# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2012


#######################################################################
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#                                CCDC 
# 
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# 
#  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. 
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#  fide research purposes only. It may contain copyright material 
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data_TTFV-Dimer-TMS
_database_code_depnum_ccdc_archive 'CCDC 845793'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H38 S8 Si2, C H2 Cl2'
_chemical_formula_sum            'C35 H40 Cl2 S8 Si2'
_chemical_formula_weight         844.26

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'
Cl Cl 0.1484 0.1585 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.853(7)
_cell_length_b                   15.935(13)
_cell_length_c                   17.189(14)
_cell_angle_alpha                113.950(4)
_cell_angle_beta                 100.455(8)
_cell_angle_gamma                100.051(9)
_cell_volume                     2095(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    6218
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      29.8

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_process_details   'T. Higashi, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            17256
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         26.50
_reflns_number_total             8552
_reflns_number_gt                6444
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_structure_solution    'SHELXS-97 (Acta Cryst.2008, A64, 112-122)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'

_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^)+(0.1153P)^2^+2.8749P] 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         8552
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0834
_refine_ls_wR_factor_ref         0.2453
_refine_ls_wR_factor_gt          0.2162
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
Cl1 Cl 0.8891(3) 0.7320(3) 0.3048(3) 0.1573(13) Uani 1 1 d . . .
Cl2 Cl 0.9355(6) 0.5915(4) 0.1470(3) 0.2048(18) Uani 1 1 d . . .
S1 S 0.73358(16) 0.01489(9) 0.44826(8) 0.0479(3) Uani 1 1 d . . .
S2 S 0.68551(16) 0.20217(8) 0.48272(8) 0.0479(3) Uani 1 1 d . . .
S3 S 0.85231(14) 0.34488(8) 0.32702(8) 0.0482(3) Uani 1 1 d . . .
S4 S 1.01557(14) 0.23095(9) 0.39102(9) 0.0520(3) Uani 1 1 d . . .
S5 S 0.70357(18) 0.03039(13) 0.62366(10) 0.0638(4) Uani 1 1 d . . .
S6 S 0.6576(2) 0.24911(13) 0.66533(9) 0.0710(5) Uani 1 1 d . . .
S7 S 1.13810(17) 0.51864(10) 0.42149(10) 0.0621(4) Uani 1 1 d . . .
S8 S 1.32264(16) 0.38691(12) 0.48608(10) 0.0675(4) Uani 1 1 d . . .
Si1 Si 0.6299(2) -0.45448(11) -0.13121(10) 0.0605(4) Uani 1 1 d . . .
Si2 Si -0.19424(15) 0.17589(10) -0.00165(9) 0.0471(3) Uani 1 1 d . . .
C1 C 0.7081(6) 0.0829(4) 0.5522(3) 0.0479(11) Uani 1 1 d . . .
C2 C 0.6831(6) 0.1674(4) 0.5678(3) 0.0470(11) Uani 1 1 d . . .
C3 C 0.7066(5) 0.0956(3) 0.4045(3) 0.0392(9) Uani 1 1 d . . .
C4 C 0.7060(5) 0.0820(3) 0.3221(3) 0.0374(9) Uani 1 1 d . . .
C5 C 0.7007(5) 0.1644(3) 0.3020(3) 0.0375(9) Uani 1 1 d . . .
C6 C 0.8363(5) 0.2369(3) 0.3341(3) 0.0414(10) Uani 1 1 d . . .
C7 C 1.0496(6) 0.3997(3) 0.3937(3) 0.0466(11) Uani 1 1 d . . .
C8 C 1.1258(6) 0.3474(3) 0.4209(3) 0.0489(11) Uani 1 1 d . . .
C9 C 0.7041(5) -0.0090(3) 0.2483(3) 0.0378(9) Uani 1 1 d . . .
C10 C 0.6186(6) -0.0960(3) 0.2389(3) 0.0469(11) Uani 1 1 d . . .
H10 H 0.5632 -0.0976 0.2810 0.056 Uiso 1 1 calc R . .
C11 C 0.6135(6) -0.1800(3) 0.1690(3) 0.0477(11) Uani 1 1 d . . .
H11 H 0.5543 -0.2391 0.1630 0.057 Uiso 1 1 calc R . .
C12 C 0.6944(5) -0.1789(3) 0.1073(3) 0.0417(10) Uani 1 1 d . . .
C13 C 0.7775(5) -0.0926(3) 0.1139(3) 0.0431(10) Uani 1 1 d . . .
H13 H 0.8305 -0.0912 0.0710 0.052 Uiso 1 1 calc R . .
C14 C 0.7810(5) -0.0085(3) 0.1850(3) 0.0421(10) Uani 1 1 d . . .
H14 H 0.8377 0.0509 0.1904 0.050 Uiso 1 1 calc R . .
C15 C 0.6821(6) -0.2682(3) 0.0327(3) 0.0479(11) Uani 1 1 d . . .
C16 C 0.6655(6) -0.3436(4) -0.0295(3) 0.0515(12) Uani 1 1 d . . .
C17 C 0.5465(5) 0.1620(3) 0.2497(3) 0.0378(9) Uani 1 1 d . . .
C18 C 0.4039(6) 0.1156(3) 0.2571(3) 0.0483(11) Uani 1 1 d . . .
H18 H 0.4079 0.0837 0.2933 0.058 Uiso 1 1 calc R . .
C19 C 0.2571(6) 0.1157(4) 0.2120(3) 0.0487(11) Uani 1 1 d . . .
H19 H 0.1616 0.0855 0.2191 0.058 Uiso 1 1 calc R . .
C20 C 0.2484(5) 0.1596(3) 0.1566(3) 0.0451(10) Uani 1 1 d . . .
C21 C 0.3919(6) 0.2022(3) 0.1475(3) 0.0468(11) Uani 1 1 d . . .
H21 H 0.3887 0.2310 0.1087 0.056 Uiso 1 1 calc R . .
C22 C 0.5360(5) 0.2035(3) 0.1928(3) 0.0417(10) Uani 1 1 d . . .
H22 H 0.6311 0.2334 0.1853 0.050 Uiso 1 1 calc R . .
C23 C 0.0986(6) 0.1617(4) 0.1084(3) 0.0489(11) Uani 1 1 d . . .
C24 C -0.0178(6) 0.1681(4) 0.0667(3) 0.0517(12) Uani 1 1 d . . .
C25 C 0.8929(10) 0.0070(7) 0.6367(6) 0.103(3) Uani 1 1 d . . .
H25A H 0.8967 -0.0421 0.5802 0.124 Uiso 1 1 calc R . .
H25B H 0.9097 -0.0155 0.6820 0.124 Uiso 1 1 calc R . .
H25C H 0.9769 0.0657 0.6551 0.124 Uiso 1 1 calc R . .
C26 C 0.4676(11) 0.2602(7) 0.6281(5) 0.113(3) Uani 1 1 d . . .
H26A H 0.4701 0.2873 0.5862 0.136 Uiso 1 1 calc R . .
H26B H 0.4368 0.3025 0.6788 0.136 Uiso 1 1 calc R . .
H26C H 0.3897 0.1972 0.5986 0.136 Uiso 1 1 calc R . .
C27 C 1.4270(7) 0.3639(5) 0.4017(5) 0.092(2) Uani 1 1 d . . .
H27A H 1.4085 0.2948 0.3676 0.110 Uiso 1 1 calc R . .
H27B H 1.5417 0.3943 0.4299 0.110 Uiso 1 1 calc R . .
H27C H 1.3872 0.3900 0.3619 0.110 Uiso 1 1 calc R . .
C28 C 0.9852(7) 0.5511(4) 0.3673(4) 0.0709(17) Uani 1 1 d . . .
H28A H 0.9634 0.5146 0.3030 0.085 Uiso 1 1 calc R . .
H28B H 1.0199 0.6195 0.3845 0.085 Uiso 1 1 calc R . .
H28C H 0.8879 0.5370 0.3846 0.085 Uiso 1 1 calc R . .
C29 C 0.6179(13) -0.5539(5) -0.1040(5) 0.108(3) Uani 1 1 d . . .
H29A H 0.7189 -0.5433 -0.0622 0.130 Uiso 1 1 calc R . .
H29B H 0.5978 -0.6132 -0.1582 0.130 Uiso 1 1 calc R . .
H29C H 0.5304 -0.5586 -0.0769 0.130 Uiso 1 1 calc R . .
C30 C 0.4403(10) -0.4687(6) -0.2088(5) 0.106(3) Uani 1 1 d . . .
H30A H 0.3519 -0.4759 -0.1829 0.127 Uiso 1 1 calc R . .
H30B H 0.4202 -0.5255 -0.2652 0.127 Uiso 1 1 calc R . .
H30C H 0.4490 -0.4121 -0.2191 0.127 Uiso 1 1 calc R . .
C31 C 0.7890(9) -0.4414(5) -0.1833(5) 0.093(2) Uani 1 1 d . . .
H31A H 0.7930 -0.3860 -0.1952 0.111 Uiso 1 1 calc R . .
H31B H 0.7677 -0.4991 -0.2391 0.111 Uiso 1 1 calc R . .
H31C H 0.8916 -0.4319 -0.1434 0.111 Uiso 1 1 calc R . .
C32 C -0.3649(6) 0.0770(4) -0.0227(4) 0.0578(13) Uani 1 1 d . . .
H32A H -0.3395 0.0161 -0.0507 0.069 Uiso 1 1 calc R . .
H32B H -0.4596 0.0773 -0.0621 0.069 Uiso 1 1 calc R . .
H32C H -0.3861 0.0851 0.0336 0.069 Uiso 1 1 calc R . .
C33 C -0.1527(7) 0.1661(5) -0.1072(4) 0.0699(16) Uani 1 1 d . . .
H33A H -0.0503 0.2117 -0.0937 0.084 Uiso 1 1 calc R . .
H33B H -0.2381 0.1804 -0.1405 0.084 Uiso 1 1 calc R . .
H33C H -0.1478 0.1011 -0.1428 0.084 Uiso 1 1 calc R . .
C34 C -0.2295(7) 0.2942(4) 0.0572(4) 0.0642(15) Uani 1 1 d . . .
H34A H -0.2135 0.3105 0.1201 0.077 Uiso 1 1 calc R . .
H34B H -0.3393 0.2917 0.0312 0.077 Uiso 1 1 calc R . .
H34C H -0.1545 0.3428 0.0513 0.077 Uiso 1 1 calc R . .
C35 C 0.9298(14) 0.7041(11) 0.2064(9) 0.158(5) Uani 1 1 d . . .
H35A H 0.8486 0.7181 0.1692 0.190 Uiso 1 1 calc R . .
H35B H 1.0346 0.7476 0.2175 0.190 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
Cl1 0.111(2) 0.186(3) 0.244(4) 0.155(3) 0.056(2) 0.052(2)
Cl2 0.208(4) 0.238(5) 0.206(4) 0.125(4) 0.049(3) 0.099(4)
S1 0.0616(8) 0.0472(7) 0.0425(6) 0.0237(5) 0.0164(5) 0.0228(6)
S2 0.0622(8) 0.0409(6) 0.0388(6) 0.0149(5) 0.0144(5) 0.0174(5)
S3 0.0425(6) 0.0389(6) 0.0539(7) 0.0220(5) -0.0017(5) 0.0024(5)
S4 0.0395(6) 0.0494(7) 0.0640(8) 0.0294(6) 0.0020(5) 0.0087(5)
S5 0.0615(8) 0.0950(11) 0.0617(9) 0.0528(8) 0.0252(7) 0.0337(8)
S6 0.0850(11) 0.0817(11) 0.0395(7) 0.0146(7) 0.0190(7) 0.0375(9)
S7 0.0548(8) 0.0436(7) 0.0654(9) 0.0195(6) -0.0047(6) -0.0045(6)
S8 0.0437(7) 0.0740(10) 0.0652(9) 0.0284(7) -0.0087(6) 0.0020(7)
Si1 0.0664(10) 0.0412(8) 0.0562(9) 0.0056(6) 0.0196(7) 0.0113(7)
Si2 0.0345(6) 0.0560(8) 0.0493(7) 0.0253(6) 0.0055(5) 0.0115(6)
C1 0.043(2) 0.062(3) 0.038(2) 0.024(2) 0.0073(19) 0.014(2)
C2 0.050(3) 0.055(3) 0.037(2) 0.020(2) 0.011(2) 0.018(2)
C3 0.037(2) 0.035(2) 0.038(2) 0.0125(17) 0.0068(18) 0.0069(18)
C4 0.035(2) 0.038(2) 0.037(2) 0.0160(18) 0.0078(17) 0.0084(18)
C5 0.035(2) 0.041(2) 0.034(2) 0.0165(18) 0.0063(17) 0.0081(18)
C6 0.043(2) 0.039(2) 0.041(2) 0.0182(19) 0.0105(19) 0.0078(19)
C7 0.043(2) 0.048(3) 0.043(2) 0.020(2) 0.006(2) 0.006(2)
C8 0.043(2) 0.045(3) 0.046(3) 0.018(2) 0.002(2) 0.001(2)
C9 0.036(2) 0.041(2) 0.030(2) 0.0119(17) 0.0045(16) 0.0116(18)
C10 0.054(3) 0.047(3) 0.038(2) 0.017(2) 0.013(2) 0.014(2)
C11 0.055(3) 0.037(2) 0.042(2) 0.0138(19) 0.010(2) 0.005(2)
C12 0.044(2) 0.042(2) 0.036(2) 0.0159(19) 0.0065(18) 0.014(2)
C13 0.041(2) 0.044(2) 0.042(2) 0.0153(19) 0.0112(19) 0.015(2)
C14 0.041(2) 0.039(2) 0.041(2) 0.0153(19) 0.0081(18) 0.0099(19)
C15 0.053(3) 0.042(3) 0.050(3) 0.021(2) 0.015(2) 0.015(2)
C16 0.058(3) 0.045(3) 0.049(3) 0.019(2) 0.014(2) 0.016(2)
C17 0.036(2) 0.034(2) 0.032(2) 0.0075(16) 0.0024(16) 0.0069(17)
C18 0.046(3) 0.049(3) 0.054(3) 0.029(2) 0.010(2) 0.014(2)
C19 0.038(2) 0.049(3) 0.055(3) 0.025(2) 0.008(2) 0.004(2)
C20 0.040(2) 0.043(2) 0.043(2) 0.016(2) 0.0000(19) 0.012(2)
C21 0.045(3) 0.048(3) 0.041(2) 0.019(2) 0.0020(19) 0.009(2)
C22 0.037(2) 0.043(2) 0.038(2) 0.0176(19) 0.0043(18) 0.0022(19)
C23 0.042(3) 0.050(3) 0.046(3) 0.019(2) 0.001(2) 0.008(2)
C24 0.043(3) 0.055(3) 0.052(3) 0.024(2) 0.005(2) 0.009(2)
C25 0.103(6) 0.160(8) 0.129(7) 0.116(7) 0.057(5) 0.084(6)
C26 0.137(7) 0.118(7) 0.086(5) 0.024(5) 0.039(5) 0.088(6)
C27 0.045(3) 0.074(4) 0.101(5) -0.003(4) 0.014(3) -0.003(3)
C28 0.071(4) 0.040(3) 0.085(4) 0.024(3) 0.004(3) 0.007(3)
C29 0.186(9) 0.050(4) 0.088(5) 0.024(4) 0.052(6) 0.033(5)
C30 0.090(5) 0.079(5) 0.093(6) 0.001(4) -0.004(4) 0.020(4)
C31 0.100(5) 0.077(5) 0.077(5) 0.007(4) 0.038(4) 0.021(4)
C32 0.042(3) 0.058(3) 0.059(3) 0.016(3) 0.008(2) 0.010(2)
C33 0.059(3) 0.098(5) 0.064(4) 0.047(3) 0.017(3) 0.023(3)
C34 0.051(3) 0.061(3) 0.079(4) 0.031(3) 0.013(3) 0.017(3)
C35 0.139(9) 0.249(16) 0.202(13) 0.172(13) 0.080(9) 0.121(10)

