# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

# 1. SUBMISSION DETAILS

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Evans, P. Andrew'
_publ_contact_author_address     
;
Department of Chemistry
800 E. Kirkwood Ave
Bloomington, IN 47405-7108
USA
;
_publ_contact_author_phone       '001 812 855 7368'
_publ_contact_author_fax         '001 812 855 8300'
_publ_contact_author_email       paevans@indiana.edu

loop_
_publ_author_name
_publ_author_address
P.A.Evans
; Department of Chemistry
800 E. Kirkwood Ave
Bloomington, IN 47405-7108
USA
;
J.Sawyer
; Department of Chemistry
800 E. Kirkwood Ave
Bloomington, IN 47405-7108
USA
;
K.W.Lai
; Department of Chemistry
800 E. Kirkwood Ave
Bloomington, IN 47405-7108
USA
;
J.C.Huffman
; Department of Chemistry
800 E. Kirkwood Ave
Bloomington, IN 47405-7108
USA
;

_publ_section_title              
;
Intermolecular rhodium-catalyzed [2+2+2]
carbocyclization reactions of 1,6-enynes with symmetrical and
unsymmetrical alkynes
;

data_05060
_database_code_depnum_ccdc_archive 'CCDC 269096'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H21 N O4 S'
_chemical_formula_weight         347.42

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'
N N 0.0061 0.0033 '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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c '

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

_cell_length_a                   5.9474(8)
_cell_length_b                   19.586(2)
_cell_length_c                   14.4749(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.260(4)
_cell_angle_gamma                90.00
_cell_volume                     1672.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    119(2)
_cell_measurement_reflns_used    1139
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      26.82

_exptl_crystal_description       wedge
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      119(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_details      
' 0.30 degree frames measured for 5.17 seconds each'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_detector_area_resol_mean 44.52
_diffrn_standards_decay_%        0.0

