(8) . . . . ?
C12 C13 C14 C15 166.8(6) . . . . ?
C17 C13 C14 C15 47.1(7) . . . . ?
C8 C14 C15 C16 -163.3(6) . . . . ?
C13 C14 C15 C16 -36.2(7) . . . . ?
C14 C15 C16 C17 10.3(8) . . . . ?
C18 C13 C17 C20 -49.5(10) . . . . ?
C12 C13 C17 C20 78.8(9) . . . . ?
C14 C13 C17 C20 -169.2(7) . . . . ?
C18 C13 C17 C16 79.7(8) . . . . ?
C12 C13 C17 C16 -152.0(7) . . . . ?
C14 C13 C17 C16 -40.1(7) . . . . ?
C15 C16 C17 C20 153.4(7) . . . . ?
C15 C16 C17 C13 19.1(8) . . . . ?
C13 C17 C20 O1 65.9(9) . . . . ?
C16 C17 C20 O1 -59.8(8) . . . . ?
C13 C17 C20 C21 -52.7(11) . . . . ?
C16 C17 C20 C21 -178.4(8) . . . . ?
C13 C17 C20 C22 -178.8(7) . . . . ?
C16 C17 C20 C22 55.4(9) . . . . ?
O1 C20 C22 S2B 31.7(10) . . . . ?
C21 C20 C22 S2B 148.7(8) . . . . ?
C17 C20 C22 S2B -84.1(9) . . . . ?
O1 C20 C22 S1C 158.1(8) . . . . ?
C21 C20 C22 S1C -84.9(11) . . . . ?
C17 C20 C22 S1C 42.3(11) . . . . ?
O1 C20 C22 S2A -45.6(10) . . . . ?
C21 C20 C22 S2A 71.4(10) . . . . ?
C17 C20 C22 S2A -161.4(7) . . . . ?
O1 C20 C22 S2C -64.4(8) . . . . ?
C21 C20 C22 S2C 52.6(9) . . . . ?
C17 C20 C22 S2C 179.8(7) . . . . ?
O1 C20 C22 S1B 174.6(7) . . . . ?
C21 C20 C22 S1B -68.4(10) . . . . ?
C17 C20 C22 S1B 58.8(9) . . . . ?
O1 C20 C22 S1A -174.6(7) . . . . ?
C21 C20 C22 S1A -57.6(9) . . . . ?
C17 C20 C22 S1A 69.7(8) . . . . ?
O2 Si1 C28 C30 176.2(7) . . . . ?
C26 Si1 C28 C30 58.2(9) . . . . ?
C27 Si1 C28 C30 -62.7(9) . . . . ?
O2 Si1 C28 C29 -63.2(7) . . . . ?
C26 Si1 C28 C29 178.8(7) . . . . ?
C27 Si1 C28 C29 58.0(8) . . . . ?
O2 Si1 C28 C31 56.6(8) . . . . ?
C26 Si1 C28 C31 -61.4(8) . . . . ?
C27 Si1 C28 C31 177.7(7) . . . . ?
C20 C22 S1A C23A -162.2(11) . . . . ?
S2B C22 S1A C23A -10.9(15) . . . . ?
S1C C22 S1A C23A -29.1(11) . . . . ?
S2A C22 S1A C23A 64.4(12) . . . . ?
S2C C22 S1A C23A 80.5(11) . . . . ?
S1B C22 S1A C23A -38(3) . . . . ?
C22 S1A C23A C24A -52(4) . . . . ?
S1A C23A C24A C25A 38(8) . . . . ?
C23A C24A C25A S2A -29(8) . . . . ?
C20 C22 S2A C25A 176.1(13) . . . . ?
S2B C22 S2A C25A 63.7(12) . . . . ?
S1C C22 S2A C25A -24.7(13) . . . . ?
S2C C22 S2A C25A -116(2) . . . . ?
S1B C22 S2A C25A -45.3(14) . . . . ?
S1A C22 S2A C25A -58.4(13) . . . . ?
C24A C25A S2A C22 35(4) . . . . ?
C20 C22 S1B C23B 146.4(10) . . . . ?
S2B C22 S1B C23B -68.9(12) . . . . ?
S1C C22 S1B C23B -79.0(18) . . . . ?
S2A C22 S1B C23B 4.3(12) . . . . ?
S2C C22 S1B C23B 22.8(11) . . . . ?
S1A C22 S1B C23B 88(3) . . . . ?
C22 S1B C23B C24B 54.5(17) . . . . ?
S1B C23B C24B C25B -60(4) . . . . ?
C23B C24B C25B S2B 52(5) . . . . ?
C20 C22 S2B C25B -160.6(15) . . . . ?
S1C C22 S2B C25B 61.4(15) . . . . ?
S2A C22 S2B C25B -48.6(14) . . . . ?
S2C C22 S2B C25B -48.4(15) . . . . ?
S1B C22 S2B C25B 58.0(16) . . . . ?
S1A C22 S2B C25B 52.0(17) . . . . ?
C24B C25B S2B C22 -50(4) . . . . ?
C20 C22 S1C C23C -160.8(12) . . . . ?
S2B C22 S1C C23C -25.0(13) . . . . ?
S2A C22 S1C C23C 41.1(14) . . . . ?
S2C C22 S1C C23C 61.1(13) . . . . ?
S1B C22 S1C C23C 146(2) . . . . ?
S1A C22 S1C C23C 140.5(15) . . . . ?
C22 S1C C23C C24C -71(3) . . . . ?
S1C C23C C24C C25C 79(2) . . . . ?
C23C C24C C25C S2C -84(2) . . . . ?
C20 C22 S2C C25C 151.6(13) . . . . ?
S2B C22 S2C C25C 30.9(13) . . . . ?
S1C C22 S2C C25C -64.8(14) . . . . ?
S2A C22 S2C C25C 31.4(18) . . . . ?
S1B C22 S2C C25C -84.9(13) . . . . ?
S1A C22 S2C C25C -96.2(13) . . . . ?
C24C C25C S2C C22 67.2(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.042