_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
Cl1 C35 1.690(12) . ?
Cl2 C35 1.682(14) . ?
S1 C1 1.754(5) . ?
S1 C3 1.762(5) . ?
S2 C3 1.754(4) . ?
S2 C2 1.764(5) . ?
S3 C7 1.748(5) . ?
S3 C6 1.756(5) . ?
S4 C6 1.747(5) . ?
S4 C8 1.753(5) . ?
S5 C1 1.747(5) . ?
S5 C25 1.774(7) . ?
S6 C2 1.740(5) . ?
S6 C26 1.753(8) . ?
S7 C7 1.745(5) . ?
S7 C28 1.773(6) . ?
S8 C8 1.739(5) . ?
S8 C27 1.806(7) . ?
Si1 C29 1.816(8) . ?
Si1 C31 1.826(7) . ?
Si1 C16 1.838(5) . ?
Si1 C30 1.859(8) . ?
Si2 C24 1.833(5) . ?
Si2 C32 1.845(6) . ?
Si2 C34 1.857(6) . ?
Si2 C33 1.867(6) . ?
C1 C2 1.329(7) . ?
C3 C4 1.341(6) . ?
C4 C9 1.484(6) . ?
C4 C5 1.495(6) . ?
C5 C6 1.356(6) . ?
C5 C17 1.477(6) . ?
C7 C8 1.329(7) . ?
C9 C14 1.387(6) . ?
C9 C10 1.389(7) . ?
C10 C11 1.374(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.390(7) . ?
C12 C15 1.447(6) . ?
C13 C14 1.390(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.203(7) . ?
C17 C22 1.384(6) . ?
C17 C18 1.401(7) . ?
C18 C19 1.388(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.400(7) . ?
C20 C23 1.445(6) . ?
C21 C22 1.361(6) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.188(7) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 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
C1 S1 C3 96.6(2) . . ?
C3 S2 C2 96.8(2) . . ?
C7 S3 C6 95.9(2) . . ?
C6 S4 C8 96.3(2) . . ?
C1 S5 C25 102.1(3) . . ?
C2 S6 C26 101.9(3) . . ?
C7 S7 C28 103.4(3) . . ?
C8 S8 C27 100.5(3) . . ?
C29 Si1 C31 112.3(4) . . ?
C29 Si1 C16 109.2(3) . . ?
C31 Si1 C16 109.1(3) . . ?
C29 Si1 C30 111.8(5) . . ?
C31 Si1 C30 107.2(4) . . ?
C16 Si1 C30 107.1(3) . . ?
C24 Si2 C32 107.8(3) . . ?
C24 Si2 C34 109.3(3) . . ?
C32 Si2 C34 111.8(3) . . ?
C24 Si2 C33 108.2(3) . . ?
C32 Si2 C33 111.3(3) . . ?
C34 Si2 C33 108.3(3) . . ?
C2 C1 S5 125.2(4) . . ?
C2 C1 S1 117.4(4) . . ?
S5 C1 S1 117.2(3) . . ?
C1 C2 S6 126.6(4) . . ?
C1 C2 S2 116.5(4) . . ?
S6 C2 S2 116.9(3) . . ?
C4 C3 S2 121.5(4) . . ?
C4 C3 S1 126.1(3) . . ?
S2 C3 S1 112.4(3) . . ?
C3 C4 C9 125.6(4) . . ?
C3 C4 C5 117.2(4) . . ?
C9 C4 C5 117.2(4) . . ?
C6 C5 C17 124.5(4) . . ?
C6 C5 C4 118.1(4) . . ?
C17 C5 C4 117.4(4) . . ?
C5 C6 S4 121.2(4) . . ?
C5 C6 S3 125.6(4) . . ?
S4 C6 S3 113.2(2) . . ?
C8 C7 S7 122.9(4) . . ?
C8 C7 S3 117.4(4) . . ?
S7 C7 S3 119.7(3) . . ?
C7 C8 S8 125.1(4) . . ?
C7 C8 S4 116.8(4) . . ?
S8 C8 S4 118.1(3) . . ?
C14 C9 C10 118.7(4) . . ?
C14 C9 C4 120.6(4) . . ?
C10 C9 C4 120.6(4) . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C13 120.3(4) . . ?
C11 C12 C15 119.2(4) . . ?
C13 C12 C15 120.4(4) . . ?
C12 C13 C14 118.4(4) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C9 C14 C13 121.7(4) . . ?
C9 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C16 C15 C12 177.3(5) . . ?
C15 C16 Si1 174.4(5) . . ?
C22 C17 C18 118.0(4) . . ?
C22 C17 C5 122.8(4) . . ?
C18 C17 C5 119.3(4) . . ?
C19 C18 C17 120.8(5) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.6(4) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C21 117.8(4) . . ?
C19 C20 C23 122.7(4) . . ?
C21 C20 C23 119.6(4) . . ?
C22 C21 C20 121.6(5) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C21 C22 C17 121.2(4) . . ?
C21 C22 H22 119.4 . . ?
C17 C22 H22 119.4 . . ?
C24 C23 C20 174.8(6) . . ?
C23 C24 Si2 177.6(5) . . ?
S5 C25 H25A 109.5 . . ?
S5 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
S5 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
S6 C26 H26A 109.5 . . ?
S6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
S6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
S8 C27 H27A 109.5 . . ?
S8 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
S8 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
S7 C28 H28A 109.5 . . ?
S7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
S7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Si2 C33 H33A 109.5 . . ?
Si2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
Si2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si2 C34 H34A 109.5 . . ?
Si2 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
Si2 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Cl2 C35 Cl1 117.7(7) . . ?
Cl2 C35 H35A 107.9 . . ?
Cl1 C35 H35A 107.9 . . ?
Cl2 C35 H35B 107.9 . . ?
Cl1 C35 H35B 107.9 . . ?
H35A C35 H35B 107.2 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.092