_diffrn_reflns_number            9109
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         27.55
_reflns_number_total             3854
_reflns_number_gt                2166
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1999)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local program)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0521P)^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_number_reflns         3854
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1242
_refine_ls_wR_factor_gt          0.1090
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_restrained_S_all      0.868
_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
S15 S 0.10210(11) 0.65696(3) 0.70162(5) 0.0411(2) Uani 1 1 d . A 1
O12 O 0.8589(5) 0.37647(12) 0.99652(16) 0.0878(10) Uani 1 1 d . A 1
O13 O 1.1158(3) 0.36187(9) 0.90045(11) 0.0408(5) Uani 1 1 d . A 1
O16 O 0.0898(4) 0.66990(10) 0.60339(13) 0.0609(7) Uani 1 1 d . A 1
O17 O -0.1000(3) 0.64936(9) 0.74433(16) 0.0558(6) Uani 1 1 d . A 1
N6 N 0.2461(3) 0.58645(10) 0.71976(15) 0.0361(5) Uani 1 1 d . A 1
C1 C 0.8487(4) 0.43352(12) 0.76377(16) 0.0301(5) Uani 1 1 d . A 1
C2 C 0.7324(4) 0.47956(11) 0.69300(16) 0.0272(5) Uani 1 1 d . A 1
C3 C 0.8162(5) 0.48317(14) 0.60055(19) 0.0353(6) Uani 1 1 d . A 1
C4 C 0.5626(4) 0.51657(12) 0.71750(17) 0.0335(6) Uani 1 1 d . A 1
C5 C 0.4310(5) 0.57198(13) 0.66342(19) 0.0355(6) Uani 1 1 d . A 1
C7 C 0.3126(5) 0.56305(13) 0.8164(2) 0.0392(7) Uani 1 1 d . A 1
C8 C 0.4613(8) 0.5005(3) 0.8092(2) 0.0348(14) Uani 0.747(13) 1 d P A 1
C8A C 0.534(2) 0.5337(7) 0.8123(6) 0.022(3) Uiso 0.253(13) 1 d P A 2
C9 C 0.6297(7) 0.47986(19) 0.8821(2) 0.0673(12) Uani 1 1 d . A 1
C10 C 0.8038(4) 0.43290(11) 0.85178(17) 0.0305(6) Uani 1 1 d . A 1
C11 C 0.9266(5) 0.38855(12) 0.92348(18) 0.0378(6) Uani 1 1 d . A 1
C14 C 1.2425(5) 0.31812(16) 0.9689(2) 0.0400(7) Uani 1 1 d . A 1
C18 C 0.2618(4) 0.72199(11) 0.76236(16) 0.0271(5) Uani 1 1 d . A 1
C19 C 0.4430(5) 0.75066(12) 0.72520(19) 0.0336(6) Uani 1 1 d . A 1
C20 C 0.5804(5) 0.79683(12) 0.7766(2) 0.0364(6) Uani 1 1 d . A 1
C21 C 0.5389(4) 0.81574(11) 0.86537(17) 0.0313(6) Uani 1 1 d . A 1
C22 C 0.6953(6) 0.86538(15) 0.9213(3) 0.0472(8) Uani 1 1 d . A 1
C23 C 0.3552(5) 0.78743(12) 0.90151(18) 0.0312(6) Uani 1 1 d . A 1
C24 C 0.2166(4) 0.74041(12) 0.85045(18) 0.0308(6) Uani 1 1 d . A 1
H25 H 0.963(5) 0.4005(13) 0.7442(17) 0.049(8) Uiso 1 1 d . B 1
H26 H 0.822(4) 0.4364(12) 0.5743(16) 0.034(7) Uiso 1 1 d . C 1
H27 H 0.721(5) 0.5113(13) 0.5572(19) 0.048(8) Uiso 1 1 d . D 1
H28 H 0.965(6) 0.5011(16) 0.604(2) 0.074(11) Uiso 1 1 d . E 1
H29 H 0.364(5) 0.5583(12) 0.5996(19) 0.047(7) Uiso 1 1 d . F 1
H30 H 0.528(4) 0.6119(12) 0.6573(16) 0.034(7) Uiso 1 1 d . G 1
H31 H 0.375(6) 0.5983(16) 0.851(2) 0.066(10) Uiso 1 1 d . H 1
H32 H 0.192(6) 0.5544(16) 0.845(2) 0.075(11) Uiso 1 1 d . I 1
H33 H 0.375(5) 0.4540(16) 0.807(2) 0.029(9) Uiso 0.747(13) 1 d P A 1
H33A H 0.647(13) 0.569(4) 0.829(5) 0.007(19) Uiso 0.253(13) 1 d P A 2
H34 H 0.579(4) 0.4664(12) 0.9395(18) 0.035(7) Uiso 1 1 d . J 1
H35 H 0.704(10) 0.530(3) 0.898(4) 0.18(2) Uiso 1 1 d . K 1
H36 H 1.231(5) 0.3344(14) 1.026(2) 0.055(9) Uiso 1 1 d . L 1
H37 H 1.406(6) 0.3179(13) 0.9511(19) 0.056(9) Uiso 1 1 d . M 1
H38 H 1.165(5) 0.2729(15) 0.968(2) 0.059(9) Uiso 1 1 d . N 1
H39 H 0.471(5) 0.7366(12) 0.6653(19) 0.046(8) Uiso 1 1 d . O 1
H40 H 0.712(5) 0.8149(12) 0.7522(17) 0.039(7) Uiso 1 1 d . P 1
H41 H 0.857(8) 0.8531(19) 0.922(3) 0.108(14) Uiso 1 1 d . Q 1
H42 H 0.644(6) 0.8677(16) 0.981(2) 0.073(12) Uiso 1 1 d . R 1
H43 H 0.676(6) 0.9111(17) 0.899(2) 0.074(10) Uiso 1 1 d . S 1
H44 H 0.327(5) 0.7994(13) 0.9591(19) 0.050(8) Uiso 1 1 d . T 1
H45 H 0.097(5) 0.7198(12) 0.8756(17) 0.043(8) Uiso 1 1 d . U 1