data_6a
_database_code_depnum_ccdc_archive 'CCDC 888258'

_vrf_PLAT112_6a                  
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem...Y
RESPONSE: PLATON's ADDSYM did not suggest any change in
space group. PLATON's Space Group from Extinctions was
consistent with P-1, as used for this model.
;
_vrf_PLAT220_6a                  
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ...4.1 Ratio
RESPONSE: This is C31, which is a terminal S-methyl group.
A similarity restraint was applied here. This does not
indicate that an atom-type has been incorrectly assigned.
;
_vrf_PLAT094_6a                  
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....2.36
RESPONSE: From shelxl.lst:
Electron density synthesis with coefficients Fo-Fc

Highest peak 1.16 at 0.1219 0.1422 0.2811 [ 0.10 A from S3 ]
Deepest hole -0.49 at 0.4772 0.9614 0.2860 [ 0.87 A from S2 ]
;
_vrf_PLAT213_6a                  
;
PROBLEM: Atom C31 has ADP max/min Ratio ..... 3.2 prola
RESPONSE: C31 is a terminal S-methyl group.
A similarity restraint was applied here. This does not
indicate that an atom-type has been incorrectly assigned.
;
_vrf_PLAT242_6a                  
;
PROBLEM: Check Low Ueq as Compared to Neighbors for S7
RESPONSE: S7 is adjacent to the large, terminal methyl, C31
A similarity restraint was applied here. This does not
indicate that an atom-type has been incorrectly assigned.
;
_vrf_PLAT003_6a                  
;
PROBLEM: Number of Uiso or Uij Restrained Atom Sites ....2
RESPONSE: S7 is adjacent to the large, terminal methyl, C31
A similarity restraint was applied here. Please see
iucr_refine_instructions_details for more information.
;
_vrf_PLAT860_6a                  
;
PROBLEM: Note: Number of Least-Squares Restraints ....... 6
RESPONSE: S7 is adjacent to the large, terminal methyl, C31
A similarity restraint was applied here. Please see
iucr_refine_instructions_details for more information.

# end Validation Reply Form
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 S8'
_chemical_formula_sum            'C32 H26 S8'
_chemical_formula_weight         667.04

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'
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   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.433(8)
_cell_length_b                   12.641(8)
_cell_length_c                   12.954(8)
_cell_angle_alpha                66.52(3)
_cell_angle_beta                 73.94(2)
_cell_angle_gamma                83.87(3)
_cell_volume                     1505.8(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    4114
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      29.8

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_process_details   'T.Higashi, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      163(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            11348
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5514
_reflns_number_gt                3999
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_structure_solution    'SHELXS-97 (Acta Cryst.2008, A64, 112-122)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'

_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^)+(0.1620P)^2^+1.9725P] 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         5514
_refine_ls_number_parameters     365
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0987
_refine_ls_wR_factor_ref         0.3004
_refine_ls_wR_factor_gt          0.2593
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.090
_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 0.74679(15) 0.04293(13) 0.54583(12) 0.0532(4) Uani 1 1 d . . .
S2 S 0.54912(16) 0.09125(14) 0.73153(12) 0.0570(5) Uani 1 1 d . . .
S3 S 0.88568(17) -0.13787(15) 0.71239(16) 0.0649(5) Uani 1 1 d . . .
S4 S 0.6611(2) -0.08702(16) 0.92109(14) 0.0685(5) Uani 1 1 d . . .
S5 S 0.26181(15) 0.44333(13) 0.44935(12) 0.0522(4) Uani 1 1 d . . .
S6 S 0.43287(15) 0.37003(13) 0.26780(12) 0.0519(4) Uani 1 1 d . . .
S7 S 0.12604(19) 0.62781(16) 0.28265(18) 0.0713(6) Uani 1 1 d U . .
S8 S 0.32471(17) 0.55206(14) 0.07728(13) 0.0595(5) Uani 1 1 d . . .
C1 C 0.6037(5) 0.1235(5) 0.5820(5) 0.0476(13) Uani 1 1 d . . .
C2 C 0.7550(6) -0.0425(5) 0.6886(5) 0.0512(14) Uani 1 1 d . . .
C3 C 0.6642(6) -0.0207(5) 0.7739(5) 0.0543(15) Uani 1 1 d . . .
C4 C 0.5541(5) 0.2019(5) 0.4909(4) 0.0476(13) Uani 1 1 d . . .
C5 C 0.4450(6) 0.2778(5) 0.5050(4) 0.0452(12) Uani 1 1 d . . .
C6 C 0.3917(5) 0.3527(5) 0.4144(4) 0.0468(13) Uani 1 1 d . . .
C7 C 0.2439(5) 0.5165(5) 0.3089(5) 0.0481(13) Uani 1 1 d . . .
C8 C 0.3205(5) 0.4834(5) 0.2257(5) 0.0491(13) Uani 1 1 d . . .
C9 C 0.6321(5) 0.2106(5) 0.3715(4) 0.0426(12) Uani 1 1 d . . .
C10 C 0.6102(6) 0.1382(5) 0.3238(5) 0.0514(14) Uani 1 1 d . . .
H10 H 0.5408 0.0824 0.3652 0.062 Uiso 1 1 calc R . .
C11 C 0.6888(7) 0.1445(6) 0.2143(5) 0.0607(16) Uani 1 1 d . . .
H11 H 0.6727 0.0934 0.1817 0.073 Uiso 1 1 calc R . .
C12 C 0.7897(6) 0.2256(6) 0.1544(5) 0.0611(16) Uani 1 1 d . . .
H12 H 0.8416 0.2306 0.0797 0.073 Uiso 1 1 calc R . .
C13 C 0.8172(6) 0.2999(5) 0.2005(5) 0.0511(14) Uani 1 1 d . . .
C14 C 0.9243(6) 0.3812(6) 0.1427(5) 0.0609(17) Uani 1 1 d . . .
H14 H 0.9804 0.3848 0.0699 0.073 Uiso 1 1 calc R . .
C15 C 0.9476(7) 0.4533(6) 0.1895(6) 0.0672(18) Uani 1 1 d . . .
H15 H 1.0188 0.5074 0.1486 0.081 Uiso 1 1 calc R . .
C16 C 0.8692(6) 0.4494(5) 0.2958(5) 0.0558(15) Uani 1 1 d . . .
H16 H 0.8861 0.5010 0.3274 0.067 Uiso 1 1 calc R . .
C17 C 0.7670(5) 0.3711(5) 0.3558(5) 0.0496(13) Uani 1 1 d . . .
H17 H 0.7150 0.3680 0.4299 0.060 Uiso 1 1 calc R . .
C18 C 0.7372(5) 0.2954(5) 0.3105(4) 0.0462(13) Uani 1 1 d . . .
C19 C 0.3831(5) 0.2811(5) 0.6221(5) 0.0451(12) Uani 1 1 d . . .
C20 C 0.4349(6) 0.3513(5) 0.6579(5) 0.0531(14) Uani 1 1 d . . .
H20 H 0.5113 0.3967 0.6076 0.064 Uiso 1 1 calc R . .
C21 C 0.3788(7) 0.3585(5) 0.7668(5) 0.0640(17) Uani 1 1 d . . .
H21 H 0.4186 0.4063 0.7904 0.077 Uiso 1 1 calc R . .
C22 C 0.2672(7) 0.2964(6) 0.8379(5) 0.0645(18) Uani 1 1 d . . .
H22 H 0.2287 0.3016 0.9113 0.077 Uiso 1 1 calc R . .
C23 C 0.2073(6) 0.2241(5) 0.8042(5) 0.0561(16) Uani 1 1 d . . .
C24 C 0.0913(7) 0.1596(7) 0.8757(6) 0.077(2) Uani 1 1 d . . .
H24 H 0.0501 0.1650 0.9487 0.092 Uiso 1 1 calc R . .
C25 C 0.0375(8) 0.0899(7) 0.8418(7) 0.083(2) Uani 1 1 d . . .
H25 H -0.0414 0.0477 0.8912 0.100 Uiso 1 1 calc R . .
C26 C 0.0956(7) 0.0788(6) 0.7360(6) 0.074(2) Uani 1 1 d . . .
H26 H 0.0571 0.0291 0.7137 0.089 Uiso 1 1 calc R . .
C27 C 0.2087(6) 0.1403(5) 0.6643(5) 0.0565(15) Uani 1 1 d . . .
H27 H 0.2492 0.1317 0.5928 0.068 Uiso 1 1 calc R . .
C28 C 0.2665(5) 0.2165(5) 0.6947(5) 0.0491(13) Uani 1 1 d . . .
C29 C 0.9087(7) -0.1922(6) 0.6024(6) 0.0687(18) Uani 1 1 d . . .
H29A H 0.8231 -0.2197 0.6049 0.082 Uiso 1 1 calc R . .
H29B H 0.9722 -0.2562 0.6150 0.082 Uiso 1 1 calc R . .
H29C H 0.9436 -0.1308 0.5261 0.082 Uiso 1 1 calc R . .
C30 C 0.4962(8) -0.1529(7) 0.9850(6) 0.085(2) Uani 1 1 d . . .
H30A H 0.4283 -0.0926 0.9818 0.102 Uiso 1 1 calc R . .
H30B H 0.4887 -0.2048 1.0663 0.102 Uiso 1 1 calc R . .
H30C H 0.4826 -0.1969 0.9413 0.102 Uiso 1 1 calc R . .
C31 C 0.1370(14) 0.6923(11) 0.3701(12) 0.176(7) Uani 1 1 d U . .
H31A H 0.1261 0.6347 0.4496 0.211 Uiso 1 1 calc R . .
H31B H 0.0668 0.7505 0.3691 0.211 Uiso 1 1 calc R . .
H31C H 0.2245 0.7295 0.3428 0.211 Uiso 1 1 calc R . .
C32 C 0.3048(7) 0.4320(6) 0.0406(6) 0.0689(18) Uani 1 1 d . . .
H32A H 0.3881 0.3882 0.0358 0.083 Uiso 1 1 calc R . .
H32B H 0.2828 0.4610 -0.0347 0.083 Uiso 1 1 calc R . .
H32C H 0.2328 0.3816 0.1007 0.083 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 0.0468(8) 0.0604(9) 0.0434(8) -0.0137(7) -0.0121(6) 0.0133(7)
S2 0.0562(9) 0.0610(10) 0.0418(8) -0.0132(7) -0.0122(7) 0.0215(7)
S3 0.0617(10) 0.0688(11) 0.0738(11) -0.0314(9) -0.0365(9) 0.0274(8)
S4 0.0815(12) 0.0727(11) 0.0481(9) -0.0170(8) -0.0295(8) 0.0220(9)
S5 0.0504(9) 0.0604(9) 0.0443(8) -0.0199(7) -0.0165(6) 0.0177(7)
S6 0.0471(8) 0.0592(9) 0.0428(8) -0.0173(6) -0.0111(6) 0.0164(6)
S7 0.0712(11) 0.0697(11) 0.0935(13) -0.0418(10) -0.0495(10) 0.0335(9)
S8 0.0622(10) 0.0619(10) 0.0454(8) -0.0089(7) -0.0205(7) 0.0072(7)
C1 0.035(3) 0.053(3) 0.046(3) -0.010(2) -0.013(2) 0.008(2)
C2 0.053(3) 0.052(3) 0.049(3) -0.016(3) -0.021(3) 0.005(3)
C3 0.056(3) 0.058(4) 0.044(3) -0.015(3) -0.019(3) 0.019(3)
C4 0.041(3) 0.054(3) 0.039(3) -0.010(2) -0.010(2) 0.006(2)
C5 0.048(3) 0.043(3) 0.039(3) -0.010(2) -0.013(2) 0.004(2)
C6 0.042(3) 0.056(3) 0.040(3) -0.017(2) -0.013(2) 0.013(2)
C7 0.044(3) 0.044(3) 0.057(3) -0.017(3) -0.021(3) 0.011(2)
C8 0.045(3) 0.054(3) 0.043(3) -0.010(2) -0.019(2) 0.007(2)
C9 0.038(3) 0.046(3) 0.040(3) -0.014(2) -0.009(2) 0.007(2)
C10 0.054(3) 0.053(3) 0.049(3) -0.023(3) -0.015(3) 0.007(3)
C11 0.066(4) 0.071(4) 0.050(3) -0.030(3) -0.020(3) 0.020(3)
C12 0.059(4) 0.078(4) 0.042(3) -0.025(3) -0.011(3) 0.020(3)
C13 0.045(3) 0.058(3) 0.038(3) -0.012(2) -0.008(2) 0.016(3)
C14 0.051(3) 0.070(4) 0.034(3) 0.001(3) -0.001(2) 0.008(3)
C15 0.053(4) 0.078(5) 0.061(4) -0.013(3) -0.018(3) -0.006(3)
C16 0.047(3) 0.057(3) 0.055(3) -0.015(3) -0.008(3) -0.003(3)
C17 0.044(3) 0.054(3) 0.048(3) -0.021(3) -0.008(2) 0.007(2)
C18 0.032(3) 0.061(3) 0.036(3) -0.014(2) -0.006(2) 0.014(2)
C19 0.040(3) 0.053(3) 0.043(3) -0.017(2) -0.013(2) 0.005(2)
C20 0.054(3) 0.048(3) 0.052(3) -0.016(3) -0.016(3) 0.017(3)
C21 0.090(5) 0.050(3) 0.058(4) -0.025(3) -0.026(4) 0.009(3)
C22 0.086(5) 0.057(4) 0.048(3) -0.024(3) -0.018(3) 0.027(3)
C23 0.052(3) 0.057(4) 0.036(3) -0.005(2) -0.004(2) 0.024(3)
C24 0.060(4) 0.071(5) 0.059(4) -0.002(3) 0.004(3) 0.019(4)
C25 0.061(4) 0.080(5) 0.070(5) 0.008(4) -0.010(4) 0.000(4)
C26 0.062(4) 0.075(5) 0.070(4) -0.003(4) -0.025(4) -0.009(3)
C27 0.058(4) 0.060(4) 0.047(3) -0.011(3) -0.018(3) -0.003(3)
C28 0.041(3) 0.053(3) 0.045(3) -0.011(2) -0.014(2) 0.015(2)
C29 0.068(4) 0.063(4) 0.079(5) -0.033(4) -0.022(4) 0.015(3)
C30 0.093(6) 0.087(5) 0.064(4) -0.025(4) -0.013(4) 0.010(4)
C31 0.249(15) 0.162(11) 0.236(14) -0.155(11) -0.189(13) 0.160(11)
C32 0.061(4) 0.083(5) 0.061(4) -0.032(3) -0.010(3) 0.005(3)

_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 C2 1.752(6) . ?
S1 C1 1.777(6) . ?
S2 C1 1.746(6) . ?
S2 C3 1.769(6) . ?
S3 C2 1.730(6) . ?
S3 C29 1.765(7) . ?
S4 C3 1.743(6) . ?
S4 C30 1.819(8) . ?
S5 C7 1.735(6) . ?
S5 C6 1.759(6) . ?
S6 C6 1.754(5) . ?
S6 C8 1.760(6) . ?
S7 C31 1.669(10) . ?
S7 C7 1.757(6) . ?
S8 C8 1.756(6) . ?
S8 C32 1.808(7) . ?
C1 C4 1.393(7) . ?
C2 C3 1.342(8) . ?
C4 C5 1.428(8) . ?
C4 C9 1.501(7) . ?
C5 C6 1.396(7) . ?
C5 C19 1.491(7) . ?
C7 C8 1.337(8) . ?
C9 C10 1.358(8) . ?
C9 C18 1.440(8) . ?
C10 C11 1.405(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(9) . ?
C12 H12 0.9500 . ?
C13 C18 1.420(7) . ?
C13 C14 1.427(9) . ?
C14 C15 1.351(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.369(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.404(8) . ?
C17 H17 0.9500 . ?
C19 C20 1.366(8) . ?
C19 C28 1.413(8) . ?
C20 C21 1.405(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.359(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.417(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.406(9) . ?
C23 C28 1.419(8) . ?
C24 C25 1.354(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.369(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.415(8) . ?
C27 H27 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