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
S15 0.0268(4) 0.0350(3) 0.0561(5) -0.0132(3) -0.0165(3) 0.0066(3)
O12 0.108(2) 0.0990(17) 0.0678(16) 0.0486(14) 0.0571(16) 0.0678(16)
O13 0.0333(11) 0.0604(11) 0.0287(9) 0.0095(8) 0.0047(8) 0.0158(9)
O16 0.0669(15) 0.0586(12) 0.0458(12) -0.0154(9) -0.0368(11) 0.0241(11)
O17 0.0226(10) 0.0395(10) 0.1030(17) -0.0216(10) -0.0012(11) 0.0015(8)
N6 0.0240(12) 0.0342(11) 0.0473(13) -0.0123(10) -0.0061(10) 0.0049(9)
C1 0.0242(13) 0.0357(13) 0.0292(13) -0.0045(10) -0.0012(10) 0.0044(10)
C2 0.0240(13) 0.0287(11) 0.0275(12) -0.0057(9) -0.0021(10) -0.0022(10)
C3 0.0390(17) 0.0329(14) 0.0338(15) 0.0030(12) 0.0036(13) 0.0043(12)
C4 0.0262(14) 0.0419(13) 0.0302(13) -0.0059(11) -0.0046(11) 0.0048(11)
C5 0.0271(14) 0.0341(13) 0.0422(16) -0.0078(12) -0.0074(12) 0.0032(11)
C7 0.0335(16) 0.0295(14) 0.0563(19) 0.0023(13) 0.0124(14) 0.0020(12)
C8 0.032(2) 0.030(3) 0.043(2) -0.0006(15) 0.0064(16) 0.004(2)
C9 0.082(3) 0.074(2) 0.055(2) 0.0334(18) 0.045(2) 0.051(2)
C10 0.0285(14) 0.0267(12) 0.0377(14) -0.0009(10) 0.0092(11) 0.0004(10)
C11 0.0443(17) 0.0357(13) 0.0357(15) 0.0035(11) 0.0143(13) 0.0084(12)
C14 0.0409(18) 0.0512(17) 0.0270(15) 0.0077(13) 0.0003(13) 0.0104(14)
C18 0.0217(13) 0.0257(11) 0.0317(13) -0.0006(10) -0.0047(10) 0.0051(9)
C19 0.0365(16) 0.0332(13) 0.0319(14) -0.0001(11) 0.0074(12) 0.0039(11)
C20 0.0272(15) 0.0283(12) 0.0553(18) 0.0037(12) 0.0114(13) -0.0014(11)
C21 0.0292(14) 0.0233(11) 0.0377(14) 0.0023(10) -0.0098(11) 0.0038(10)
C22 0.0407(19) 0.0322(15) 0.062(2) -0.0038(14) -0.0187(16) -0.0029(12)
C23 0.0386(16) 0.0303(12) 0.0233(13) 0.0018(10) -0.0015(11) 0.0031(11)
C24 0.0273(14) 0.0299(12) 0.0358(14) 0.0043(10) 0.0063(11) 0.0008(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
S15 O17 1.427(2) . ?
S15 O16 1.437(2) . ?
S15 N6 1.629(2) . ?
S15 C18 1.757(2) . ?
O12 C11 1.201(3) . ?
O13 C11 1.321(3) . ?
O13 C14 1.448(3) . ?
N6 C5 1.477(3) . ?
N6 C7 1.477(3) . ?
C1 C10 1.334(3) . ?
C1 C2 1.470(3) . ?
C1 H25 1.01(3) . ?
C2 C4 1.327(3) . ?
C2 C3 1.487(4) . ?
C3 H26 1.00(2) . ?
C3 H27 0.96(3) . ?
C3 H28 0.95(4) . ?
C4 C5 1.500(3) . ?
C4 C8 1.558(5) . ?
C5 H29 1.00(3) . ?
C5 H30 0.98(2) . ?
C7 C8 1.523(4) . ?
C7 H31 0.90(3) . ?
C7 H32 0.89(3) . ?
C8 C9 1.418(5) . ?
C8 H33 1.04(3) . ?
C8A H33A 0.96(7) . ?
C8A H35 1.50(6) . ?
C9 C10 1.492(4) . ?
C9 H34 0.96(2) . ?
C9 H35 1.08(6) . ?
C10 C11 1.474(3) . ?
C14 H36 0.89(3) . ?
C14 H37 1.04(3) . ?
C14 H38 1.00(3) . ?
C18 C19 1.383(3) . ?
C18 C24 1.384(3) . ?
C19 C20 1.373(4) . ?