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
C2 S1 C1 97.1(3) . . ?
C1 S2 C3 96.8(3) . . ?
C2 S3 C29 102.6(3) . . ?
C3 S4 C30 102.1(3) . . ?
C7 S5 C6 96.2(3) . . ?
C6 S6 C8 95.6(3) . . ?
C31 S7 C7 103.0(4) . . ?
C8 S8 C32 102.1(3) . . ?
C4 C1 S2 130.1(4) . . ?
C4 C1 S1 117.5(4) . . ?
S2 C1 S1 112.4(3) . . ?
C3 C2 S3 123.5(5) . . ?
C3 C2 S1 116.4(5) . . ?
S3 C2 S1 119.8(3) . . ?
C2 C3 S4 124.4(5) . . ?
C2 C3 S2 117.1(4) . . ?
S4 C3 S2 118.3(3) . . ?
C1 C4 C5 124.2(5) . . ?
C1 C4 C9 115.1(5) . . ?
C5 C4 C9 120.5(5) . . ?
C6 C5 C4 124.1(5) . . ?
C6 C5 C19 116.2(5) . . ?
C4 C5 C19 119.7(5) . . ?
C5 C6 S6 129.6(4) . . ?
C5 C6 S5 116.8(4) . . ?
S6 C6 S5 113.5(3) . . ?
C8 C7 S5 117.5(4) . . ?
C8 C7 S7 123.2(4) . . ?
S5 C7 S7 119.3(3) . . ?
C7 C8 S8 124.4(4) . . ?
C7 C8 S6 117.1(4) . . ?
S8 C8 S6 118.4(3) . . ?
C10 C9 C18 120.4(5) . . ?
C10 C9 C4 122.1(5) . . ?
C18 C9 C4 117.5(5) . . ?
C9 C10 C11 121.0(6) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 119.3(6) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 121.7(6) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C12 C13 C18 119.4(6) . . ?
C12 C13 C14 122.9(6) . . ?
C18 C13 C14 117.7(6) . . ?
C15 C14 C13 121.4(6) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 120.8(6) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 120.1(6) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 121.5(5) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C13 118.6(5) . . ?
C17 C18 C9 123.3(5) . . ?
C13 C18 C9 118.1(5) . . ?
C20 C19 C28 119.2(5) . . ?
C20 C19 C5 120.1(5) . . ?
C28 C19 C5 120.6(5) . . ?
C19 C20 C21 122.1(6) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C22 C21 C20 119.3(6) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 121.0(6) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 122.2(6) . . ?
C24 C23 C28 118.9(7) . . ?
C22 C23 C28 118.9(6) . . ?
C25 C24 C23 120.8(7) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 121.4(7) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C27 C26 C25 119.4(7) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 121.3(6) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C19 C28 C27 122.3(5) . . ?
C19 C28 C23 119.4(6) . . ?
C27 C28 C23 118.2(5) . . ?
S3 C29 H29A 109.5 . . ?
S3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
S3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
S4 C30 H30A 109.5 . . ?
S4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
S4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
S7 C31 H31A 109.5 . . ?
S7 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
S7 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
S8 C32 H32A 109.5 . . ?
S8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

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 S2 C1 C4 176.6(6) . . . . ?
C3 S2 C1 S1 -4.6(4) . . . . ?
C2 S1 C1 C4 -176.5(5) . . . . ?
C2 S1 C1 S2 4.5(4) . . . . ?
C29 S3 C2 C3 148.3(6) . . . . ?
C29 S3 C2 S1 -38.6(4) . . . . ?
C1 S1 C2 C3 -2.6(5) . . . . ?
C1 S1 C2 S3 -176.2(4) . . . . ?
S3 C2 C3 S4 -1.7(9) . . . . ?
S1 C2 C3 S4 -175.0(4) . . . . ?
S3 C2 C3 S2 173.0(3) . . . . ?
S1 C2 C3 S2 -0.3(7) . . . . ?
C30 S4 C3 C2 -121.9(6) . . . . ?
C30 S4 C3 S2 63.5(5) . . . . ?
C1 S2 C3 C2 3.1(6) . . . . ?
C1 S2 C3 S4 178.1(4) . . . . ?
S2 C1 C4 C5 2.6(9) . . . . ?
S1 C1 C4 C5 -176.1(5) . . . . ?
S2 C1 C4 C9 176.9(4) . . . . ?
S1 C1 C4 C9 -1.8(7) . . . . ?
C1 C4 C5 C6 -177.1(5) . . . . ?
C9 C4 C5 C6 8.9(9) . . . . ?
C1 C4 C5 C19 4.0(9) . . . . ?
C9 C4 C5 C19 -170.0(5) . . . . ?
C4 C5 C6 S6 3.7(9) . . . . ?
C19 C5 C6 S6 -177.4(4) . . . . ?
C4 C5 C6 S5 -177.4(5) . . . . ?
C19 C5 C6 S5 1.5(7) . . . . ?
C8 S6 C6 C5 -177.9(6) . . . . ?
C8 S6 C6 S5 3.2(4) . . . . ?
C7 S5 C6 C5 177.4(5) . . . . ?
C7 S5 C6 S6 -3.5(4) . . . . ?
C6 S5 C7 C8 2.6(5) . . . . ?
C6 S5 C7 S7 -178.3(3) . . . . ?
C31 S7 C7 C8 -143.0(8) . . . . ?
C31 S7 C7 S5 38.0(7) . . . . ?
S5 C7 C8 S8 -175.9(3) . . . . ?
S7 C7 C8 S8 5.1(8) . . . . ?
S5 C7 C8 S6 -0.8(7) . . . . ?
S7 C7 C8 S6 -179.8(3) . . . . ?
C32 S8 C8 C7 -130.4(6) . . . . ?
C32 S8 C8 S6 54.6(4) . . . . ?
C6 S6 C8 C7 -1.5(5) . . . . ?
C6 S6 C8 S8 173.9(4) . . . . ?
C1 C4 C9 C10 85.6(7) . . . . ?
C5 C4 C9 C10 -99.8(7) . . . . ?
C1 C4 C9 C18 -91.1(6) . . . . ?
C5 C4 C9 C18 83.5(7) . . . . ?
C18 C9 C10 C11 -0.3(9) . . . . ?
C4 C9 C10 C11 -176.9(5) . . . . ?
C9 C10 C11 C12 0.0(9) . . . . ?
C10 C11 C12 C13 1.1(9) . . . . ?
C11 C12 C13 C18 -2.0(9) . . . . ?
C11 C12 C13 C14 177.3(6) . . . . ?
C12 C13 C14 C15 179.3(6) . . . . ?
C18 C13 C14 C15 -1.4(9) . . . . ?
C13 C14 C15 C16 0.9(10) . . . . ?
C14 C15 C16 C17 0.5(10) . . . . ?
C15 C16 C17 C18 -1.5(9) . . . . ?
C16 C17 C18 C13 1.0(8) . . . . ?
C16 C17 C18 C9 178.9(5) . . . . ?
C12 C13 C18 C17 179.8(5) . . . . ?
C14 C13 C18 C17 0.4(8) . . . . ?
C12 C13 C18 C9 1.7(8) . . . . ?
C14 C13 C18 C9 -177.7(5) . . . . ?
C10 C9 C18 C17 -178.6(5) . . . . ?
C4 C9 C18 C17 -1.8(8) . . . . ?
C10 C9 C18 C13 -0.6(8) . . . . ?
C4 C9 C18 C13 176.2(5) . . . . ?
C6 C5 C19 C20 -92.6(7) . . . . ?
C4 C5 C19 C20 86.4(7) . . . . ?
C6 C5 C19 C28 84.2(7) . . . . ?
C4 C5 C19 C28 -96.9(7) . . . . ?
C28 C19 C20 C21 2.3(8) . . . . ?
C5 C19 C20 C21 179.1(5) . . . . ?
C19 C20 C21 C22 -1.9(9) . . . . ?
C20 C21 C22 C23 0.4(9) . . . . ?
C21 C22 C23 C24 -179.5(6) . . . . ?
C21 C22 C23 C28 0.5(9) . . . . ?
C22 C23 C24 C25 -179.0(6) . . . . ?
C28 C23 C24 C25 0.9(9) . . . . ?
C23 C24 C25 C26 0.6(11) . . . . ?
C24 C25 C26 C27 -0.5(11) . . . . ?
C25 C26 C27 C28 -1.1(10) . . . . ?
C20 C19 C28 C27 -178.7(5) . . . . ?
C5 C19 C28 C27 4.5(8) . . . . ?
C20 C19 C28 C23 -1.2(8) . . . . ?
C5 C19 C28 C23 -178.0(5) . . . . ?
C26 C27 C28 C19 -179.8(6) . . . . ?
C26 C27 C28 C23 2.6(9) . . . . ?
C24 C23 C28 C19 179.9(5) . . . . ?
C22 C23 C28 C19 -0.1(8) . . . . ?
C24 C23 C28 C27 -2.5(8) . . . . ?
C22 C23 C28 C27 177.4(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.118