C19 H39 0.95(3) . ?
C20 C21 1.389(4) . ?
C20 H40 0.96(3) . ?
C21 C23 1.386(4) . ?
C21 C22 1.509(4) . ?
C22 H41 0.99(5) . ?
C22 H42 0.95(3) . ?
C22 H43 0.95(3) . ?
C23 C24 1.386(3) . ?
C23 H44 0.90(3) . ?
C24 H45 0.93(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
O17 S15 O16 120.43(14) . . ?
O17 S15 N6 107.22(11) . . ?
O16 S15 N6 105.61(11) . . ?
O17 S15 C18 106.90(11) . . ?
O16 S15 C18 108.91(12) . . ?
N6 S15 C18 107.10(10) . . ?
C11 O13 C14 116.6(2) . . ?
C5 N6 C7 109.5(2) . . ?
C5 N6 S15 119.12(17) . . ?
C7 N6 S15 119.22(16) . . ?
C10 C1 C2 122.5(2) . . ?
C10 C1 H25 119.2(14) . . ?
C2 C1 H25 118.3(14) . . ?
C4 C2 C1 117.1(2) . . ?
C4 C2 C3 124.5(2) . . ?
C1 C2 C3 118.3(2) . . ?
C2 C3 H26 109.4(13) . . ?
C2 C3 H27 112.1(16) . . ?
H26 C3 H27 109(2) . . ?
C2 C3 H28 113(2) . . ?
H26 C3 H28 107(2) . . ?
H27 C3 H28 107(2) . . ?
C2 C4 C5 128.4(2) . . ?
C2 C4 C8 120.4(2) . . ?
C5 C4 C8 111.0(2) . . ?
N6 C5 C4 103.1(2) . . ?
N6 C5 H29 108.9(16) . . ?
C4 C5 H29 114.3(14) . . ?
N6 C5 H30 112.5(14) . . ?
C4 C5 H30 110.5(15) . . ?
H29 C5 H30 108(2) . . ?
N6 C7 C8 105.9(2) . . ?
N6 C7 H31 109.0(19) . . ?
C8 C7 H31 117(2) . . ?
N6 C7 H32 111(2) . . ?
C8 C7 H32 113(2) . . ?
H31 C7 H32 101(3) . . ?
C9 C8 C7 122.7(3) . . ?
C9 C8 C4 112.2(3) . . ?
C7 C8 C4 100.7(3) . . ?
C9 C8 H33 94.1(17) . . ?
C7 C8 H33 114.6(17) . . ?
C4 C8 H33 113.2(16) . . ?
H33A C8A H35 57(4) . . ?
C8 C9 C10 114.1(3) . . ?
C8 C9 H34 117.0(16) . . ?
C10 C9 H34 113.1(15) . . ?
C8 C9 H35 97(3) . . ?
C10 C9 H35 110(3) . . ?
H34 C9 H35 104(3) . . ?
C1 C10 C11 122.4(2) . . ?
C1 C10 C9 120.3(2) . . ?
C11 C10 C9 117.2(2) . . ?
O12 C11 O13 122.4(2) . . ?
O12 C11 C10 123.0(2) . . ?
O13 C11 C10 114.7(2) . . ?
O13 C14 H36 109.2(18) . . ?
O13 C14 H37 104.8(16) . . ?
H36 C14 H37 114(3) . . ?
O13 C14 H38 108.4(18) . . ?
H36 C14 H38 104(2) . . ?
H37 C14 H38 116(2) . . ?
C19 C18 C24 120.3(2) . . ?
C19 C18 S15 119.90(19) . . ?
C24 C18 S15 119.61(19) . . ?
C20 C19 C18 119.8(2) . . ?
C20 C19 H39 121.8(17) . . ?
C18 C19 H39 118.4(17) . . ?
C19 C20 C21 120.9(2) . . ?
C19 C20 H40 119.8(15) . . ?
C21 C20 H40 119.2(15) . . ?
C23 C21 C20 118.9(2) . . ?
C23 C21 C22 121.1(3) . . ?
C20 C21 C22 119.9(3) . . ?
C21 C22 H41 113(2) . . ?
C21 C22 H42 106(2) . . ?
H41 C22 H42 115(3) . . ?
C21 C22 H43 112(2) . . ?
H41 C22 H43 108(3) . . ?
H42 C22 H43 103(3) . . ?
C21 C23 C24 120.6(2) . . ?
C21 C23 H44 119.6(19) . . ?
C24 C23 H44 119.8(19) . . ?
C18 C24 C23 119.5(2) . . ?
C18 C24 H45 119.7(16) . . ?
C23 C24 H45 120.8(16) . . ?