_iucr_refine_instructions_details 
;
TITL _6a
CELL 0.71075 10.43300 12.64100 12.95400 66.520 73.940 83.870
ZERR 2 0.00800 0.00800 0.00800 0.030 0.020 0.030
LATT 1
SFAC C H S
UNIT 64 52 16
SHEL 8.147180 0.825472
L.S. 5
FMAP 2
PLAN -25
TEMP -110.0
CONF
BOND $H
ACTA
SIMU 0.05 0.1 1.7 S7 C31
SIZE 0.070 0.130 0.160
WGHT 0.162000 1.972500
FVAR 0.38266
S1 3 0.746788 0.042926 0.545835 11.00000 0.04679 0.06039 =
0.04337 -0.01368 -0.01207 0.01334
S2 3 0.549117 0.091250 0.731529 11.00000 0.05624 0.06095 =
0.04178 -0.01317 -0.01218 0.02146
S3 3 0.885679 -0.137867 0.712390 11.00000 0.06170 0.06879 =
0.07379 -0.03145 -0.03654 0.02744
S4 3 0.661115 -0.087025 0.921087 11.00000 0.08151 0.07265 =
0.04808 -0.01697 -0.02949 0.02200
S5 3 0.261811 0.443332 0.449353 11.00000 0.05035 0.06039 =
0.04426 -0.01990 -0.01653 0.01771
S6 3 0.432869 0.370028 0.267798 11.00000 0.04715 0.05921 =
0.04277 -0.01731 -0.01113 0.01637
S7 3 0.126041 0.627809 0.282653 11.00000 0.07123 0.06966 =
0.09348 -0.04175 -0.04947 0.03347
S8 3 0.324712 0.552058 0.077280 11.00000 0.06220 0.06190 =
0.04543 -0.00889 -0.02052 0.00717
C1 1 0.603670 0.123533 0.582047 11.00000 0.03510 0.05337 =
0.04572 -0.01047 -0.01332 0.00796
C2 1 0.755015 -0.042482 0.688606 11.00000 0.05341 0.05169 =
0.04851 -0.01561 -0.02076 0.00547
C3 1 0.664224 -0.020687 0.773896 11.00000 0.05606 0.05810 =
0.04422 -0.01536 -0.01930 0.01862
C4 1 0.554062 0.201932 0.490904 11.00000 0.04104 0.05412 =
0.03858 -0.00993 -0.01038 0.00557
C5 1 0.445038 0.277776 0.504981 11.00000 0.04782 0.04315 =
0.03924 -0.00980 -0.01326 0.00369
C6 1 0.391684 0.352742 0.414387 11.00000 0.04187 0.05559 =
0.04008 -0.01669 -0.01321 0.01255
C7 1 0.243917 0.516533 0.308890 11.00000 0.04428 0.04388 =
0.05679 -0.01721 -0.02139 0.01090
C8 1 0.320544 0.483386 0.225693 11.00000 0.04523 0.05372 =
0.04299 -0.00982 -0.01928 0.00745
C9 1 0.632076 0.210618 0.371522 11.00000 0.03761 0.04615 =
0.03955 -0.01404 -0.00907 0.00678
C10 1 0.610243 0.138172 0.323844 11.00000 0.05403 0.05321 =
0.04939 -0.02299 -0.01473 0.00735
AFIX 43
H10 2 0.540786 0.082404 0.365232 11.00000 -1.20000
AFIX 0
C11 1 0.688817 0.144465 0.214253 11.00000 0.06637 0.07132 =
0.05003 -0.03044 -0.02047 0.01996
AFIX 43
H11 2 0.672705 0.093420 0.181654 11.00000 -1.20000
AFIX 0
C12 1 0.789697 0.225610 0.154423 11.00000 0.05883 0.07839 =
0.04232 -0.02546 -0.01119 0.01971
AFIX 43
H12 2 0.841626 0.230627 0.079712 11.00000 -1.20000
AFIX 0
C13 1 0.817170 0.299922 0.200514 11.00000 0.04492 0.05794 =
0.03815 -0.01153 -0.00826 0.01623
C14 1 0.924288 0.381248 0.142743 11.00000 0.05092 0.06953 =
0.03389 0.00068 -0.00133 0.00768
AFIX 43
H14 2 0.980425 0.384778 0.069858 11.00000 -1.20000
AFIX 0
C15 1 0.947566 0.453322 0.189490 11.00000 0.05303 0.07797 =
0.06068 -0.01316 -0.01755 -0.00562
AFIX 43
H15 2 1.018824 0.507385 0.148600 11.00000 -1.20000
AFIX 0
C16 1 0.869175 0.449351 0.295784 11.00000 0.04685 0.05712 =
0.05479 -0.01539 -0.00827 -0.00273
AFIX 43
H16 2 0.886085 0.500958 0.327432 11.00000 -1.20000
AFIX 0
C17 1 0.766958 0.371133 0.355838 11.00000 0.04373 0.05422 =
0.04766 -0.02054 -0.00795 0.00668
AFIX 43
H17 2 0.714976 0.368023 0.429889 11.00000 -1.20000
AFIX 0
C18 1 0.737194 0.295407 0.310491 11.00000 0.03248 0.06062 =
0.03631 -0.01442 -0.00638 0.01412
C19 1 0.383051 0.281100 0.622075 11.00000 0.03996 0.05253 =
0.04262 -0.01749 -0.01332 0.00452
C20 1 0.434908 0.351324 0.657915 11.00000 0.05391 0.04778 =
0.05205 -0.01615 -0.01581 0.01656
AFIX 43
H20 2 0.511348 0.396748 0.607603 11.00000 -1.20000
AFIX 0
C21 1 0.378840 0.358533 0.766784 11.00000 0.08967 0.04985 =
0.05849 -0.02465 -0.02552 0.00853
AFIX 43
H21 2 0.418569 0.406347 0.790446 11.00000 -1.20000
AFIX 0
C22 1 0.267188 0.296416 0.837913 11.00000 0.08600 0.05745 =
0.04763 -0.02371 -0.01799 0.02657
AFIX 43
H22 2 0.228712 0.301561 0.911337 11.00000 -1.20000
AFIX 0
C23 1 0.207329 0.224111 0.804194 11.00000 0.05177 0.05740 =
0.03561 -0.00509 -0.00352 0.02431
C24 1 0.091266 0.159582 0.875724 11.00000 0.05977 0.07133 =
0.05943 -0.00227 0.00439 0.01939
AFIX 43
H24 2 0.050091 0.164951 0.948677 11.00000 -1.20000
AFIX 0
C25 1 0.037521 0.089872 0.841794 11.00000 0.06121 0.07957 =
0.06964 0.00765 -0.01011 -0.00009
AFIX 43
H25 2 -0.041409 0.047652 0.891174 11.00000 -1.20000
AFIX 0
C26 1 0.095613 0.078809 0.735961 11.00000 0.06160 0.07484 =
0.06989 -0.00336 -0.02485 -0.00859
AFIX 43
H26 2 0.057074 0.029057 0.713732 11.00000 -1.20000
AFIX 0
C27 1 0.208715 0.140295 0.664338 11.00000 0.05754 0.05956 =
0.04683 -0.01055 -0.01837 -0.00332
AFIX 43
H27 2 0.249225 0.131660 0.592840 11.00000 -1.20000
AFIX 0
C28 1 0.266531 0.216501 0.694686 11.00000 0.04130 0.05261 =
0.04453 -0.01126 -0.01386 0.01450
C29 1 0.908698 -0.192190 0.602355 11.00000 0.06790 0.06348 =
0.07870 -0.03279 -0.02236 0.01526
AFIX 137
H29A 2 0.823095 -0.219672 0.604883 11.00000 -1.20000
H29B 2 0.972189 -0.256207 0.614988 11.00000 -1.20000
H29C 2 0.943589 -0.130847 0.526109 11.00000 -1.20000
AFIX 0
C30 1 0.496167 -0.152916 0.985006 11.00000 0.09298 0.08726 =
0.06433 -0.02477 -0.01298 0.00997
AFIX 137
H30A 2 0.428320 -0.092573 0.981839 11.00000 -1.20000
H30B 2 0.488740 -0.204821 1.066290 11.00000 -1.20000
H30C 2 0.482577 -0.196853 0.941325 11.00000 -1.20000
AFIX 0
C31 1 0.136969 0.692299 0.370056 11.00000 0.24882 0.16184 =
0.23573 -0.15460 -0.18867 0.16006
AFIX 137
H31A 2 0.126083 0.634707 0.449633 11.00000 -1.20000
H31B 2 0.066785 0.750508 0.369077 11.00000 -1.20000
H31C 2 0.224457 0.729544 0.342774 11.00000 -1.20000
AFIX 0
C32 1 0.304817 0.431982 0.040580 11.00000 0.06135 0.08316 =
0.06111 -0.03190 -0.00967 0.00480
AFIX 137
H32A 2 0.388147 0.388224 0.035846 11.00000 -1.20000
H32B 2 0.282769 0.461006 -0.034740 11.00000 -1.20000
H32C 2 0.232752 0.381643 0.100745 11.00000 -1.20000
HKLF 4

REM _6a
REM R1 = 0.0987 for 3999 Fo > 4sig(Fo) and 0.1235 for all 5514 data
REM 365 parameters refined using 6 restraints

END

WGHT 0.1622 1.9653
REM Highest difference peak 1.159, deepest hole -0.491, 1-sigma level 0.118
Q1 1 0.5893 0.1378 0.7344 11.00000 0.05 0.98
Q2 1 0.7200 -0.0400 0.9072 11.00000 0.05 0.84
Q3 1 0.1015 0.6125 0.3479 11.00000 0.05 0.72
Q4 1 0.9214 -0.0975 0.6679 11.00000 0.05 0.68
Q5 1 0.6781 0.0461 0.9657 11.00000 0.05 0.65
Q6 1 0.2667 0.5968 0.1005 11.00000 0.05 0.58
Q7 1 0.2206 0.7253 0.2906 11.00000 0.05 0.55
Q8 1 0.1011 0.6979 0.3885 11.00000 0.05 0.55
Q9 1 0.0599 0.5593 0.3346 11.00000 0.05 0.50
Q10 1 0.5845 0.2003 0.4362 11.00000 0.05 0.47
Q11 1 0.3431 0.2384 0.6645 11.00000 0.05 0.44
Q12 1 0.2012 0.2622 0.9000 11.00000 0.05 0.43
Q13 1 0.2373 0.1568 0.6210 11.00000 0.05 0.41
Q14 1 0.8992 0.3382 0.0986 11.00000 0.05 0.40
Q15 1 0.7958 -0.0073 0.6779 11.00000 0.05 0.40
Q16 1 0.7335 0.0188 0.7463 11.00000 0.05 0.39
Q17 1 0.1225 0.0653 0.7224 11.00000 0.05 0.39
Q18 1 0.8946 0.4062 0.2477 11.00000 0.05 0.38
Q19 1 0.5934 0.1401 0.5534 11.00000 0.05 0.37
Q20 1 0.8009 0.2489 0.1015 11.00000 0.05 0.37
Q21 1 0.3797 0.3480 0.6643 11.00000 0.05 0.36
Q22 1 0.7746 0.2244 0.1806 11.00000 0.05 0.35
Q23 1 0.7328 0.2034 0.1649 11.00000 0.05 0.34
Q24 1 1.0040 0.3286 0.0890 11.00000 0.05 0.34
Q25 1 0.3028 0.3304 0.7803 11.00000 0.05 0.33
;


data_6b
_database_code_depnum_ccdc_archive 'CCDC 888259'
#TrackingRef 'Combined.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 S8'
_chemical_formula_sum            'C32 H26 S8'
_chemical_formula_weight         667.04

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'
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   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   20.472(8)
_cell_length_b                   9.432(3)
_cell_length_c                   15.900(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.519(5)
_cell_angle_gamma                90.00
_cell_volume                     3064.4(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    163(2)
_cell_measurement_reflns_used    4291
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      29.8

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_process_details   'T. Higashi, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      163(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 14.63
_diffrn_reflns_number            20685
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.46
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3517
_reflns_number_gt                3380
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'

_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^)+(0.0910P)^2^+3.3572P] 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         3517
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1647
_refine_ls_wR_factor_gt          0.1624
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.182
_refine_ls_shift/su_max          0.002
_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 0.39872(3) 0.96945(7) 0.19556(4) 0.0371(2) Uani 1 1 d . . .
S2 S 0.36841(3) 0.88297(7) 0.36632(4) 0.0362(2) Uani 1 1 d . . .
S3 S 0.27156(4) 1.12842(9) 0.16566(5) 0.0513(2) Uani 1 1 d . . .
S4 S 0.23495(3) 1.01615(8) 0.35318(4) 0.0428(2) Uani 1 1 d . . .
C1 C 0.42418(11) 0.8735(2) 0.28689(14) 0.0313(5) Uani 1 1 d . . .
C2 C 0.32294(11) 1.0215(3) 0.22973(15) 0.0347(5) Uani 1 1 d . . .
C3 C 0.30877(11) 0.9795(3) 0.30731(15) 0.0352(5) Uani 1 1 d . . .
C4 C 0.48148(10) 0.8022(2) 0.28924(13) 0.0309(5) Uani 1 1 d . . .
C5 C 0.51102(10) 0.7299(2) 0.36566(14) 0.0316(5) Uani 1 1 d . . .
C6 C 0.50708(11) 0.7832(3) 0.44571(14) 0.0337(5) Uani 1 1 d . . .
H6 H 0.4824 0.8670 0.4534 0.040 Uiso 1 1 calc R . .
C7 C 0.53884(11) 0.7164(3) 0.51727(14) 0.0336(5) Uani 1 1 d . . .
C8 C 0.53640(13) 0.7726(3) 0.59955(15) 0.0410(5) Uani 1 1 d . . .
H8 H 0.5120 0.8564 0.6085 0.049 Uiso 1 1 calc R . .
C9 C 0.56928(15) 0.7064(3) 0.66656(17) 0.0482(7) Uani 1 1 d . . .
H9 H 0.5670 0.7446 0.7216 0.058 Uiso 1 1 calc R . .
C10 C 0.60599(14) 0.5841(3) 0.65501(17) 0.0486(7) Uani 1 1 d . . .
H10 H 0.6290 0.5408 0.7019 0.058 Uiso 1 1 calc R . .
C11 C 0.60897(13) 0.5262(3) 0.57611(18) 0.0435(6) Uani 1 1 d . . .
H11 H 0.6336 0.4422 0.5690 0.052 Uiso 1 1 calc R . .
C12 C 0.57558(11) 0.5905(3) 0.50489(15) 0.0353(5) Uani 1 1 d . . .
C13 C 0.57807(11) 0.5353(3) 0.42241(15) 0.0376(5) Uani 1 1 d . . .
H13 H 0.6010 0.4494 0.4138 0.045 Uiso 1 1 calc R . .
C14 C 0.54790(11) 0.6040(3) 0.35485(15) 0.0346(5) Uani 1 1 d . . .
H14 H 0.5516 0.5670 0.2998 0.041 Uiso 1 1 calc R . .
C15 C 0.3085(3) 1.1226(7) 0.0690(2) 0.129(3) Uani 1 1 d . . .
H15A H 0.3503 1.1737 0.0740 0.155 Uiso 1 1 calc R . .
H15B H 0.2796 1.1672 0.0253 0.155 Uiso 1 1 calc R . .
H15C H 0.3164 1.0237 0.0537 0.155 Uiso 1 1 calc R . .
C16 C 0.24673(18) 1.1998(4) 0.3843(2) 0.0627(9) Uani 1 1 d . . .
H16A H 0.2865 1.2082 0.4215 0.075 Uiso 1 1 calc R . .
H16B H 0.2090 1.2322 0.4140 0.075 Uiso 1 1 calc R . .
H16C H 0.2511 1.2584 0.3340 0.075 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 0.0321(3) 0.0472(4) 0.0326(3) 0.0071(2) 0.0071(2) 0.0069(2)
S2 0.0299(3) 0.0473(4) 0.0322(3) 0.0053(2) 0.0083(2) 0.0046(2)
S3 0.0428(4) 0.0643(5) 0.0467(4) 0.0102(3) 0.0007(3) 0.0179(3)
S4 0.0287(3) 0.0546(4) 0.0460(4) -0.0027(3) 0.0100(3) 0.0044(2)
C1 0.0269(10) 0.0388(12) 0.0285(10) 0.0010(8) 0.0044(8) -0.0025(8)
C2 0.0292(11) 0.0390(12) 0.0358(12) -0.0010(9) 0.0017(9) 0.0030(9)
C3 0.0275(10) 0.0429(13) 0.0355(12) 0.0005(9) 0.0053(9) 0.0036(9)
C4 0.0271(10) 0.0363(11) 0.0296(11) -0.0013(9) 0.0054(8) -0.0022(8)
C5 0.0253(9) 0.0372(11) 0.0327(11) 0.0014(9) 0.0045(8) -0.0021(8)
C6 0.0331(11) 0.0359(12) 0.0320(11) 0.0022(9) 0.0019(9) -0.0007(9)
C7 0.0300(10) 0.0387(12) 0.0320(11) 0.0018(9) 0.0008(8) -0.0064(9)
C8 0.0446(13) 0.0441(13) 0.0339(12) -0.0016(10) 0.0004(10) -0.0054(11)
C9 0.0510(15) 0.0588(17) 0.0338(13) 0.0034(11) -0.0043(11) -0.0141(13)
C10 0.0412(13) 0.0606(17) 0.0430(14) 0.0180(13) -0.0065(11) -0.0080(12)
C11 0.0346(12) 0.0483(15) 0.0475(14) 0.0143(11) 0.0009(10) -0.0003(10)
C12 0.0251(10) 0.0415(12) 0.0392(12) 0.0060(10) 0.0023(9) -0.0048(9)
C13 0.0306(11) 0.0406(13) 0.0423(14) 0.0030(10) 0.0072(10) 0.0028(9)
C14 0.0284(10) 0.0408(13) 0.0350(12) -0.0018(9) 0.0060(9) 0.0039(9)
C15 0.169(5) 0.179(6) 0.0404(19) 0.034(3) 0.021(2) 0.122(5)
C16 0.0650(19) 0.0573(18) 0.068(2) -0.0150(16) 0.0257(16) 0.0066(15)

_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 C2 1.745(2) . ?
S1 C1 1.763(2) . ?
S2 C3 1.749(2) . ?
S2 C1 1.756(2) . ?
S3 C2 1.741(2) . ?
S3 C15 1.755(4) . ?
S4 C3 1.752(2) . ?
S4 C16 1.814(3) . ?
C1 C4 1.351(3) . ?
C2 C3 1.344(4) . ?
C4 C5 1.489(3) . ?
C4 C4 1.499(4) 2_655 ?
C5 C6 1.376(3) . ?
C5 C14 1.423(3) . ?
C6 C7 1.423(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.415(3) . ?
C7 C12 1.425(3) . ?
C8 C9 1.375(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.422(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.415(3) . ?
C13 C14 1.369(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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
C2 S1 C1 96.39(11) . . ?
C3 S2 C1 95.97(11) . . ?
C2 S3 C15 102.52(16) . . ?
C3 S4 C16 101.43(14) . . ?
C4 C1 S2 127.39(18) . . ?
C4 C1 S1 119.40(17) . . ?
S2 C1 S1 113.20(13) . . ?
C3 C2 S3 123.4(2) . . ?
C3 C2 S1 116.68(19) . . ?
S3 C2 S1 119.83(14) . . ?
C2 C3 S2 117.56(19) . . ?
C2 C3 S4 124.3(2) . . ?
S2 C3 S4 118.09(14) . . ?
C1 C4 C5 124.0(2) . . ?
C1 C4 C4 117.4(2) . 2_655 ?
C5 C4 C4 118.6(2) . 2_655 ?
C6 C5 C14 118.6(2) . . ?
C6 C5 C4 122.9(2) . . ?
C14 C5 C4 118.4(2) . . ?
C5 C6 C7 121.9(2) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 122.2(2) . . ?
C8 C7 C12 119.3(2) . . ?
C6 C7 C12 118.5(2) . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 121.0(3) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 120.2(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.8(3) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 122.6(2) . . ?
C13 C12 C7 118.9(2) . . ?
C11 C12 C7 118.5(2) . . ?
C14 C13 C12 120.8(2) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C5 121.2(2) . . ?
C13 C14 H14 119.4 . . ?
C5 C14 H14 119.4 . . ?
S3 C15 H15A 109.5 . . ?
S3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
S3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
S4 C16 H16A 109.5 . . ?
S4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