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
O17 S15 N6 C5 163.89(18) . . . . ?
O16 S15 N6 C5 34.3(2) . . . . ?
C18 S15 N6 C5 -81.7(2) . . . . ?
O17 S15 N6 C7 -57.5(2) . . . . ?
O16 S15 N6 C7 172.9(2) . . . . ?
C18 S15 N6 C7 56.9(2) . . . . ?
C10 C1 C2 C4 -6.5(4) . . . . ?
C10 C1 C2 C3 171.7(2) . . . . ?
C1 C2 C4 C5 173.4(2) . . . . ?
C3 C2 C4 C5 -4.7(4) . . . . ?
C1 C2 C4 C8 -12.3(4) . . . . ?
C3 C2 C4 C8 169.6(3) . . . . ?
C7 N6 C5 C4 21.5(3) . . . . ?
S15 N6 C5 C4 163.71(16) . . . . ?
C2 C4 C5 N6 172.0(2) . . . . ?
C8 C4 C5 N6 -2.7(3) . . . . ?
C5 N6 C7 C8 -32.7(3) . . . . ?
S15 N6 C7 C8 -174.9(3) . . . . ?
N6 C7 C8 C9 153.4(4) . . . . ?
N6 C7 C8 C4 28.0(4) . . . . ?
C2 C4 C8 C9 36.9(5) . . . . ?
C5 C4 C8 C9 -147.8(3) . . . . ?
C2 C4 C8 C7 169.1(3) . . . . ?
C5 C4 C8 C7 -15.7(4) . . . . ?
C7 C8 C9 C10 -161.0(4) . . . . ?
C4 C8 C9 C10 -41.0(5) . . . . ?
C2 C1 C10 C11 -177.6(2) . . . . ?
C2 C1 C10 C9 0.2(4) . . . . ?
C8 C9 C10 C1 25.5(5) . . . . ?
C8 C9 C10 C11 -156.6(3) . . . . ?
C14 O13 C11 O12 -1.4(4) . . . . ?
C14 O13 C11 C10 179.8(2) . . . . ?
C1 C10 C11 O12 -163.8(3) . . . . ?
C9 C10 C11 O12 18.4(4) . . . . ?
C1 C10 C11 O13 15.0(4) . . . . ?
C9 C10 C11 O13 -162.9(3) . . . . ?
O17 S15 C18 C19 -166.41(19) . . . . ?
O16 S15 C18 C19 -34.8(2) . . . . ?
N6 S15 C18 C19 78.9(2) . . . . ?
O17 S15 C18 C24 18.7(2) . . . . ?
O16 S15 C18 C24 150.23(19) . . . . ?
N6 S15 C18 C24 -96.0(2) . . . . ?
C24 C18 C19 C20 1.0(4) . . . . ?
S15 C18 C19 C20 -173.89(18) . . . . ?
C18 C19 C20 C21 -0.6(4) . . . . ?
C19 C20 C21 C23 -0.2(4) . . . . ?
C19 C20 C21 C22 178.7(2) . . . . ?
C20 C21 C23 C24 0.7(3) . . . . ?
C22 C21 C23 C24 -178.1(2) . . . . ?
C19 C18 C24 C23 -0.5(3) . . . . ?
S15 C18 C24 C23 174.40(18) . . . . ?
C21 C23 C24 C18 -0.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.064