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 S2 C1 C4 -175.2(2) . . . . ?
C3 S2 C1 S1 4.30(15) . . . . ?
C2 S1 C1 C4 176.0(2) . . . . ?
C2 S1 C1 S2 -3.52(15) . . . . ?
C15 S3 C2 C3 -170.7(3) . . . . ?
C15 S3 C2 S1 12.0(3) . . . . ?
C1 S1 C2 C3 1.0(2) . . . . ?
C1 S1 C2 S3 178.49(15) . . . . ?
S3 C2 C3 S2 -175.42(14) . . . . ?
S1 C2 C3 S2 2.0(3) . . . . ?
S3 C2 C3 S4 4.1(4) . . . . ?
S1 C2 C3 S4 -178.47(14) . . . . ?
C1 S2 C3 C2 -3.8(2) . . . . ?
C1 S2 C3 S4 176.57(15) . . . . ?
C16 S4 C3 C2 -77.5(3) . . . . ?
C16 S4 C3 S2 102.08(19) . . . . ?
S2 C1 C4 C5 -7.0(4) . . . . ?
S1 C1 C4 C5 173.58(17) . . . . ?
S2 C1 C4 C4 175.88(15) . . . 2_655 ?
S1 C1 C4 C4 -3.6(3) . . . 2_655 ?
C1 C4 C5 C6 -36.3(3) . . . . ?
C4 C4 C5 C6 140.83(19) 2_655 . . . ?
C1 C4 C5 C14 147.1(2) . . . . ?
C4 C4 C5 C14 -35.8(3) 2_655 . . . ?
C14 C5 C6 C7 0.2(3) . . . . ?
C4 C5 C6 C7 -176.4(2) . . . . ?
C5 C6 C7 C8 178.3(2) . . . . ?
C5 C6 C7 C12 -0.1(3) . . . . ?
C6 C7 C8 C9 -178.3(2) . . . . ?
C12 C7 C8 C9 0.1(4) . . . . ?
C7 C8 C9 C10 0.6(4) . . . . ?
C8 C9 C10 C11 -1.1(4) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 179.2(2) . . . . ?
C10 C11 C12 C7 -0.1(4) . . . . ?
C8 C7 C12 C13 -179.7(2) . . . . ?
C6 C7 C12 C13 -1.2(3) . . . . ?
C8 C7 C12 C11 -0.4(3) . . . . ?
C6 C7 C12 C11 178.1(2) . . . . ?
C11 C12 C13 C14 -176.8(2) . . . . ?
C7 C12 C13 C14 2.5(3) . . . . ?
C12 C13 C14 C5 -2.4(4) . . . . ?
C6 C5 C14 C13 1.1(3) . . . . ?
C4 C5 C14 C13 177.8(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.077

_iucr_refine_instructions_details 
;
TITL _6b
CELL 0.71075 20.47200 9.43200 15.90000 90.000 93.519 90.000
ZERR 4 0.00800 0.00300 0.00600 0.000 0.005 0.000
LATT 7
SYMM -X, +Y, .50-Z
SFAC C H S
UNIT 128 104 32
SHEL 8.147180 0.769629
OMIT -2 0 2
L.S. 5
FMAP 2
PLAN -25
BOND $H
CONF
LIST 4
TEMP -110.0
ACTA
SIZE 0.070 0.140 0.163
WGHT 0.091000 3.357200
FVAR 0.33507
S1 3 0.398723 0.969446 0.195558 11.00000 0.03210 0.04720 =
0.03257 0.00707 0.00710 0.00687
S2 3 0.368408 0.882974 0.366322 11.00000 0.02991 0.04729 =
0.03220 0.00532 0.00833 0.00457
S3 3 0.271557 1.128420 0.165661 11.00000 0.04276 0.06430 =
0.04667 0.01025 0.00067 0.01789
S4 3 0.234952 1.016149 0.353180 11.00000 0.02875 0.05459 =
0.04599 -0.00273 0.00998 0.00440
C1 1 0.424179 0.873482 0.286886 11.00000 0.02694 0.03883 =
0.02848 0.00102 0.00441 -0.00246
C2 1 0.322937 1.021451 0.229733 11.00000 0.02923 0.03904 =
0.03582 -0.00102 0.00165 0.00304
C3 1 0.308769 0.979509 0.307312 11.00000 0.02753 0.04293 =
0.03548 0.00052 0.00531 0.00355
C4 1 0.481477 0.802151 0.289241 11.00000 0.02714 0.03631 =
0.02955 -0.00127 0.00542 -0.00221
C5 1 0.511024 0.729876 0.365660 11.00000 0.02530 0.03719 =
0.03268 0.00143 0.00452 -0.00205
C6 1 0.507075 0.783201 0.445707 11.00000 0.03310 0.03594 =
0.03200 0.00221 0.00194 -0.00070
AFIX 43
H6 2 0.482438 0.867047 0.453428 11.00000 -1.20000
AFIX 0
C7 1 0.538841 0.716357 0.517272 11.00000 0.02997 0.03875 =
0.03196 0.00176 0.00081 -0.00636
C8 1 0.536404 0.772631 0.599546 11.00000 0.04462 0.04411 =
0.03395 -0.00162 0.00037 -0.00545
AFIX 43
H8 2 0.511988 0.856365 0.608484 11.00000 -1.20000
AFIX 0
C9 1 0.569281 0.706419 0.666562 11.00000 0.05100 0.05884 =
0.03377 0.00336 -0.00434 -0.01415
AFIX 43
H9 2 0.566961 0.744553 0.721598 11.00000 -1.20000
AFIX 0
C10 1 0.605990 0.584135 0.655014 11.00000 0.04120 0.06058 =
0.04296 0.01799 -0.00653 -0.00801
AFIX 43
H10 2 0.629018 0.540763 0.701913 11.00000 -1.20000
AFIX 0
C11 1 0.608965 0.526216 0.576113 11.00000 0.03460 0.04832 =
0.04748 0.01427 0.00085 -0.00033
AFIX 43
H11 2 0.633618 0.442193 0.569018 11.00000 -1.20000
AFIX 0
C12 1 0.575579 0.590522 0.504891 11.00000 0.02508 0.04154 =
0.03921 0.00604 0.00229 -0.00480
C13 1 0.578074 0.535286 0.422413 11.00000 0.03062 0.04056 =
0.04233 0.00299 0.00716 0.00283
AFIX 43
H13 2 0.600984 0.449417 0.413811 11.00000 -1.20000
AFIX 0
C14 1 0.547899 0.603991 0.354849 11.00000 0.02836 0.04081 =
0.03503 -0.00175 0.00597 0.00391
AFIX 43
H14 2 0.551642 0.566985 0.299783 11.00000 -1.20000
AFIX 0
C15 1 0.308518 1.122584 0.068994 11.00000 0.16918 0.17862 =
0.04036 0.03443 0.02102 0.12205
AFIX 137
H15A 2 0.350256 1.173679 0.074049 11.00000 -1.20000
H15B 2 0.279577 1.167156 0.025275 11.00000 -1.20000
H15C 2 0.316356 1.023659 0.053684 11.00000 -1.20000
AFIX 0
C16 1 0.246731 1.199818 0.384262 11.00000 0.06502 0.05729 =
0.06846 -0.01504 0.02574 0.00658
AFIX 137
H16A 2 0.286479 1.208188 0.421535 11.00000 -1.20000
H16B 2 0.208952 1.232160 0.414044 11.00000 -1.20000
H16C 2 0.251127 1.258360 0.334003 11.00000 -1.20000
HKLF 4

REM _6b
REM R1 = 0.0568 for 3380 Fo > 4sig(Fo) and 0.0586 for all 3517 data
REM 183 parameters refined using 0 restraints

END

WGHT 0.0907 3.3791
REM Highest difference peak 0.826, deepest hole -0.559, 1-sigma level 0.077
Q1 1 0.5336 0.5325 0.2345 11.00000 0.05 0.48
Q2 1 0.5028 0.6204 0.4109 11.00000 0.05 0.36
Q3 1 0.6312 0.8358 0.6324 11.00000 0.05 0.33
Q4 1 0.3977 1.0968 0.2029 11.00000 0.05 0.33
Q5 1 0.4010 1.2682 0.1849 11.00000 0.05 0.32
Q6 1 0.3513 1.0142 0.2176 11.00000 0.05 0.32
Q7 1 0.3205 1.1439 0.0632 11.00000 0.05 0.32
Q8 1 0.3361 1.0286 0.0416 11.00000 0.05 0.29
Q9 1 0.5030 0.9738 0.6161 11.00000 0.05 0.29
Q10 1 0.5305 0.8773 0.7117 11.00000 0.05 0.28
Q11 1 0.2770 1.0768 0.0660 11.00000 0.05 0.28
Q12 1 0.5199 0.7391 0.4852 11.00000 0.05 0.28
Q13 1 0.6193 0.6897 0.3236 11.00000 0.05 0.27
Q14 1 0.6277 0.4606 0.4243 11.00000 0.05 0.27
Q15 1 0.3003 1.1856 0.1672 11.00000 0.05 0.25
Q16 1 0.2712 1.0611 0.1276 11.00000 0.05 0.25
Q17 1 0.3674 1.0608 0.3732 11.00000 0.05 0.24
Q18 1 0.2732 1.2511 0.1513 11.00000 0.05 0.24
Q19 1 0.6011 0.3747 0.3274 11.00000 0.05 0.24
Q20 1 0.2430 0.9665 0.2773 11.00000 0.05 0.23
Q21 1 0.3042 1.0285 -0.0099 11.00000 0.05 0.23
Q22 1 0.5601 0.9610 0.5370 11.00000 0.05 0.23
Q23 1 0.4016 0.7890 0.1928 11.00000 0.05 0.22
Q24 1 0.1999 0.8849 0.0248 11.00000 0.05 0.22
Q25 1 0.5346 0.8982 0.4294 11.00000 0.05 0.22
;